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Black liquor concentration

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Inside Cover
Acknowledgments
Disclaimer
This roadmap was developed under the guidance This report was prepared as an account of work
of David Turpin, Executive Director of the sponsored in part by agencies of the U.S.
Agenda 2020 Technology Alliance, with the government. Neither the U.S. government, nor
financial support of Agenda 2020 and with any agency thereof nor any of their employees
funding from a National Institute of Standards make any warranty, expressed or implied, or
and Technology (NIST) Advanced assume any legal liability or responsibility for
Manufacturing Technology Consortia (AMTech) the accuracy completeness, or usefulness of any
Planning Grant. information, apparatus, product, or process
disclosed, or represent that its use would not
This roadmap was created through the work of infringe on privately owned rights. Reference
many individuals representing pulp and paper herein to any specific commercial product,
companies, industry suppliers, government process, or service by trade name, trademark,
agencies, universities, and other organizations. manufacturer, or otherwise does not constitute or
imply its endorsement, recommendation, or
A full list of contributors can be found in favoring by the U.S. government or any agency
Appendix D. thereof. This report represents the views and
opinions of individuals from the forest products
The principle writers were Victoria Brun and
industry and not those of the U.S. government or
Fred Hansen of Energetics Incorporated, David
any agency thereof.
Turpin, Kathleen Bennett, Chris Verrill of
International Paper Company, and members of
the Agenda 2020 Black Liquor Concentration
Team. Chris Verrill and Takis Taosakis of
MeadWestvaco (now WestRock) originally led
the team, and Ricardo Santos, WestRock, served
as team manager. In 2015, Jim Bradbury, Verso
Paper, became co-lead, replacing Takis
Taosakis. Special acknowledgement and thanks
to Greg Burns, Kapstone Paper, for his work in
developing the WinGEMS model described in
this roadmap. The document was designed by
Julie Chappell of Energetics Incorporated.

Copyright Information
The information in this document is meant to be
distributed widely throughout the forest products
industry and the broader research community.
The sponsors encourage reproduction and
dissemination of the entire document, or
portions thereof, with attribution and without
changes.
Table of Contents
Executive Summary ............................................ i Appendix A: High-Priority R&D Project Maps17
Black Liquor Concentration Roadmap .............. i
Agenda 2020’s Strategy ..................................... i Appendix B: Additional Background and
Agenda 2020 .....................................................ii Modeling Results ...................................... 30
Technology Development Projects ...................ii Additional Background ................................... 30
Membrane Technology Program Projects.........ii Development of Process Model ...................... 32
Path Forward ....................................................iii Non-Membrane Technologies Considered ..... 36
Longer-Term Research Opportunities ............ 38
1. Introduction ................................................. 1
Background ....................................................... 1 Appendix C: Additional Content for the
Agenda 2020 Vision ......................................... 1 Membrane Technology Program............... 41
Focus on Black Liquor Concentration .............. 2 Challenges and Knowledge Gaps ................... 41
Potential Benefit ............................................... 3 R&D Projects .................................................. 44
Structure of this Report ..................................... 3 Appendix D: Contributors ............................... 47
2. Technology Overview and Modeling Agenda 2020 Black Liquor Team Members ... 47
Results ......................................................... 4 Technology Presentations ............................... 48
Technical Review ............................................. 4 Literature Surveys ........................................... 49
Modeling Study ................................................ 5 Model Development ....................................... 49
Membrane Workshop Participants (Phase II
3. Technology Development Projects.............. 7 Workshop) ...................................................... 49
Introduction ...................................................... 7
Focused Development Projects ......................... 7 Appendix E: Workshop Agenda ...................... 51
4. Development of a Membrane Technology
Program ..................................................... 10
Introduction .................................................... 10
Requirements for a Membrane Solution ......... 10
Technical Issues .............................................. 11
The Membrane Technology Program ............. 12
High-Priority R&D Projects ........................... 13
5. Conclusion ................................................. 15
Executive Summary
The United States faces critical energy challenges. tons per day of pulp, integrating membrane-based
Energy is at the nexus of national security, global black liquor concentration technology has the
climate change policy, and economic prosperity. potential to reduce annual energy costs by $2–$3
The United States is currently the world’s second- million. Therefore, reducing the energy demand
largest consumer of energy, and U.S. energy devoted to the concentration of weak black liquor
consumption is projected to grow through 2040, represents a significant area of opportunity for
making the need for increasing energy efficiency a decreasing energy usage.
national imperative.1 For industry, the volatility of
energy prices in recent years has become a major This roadmap presents six concrete research and
risk factor, and energy efficiency is now seen as an development (R&D) projects to develop advanced
essential risk management strategy.2 Improving membrane technologies to decrease the energy
energy efficiency is one of the most constructive used in concentrating black liquor.
and cost-effective ways to reduce energy use and
thereby improve energy security and
independence, and reduce carbon emissions.3 Agenda 2020’s Strategy
The Agenda 2020 Black Liquor Concentration
Black Liquor Concentration Team utilized a methodical strategy (see Figure
ES-1) to identify opportunities to reduce energy
Roadmap use through the advancement of black liquor
As the third largest manufacturing user of energy, concentration technology. The team first
the U.S. pulp and paper industry is considered an conducted a thorough investigation of the current
energy-intensive sector. About 7% of pulp and state and examined a range of potential
paper energy usage, or nearly 164 trillion Btu, is technologies. The team also considered industry
used to remove water from black liquor in U.S. needs with regard to black liquor concentration
kraft mills.4 Concentrating black liquor is an and conducted a modeling study to predict the
energy-intensive step in recovering pulping process implications and impacts within typical
chemicals and generating high-pressure steam kraft mill.
from dissolved wood solids.
Based on this analysis the team chose to focus the
This roadmap—which is part of a series of five roadmap on membrane technology. The team then
Agenda 2020 roadmaps—specifically looks to identified current projects developing membrane-
reduce the energy used in concentrating weak based separation technologies that have the
greatest promise for near-term improvement.
Executive Summary
black liquor. According to material and energy
models for a typical mill producing 2,000 air-dried Agenda 2020 became involved with each of these
projects in order to advance a membrane solution
1
U.S. Energy Information Administration (EIA). 2015.
for the pulp and paper industry.
Annual Energy Outlook 2015. DOE/EIA-0383. EIA.
https://www.eia.gov/forecasts/aeo/executive_summary.cfm. In addition, the team decided to take a more
2
Industrial Energy Efficiency as a Risk Management comprehensive look at the enabling factors
Strategy. 2007. ACEEE Summer Study on Energy Efficiency surrounding membrane-based separation
in Industry. technology. The team developed specific
3
U.S. Environmental Protect Agency (EPA). 2015. “Energy
Efficiency (EE).” EPA. requirements for the implementation of membrane
http://www3.epa.gov/statelocalclimate/local/topics/energy- systems in partial black liquor concentration. The
efficiency.html. team examined the broader, precompetitive issues
4
RISI Mill Asset Database, January 2014.

Reuse of Process Effluents Research Roadmap i


involved in enabling new technology to meet these ■ Develop a membrane process simulation to
requirements and developed a Membrane predict permeate stream compositions based on
Technology Program. The program maps out a set inputs, membranes, and configuration
of projects to produce knowledge, instrumentation,
■ Develop new instrumentation to
and testing platforms to enable the
operate/control membrane systems
commercialization and implementation of new
membrane technologies. The project maps for these six high-priority
Executive Summary

projects are presented in Appendix A. Each map


provides a detailed plan that is intended to guide
Technology Development the implementation of the R&D project and
provide a basis for securing funding and
Projects establishing partnerships.
The team identified three membrane technologies
that have the potential for breakthroughs which
would accelerate development:
Agenda 2020
The Agenda 2020 Technology Alliance is a non-profit
■ Membranes with sacrificial protective coatings organization working to identify high-priority, pre-
(a Teledyne project under contract with the competitive technology challenges for the pulp and paper
U.S. Department of Energy) industry and to promote scientific R&D projects to address
them.
■ Robust membranes (a project being undertaken The goals of the organization are the following:
at Georgia Tech)
■ Reduce water consumption and enhance water reuse
■ High-Performance Architectured System
(HiPAS) membrane technology at Oak Ridge ■ Reduce energy use and carbon emissions
The team has facilitated Agenda 2020’s ■ Increase manufacturing process efficiency
participation in and/or sponsoring of current ■ Improve raw material yield
projects to develop these technologies and make
them commercially available to the pulp and paper ■ Develop new biobased products
industry. The Agenda 2020 Technology Alliance is committed to
transforming the paper and forest products industry through
innovation in its manufacturing processes and products.
Agenda 2020 is uniquely qualified to meet this goal because
Membrane Technology of its ability to bring together subject-matter experts and
promote cooperation among universities, research institutions,
Program Projects and government agencies. Collaborative R&D programs that
bring together diverse expertise are essential for addressing
The Membrane Technology Program consists of industry needs and national sustainability goals.
six actionable R&D projects: ■ Agenda 2020 has developed five R&D roadmaps: Reuse
of Process Effluents
■ Conduct a modeling study to establish
acceptable permeate quality specifications and ■ Drier Web before Dryer Section
process integration alternatives ■ Black Liquor Concentration
■ Characterize the capability of existing ■ Next-Generation Pulping
membrane technology
■ Cellulose Nanomaterials
■ Characterize process streams across
Each roadmap topic aligns with Agenda 2020’s vision and
membranes and conduct bench-scale was selected after a careful analysis of industry needs and
membrane performance screening and research current and emerging technology.
■ Develop a portable test skid for the purpose of
analyzing and optimizing membrane
technology

ii Reuse of Process Effluents Research Roadmap


Path Forward This roadmap is designed to spur this critical
collective action and serve as an invitation and as
Developing breakthrough technologies to increase guidance for future R&D efforts.
the reuse of process effluents is beyond the scope
and means of a single organization. Effectively We look forward to engaging the research
implementing the identified R&D projects and community to address this challenge, and we
achieving the resulting benefits of reduced water welcome the input and engagement of industry,
usage and reduced energy use will require universities, research institutions, national
collaborative effort with diverse partners. laboratories, and public agencies in developing
technology options—and in further defining the
questions and challenges.

Executive Summary

Figure ES-1. Overview of the Roadmap Strategy

Reuse of Process Effluents Research Roadmap iii


ii Reuse of Process Effluents Research Roadmap
1. Introduction
Background Vision 2030
This roadmap is part of a series of research and
development (R&D) roadmaps developed by the If these projects were successful and broadly
Agenda 2020 Technology Alliance in part with implemented, the U.S. pulp and paper industry
funding from an award from the National Institute could accomplish the following by 2030:
of Standards and Technology (NIST) Advanced ■ Reduce purchased energy by 50%, saving
Manufacturing Technology Consortia (AMTech) over 500 TBtu per year.
program.
■ Reduce water used per ton by 50%,
After careful analysis of trends and drivers shaping reducing water discharge nationally by 480
the industry, key challenges and opportunities, and billion gallons per year.
barriers to industry sustainability and
■ Develop new biobased products worth
competitiveness, a steering committee selected
$5 billion in sales per year.
reducing the energy used in concentrating weak
black liquor as the topic for this roadmap. ■ Protect 370,000 existing jobs by making
359 mills in 40 states more sustainable
The development of this roadmap followed a economically, environmentally, and
slightly different path than the other roadmaps. socially.
First, the Agenda 2020 Black Liquor
Concentration Team investigated a range of ■ Dramatically improve the life-cycle
alternative technologies and determined that sustainability of its products.
membrane technology should be the focus of this
industry. The implementation of the Membrane
roadmap. Next, the team identified three
membrane technologies that have the potential for Technology Program will produce knowledge,
instrumentation, and testing platforms designed to
near-term success and facilitated Agenda 2020’s
participation in current and planned projects to enable the commercialization and implementation
of new membrane technologies.
develop these technologies. Finally, the team
developed a broader Membrane Technology
Program that mapped out a set of six projects
focused on research to enable technology Agenda 2020 Vision
development.
The U.S. pulp and paper manufacturing industry
In all phases, the team used workshops and other through Agenda 2020 is actively addressing
interactions to draw on the diverse expertise and national goals of sustainability, energy
productivity, full employment, and healthy, 1. Introduction
perspectives of subject-matter experts from
industry, national laboratories, government, and resilient forests. Pulp and paper manufacturers
academia. need new breakthrough technologies that can meet
key industry needs. However, such research is
Accordingly, this roadmap describes the three capital-, equipment-, and resource-intensive, and
technology development projects. It also provides no company is likely to discover a breakthrough
detailed R&D project maps for the set of projects technology alone. These roadmaps seek to address
comprising the broader program. The specific needs and to encourage the interest of
implementation of technology focused projects is research institutes and government agencies in this
specifically designed to produce a viable challenging and promising endeavor in the
membrane technology for the pulp and paper national interest.

Reuse of Process Effluents Research Roadmap 1


1. Introduction

Figure 1. Roadmaps Driven by Vision and Need

The roadmaps are driven by the Agenda 2020 evaporation and concentration of weak black
Vision for the pulp and paper industry. This vision liquor is an important area of opportunity toward
encompasses specific industry goals and is aligned meeting this objective.
with broader national priorities (Figure 1). In
identifying high-priority R&D projects for the The focus of the Black Liquor Concentration
industry, each roadmap maintains a line of sight to roadmap is on the facilitation of research to
the vision and to particular industry goals and develop an energy-efficient, breakthrough method
societal priorities. This line of sight ensures that to remove water from kraft pulp mill black liquor,
the research described in the roadmaps will integrated synergistically with other pulp and
directly contribute to the realization of the Agenda paper manufacturing systems that will surpass
2020 Vision and thus provides the purpose, current BAT while providing superior economics.
rationale, and measure of success for the
roadmaps. Agenda 2020 member companies seek further
investigation and development of new and
promising technologies as well as additional
strategies to reduce the energy requirements of
Focus on Black Liquor concentrating weak black liquor. The Agenda
Concentration 2020 Black Liquor Concentration Team examined
a range of possibilities related to membrane
As part of its vision, Agenda 2020 has a goal to separations and other technologies, including
reduce purchased energy demand per ton of freeze crystallization, electrolysis, dialysis,
product by half, from an estimated 13 million precipitation of lignin, adsorption, and others.
Btu/ton in 2010 to 6.5 million Btu/ton by 2030. Although the team ultimately chose to focus this
Reducing the energy demand devoted to roadmap on membrane technologies, the team is

2 Reuse of Process Effluents Research Roadmap


not discounting other approaches and invites Structure of this Report
researchers to pursue these areas and to develop
additional ideas. The remainder of this report is organized as
follows:
The Agenda 2020 Technology Alliance is working
with companies and with partners in universities, ■ Chapter 2, which follows, presents an overview
research institutions, national laboratories, and of best available technology and the results of
public agencies to advance R&D projects and the modeling study that helped establish the
encourage participation, project funding, and rapid case for pursuing membrane technologies.
progress.
■ Chapter 3 describes the three technology
development projects focused specific
membrane technologies.
Potential Benefit
■ Chapter 4 presents the Membrane Technology
Advanced systems based on membrane Program, including the requirements for new
concentration of weak black liquor that replace technologies and the six enabling research
two stages in multiple-effect evaporators could projects.
make a significant contribution toward the
■ Chapter 5 presents conclusions and outlines a
industries energy reduction goal. According to
path forwards. It also puts forth a call to action.
material and energy models, this technology has
the potential to save as much as 0.75 million Btu In addition, a series of appendices provides
per ton of pulp. If the savings achievable in the extensive detail of this roadmapping effort,
model mill could be widely implemented across all including the project maps for the four high-
U.S. mills (of course, individual mill priority projects.
configurations differ), this strategy would reduce
energy consumption nationally by 23 trillion
Btu/year, which would have an economic value
between $70 and $120 million annually.

1. Introduction

Reuse of Process Effluents Research Roadmap 3


2. Technology Overview and
Modeling Results
2. Technology Overview and Modeling
Results

The Black Liquor Concentration Team chose to usage is used to remove water from black liquor in
focus this roadmap on membrane technologies U.S. kraft mills.7
based on a review of a range of alternative
technologies. These included membrane Reducing energy in concentrating black liquor for
separation technologies, freeze crystallization, chemical recovery and steam and power
electrolysis, dialysis, precipitation of lignin, generation is important for achieving a more
adsorption, and others. In addition, the team sustainable approach for pulp and paper
developed a model of a typical mill to predict the manufacturing. Advanced technologies can benefit
process implications and economic results of many mills by reducing energy demand, input
membrane technology. costs, and greenhouse gas emissions. New
developments are expected to be cost-effective to
This chapter presents a brief overview of this implement in many mills but, because this depends
technical review and the results of the modeling on site-specific conditions, not all mills will
study for membrane-based weak black liquor benefit equally. Achieving substantial energy
concentration. Additional background information savings from advanced technologies for black
and modeling results may be found in Appendix liquor concentration will require new technologies
B. The purpose of this section is to provide the and solutions that are cost-effective and that can
reader with access to and understanding of the
basis for the team’s decision to focus on
membrane technologies.

Technical Review
Concentrating black liquor is an energy-intensive
step in recovering pulping chemicals and
generating high-pressure steam from dissolved
wood solids. The U.S. manufacturing sector
utilizes approximately 22.7 quadrillion Btu (quad)
of energy annually.5 Pulp and paper manufacturing
is the third-largest consumer of energy in the
manufacturing sector, earning it the label as an
energy-intensive manufacturer.6 Black liquor
concentration has been listed as one of the top
Figure 2. U.S. Energy Usage
contributors to this figure; nearly 164 trillion Btu
per year or about 7% of pulp and paper energy
be applied broadly in many mills.

5
U.S. Department of Energy, Pulp and Paper Industry Energy
Bandwidth Study, 2013.
6
U.S. Department of Energy Information Administration,
7
2011. RISI Mill Asset Database, January 2014.

4 Reuse of Process Effluents Research Roadmap


Current Practices Best Available Technology
The United States has 99 kraft pulp mills in 24 The best technology in use today is falling-film,
states,8 which produce 45 million tons of pulp a multiple-effect evaporation with six or seven
year. A typical kraft mill today produces 2,600 to stages, having steam economies of 5.0 to 5.8
3,000 pounds of black liquor solids per ton of air- pounds of water evaporated per pound of steam
dried unbleached pulp. The actual value varies by used. Exit solids content ranges from 75% to 85%.
pulping yield, with brown grades at the lower end BAT evaporator systems also typically include
of the range and bleachable grades at the upper condensate segregation to separate the cleaner
end. Weak black liquor from the washers is made process condensates for direct reuse in pulp
up of about 15%–20% solids and 80%–85% water. washing. They also have integrated steam-
Black liquor entering the recovery boiler is stripping operations to purify foul process
typically 65%–85% solids. Concentrating the condensates for reuse. Waste heat from BAT
black liquor is typically accomplished in one or evaporator condensers is typically utilized for
more sets of multiple-effect evaporators. Three heating process water streams. Assuming that
technologies are commonly employed: black liquor is concentrated from 15% to 80%
solids content in a seven-effect evaporator, the
■ Pre-evaporators operating on secondary heat evaporation duty would require 3.0 million Btu
from batch digester blow-heat systems or black energy (as compared to 3.5 million Btu for more
liquor concentrators, employing two to five typical systems) per air-dry ton of unbleached
effects or stages of heat utilization, with pulp.10
product liquor concentration of 20%–30%
solids content Some mills have older recovery boiler technology
that uses direct contact of hot flue gases with black
■ Evaporators operating on low-pressure steam
liquor to achieve the final stage of concentration to
of rising-film and/or falling-film design,
65%–70% solids. Evaporators for these mills
employing four to eight effects or stages of
would be limited to concentrating black liquor to
heat utilization, with product liquor
only 50% solids content. A BAT evaporator
concentration of 45%–55% solids content
system for such an application is shown in Figure
■ Concentrators, designed to manage the 6 in Appendix B.
concentration of sodium salts that occurs when
black liquor is concentrated above ~50% solids
content; these operate on low- or medium- Modeling Study
pressure steam with product liquor
concentration of 65%–85% solids content. In 2014, the Agenda 2020 Black Liquor
Concentrators can be integrated as first-effect Concentration Team developed a model of a
bodies of multiple-effect evaporators or one- to typical mill to predict the process implications and
two-effect stand-alone units, or coupled with impacts of incorporating membrane technology

2. Technology Overview and Modeling


pre-evaporators. under various scenarios. (See Appendix B for
more details). Using the model, the team
Using conservative estimates that the typical solids developed the following table, which provides
concentration in weak black liquor into a typical example savings calculation for integrating a
Results
six-effect evaporator is 45%, the evaporation duty membrane system for concentrating black liquor
requires 3.5 mm Btu of heat energy (typically in from 15% to 30% solids content with a four-stage
the form of low-pressure steam) per air-dried ton conventional black liquor evaporator and two-
of pulp.9 stage concentrator to produce 70% solids liquor
for burning in a recovery boiler.
8
RISI Mill Asset Database, January 2014.
9
Kinstrey, R., and D. White. “Pulp & Paper Industry Energy
Bandwidth Study,” Paper 27-1 at 2007 TAPPI engineering,
Pulping & Environmental Conference, Jacksonville, FL,
10
October 2007. Ibid.

Reuse of Process Effluents Research Roadmap 5


Table 1. Example Savings for Membrane-Based

Typical Mill
Production (unbleached) 700,000 ADT/year
2. Technology Overview and Modeling

Weak black liquor solids 15%


Membrane retentate solids 30%
Incremental Energy Cost
Incremental boiler fuel cost (mid-point of $3-5 range, based on 2012 DoE Energy Information $ 4.00 MM/Btu
Results

Administration data as updated by 2014 company estimates)


Purchased electricity cost (team benchmark, 2014 estimate) $50.00/MWh
Differential Energy Quantities from Preliminary Process Model
Boiler steam savings 1.49 MM Btu/ADT
Purchased power increase 0.07 MW/ADT
Boiler fuel efficiency† 80%
Boiler fuel savings $5,215,000/year
Purchased electricity cost increase $2,450,000/year
Net annual savings $2,765,000/year

Typical boiler efficiency for natural gas

Weak Black Liquor Concentration Assuming that the modeled purchased-energy


According to preliminary model results, advanced reduction of 0.5 million Btu per ton could be
systems based on membrane concentration of achieved on average across all 47 million tons per
weak black liquor that raise the solids from 15% to year of kraft pulp produced in the United States,
30% have the potential to save as much as 1.5 concentration with advanced membrane systems
million Btu fuel-based energy per ton of pulp. The could reduce energy consumption nationally by 23
net energy-saving potential varies considerably trillion Btu per year. The economic value of this
from mill to mill, depending on the configuration energy saving would be $70 to $120 million per
of mill steam and power systems. For typical mills year, based on energy costs of $3 to $5 per million
producing 2,000 air-dried ton per day of pulp there Btu.
is a $2–3 million annual energy cost savings
potential for integrating membrane-based black Given the likelihood of a viable business case for
liquor concentration technology. Large-production one or more membrane technologies, the Agenda
mills with weak black liquor solids content below 2020 Black Liquor Concentration Team has
15% could realize as much as $5–6 million in developed a research initiative to explore this
annual energy cost savings. option in detail.

6 Reuse of Process Effluents Research Roadmap


3. Technology Development
Projects
Introduction Membranes with Sacrificial Protective
Using membrane systems for pressure-driven Coatings
separation of water from black liquor to raise
solids content from about 15 percent to near 30 Description and Advantages
percent is a promising approach to achieve The Teledyne membrane system applies a
considerable reduction in the steam energy sacrificial coating to off-the-shelf membrane
required for concentration. However, there is no modules to reduce or eliminate membrane fouling.
membrane technology yet proven for black liquor The coating resists fouling by black liquor and, as
concentration and a number of performance a result, the membrane system maintains higher
challenges such as fouling, high flux, and ability to average flux. Foulants adhere weakly to the
withstand high-temperatures still need to be coating. The coating is periodically reapplied in
addressed. the field by taking one module out of service at a
time while a clean-in-place operation is done. The
Accordingly, the Agenda 2020 Team investigated reformation of the coating can be automated.
new membrane technologies that would have the
greatest potential to be an effective solution for Teledyne has demonstrated success of
black liquor concentration. In addition, the team concentrating weak black liquor in a laboratory
sought technologies for which development set-up using actual black liquor from a mill and
projects are planned or under way and thus would heating it to 85oC. Coating material stability on
present an opportunity for Agenda 2020 to become chosen membranes at pH 13–14 was satisfactory,
actively involved and advance the technology for and the permeate (separated water) quality met the
the pulp and paper industry. DOE contract targets; however, the impurities are
presently too high for this stream to be readily
integrated into an existing pulp mill.
Focused Development Projects
The company has demonstrated successful black
The Black Liquor Concentration Team identified liquor treatment for more than seven days with

3. Technology Development Projects


and is assisting or monitoring two membrane <20% drop in total flux with semi-automated
technology development projects: (1) membranes backflush, chemical clean, and coating
with sacrificial protective coatings (a Teledyne reformation. Preliminary nanofiltration (NF) tests
project under contract with the U.S. Department of suggest that permeate total dissolved solids (TDS)
Energy [DOE]), (2) robust membranes (a project concentration <1000 ppm is possible.
being undertaken at Georgia Tech). In addition,
the team is also considering a project to evaluate Knowledge Gaps and Challenges
the High-Performance Architectured System The knowledge gaps for membranes with
(HiPAS) membrane technology at Oak Ridge. sacrificial protective coating technology are
described below:
For each membrane technology, the team explored
its advantages and challenges. It has also provided 1. What is the solids content of the permeate from
input for current research plans and identified sacrificial-coatings membranes? If permeate of
additional research needed.

Reuse of Process Effluents Research Roadmap 7


0.1% solids or less can be achieved, it can be Robust Membranes
used as shower water in brownstock washing.
Description and Advantages
2. It is unknown whether the membrane system
A Georgia Tech team (Nair, Shofner, and
can be successfully operated at 95°C instead of
Sinquefield) has been conducting a two-year
3. Technology Development Projects

~80°C; the higher temperature would be


project to develop new robust membranes that can
representative of worst-case operating
withstand the harsh environment posed by the
conditions in a mill.
black liquors leaving the kraft digester. The team
3. Greater understanding of methanol partitioning plans to explore separation efficiency and fouling
and characterization of streams is needed. tendency under black liquor permeation
conditions. Achieving all of the goals in this
4. It is unknown whether the system would be project would prepare the technology for
able to run using the liquor from 100% integration at the bench scale.
southern pine furnish; the question is whether
soap from that species would create Knowledge Gaps/Challenges
insurmountable operating problems. There are three critical challenges that hinder
progress on this technology:
5. The sources and nature of fouling are not yet
fully identified or understood, nor are their 1. A key challenge is that—unlike conventional NF
potential impacts on flux. and reverse-osmosis (RO) membranes for water
purification/desalination applications—the
6. The fate/transport/environmental health and membranes required here must be capable of
safety (EHS) impacts of cleaning agents must withstanding the high pH (>12), high
be understood and potential conflicts temperature (80–95°C), and different fouling
addressed. The stewardship implications of species in black liquor. This project will focus
cleaning agents must be investigated mainly on CMS membranes and, to a lesser
Further Research Under Way or Planned extent, on zeolite membranes. Early work
identified CMS membranes as the more viable
As part of the Teledyne project under contract
candidate based upon its excellent pH and
with the DOE, the following steps are planned:
temperature stability.
1. The project will target permeate of 0.1% solids
2. There is currently little knowledge of the
or less so it can be used as shower water in
synthesis-structure-separation-fouling
brownstock washing.
relationships of CMS and zeolite membranes
2. The membrane system will be developed and under black liquor permeation conditions. In
operated at 95°C instead of ~80°C in order to particular, the project seeks to determine the
cover the worst-case operating conditions in a long-term chemical and mechanical stability,
mill. and long-term performance characteristics,
under realistic conditions.
3. Streams from test runs will be characterized to
provide some early indication of methanol 3. A detailed literature survey indicates a very
partitioning. large variation in the quality and performance
characteristics of membranes reported in the
4. Pure pine feed-liquor will be tested to evaluate literature. The economic/business case can only
potential issues from soap. It is important to be reliably quantified with measurement-based
obtain results from a true worst-case furnish of estimates of feasible membrane throughput,
100% southern pine. selectivity, and composition of proposed
CMS/zeolite membranes. This project will
5. Cleaning methods and the downtime and collect such data and use it in conjunction with
fate/transport/EHS impacts of the cleaning simple cost-models to determine the realistic
agents will be described. business case.

8 Reuse of Process Effluents Research Roadmap


Further Research Under Way An economic analysis, including NPV and IRR,
In addition to the research described above, the was started early in the project and updated
Georgia Tech team also plans to develop data to throughout the project as new information about
support a quantified business case, once the performance and estimated cost of the
measurement-based estimates of throughput, membranes became available.
selectivity, and composition of the permeates have
been determined.
Oak Ridge HiPAS Membranes
The team will develop prototype CMS/zeolite
membranes with the correct range of pore size and Description and Advantages
microstructure that successfully perform black HiPAS consist of multi-layered membranes with
liquor concentration. To reduce fouling/plugging molecular or polymeric functionalities enabling
by reactions with the retentate species, the team specific separations capabilities. They are applied
will also optimize CMS and zeolite membranes either by dip- or spray-coating a surface, either
with appropriate pore structure and surface inside or outside of a porous tube. The layers
microstructure. typically consist of a solid or flexible support, an
architectured layer facilitating high flux, and a
The team plans to develop data from extended highly selective surface layer, with tunable
measurements with both model streams and actual superhydrophilic (SHI) or superhydrophobic
black liquor streams to determine the long-term (SHO) characteristics. A significant advantage of
resistance of the membranes to the caustic liquor. the HiPAS membrane technology is the ability to
The target performance deliverables are: (1) preferentially separate water from other materials
greater than 95% rejection of salts and (2) greater in a stream because of the surface tension and
than 99% rejection of larger organic solutes. molecular affinity. Another advantage is the
apparent ability to achieve greater than 99.5%
Preliminary process calculations should separation of like materials, such as ethanol and
incorporate performance parameters of the water. This ability suggests the possibility of
membranes obtained from the three challenges uncomplicated separation of methanol from the
listed above. The calculations will also provide flash vapor of the feed evaporator effect.
quantitative estimates of the production rates of
water, salt solutions, concentration black liquor, Knowledge Gaps and Challenges
and energy consumption. This will provide Potential barriers include fouling tendencies, poor
information required to tune the optimal separation of methanol and/or sodium and sulfur
throughput rates (fluxes) of the membranes. ions, soap separation issues, and pH/temperature/
viscosity issues as the black liquor solids increase.

3. Technology Development Projects

Reuse of Process Effluents Research Roadmap 9


4. Development of a Membrane
Technology Program
4. Development of a Membrane
Technology Program

Introduction high-priority R&D projects that would result in


enabling solutions for membrane technology.
In addition to helping advance the development of
the three technologies for black liquor This process ensures that implementation of the
concentration, the Agenda 2020 team also decided high-priority R&D projects will be guided by a
that a more comprehensive look at the issues line of sight to the technical requirements. Figure
surrounding membrane separation technology was 4 illustrates this line of sight that helps align
merited. In particular, the team decided to examine research and industry need.
the broader, precompetitive issues hindering
The projects are intended to comprise an
membrane technologies.
integrated program of research. For each of the
The team began this effort by identifying the R&D projects, the team has developed project
requirements that a membrane solution would maps (see Appendix A) to guide the
have to meet in order to be a viable option for implementation of the high-priority projects. The
partial black liquor concentration. Given these R&D project maps represent the ultimate output of
requirements, the team then identified technical this roadmap. They are intended to provide a
issues that must be addressed in order to enable business case and research plan that engages
membrane technology to meet the requirements. In funding sources, informs and shapes request for
other words, what are the specific technical proposal development, and guides the actual
challenges and/or knowledge gaps that currently implementation of research projects.
prevent membranes systems from meeting the
requirements?
Requirements for a Membrane
Solution
Based on this analysis, the team established a set
of goals for partial black liquor concentration via
membranes. A modified black liquor concentration
process, when compared to the current process,
should provide the following:

■ Concentration of black liquor from 15%–30%


solids (50% stretch goal)
■ Overall energy savings of at least 0.50 million
Btu per ton of pulp per evaporator line and
lower operating cost than current multiple-
Figure 3. Line of Sight to Requirements
effect evaporation technology
Next, the team identified four areas of research ■ Sufficient payback to justify the capital
that would address the technical issues and help expenditure to modify the process (return on
enable a membrane-based solution for black liquor investment [ROI] >30%)
concentration. Finally, the team generated a set of
■ Development within the next 3 to 10 years

10 Reuse of Process Effluents Research Roadmap


■ Reasonable prospect of adoption across 10% of 5. Integration with existing pulp mill processes
available units in the industry within 10 years and systems
Membrane technology exists and is believed to be □ There must be no major negative impact on
a viable alternative to evaporation. However, there the various critical balances in the mill
are a number of performance challenges that need (energy, steam, power, waste heat, water,
to be addressed for this technology to work and chemical).
effectively as an alternative to evaporation.
Therefore, the team identified a set of more □ The technology must function with
specific requirements: hardwood and softwood liquors.
Addressing these requirements would enable
1. Advanced high-flux membrane systems
membranes to provide a more energy-efficient
□ The new technology must be able to handle alternative to evaporation and make a reduction in
the throughput/flux volumes experienced at energy usage significant enough to justify the
a 1,000 ton per day pulp mill line, estimated expenditure of installing the process.
to be 1,200 to 1,800 gallons per minute of
weak black liquor per evaporator line.
□ The footprint of the membrane system must
Technical Issues
fit practically within the traditional recovery The team identified the challenges and/or
system area. knowledge gaps that currently prevent membranes
2. Optimal separations of water, ions, and systems from meeting the requirements. Below is
organics a summary of the challenges and knowledge gaps
relative to meeting each of the requirements:
□ Separation technologies must show
separation effectiveness. Ideally, the quality ■ High Flux/Throughput: A membrane system
of the exit water stream would be suitable must be able to handle the high-flux volumes
for reuse elsewhere in the process and, at a experienced at the mill. Currently, there is a
minimum, would not interfere with existing significant knowledge gap regarding the flux of
wastewater treatment processes. The target black liquor through known membranes, which
is 0.1% solids in the permeate. hinders progress in this area. The variability of
black liquor component composition from
3. Withstand high-temperature, high-pH facility to facility poses a significant challenge
environments to water removal.
□ Separation technologies must be able to ■ Membrane Systems: It is not known what
process black liquor (solids = 30+% salt, membrane system configuration can work in
35% organics; 1,000 ppm MeOH; pH 12+; this application. The relationship between
operating temperatures of 80–95°C). membrane life and costs is unknown, and more

4. Development of a Membrane
knowledge is needed regarding the life-cycle

Technology Program
4. Fouling resistance/system availability considerations. Another issue is that some
technologies will not work with high-feed
□ Membrane fouling must be monitored and
solids, and other limitations of the various
controlled.
separation technologies are also unknown.
□ Membrane technology must require less Research is needed to explore the potential for
downtime for cleaning/maintenance than changing the feed instead of changing the
current evaporators. membrane. Altering the feedstock liquor, if
□ Membrane materials must be reasonable in practicable, could make it more compatible
cost and durability such that operating costs with existing commercial processes. There is a
do not outweigh the energy savings. need for further exploration of the process
options that could make membrane technology
more feasible.

Reuse of Process Effluents Research Roadmap 11


■ Robust Materials: In order to achieve 0.1% conducted and the anticipated R&D outputs. The
solids permeate, reverse osmosis (RO) would four areas are summarized below:
be required. Current RO systems cannot run at
the high-pH and high-temperature levels
required because most are based on thin-film Modeling and Simulation
polyamide technology, and thermal cycles Modeling and simulation is needed to identify the
4. Development of a Membrane

damage membrane systems. A greater acceptable range of salts and organic materials at
Technology Program

understanding of the characteristics of black target destinations for permeate reuse and, if the
liquor going into the system, including permeate salts and organics fall outside the target
composition, pH, and temperature, is also range, determine whether the permeate could be
needed to develop more robust materials. The used elsewhere.
current understanding of the long-term effects
Membrane process modeling and simulation
of black liquor on membrane and module
capability is also needed to predict stream
materials is not sufficient.
compositions based on various inputs, membranes,
■ Resistance to Fouling/Decreasing Downtime: and configurations. The research should include
The primary fouling mechanisms are not energy balances to explore impacts on stream
currently known and, thus, fouling is poorly temperature such as lowering feed temperatures.
understood. It is not clear what fouls the Simulation will be a major input to determining
membranes or whether the concentration the industrial business case and will quickly show
change of components affects fouling. It is not potential integration benefits and liabilities.
clear what chemistries and reactions occur at Results gained from modeling will drive design
the fouling site. A greater understanding of the targets.
correlation between fouling rates and fiber
content and size is needed. To gain a greater
understanding of fouling, a method to test and Black Liquor Characterization Studies
characterize fouling mechanisms is required. for Compatibility with Membrane
■ Mill Integration: There are numerous Systems
knowledge gaps related to mill integration. A R&D is needed to study and characterize black
greater understanding of the capacity of liquor properties in terms of variables that impact
existing membrane technology to perform membrane pressure-based separations, including
these separations on black liquor is needed, as osmotic pressure, temperature, and pH. R&D
is a greater understanding of the feed should foster a greater understanding of the
properties. The gap between today’s influence of non-process elements (NPE) on black
performance and the desired performance is liquor solids removal and influence in the
not clearly defined. There is currently a lack of separation process. To ensure test results on
characterization of the process components various configurations and materials are
across membranes. comparable, standardized synthetic black liquor
formulations and testing protocols for membrane
suppliers should be developed.
The Membrane Technology
Program Black Liquor Concentration Process
This roadmap is slightly different from other
Studies
Agenda 2020 Roadmaps in that the projects R&D is needed to compare alternative membrane
represent a single initiative to enable a viable process designs using best available membrane
membrane technology option. The initiative technologies. A neutral black liquor and
identifies four areas of research. For each area, the membrane testing site should be established to
team specified the nature of the research to be carry out laboratory screening and provide analytic
oversight. The research should utilize the
learnings from testing process streams across

12 Reuse of Process Effluents Research Roadmap


existing membranes to provide research guidance fouling, including alterations in temperature and
on new membranes as challenges occur. pH. Engineering studies on pretreatment options
are needed to determine the optimal solution.
Small-scale experimental studies progressing to
larger trial skid-mounted units should be used to
understand the issues associated with specific
technologies. R&D should determine the
High-Priority R&D Projects
robustness of membrane systems using extended Based on these areas, the team identified an
trials under industrial operating conditions. integrated set of six high-priority R&D projects
(see the Table 2 below). In several cases, the
Membrane Fouling and Pre-Treatment identified project integrates multiple R&D
activities that the group determined would fit
Studies together and could be carried out as a single R&D
R&D is needed to determine the causes of fouling project. The six identified highest-priority R&D
and examine the factors that affect it, including projects are the following:
temperature, pH, particulates, non-process
elements, and concentration. Studies should
investigate pretreatment alternatives to reducing

Table 2. High-Priority R&D Projects

1. Modeling study to establish acceptable permeate quality specifications and process integration
alternatives
This project could include the following:
- Identifying the acceptable range of salts and organics in permeate for reuse in pulp washing and, if they fall
outside the target range, determining whether the permeate could be used somewhere else in the mill
- Conducting a sensitivity analysis with modeling
- Using existing membranes and identifying opportunities for reuse of permeate with solids > 0.1%

2. Characterize the capability of existing membrane technology


This project could include the following:
- Utilizing membrane suppliers to establish the capability of existing technology
- Performing a literature review (and seek membrane supplier review of the Georgia Tech 2015 membrane
literature survey) - Process modeling, conducting small-scale experiments—alternative process designs using
best available membrane technologies—output, economic business case
- R&D/engineering–systems for high-temperature and pH; engineering/pretreatment with existing systems

4. Development of a Membrane
Technology Program

Reuse of Process Effluents Research Roadmap 13


3. Characterize process streams across membranes and conduct bench-scale membrane performance
screening and research
This project could include the following:
- Characterizing process streams across membranes, and conducting membrane performance screening and
research (bench-top)
4. Development of a Membrane

- Establishing a bench-scale testing site with black liquor testing capability for the purpose of analyzing and
optimizing membrane technology
Technology Program

- Developing a standardized weak black liquor (synthetic liquor formulation) and test protocols
- Establishing osmotic pressure of weak black liquor and determining required operating pressure of the NF
and RO processes
- Developing capabilities to determine the causes of fouling and related loss of membrane performance–
temperature, pH, concentration, suspended solids, turpentine, soap, etc.

4. Develop a portable test skid for the purpose of analyzing and optimizing membrane technology
This project could include the following:
- Defining membrane performance and long-term effects on membrane assemblies

5. Membrane process simulation to predict permeate stream compositions based on inputs, membranes,
and configuration
This project could include the following:
- Modeling of the split of stream components across membrane configurations
- Developing a membrane modeling program to interface with WinGEMS models of the pulp mill

6. Develop new instrumentation to operate/control membrane systems


This project could include the following:
- Surveying and testing existing characterization and measurement tools for black liquor; identifying gaps
- Developing and testing new tools to address unmet needs

Using a structured format, the team developed projects and provide a basis for securing funding
detailed R&D project maps for each of the six and establishing partnerships. The project maps
projects. These project maps are intended to guide are presented in Appendix A
the implementation of the high-priority R&D

14 Reuse of Process Effluents Research Roadmap


5. Conclusion
Energy cost reduction is a focus area for pulp and Although focused this roadmap is focused on
paper manufacturers. A published energy membrane technology, Appendix B identifies
bandwidth study performed for the U.S. other promising technology options that should
Department of Energy identified paper drying and also be considered. The implementation the team’s
black liquor concentration as the largest total membrane technology program and exploration of
energy users among pulp and paper mill unit other technologies will require broad collaboration
processes. Black liquor concentration has long across stakeholders. This roadmap is designed to
been accomplished with the use of multi-stage, spur the necessary collective action and serve as
thermally driven evaporators. However, an an invitation and as guidance for future R&D
alternative technology to thermally driven efforts.
evaporation is required to achieve greater energy
savings. We look forward to engaging the research
community to address this challenge, and we
This roadmap focuses on membranes. The model welcome the input and engagement of industry,
developed by the team suggests that, for typical universities, research institutions, national
mills producing 2,000 air-dried tons per day of laboratories, and public agencies in developing
pulp, there is a $2–3 million annual energy cost technology options—and in further defining the
savings potential for integrating membrane-based questions and challenges.
black liquor concentration technology. Large-
production mills with weak black liquor solids We are grateful to all those who have contributed
content below 15% could realize as much as $5–6 to the development of this roadmap as well as to
those who will read and consider its content.
million in annual energy cost savings.

This roadmap identifies three promising


membrane technologies. Agenda 2020 is currently
or will be participating in development projects for
each technology in order to advance a viable
membrane solution for the Pulp and Paper
industry. This roadmap also defines a program of
R&D projects to help membrane technology meet
the unique performance requirements of a mill
environment. The combination of technology
development projects and enabling R&D projects
will accelerate the deployment of a membrane-
based solution to reduce the energy cost of black 5. Conclusion
liquor evaporation.

Reuse of Process Effluents Research Roadmap 15


16 Reuse of Process Effluents Research Roadmap
Appendix A: High-Priority R&D
Project Maps
The following pages present the project maps for The projects maps are presented in the following
the four high-priority projects. These project order:
maps are intended to guide the implementation
of the research and development (R&D) projects ■ R&D Project 1: Modeling study to establish
and provide a basis for securing funding and acceptable permeate quality specifications
establishing partnerships. and process integration alternatives
■ R&D Project 2: Characterize the capability of
The initial sections of the project map describe
existing membrane technology
the larger context for the proposed effort,
including the specific technical challenges to be ■ R&D Project 3: Characterize process streams
solved by the R&D project, and the benefits to across membranes and conduct bench-scale
industry and potential impact relative to the membrane performance screening and
Agenda 2020 Vision. Understanding this larger research
context is especially important to entities that are ■ R&D Project 4: Develop a portable test skid
considering funding or contributing to the for the purpose of analyzing and optimizing
project. Funding sources are more likely to back membrane technology
projects that address key technical challenges
and demonstrate alignment to industry needs. ■ R&D Project 5: Membrane process
simulation
The project map also includes a more specific
description of the R&D work, a specific plan for ■ R&D Project 6: Develop new
carrying out the R&D project, and additional instrumentation to operate/control membrane
guidance for carrying out the research. systems

Appendix A: High-Priority R&D Project


Maps

Reuse of Process Effluents Research Roadmap 17


R&D Project 1: Modeling study to establish acceptable permeate quality
specifications and process integration alternatives
Appendix A: High-Priority R&D Project

R&D Focus

Identify the acceptable range of salts and organics in permeate and determine whether the permeate can
be used elsewhere by iterative modeling within chosen limits of permeate components.
Maps

Benefits to Industry of this Project Potential Impacts re: Agenda 2020 Vision
LOW HIGH
 Potentially broadens range of possible Create/preserve jobs
membrane systems
Reduce carbon emissions
 Potentially improves membrane cost model Reduce fresh water demand
 Promotes resource, water, and energy Increase energy productivity
efficiency
Develop new biobased products
 Potentially clarifies other research efforts by
identifying key stream elements
 Provides potential design specs to membrane
manufacturers

Current State of Technology Keys to Success & Implementation Challenges

 Current data on permeate are limited, and  Identify other locations besides pulp washers
permeate is of differing composition from for permeate re-use.
membrane to membrane
 Identify basic requirements for permeate quality
at target process destination.
 Identify basic process elements that are critical
to quality

Requirements, Challenges, &/or Knowledge Gaps Addressed

Define acceptable process stream conditions that allow economically viable permeate re-use and
membrane application.
 Identify the acceptable range of salts and organics in permeate, and if they fall outside the target
range, determine whether the permeate can be used somewhere other than pulp washing.
 Identify of opportunities for reuse of permeate with total solids concentration greater than 0.1%.

18 Reuse of Process Effluents Research Roadmap


R&D Project 1: Modeling study to establish acceptable permeate quality
specifications and process integration alternatives (continued)

Project Plan

STEPS, TASKS, and ACTIVITIES EXPERTISE/PARTNERS TIMEFRAME

1. Conduct brainstorming meeting to determine the Mill operations in pulp, 2 months


following). paper, and chemical
recovery departments
a. Potential locations
a. SMEs for as many
b. Critical stream components areas as feasible
c. Common-sense limits on component b. Membrane company
experts

2. Design the model matrix. Primary modeling 2 months


personnel and select
group of experts

3. Execute model runs. Qualified facility 6 months/1


week (outside)

4. Validate key model results. 1-2 years


a. Validate achievability of required stream a. Membrane company
component concentrations.
b. Validate pulping process results. b. Pulp and paper
industry laboratory

Other Guidance

Appendix A: High-Priority R&D Project


Successful completion of this project is important to guide all succeeding projects in this initiative

Funding Options Maps

 Member companies of Agenda 2020


 Corporate sponsors (develop a consortium, including pulp manufacturers and membrane companies)
 DOE

Reuse of Process Effluents Research Roadmap 19


R&D Project 2: Characterize the capability of existing membrane
technology

R&D Focus
Appendix A: High-Priority R&D Project

An independent membrane consultant and a pulp and paper process expert evaluate and recommend
existing commercial technologies for feasibility testing.
Maps

Benefits to Industry of this Project Potential Impacts re: Agenda 2020 Vision
LOW HIGH
 Accelerate commercialization of an alternative Create/preserve jobs
concentration process to within 3–5 years. Reduce carbon emissions

 Develop pilot testing protocol. Reduce fresh water demand

 Deliver specifications for a full-scale system. Increase energy productivity

Develop new biobased products

Current State of Technology Keys to Success & Implementation Challenges

 See BLC Roadmap  Bring together creativity and knowledge from


both membrane manufacturers and pulp and
 GT membrane literature review paper industry experts.

 Write specifications for a full-scale system that


can be implemented within 3–5 years.

 Timing is good for tapping active membrane


supplier R&D for “dirty water” application.

 Commercial configurations or materials cannot


meet process needs (a positive outcome of this
“failure” is clear definition of the R&D gaps).

Requirements, Challenges, and/or Knowledge Gaps Addressed

Match existing membrane technology capabilities to black liquor concentration needs.

20 Reuse of Process Effluents Research Roadmap


R&D Project 2: Characterize the capability of existing membrane
technology (continued)

Project Plan

STEPS, TASKS, and ACTIVITIES EXPERTISE/PARTNERS TIMEFRAME

1. The Black Liquor Concentration Team prepares Team and consultant January 2016
preliminary weak black liquor feed specifications
(temperature, pH, flow, and composition) to poll
membrane technology providers for viable
options. Membrane consultant to coordinate/
follow up with technology providers on necessary
revisions.

2. Membrane suppliers provides best estimate of Membrane developers March 1, 2016


permeate and concentrate compositions and and manufacturers
rough full-scale budget cost.

3. Independent consultant evaluates offerings, Membrane Consultant June 1, 2016


recommends viable proposals, and specifies
required testing.

4. Conduct laboratory test by chosen candidates. Membrane Providers Sept. 1, 2016

5. Develop pilot protocol and schedule. Membrane Consultant Dec. 1, 2016

6. Conduct pilot testing. Selected Parties Jun-Dec. 2017

7. Develop bid specification, job sites, and system Consultant Jun-Dec. 2018
warranties, and navigate path to
commercialization (consultant).

Other Guidance

Appendix A: High-Priority R&D Project


 Project must avoid patent constraints.
 Project must consider alternative uses of permeate. Results from the modeling study in project 1 will
provide guidance.
 Consider a trailer-mounted unit as an intermediate step between pilot- and full commercial-scale (to
Maps
mitigate some ownership risk)

Funding Options
 Independent membrane consultant fees – NIST planning grant?
 Initial screening at membrane suppliers’ expense
 Pilot testing cost-shared – NIST grant and Agenda 2020 Consortium

Reuse of Process Effluents Research Roadmap 21


R&D Project 3: Characterize process streams across membranes and bench-
scale membrane performance screening and research

R&D Focus

1. Conduct a literature search on black liquor composition as background for two reference liquors— one
Appendix A: High-Priority R&D Project

hardwood and one softwood.


2. Develop the recipe for a synthetic black liquor that can be made in the laboratory with commercial
chemicals.
3. Determine ranges of compositions for “outlier” liquors (i.e., high K, Cl¯, soap, and turpentine).
4. Compare the reference liquor with several mill liquors.
Maps

5. Conduct a literature search on osmotic pressure of black liquor; measure, if not available.
6. Work with membrane manufacturers and pulp and paper industry to determine the tests to characterize
membrane performance.
7. Set up bench-scale facility to test membranes.
8. Screen candidate membranes and analyze for fouling causes.

Benefits to Industry of this Project Potential Impacts re: Agenda 2020 Vision
LOW HIGH
 Energy savings (offsetting natural gas usage) Create/preserve jobs

 Reduced interference with current mill Reduce carbon emissions


operations during screening/testing Reduce fresh water demand

 Comparable results across mills, liquors, Increase energy productivity


membrane manufacturers, and configurations Develop new biobased products

Current State of Technology Keys to Success & Implementation Challenges


 Experience with analysis of black liquor and
 Current membranes are severely challenged
components
at high pH and temperatures >70°C.
 Consistent test methods and standard test liquor(s)
 Mill-to-mill variations in liquor could pose  Sufficiently high degree of water removal to justify
problems for existing membranes cost and complexity
 Reasonable trade-offs between steam and
electrical energy
 Convincing demonstration of viability
 Appropriate membrane cost and useful life; lower
life-cycle cost for membranes than for current
concentration technology).

Requirements, Challenges, &/or Knowledge Gaps Addressed


 Challenge is to use membranes to achieve 50% or more of the water removal from weak black liquor
leaving the digester.
 Temperature, high pH, and chemical composition all contribute to harsh environment for existing
membranes.
 Liquor characteristics vary from mill to mill, and with the wood species.
 A reference liquor(s) should be defined such that all parties (both research and suppliers) have a
common starting point from which to compare results.
 Ranges for non-process elements potassium and chlorine should also be defined.
 Analytical testing protocols should be agreed upon to evaluate membrane performance and
failure/fouling modes.

22 Reuse of Process Effluents Research Roadmap


R&D Project 3: Characterize process streams across membranes and bench-
scale membrane performance screening and research (continued)

Project Plan

STEPS, TASKS, and ACTIVITIES EXPERTISE/PARTNERS TIMEFRAME

1. Establish reference hardwood and softwood Experience with black 2 months


reference liquor as a benchmark. Manufacturers liquor research
can test in-house as they see fit. Researchers can
enter the field on common ground. Outlier liquors
can be mixed up and tested as desired.

2. Confirm that the reference liquor behaves as a Black liquor testing 2 months,
model of real liquor (constituents, viscosity, etc.). capabilities depending on
number of real
liquors for
comparison

3. Establish common evaluation metrics. Industry Depends on


industry
response and
coordination

4. Establish neutral test facility. Qualified facility 3-4 months from


start of funding;
could vary with
complexity of
set-up

5. Develop data regarding causes of fouling. Qualified researchers Depends on


scope of study

Appendix A: High-Priority R&D Project


Maps
Funding Options

 Consortium of Agenda 2020 and membrane manufacturing companies; other private companies
 NIST planning grant?
 DOE grant?

Reuse of Process Effluents Research Roadmap 23


R&D Project 4: Develop a portable test skid for the purpose of analyzing
and optimizing membrane technology
Appendix A: High-Priority R&D Project

R&D Focus

Utilize a neutral party with in-house testing capabilities to build and demonstrate pilot with ambition to test
Maps

at mill site(s).

Benefits to Industry of this Project Potential Impacts re: Agenda 2020 Vision
LOW HIGH
 More rapid achievement of goals, pooling of Create/preserve jobs
resources and funding Reduce carbon emissions

 Industry-wide precompetitive opportunity to Reduce fresh water demand


drive change Increase energy productivity

Develop new biobased products

Current State of Technology Keys to Success & Implementation Challenges

 Bench apparatus expected to be in place  Participation across industry lines (suppliers,


before development of portable test skid pulp manufacturers, membrane manufacturers,
and other separations experts)
 Good identification and engagement of the
stakeholders (membrane, separations, and
others)

Requirements, Challenges, &/or Knowledge Gaps Addressed

Define membrane performance and long-term effects of black liquor on components of membrane
assemblies.

24 Reuse of Process Effluents Research Roadmap


R&D Project 4: Simulate Proposed Water Reuse Streams to Determine
Technology Needed and Return on Investment (continued)

Project Plan

STEPS, TASKS, and ACTIVITIES EXPERTISE/PARTNERS TIMEFRAME

1. Develop specifications for portable test unit.

2. Prepare a request for proposal.

3. Select supplier and award contract.

4. Build and evaluate unit.

Other Guidance

Determine how intellectual property will be handled; needs to be flexible.

Appendix A: High-Priority R&D Project


Funding Options

 Consortium dues Maps

 Federal grant money


 Endowment related to the industry
 Government advanced manufacturing process intensification grants

Reuse of Process Effluents Research Roadmap 25


R&D Project 5: Membrane process simulation
Appendix A: High-Priority R&D Project

R&D Focus

1. Identify group of candidate membrane modules.


2. Run laboratory/pilot tests with detailed chemical analyses of streams to test black liquor separation
Maps

through each (as a function of temperature, pressure, etc.).


3. Input data into process model.

Benefits to Industry of this Project Potential Impacts re: Agenda 2020 Vision
LOW HIGH
Capability to provide good predictions of Create/preserve jobs
economic/energy usage for various black liquor Reduce carbon emissions
concentration process options as well as
Reduce fresh water demand
separation performance and permeate
characteristics Increase energy productivity

Develop new biobased products

Current State of Technology Keys to Success & Implementation Challenges

 WinGEMs is limited in capability to model,  Ensuring that inputs are characterized (e.g.,
e.g., dynamic structure. Other process which black liquor(s) is/are used for testing?
modeling software (e.g., ASPEN) provides What were the operating conditions?) and that
more flexibility, but licensing costs are higher, a robust dataset is acquired
and the learning curve can be steep.
 Ensuring that model can work with WinGEMS
 Scarcity of available data on chemical pulp mill models
composition split, flux/fouling for black liquor
through candidate membranes, and
knowledge of cleaning capability/flux
regeneration for membranes.
 WinGEMS model is available for pulp mill but
not for membrane systems

Requirements, Challenges, &/or Knowledge Gaps Addressed

Challenge: Need membrane-specific data to model black liquor separation characteristics


Requirements: Need some level of basic separation data for black liquor through various membranes to
realistically model process steps. Need detailed chemical composition splits as function of temperature
and pressure for specific membrane options
Knowledge Gaps Addressed: Prediction of stream compositions based on inputs, membranes, and
configurations. Prediction of economic/energy usage for various black liquor concentration process
options

26 Reuse of Process Effluents Research Roadmap


R&D Project 5: Membrane process simulation (continued)

Project Plan

STEPS, TASKS, and ACTIVITIES EXPERTISE/PARTNERS TIMEFRAME

1. Identify likely best candidate membrane modules Membrane module 3-6 months
to purchase/collect modules at laboratory-scale suppliers, process
size. engineers with
membrane expertise
(academic and/or
industrial)

2. Conduct laboratory/pilot testing. Membrane process 1–3 years,


engineers/R&D depending on
scientists, analytical number of
chemists, and pulp and modules and
paper engineers as detail of tests
consultants and to
supply BL

3. Develop and validate a process model. Process modeling 1-3 months


“expert” and membrane
process engineer

Other Guidance

This project is contingent on the success of the first three projects, and could proceed in parallel with
development of testing capability and the proposed portable test skid

Funding Options Appendix A: High-Priority R&D Project


Maps
 Consortium of papermaking companies
 DOE grants, if potential energy saving is a primary driver

Reuse of Process Effluents Research Roadmap 27


R&D Project 6: Develop new instrumentation to operate/control membrane
systems
Appendix A: High-Priority R&D Project

R&D Focus

 Identify existing characterization and measurement tools used for black liquor

 Identify potential tools not currently used for black liquor


Maps

 Test tools/methods.

Benefits to Industry of this Project Potential Impacts re: Agenda 2020 Vision
LOW HIGH
 Understand feed black liquor characteristics Create/preserve jobs
and process variables that impact operability of
Reduce carbon emissions
membrane systems.
Reduce fresh water demand
 Develop membrane system sensors and
Increase energy productivity
control strategies required for commercial
operation of the new technology Develop new biobased products

Current State of Technology Keys to Success & Implementation Challenges

 Membrane sensors/controls not commonly  Complexity of black liquor


utilized beyond pressure, temperature, and
conductivity.
 Black liquor characteristics (temperature, pH,
color, and corrosivity) make robustness of
current sensors poor

Requirements, Challenges, &/or Knowledge Gaps Addressed

 Knowledge of feed black liquor characteristics, such as osmotic pressure and temperature, which will
enable testing and understanding of membrane systems’ ability to perform satisfactorily under all
expected conditions.

28 Reuse of Process Effluents Research Roadmap


R&D Project 6: Develop new instrumentation to operate/control membrane
systems (continued)

Project Plan

STEPS, TASKS, and ACTIVITIES EXPERTISE/PARTNERS TIMEFRAME

1. Literature survey/state of the art/current practice. Contractor/ consultant 3 months


(pulp and paper)

2. Feedback from membrane companies regarding Membrane vendors and 6 months


primary foulants/process conditions and methods experts
to measure them—needs/want

3. Gap analysis for existing vs. needed tools/ All of the above 3-6 months
methods
- Development of new tools/methods

4. Testing Pulp and paper/ 2 years


- Laboratory – synthetic vs. actual black liquor analytical suppliers
- Pilot 3 & 4 to
- Field be done
iteratively

Appendix A: High-Priority R&D Project


Funding Options
 Industry consortium
 NIST planning grant
 NSF/NIST if for advanced analytical tools Maps
 RBI endowment

Reuse of Process Effluents Research Roadmap 29


Appendix B: Additional
Background and Modeling
Appendix B: Additional Background

Results
and Modeling Results

Additional Background to 1.1 million Btu potential reduction may be


possible through the utilization of advanced
The United States has 99 kraft pulp mills in 24 membrane systems in conjunction with current
states,11 producing 45 million tons of pulp a year. BAT. These technologies are indeed looking
Dissolved wood components and spent pulping beyond the current BATs.
chemicals are washed from pulp to become weak
black liquor, an aqueous stream in the proximity Weak black liquor from the pulp washers is about
of 15% solids (see Figure 4). Black liquor is 15% solids, consisting of inorganic salts (30%–
concentrated from near 15% solids to 50% to 85% 45%), alkali lignin (30%–45%), and wood acids
solids with steam energy in multiple-effect and polysaccharides (30%–45%), plus resins, fatty
evaporators and concentrator technology. The best acids, and methanol (3%–5%). Each air-dried ton
technology in use today for initial concentrating is of unbleached pulp delivers 2,000–3,500 pounds
falling-film of black liquor solids, depending on pulp grade
multiple-effect and wood species.
evaporators with six
or seven stages. Kraft pulping, the dominant chemical process used
These systems have to separate wood fibers, is a well optimized
steam economies up system, and black liquor concentration must
to 5.8 pounds of integrate with mill steam, power, water, and waste
water evaporated per systems for efficient and profitable operation.
pound of steam Kraft pulping requires near-complete recovery of
used. the inorganic elements—sodium and sulfur—used
Figure 4. Concentrated
Black Liquor as pulping agents to be profitable. Dissolved wood
According to a components, including lignin and hemicelluloses,
published energy bandwidth study, through have significant fuel value. By burning black
implementation of current BAT the industry could liquor to produce steam, the mill obtains energy
realize concentration energy demands of 3.0 and electricity and recovers sodium and sulfur for
million Btu per air-dried ton by incorporating reuse in pulping.
integrated seven-stage multiple effect systems
from the current industry average of 3.5 million The U.S. pulp and paper manufacturing industry is
Btu per air-dried ton.12 However, an additional 0.8 actively addressing national goals of sustainability
and energy productivity. Pulp and paper
manufacturers are interested in new breakthrough
11
RISI Mill Asset Database, January 2014.
12
Kinstrey, R., and D. White. “Pulp & Paper Industry Energy Pulping & Environmental Conference, Jacksonville, FL,
Bandwidth Study,” Paper 27-1 at 2007 TAPPI Engineering, October 2007.

30 Reuse of Process Effluents Research Roadmap


technologies that can enable large reductions in Mechanical vapor recompression (MVR), also
energy demand, and are engaged in partnerships
with private companies, federal agencies, and
academic establishments to develop these
technologies.

Surpassing Best Available Technology


—Additional Information not included in
Chapter 2
Significant improvements in technologies for
concentrating black liquor above 50% solids
content have been made in recent years by
applying concentration principles to steam-driven
evaporator designs. These improvements have Figure 5. Andritz MVR Evaporator
largely addressed equipment reliability and called vapor compression evaporation (VCE)
availability by reducing scaling and plugging technology, is one commercially available
rates. alternative to conventional thermally driven
evaporation. The water vapor evaporated from
Black liquor concentration below 50% solids black liquor is recompressed with a simple, low-
content has received less attention, yet it is in this speed centrifugal fan. After the fan, the

Appendix B: Additional Background


and Modeling Results
Figure 6. BAT Multiple Effect Evaporator for 50% Solids Concentration Black Liquor

concentration range that the greatest potential mechanically heated vapor is used as heating
energy savings exist. In a system requiring black medium in the heating elements of the same
liquor to be concentrated from 15% to 80% solids evaporator body. The technology uses electrical
content, 86% of the water removal duty will occur energy rather than thermal energy (steam) to
in raising the concentration from 15% to 50%. accomplish liquor concentration. This can be
advantageous for mills with higher fuel costs and

Reuse of Process Effluents Research Roadmap 31


lower electricity costs. Power consumption ranges retained in a BAT evaporator system when
from 14 to 18 kWh per 1,000 kg of water integrating a membrane-based concentration
evaporated. The upper limit of black liquor technology.
concentration achievable with MVR technology is
25%–30% solids content.
Base Case and BAT
Appendix B: Additional Materials,
Identification of R&D Priorities

To simulate the typical mill installation, a base-


case model incorporating a six-effect evaporator
Development of Process Model with a two-effect concentrator concentrating liquor
A WinGEMS model of a generic 2,000-tpd kraft to 70% solids was constructed using WinGEMS
mill was constructed to evaluate the overall modeling software.
process and economic impact of integrating
membrane-based concentration and mechanical A second BAT base case was built to simulate
vapor recompression technologies with mills that incorporate a BAT evaporator set. The
conventional multiple-effect evaporator BAT base-case model incorporated a seven-effect
technologies. MVR technology is commercially evaporator to concentrate liquor to 70% solids.
available, and performance parameters in the
process model were based on industrial experience Simulation Cases
with commercial installations. Because there is no Simulations were run using theoretical membrane
membrane technology yet proven for black liquor and commercially proven mechanical vapor
concentration, the separation efficiency for water recompression technologies. In each case, liquor
from black liquor was assumed. The model is a was concentrated from 15% to 30% solids, then
useful tool to estimate the opportunity for sent on to a four-effect evaporator set where the
alternative black liquor concentration technologies solids were increased to 50%, and finally sent to a
and assign priority for R&D efforts. In addition, two-effect concentrator where solids were
the model provides a framework to evaluate actual increased to 70% for firing in a recovery boiler. In
test results when they become available. the BAT case, a seven-effect evaporator was used
to increase solids from 30% feed to 70% for firing
We have assumed that membrane-based in a recovery boiler. Inadequately treated
concentration and MVR technologies can achieve whitewater that is reused in pulping and bleaching
30% black liquor solids concentration. Typical operations often contains iron and manganese,
multiple-effect evaporator systems based on rising which catalyze hydrogen peroxide decomposition.
film technology would require modification to be Chelating agents are used in bleaching with stages
able to operate on 30% solids feed-liquor. The using hydrogen peroxide to prevent the excessive
increased boiling-point rise and requirement to decomposition of the hydrogen peroxide bleaching
reduce vacuum for adequate heat transfer in the agent. Effective removal of problematic metal
last effect would not provide sufficient cations may reduce the need for costly chelating
temperature differential to operate six or more chemicals and increase whitewater reuse
effects. We have therefore assumed that opportunities in the pulping and bleaching areas.
integrating a membrane-based concentration
technology would require bypass of two effects in Treatment of Waste Heat
an existing six-effect rising film set. Because best Utilization of excess heat from the warm-water
available falling-film evaporator designs operate at return from the evaporator surface condensers will
much lower temperature differential per effect, we vary from mill to mill. To avoid the need to
have assumed that up to seven effects can be account for variation in energy saving potential

32 Reuse of Process Effluents Research Roadmap


that would result from varying waste-heat Model Runs
approaches, the team assumed that waste heat Three scenarios were run against the typical mill
associated with the evaporator surface condenser base-case and one scenario was run against the

Figure 7. Simulation of Theoretical Two-stage Membrane-based Water Removal

would be sent to a cooling tower that would swing BAT evaporator base-case.
with the various scenarios. This allowed the model
to evaluate only the impact of the steam and The first-case scenario was run modeling
electrical savings/costs associated with the black membrane technology. The first membrane case
liquor concentration technology. allowed the turbine condenser load to swing. In

Appendix B: Additional Background


this scenario, the boilers’ steam output was fixed;

and Modeling Results


It is possible that additional heat-recovery projects the decreased steam demand in the evaporators
may be required by some mills and not by others was condensed in the turbine condenser,
to address decreased excess heat available from increasing electrical power production. This
surface condenser water when membrane or MVR allowed the team to compare the benefit of
black liquor concentration technologies are increased electrical power generation in lieu of
employed. These projects are beyond the scope of fossil-fuel savings. The second membrane case
this study. was run with the model’s turbine condenser fixed
and the power boiler swinging purchased fossil
fuels to meet mill steam demand. The third case
featured a simulation of Mechanical Vapor

Reuse of Process Effluents Research Roadmap 33


Recompression (MVR) with the turbine condenser A single case was run against the BAT evaporator
load fixed. base case. In this case, a membrane model was run
with the model’s turbine condenser load fixed and
Table3:
Table 2. Summary
Summary ofofProcess
ProcessModel
ModelResults
Results
Appendix B: Additional Materials,
Identification of R&D Priorities

34 Reuse of Process Effluents Research Roadmap


the power boiler swinging purchased fossil fuels to In the membrane system with the fixed turbine
control mill steam demand, similar to the second condenser load, the overall mill thermal energy
case above. usage was decreased by 1.49 MMBtu/ADT and
the purchased electric power increased by 0.07
All simulations were run with the assumption that MW per ADT. The power requirements of the
the filtrate from the membrane and MVR membrane pumping system increased the
technologies could be collected and reused as electrical demand; in addition, the need for
shower water in the pulp mill washers, and that the purchased electricity increased to compensate for
solids concentration in the filtrate would be below the reduced power generation.
0.1%.
For the MVR system case with fixed turbine
condenser load, the overall mill thermal energy
Results
usage was decreased by 1.45 MMBtu/ADT and
The results of the various cases described above
the purchased electric energy increased by 0.12
are detailed in Table 3. The projections suggest
MW per ADT. The increase in electrical load is
that implementation of membrane technology does
attributed to the increased power requirements
have the potential to make a significant reduction
from the pumping requirements of the MVR
in evaporation energy demand and contribute in an
system, which is estimated to be greater than the
important way to the goal of 50% reduction in
membrane technology, and the decrease in
total energy.
cogeneration associated with the reduced steam
requirements of the mill.
The thermal energy and electrical power required
to manufacture one air-dried ton (ADT) of pulp
In the final case with the BAT evaporators and
was evaluated in each of the cases against the base
membrane technology, the overall mill thermal
case and BAT base case scenarios. The thermal
energy usage was decreased by 1.54 MMBtu/ADT
energy in MMBtu/ADT was calculated using net
and the purchased electric increased by 0.08 MW
output energy in steam from all boilers (recovery
per ADT. The increase in electrical load is
and power). Utilizing the net energy in the steam
attributed to the increased power requirements
output rather than fuel energy input allowed the
from the pumping requirements of the membrane
team to evaluate the energy savings regardless of
system and the decrease in cogeneration associated
fuel mix and/or boiler efficiencies.
with the reduced steam requirements of the mill.
For the first case with the membrane system and
The model suggests that for typical mills

Appendix B: Additional Background


the turbine condenser load swinging, the overall
producing 2,000 air-dried ton per day of pulp there
mill thermal energy usage decreased slightly by
is a $2–3 million annual energy cost savings

and Modeling Results


only 0.05 MMBtu/ADT and there was a reduction
of 0.02 MW per ADT of mill purchased power potential for integrating membrane-based black
versus the base case. This was the only case for liquor concentration technology, assuming that
which a decrease in purchased power was one or more can be successfully commercialized.
predicted. This decrease is attributed to the Large-production mills with weak black liquor
increase in power production due to the increase in solids content below 15% could realize as much as
condenser load. This increase was more than $5–6 million in annual energy cost savings.
enough to offset the increased electrical usage
associated with the membrane technology.

Reuse of Process Effluents Research Roadmap 35


Non-Membrane Technologies recovered with counter-flow heat exchangers. 2)
Black liquor viscosity is a strong function of solids
Considered content, and temperature. If liquor is to be freeze-
concentrated below 0°C, it is expected that a
Freeze Concentration concentration would be reached where the liquor
Appendix B: Additional Materials,
Identification of R&D Priorities

In addition to overcoming the barriers surrounding becomes too viscous to separate the ice crystals.
membrane separation technology, the Black 3) Ice forms more readily when there are
Liquor Concentration Team also considered freeze nucleation sites/surfaces present. The crystals
concentration as an approach with a potential would need to form fast enough to accommodate
thermodynamic advantage over conventional the high flow rate of liquor. Therefore it will have
evaporation technology that had not been to be determined if the crystallization rate is
commercialized. The team decided to explore the adequate or if some sort of seed material will be
barriers preventing implementation of the required.
technology and determine whether it might hold
promise today for surpassing current best available
Evaluation
technology.
Using the WinGEMS mass and energy balance
Description and Advantages software, the team evaluated the freeze
A study by Rousseau and Sharpe13 reports that concentration approach. First, the model required
weak black liquor can be concentrated by lowering adjustments to deal with temperatures below 32°F,
the temperature until ice crystals form and then and a fix was devised. A process model was then
separating them from the solution. The ice formed developed to provide the mass and energy balance
is pure (or very nearly so) water and the heat of basis for sizing the heat exchanges and process
fusion is only 15% of the heat of vaporization; vessels that would be required (see Figure 8).
thus, the technique could be viable to perform a From this information, a team member developed
portion of black liquor concentration required by a capital estimate.
the kraft chemical recovery process. Rousseau
and Sharpe’s work was limited in that they started While not rigorously evaluated, the theoretical
with 21% liquor solids and concentrated it to 24% fossil fuel energy usage of freeze concentration as
solids. Their work showed the technique to be predicted by the model would be higher than for
valid, but the concentration change would need to membrane-based systems. This is because the
be far greater to justify it as a commercial process. concentrated liquor temperature to the evaporators
is 30°F lower for the case of freeze crystallization,
There are three major issues to address. 1) Weak which would increase steam usage at the
liquor enters the evaporators at 85-90°C. If evaporators. In addition, the electrical loads
freezing is to be viable the energy savings would required for the refrigeration cycle would be
have to justify the use of refrigeration to reduce higher than the pumping requirement for a
the temperature to less than 0°C. The membrane-based system. These higher operating
concentrated liquor would then have to be costs would decrease the potential energy savings
reheated to near the boiling point at the feed point of freeze concentration over membrane-based
in the evaporators (60-80°C). Note that a technology, and the estimated capital cost is likely
significant amount of this energy could be to be higher than membrane technology. For these
reasons, the team concluded that there is not a
13
Rousseau, R. W., Sharpe, E.E., “Freeze Concentration of compelling business case for developing freeze
Black Liquor: Characteristics and Limitations,” Ind. Eng.
Chem. Process Des. Dev. 19(1):201-2004, 1980. concentration technology in the near term.

36 Reuse of Process Effluents Research Roadmap


and the lack of a means to separate clean ice
The team also noted knowledge gaps associated crystals from viscous black liquor.
with freeze concentration of black liquor,
including the viscosity of 25-30% solids The team would welcome additional information
concentration black liquor at low temperatures, or insights on this option if its proponents believe
there is a stronger case to be made.

Figure 8. Freeze Concentration Process Concept Schematic with Preliminary Mass and Energy Balance
Results
Agenda 2020 Team Work-Product
December 2015

 Black liquor pre-treatment to fundamentally

Appendix B: Additional Background


change the process of water removal
Other Technologies to be Explored (exploratory research)
The Agenda 2020 Black Liquor Concentration

and Modeling Results


Team reaffirms its priority interest in membrane-  In situ conversion of lignin into “super-
based technologies and its parallel interest in the sponge” to tie up other components in black
liquor (exploratory)
creative suggestions from experts in the field as to
reasonable next steps to develop alternative  Electrolysis for colloidal suspension
technologies. Some that we have discussed include separations
those listed below and we are open to additional  Dialysis; RO
approaches.
 Precipitation – for example, LignoboostTM for
organics removal

Reuse of Process Effluents Research Roadmap 37


 Adsorption – potential for integration with Longer-Term Research
membranes as pre- or post-processing step?
Opportunities
 Electrifying; in situ resistance heating
In addition to the shorter-term research goals
detailed above, many of these ideas also have
Appendix B: Additional Materials,
Identification of R&D Priorities

Ideas We Considered and Deferred longer-term needs that will need to be addressed
 Use less water for washing – outside scope of by development efforts. The items listed below
our team charter represent efforts that will be targeted over the next
three to five years.
 Higher concentration salts/forward osmosis
 Biological – red bacteria 1. Process development of all membrane
technologies
 Solvents – challenge for greater than binary
a. Bench-top scale experimentation
systems
1) Determine viable flux and throughput
 Supercritical fluid extraction limits
 Licella approach developed for deoxygenating 2) Develop maintenance and wear models
biomass would eliminate need for evaporators 3) Refine life cycle cost measures in
and recovery boiler (convert organics direct to reference to key process component path
biofuel), challenge is recovery of inorganics. b. Pilot-scale development
Extensive process development required to
deal with two byproduct streams (phenols) and 1) Determine practical unit size for industrial
major capital investment required application
~$100,000,000. We see no path to success at 2) Assess additional areas of limitation with
this point. mill level applications
 Recovery of sodium and sulfur without the 2. Progression to bench-top research for freeze
water concentration
o Co-react – precipitate a. Determine the process path for key
o Organically bind – ion exchange components such as methanol and soap
o Pretreatment – settling b. Determine the energy cycle cost for freeze
concentration of black liquor
o Pulping pretreatment that makes organics
easier to separate
The interest of the team remains open to additional
o GMO Tree – low lignin
technologies that experts may suggest.
o Chemically treat the wood; skip the digester
(dry pulping)
 Microwave evaporation – preliminary study Considerations for the Implementation
suggests higher energy cost than current of these Non-Membrane Technologies
multiple-effect evaporator technology Certain fundamental integration issues must be
addressed across all alternative technologies
 Forced convection only applies to liquors
explored. The new technology must be capable of
above 50% solids concentration
integration with upstream and downstream
processes. The following considerations will be
critical for this effort:

38 Reuse of Process Effluents Research Roadmap


Process Variables • Economics – What are the economics of
• Selectivity – How effectively does the existing evaporator configurations, from
technology separate the organics, inorganics, conventional to state-of-the-art systems, and
and water? what are the economics of alternative
technologies?
• Environmental Compliance – How does the
fate and transport of methanol in the new
technology affect compliance with non-
Performance Criteria
condensible gas control requirements?
In addition to the process integration requirements
• Organics Materials Balance – At what point discussed in the preceding section, overriding
does removal of organic material from the performance criteria for any replacement
liquor inhibit firing in the recovery boiler?
technology includes the following:
• Characterization – How do changes in black
liquor rheology, lignin molecular weight • Cost-effectiveness – The new technology must
distribution, etc., impact the new technology lower operating cost more than current
options? How are they impacted by new multiple-effect evaporation technology, and
technology? lower the capital cost compared to current
equipment for evaporation.
• Wood Species – How do choices of wood
species impact technology options and • Materials Compatibility – The new technology
implementation? How can we identify, must be compatible with the high-pH/high-
quantify, and address the impacts of variable temperature environment, flow rates, pressure
characteristics of wood species—e.g., the ratios drop, and uptime in the pulp mill.
of organic/inorganic materials, the silica and
• Throughput/Flux – The new technology must
soap contents, and sulfidity variability in wood
be able to handle the volumes experienced at a
species—that may impact technology
1,000- to 2,000-tpd pulp mill.
performance?
• Availability – The replacement technology
• Variability – How does variable inlet weak
must require less downtime for
liquor concentration impact the separations by
cleaning/maintenance than current evaporators.
new technologies?
• Environmental Impacts – As stated above, the
• Suspended Solids – What are the impacts of
new technology must be well integrated with
suspended solids (e.g., fiber and lime mud) on
existing wastewater treatment and gaseous
new technologies?
emission handling systems. A lower carbon
• Energy Balance – What are the energy impacts footprint is needed.

Appendix B: Additional Background


of alternative technologies? • Separation Effectiveness – Separation
• Mill Water Balance – What impacts arise from technologies must show separation

and Modeling Results


reduced availability of evaporator condensates effectiveness. Ideally, the quality of the
for reuse in the mill? Is the mill water balance permeate water stream would be suitable for
adversely affected? Do alternative sources of reuse elsewhere in the process, and at a
process water from the new technology or minimum, it must not interfere with existing
other location contain incompatible wastewater treatment processes.
contaminants? • Time Frame – The new technology must be
• Analytical Methods Advances – How do new developed within the next 3 to 10 years.
analytical capabilities enable development of Durability – The system must have a reasonable
new technologies?
lifespan. Longer-term results, perhaps through

Reuse of Process Effluents Research Roadmap 39


side-stream pilot tests, are needed to establish
commercial feasibility.
Appendix B: Additional Materials,
Identification of R&D Priorities

40 Reuse of Process Effluents Research Roadmap


Appendix C: Additional Content
for the Membrane Technology
Program

The Membrane Technology Program projects Challenges and Knowledge


arose from the Black Liquor Concentration
Technology Workshop was held on October Gaps
15‒16, 2015, at the Cincinnati Airport Hilton in
During the workshop, participants were given a
Florence, Kentucky. The workshop brought
list of the requirements for a membrane solution.
together a select group of SMEs and industry
For each requirement, participants were then asked
representatives to refine key R&D priorities and to
to identify the technical challenges and/or
map out actionable R&D projects for advancing
knowledge gaps that currently prevent membranes
new energy-efficient methods to remove water
systems from meeting that requirement.
from kraft pulp mill black liquor.

The Agenda 2020 Technology Alliance conducted


this workshop, funded by a grant from the The following tables present the workshop results
National Institute of Standards and Technology of this discussion for each breakout group. The
under the Advanced Manufacturing Technology table headings in white text represent the
Consortia (AMTech) program. The AMTech requirements, which were posted as header cards
program supports basic and applied research on for the brainstorming. The black dots following
long-term, pre-competitive, and enabling each item indicate the number of votes it received
technology development. The program goal is to during the prioritization; more votes indicate a
strengthen the capacity of U.S. industry and the higher priority.
nation to compete in global markets.

Appendix C: Additional Content for the


Membrane Technology Program

Reuse of Process Effluents Research Roadmap 41


Knowledge Gaps & Challenges – Group A

High Flux/Throughput Membrane Systems


Appendix C: Additional Content for the
Membrane Technology Program

 BL component composition variability 


 2-stage versus single-stage membrane separation process
 Need better understanding of HW/SW BL differences and paper company differences

Robust Materials
 RO required for 0.1% solids permeate; materials today can’t run at pH 12-13, +80-95C (most today are based on thin- film
polyamide technology) 
 Temperature/pH-resistant modules (membrane and materials that hold it together, adhesives, seals, etc.)
 Manufacturing scalability of membranes/module technology that meets desired process criteria

Resistance to Fouling/ Decreasing Downtime


 How do we test fouling of membranes? What fouls the membrane? 1 component, mixture, T, pH 
 Membrane fouling – does concentration change of components affect fouling? 
 Need redundant/standby capacity in today’s pulp mill

Optimal Separations
 Change the feed instead of the membrane. 
− Need to understand process options that could make membrane technology more feasible (can we lower temperature, pH,
etc.?)
− Pre-treatment vs new materials? Which is better approach? R&D vs Engineering
 Calcium removal – what are the membrane options? 
 Separation process--which compounds partition with which stream? 

Mill Integration (balances, compliance, soap, impact of new substances)


 Feed analysis & properties 
 Are there evaporation problems that could be solved by HF/UF? 
 Permeate Reuse 
 Are there pretreatments that could reduce the load to the evaporator? 
 Feed variability – daily, monthly, annual 
 Where does the methanol go? Believe that it will go right through the membrane. 
 Necessary to recover lignin or other components?
 Upstream and downstream impact of cleaning/coating agents – how to figure out?
 Ceramic – Long life, higher cost vs shorter life, lower cost – performance economics
 OPEX and the energy efficiency of the membranes has to be cheaper than evaporation technology
 Soap and Turpentine removal before or after membrane filtering
 Find alternate uses for the permeate other than pulp washing to eliminate the 0.1% solids target for permeate
 Need to determine whether soap separates in the process
 How can you measure interfacial water?

42 Reuse of Process Effluents Research Roadmap


Group A Discussion Themes

1. Understanding characteristics of BL. Strong signal here from membrane delegation. Feed analysis; osmotic pressure
2. Understanding the process options—R&D problem; If you can change the feedstock, you could make it more forgiving for
existing commercial processes. Pretreatments. RO chemistries that can run high pH, high T
3. Understanding fouling. Need a characterization technique. Rapid test?

Knowledge Gaps & Challenges – Group B

High Flux/Throughput Membrane Systems

 Potential flux of Black Liquor through a membrane is unknown ‒ We have no idea what the flux might be; no basis to size
anything 
 Pressure, flow, etc., needed for desired permeate quality

Robust Materials
 We do not understand the long-term effect of Black Liquor on membrane and module materials 
 Thermal cycles damage to membrane systems, damage from thermal cycling 
 Need to understand the character of BL going into the system (composition, pH, temperature) 
 How does turpentine affect membranes?

Resistance to Fouling/ Decreasing Downtime


 Fouling rates versus fiber content and fiber size 
 What are the primary fouling mechanisms? What are the chemistries and reactions at a fouling site? 
 Nature of fouling – BL through MF/UF/RO/NF
 Presence of micro-fibers, microparticles ‒ contents in Black Liquor
 Suspended solids--impacts on membranes?
 Cleanability of membranes is unknown. What cleaning agents will work?

Optimal Separations

Appendix C: Additional Content for the


Membrane Technology Program
 What membrane system configuration can work in this application/on Black Liquor? Life versus costs of membrane unknown.
What are the life-cycle considerations? 
 RO won’t work with high-feed TDS; is 1000 PPM TDS clean water required? 
 Don’t know the requirements of the various separations points (RO, NF, UF, MF) 
 Methanol separation from liquor – what happens? 
 Is NF-quality permeate OK? It will have low total suspended solids & color, but will be at feed TDS.
 What is the optimum concentration of BLS?

Mill Integration (balances, compliance, soap, impact of new substances)

Reuse of Process Effluents Research Roadmap 43


 What is the capability of the existing membrane technology to perform these separations on black liquor? (temp., pH, etc.)—
what is the gap between today’s performance and desired performance? 
 Lack a characterization of the process components across membranes 
 Issues with soap separation at 30% solids; managing soap separation is a challenge 
 What is an achievable concentration versus flux, fouling, cleanability, and energy? What is the optimum concentration of BLS?
Appendix C: Additional Content for the


Membrane Technology Program

 Surrogate standard BL for standardized, comparative testing 


 Membrane cleaning agent assimilation on process or disposal; fate & transport of cleaning agents
 Understanding of footprint limitations
 Disposal of used membranes?
 What is impact or benefits of retentate (stage 1) on the remaining evaporator effects? ‒ i.e., reduced fouling?

Other
 Membrane technology other that pore-size exclusion; should we explore other technologies besides pressure-driven? -
Membrane distillation; Pervaporation

Economics—Ineligible for voting right now; optimization issues


 One-step or two-step process? “Fit for purpose”
 Employee knowledge base to implement membrane technology; worker knowledge and skill requirements
 Maintenance cycle cost and time? Annual rebuilds of units? Don’t know life-cycle cost of the different configurations

Group B Discussion Themes


1. What is the capability of existing membrane technology on BL? What is the gap between existing technology and desired
performance? [Runaway favorite]
2. What meets the objectives?
3. Fouling rate vs fiber content and size; mechanisms; nature of resulting compounds
4. Long-term effects on the membrane of the material going through it? Impacts of those effects? What can we recognize now
to narrow the field?

R&D Projects
Following the problem definition discussion
above, participants were asked to identify R&D
projects to address the knowledge gaps and
challenges. The results of this discussion are
presented in the tables below. The black dots
following each item indicate the number of votes
it received; more votes indicate a higher priority.

44 Reuse of Process Effluents Research Roadmap


RD&D Projects – Group A
Black Liquor Studies

 Study and characterize feed variability in terms of osmotic pressure, temperature, pH, etc. using on-line monitoring at mill of
weak black liquor 
 Study dead-load removal re white and black liquor ‒ conduct a lab-scale test of white and black liquor to determine what
membranes can do 
 Characterize and document black liquor that comes from various woods and processes

Process Studies
 Use process modeling and small-scale experimental studies to compare alternative process designs using best available
membrane technologies in order to understand the economic case for pursuing 
 Study use of existing membranes to identify opportunities for reuse of permeate with solids > 0.1% 
 Study to determine where the methanol (MeOH) goes using a lab/portable test skid
 Conduct an overall study of process, starting with kraft liquor using onsite measurement & analysis at a pilot plant
 Study optimal separations – explore catalytic solutions
 Conduct small-scale lab study to determine process optimization for membranes
 Conduct pilot/demonstration studies of single- versus 2-stage (multiple-stage) separations

Membrane Options Study


 Membrane Screening; bench-top and in pilot plant 
 Membrane material development and demonstration: RO separation studies; stable at > 85°C, > pH12
 Study of membrane sensitivity to varying black liquor samples: test different membranes with different black liquor samples to
determine how much variability each can take

Develop Research Site & Tools


 Establish a black liquor/membrane consortium in order to create a portable skid at a neutral site like GA Tech – RBI that can
also be used to test black liquor ‒ a one- stop research site 
 Develop R&D onsite measures and analysis tools 

Fouling Studies
 Determine what causes fouling and factors that affect it: temperature, pH, particulates, concentration 
 Study how pretreatment can reduce fouling 

Appendix C: Additional Content for the


Membrane Technology Program
Pre-Treatment Studies
 Conduct R&D on systems or system changes for increasing temperature and decreasing pH and engineering studies on
pretreatment with existing systems, in series or in parallel, in order to determine the best solution 

Reuse of Process Effluents Research Roadmap 45


RD&D Projects – Group B
Basic Research
Appendix C: Additional Content for the

 Characterize process streams across membranes utilizing Lund University or RBI or Econotech to test streams as membrane
Membrane Technology Program

research continues 


− Characterization of process components: 1) select university for lab screening with appropriate capability, 2) develop
adequate budget for testing
− Membrane test bed for long- & short-term testing; third-party university/research institute with analytic oversight
 Identify the acceptable table range of salts and organics and determine whether it can be used somewhere else and where

 Conduct simple testing to establish osmotic pressure of black liquor and determine required operating pressure of the NF and
RO processes 
 Study demineralization: Determine osmotic pressure, permeate quality NF & RO; osmotic membrane distillation; fouling index
with pretreatment permeate
 Develop online weak liquor characterization so plant changes are immediately known (what lab tests are needed?)
 Study fouling rates – survey of weak black liquors for suspended solids; RBI ideal provider, but who pays the bill?

Materials Research
 Define membrane performance and long-term effects – Develop standardized weak black liquor 
 Determine long-term effects of black liquor on membrane assemblies; develop a synthetic black liquor formulation for
membrane suppliers to use
 Determine chemical and thermal compatibility – conduct literature search on polymeric and metallic; identify potential
candidates; conduct long-term exposure tests re tensile, swelling, integrity
 Determine long-term effect of black liquor on membranes – add coupon- style tests to existing research efforts, add other
sample by suggestion

Demonstration & Testing


 Coordinate pilot studies at a university – can determine permeate and concentration stream makeup and how it can be used in
plant, and establish permeate criteria 
 Identify what the fouling mechanism are: fouling agent characterization – tests components of black liquor alone and in
mixtures to identify foulants and effect on different membrane types; use lab tests and analytical autopsy 
 Determine separation requirements: Membrane suppliers give best guess of what current technologies can provide; Agenda
2020 investigates where best to reincorporate those stream and models with WinGEMS
 Element formats – cost/benefit/ feasibility; tubular/HF/Spiral combo 

Modeling and Simulation


 Process simulation/modeling to predict stream compositions based on inputs/ membranes/ configuration 
 Run more/different WinGEMS simulations to evaluate the impact on the overall process
 Use WinGEMS simulation of BL-BL heat exchanger to study lowering feed temperature 
 Simulate using permeate as bulking liquor for batch digesters
 Run simulation/economics on lower solids to evaporator but less fouling

Mill Integration (balances, compliance, soap, impact of new substances)


 Determine what existing membrane technology is capable of: Utilize membrane suppliers to establish existing basis; perform lit
review 

46 Reuse of Process Effluents Research Roadmap


Appendix D: Contributors
The Agenda 2020 Black Liquor Concentration Team acknowledges and thanks the many people who
contributed knowledge, expertise, time, and energy to production of this research roadmap. We ask the
indulgence of any whom we may have inadvertently omitted.

Agenda 2020 Black Liquor Team Members


Name Organization
Chris Verrill, Co-lead International Paper
Takis Taousakis, Co-lead (2013 –14) MWV/WestRock
Sean Ireland Verso Paper
Fritz Paulsen Kapstone Paper
Jim Bradbury, Co-Lead New Page/Verso
Greg Burns Kapstone Paper
Chris Edgcumbe SAPPI
Don Guay New Page/Verso
Jarmo Kaila Andritz
Sergey Shevchenko Nalco
Ricardo Santos, team manager MWV/WestRock
Jason Smith Kadant
Ron Brown, Executive Director (retired) Agenda 2020
David Turpin, Executive Director Agenda 2020

Appendix C: Additional Content for the


Membrane Technology Program
Kathleen Bennett Agenda 2020

Reuse of Process Effluents Research Roadmap 47


Technology Presentations
The Black Liquor Concentration held a workshop September 5, 2013, at which several invited experts
gave presentations on emerging technologies. The team acknowledges and thanks these speakers, and the
many individuals who contributed their insights as participants at the event. Speakers included the
following:
Appendix E: Workshop Agenda

Larry Stowell, NewLogic Membrane Technology for Pre-Evaporation


Sankar Nair, Georgia Tech Robust Membranes for Concentrating Black Liquor
Vivek Mehrotra, Teledyne Sacrificial Coatings for Membranes
Brian Bischoff Membrane Capabilities at Oak Ridge National Laboratory

In addition to these presenters, participants at the 2013 workshop included pulp and equipment
manufacturers, academics, and other experts.

Black Liquor Concentration Workshop


September 5, 2013
Name Organization
Chris Verrill International Paper
Brian Bischoff Oak Ridge National Lab
Dan Bloom Lundberg
Marko Hakovirta Auburn
Sankar Nair Georgia Tech
Ron Rousseau Georgia Tech
Norman Marsolan Georgia Tech/IPST (now RBI)
Scott Sinquefield Georgia Tech/IPST (now RBI)
Cyrus Aidun Georgia Tech
James Cantrell Jacobs
Bob Kinstrey Jacobs
Larry Stowell New Logic Research
Alan Rudie USDA Forest Products Lab
Bhima Sastri US Dept of Energy AMO
Greg Burns KapStone Paper
Sergey Shevchenko Nalco
Jason Smith Andritz
Sean Ireland Verso Paper
Fritz Paulsen KapStone
Beth Cormier Sappi
Gopal Goyal International Paper
Mark Watkins MeadWestvaco
Kathleen Bennett Agenda 2020
Ron Brown Agenda 2020

48 Reuse of Process Effluents Research Roadmap


Literature Surveys insights underlying the development of this
roadmap and will continue to serve the industry
Two literature surveys were conducted as part of in evaluating scenarios as actual data are
the development of the roadmap: the first, by developed. Further information on model
Nikita Kevlich, a post-doctoral student working development and assumptions can be obtained
by contacting Agenda 2020.
with Sankar Nair of Georgia Tech on the Robust
Membranes project, is a study of literature
related to membrane technology. The second is a Membrane Workshop
survey of research related to non-membrane Participants (Phase II
technology approaches to the concentration of
black liquor; it was conducted by Scott Workshop)
Sinquefield of Georgia Tech. Dr. Sinquefield The team conducted a workshop in October
also contributed to the team’s consideration of 2015 to explore the membrane-based separation
freeze concentration technology. option in detail. The team appreciates the
considerable representation by membrane
manufacturers and experts, and their many
Model Development contributions to the endeavor. In particular, Dr.
Munir Cheryan provided a keynote address and
As discussed in Chapter 2, the team developed a educational presentation discussing the range of
model to predict the energy and economic membrane technologies, design considerations,
impacts of incorporation of membrane and critical success factors. Dr. Fareshteh
technology under various scenarios. The team is Rashidi of Georgia Tech gave a presentation on
grateful to Greg Burns of KapStone, who served the Robust Membranes Project on behalf of the
as the principal developer, and to Takis research team headed by Dr. Sankar Nair. Nikita
Taousakis, MWV, who provided guidance and Kevlich presented a literature survey of
membrane use in black liquor concentration.
assistance. The model provided significant

2015 Membrane Technology Workshop Participants


Name Organization
Wayne Bates Hydranautics
Wayne Bagley Veolia Water Technologies
Kathleen Bennett Agenda 2020
Brian Bischoff Oak Ridge National Laboratory

Appendix D: Contributors
Dan Bloom Lundberg
Jim Bradbury Verso Corporation
Jeffrey Brown Georgia Pacific
Gregory Burns KapStone Paper
Munir Cheryan Membrane Consultants LLC
Rahul Ganguli Teledyne Scientific Company
Gopal Goyal International Paper
Takashi Harada TJS Aqua Solution

Reuse of Process Effluents Research Roadmap 49


Brandon Hastings Sappi
Richard Higgins Veolia
Peter Malati Teledyne Scientific Company
Vivek Mehrotra Teledyne Scientific Company
Appendix D: Contributors

Leif Nilsson Membrane Specialists LLC


Lewis Pain Membrane Specialists LLC
Fritz Paulsen KapStone Paper & Packaging
David Pearson Membrane Specialists LLC
Fereshteh Rashidi Georgia Institute of Technology
Ricardo Santos WestRock
Sergey Shevchenko Nalco-Ecolab
Scott Sinquefield RBI at GA Tech
Jason Smith Kadant Black Clawson
Jean-Louis Staudenmann NIST
Arun Suresh Domtar
David Turpin Agenda 2020 Technology Alliance
Leland Vane U.S. EPA
Chris Verrill International Paper
Henia Yacubowicz Koch Membrane Systems
Scott Yaeger FAST Int’l Inc.

50 Reuse of Process Effluents Research Roadmap


Appendix E: Workshop Agenda

Day 1: Tuesday June 9, 2015 12:30pm–5:15pm


Time Activity
10:00– Opening
10:30am The purpose of the opening is to provide important background information on the AMTech award,
the purpose of the current workshop, and the progress of work to this point. The session will also
describe the R&D priorities that came out of the 2014 roadmap and that represent the starting
point for this workshop.

 Introductions & opening remarks Outcomes:


- Participants understand the big
 Background/Agenda 2020 and AMTech Project Overview picture

 2014 Roadmap - Participants understand what they


must do to conduct a successful
 Products of the Workshop workshop

10:30– Plenary Presentations


12:00pm A series of presentations will provide important background information for participants and
inform representatives of the membrane industry about the kraft recovery process, black liquor
concentration need, business case, etc.

 BLC Background (Chris Verrill) Outcomes:


- Membrane industry guests
understand the required
 Black Liquor Systems Today and Tomorrow (Jason Smith) performance, context, and
operational challenges

 Membrane Technology: Literature Review (Nikita Kevlich)


- Shared understa

12:00–
Lunch
12:45pm

12:45– Plenary Presentations — continued


1:50pm

Appendix D: Contributors
The plenary presentations continue after lunch.

 Current Black Liquor Membrane Research Outcomes:


- Everyone understands current
o RBI-GA Tech – Robust Membranes projects and status
o Teledyne – Sacrifical Coatings
- Membrane industry reps grasp
o Oak Ridge - HiPAS Membranes the business case and economic
requirements and the reasons for
them
 Mass Balance and Economic Drivers (Burns)

1:50– 2:00pm Break

Reuse of Process Effluents Research Roadmap 51


Time Activity
2:00– 3:45pm Overview of Membrane Technology
Highlight presentation by a leading membrane industry expert reviewing advantages and
limitations of membranes compared to conventional evaporation systems
Appendix E Workshop Agenda

 Munir Cheryan, PhD Outcomes:


o Founder & President, Membrane Consultants, LLC; Professor - P&P industry ga
Emeritus, University of Illinois-Champaign/Urbana

 Group Discussion – Q&A


 Technology Showcase
o Brief presentations by membrane manufacturers and
implementers and academics concerning their capabilities to
contribute knowledge and expertise.

 Overview of the breakout group process

3:45–
Break
4:00pm

4:00– 5:00pm Breakout Discussion 1: Challenges and Knowledge Gaps for Membrane-based
Concentration of Black Liquor
This will be an interactive breakout group discussion focused on problem definition. The purpose is
to arrive at a vetted list of challenges and knowledge gaps that define the technical “problems to be
solved.” The intent is to keep this generic, identifying additional potential barriers and novel
approaches, beyond the ones that the pulp and paper industry—non-experts in membrane
potential—developed in 2014.

 Problem Definition Brainstorming Outcomes:


- A vetted list of challenges and
 Identification of Themes knowledge gaps

5:00– 5:30pm Plenary Session: Review & Wrap-up


The wrap-up for Day 1 will include a brief review and summary of the key points of the
day and a preview of the activities for Day 2.

Outcomes:
 Breakout group reports
- Participants have a clear and
common understanding of
 Review and summary of Day 1; Instructions for Day 2 progress and plans for Day 2

6:00pm No-host Dinner & Networking Opportunity (optional)

52 Reuse of Process Effluents Research Roadmap


Day 2: Wednesday, June 10, 2015 8:00am–3:30pm
Time Activity
8:00– Day 2 Introduction
8:15am Participants will reconvene as a large group for a brief recap of the purpose and structure of the
workshop, including a review of Day 1 and a preview of Day 2.

 Introduction & opening remarks Outcomes:


- Participants have a renewed
clarity of purpose

8:15– 9:15am Breakout Discussion 2: Identify RD&D Projects


In this second breakout discussion, participants will move from problem definition to solution
specification. Participants will identify RD&D Projects that address the challenges and knowledge
gaps determined on Day 1. Participants will consider current and emerging approaches that could
address these challenges, and will be instructed to keep this pre-competitive! Participants will
prioritize the promising projects.

 Brainstorm RD&D Projects Outcomes:


- List of RD&D projects to explore
o Participants will consider the barriers identified in Day 1 along further
with current and emerging technology approaches and suggest
potential projects to overcoming the barriers.
 Consolidate and prioritize
o Suggestions from the group will be consolidated into a defined
set of promising projects, which will then be prioritized for
further action.

9:15–10:00am Plenary: Review & Integration


Participants will reconvene as a large group to review the R&D projects identified in their
respective groups and select those to develop in small groups. The full group will address any
overlap among the projects and identify a final list of projects for further exploration and
refinement during the next session.

 Breakout Group Reports Outcomes:


- List of RD&D projects to explore
 Consolidation further

 Selection of Projects for Development

Appendix E: Workshop Agenda


10:00–
Break
10:15am

Reuse of Process Effluents Research Roadmap 53


Time Activity
10:15– Small Group Work: Pushing the Boundaries
11:45am For this session, participants will divide into small groups of 3-5 people. Each small group will be
assigned a project and given the task of mapping out a plan for implementing the project using the
Appendix E Workshop Agenda

planning worksheet template.

 Small Group Work Outcomes:


- Research outlines for promising
o Participants in small groups will map out the knowledge gaps, projects; content needed in final
expertise needs, and key milestones needed to address the roadmap
barriers via the projects suggested using a template provided.
o The template when completed will begin to outline the key
next steps and ideas that need to be included in the final
roadmap

11:45am–
Lunch
12:15pm

12:15– Plenary Session: Review of Small Group Output


1:30pm For this session, the work product of the small groups will be reviewed by the entire group.
Participants will provide comments and feedback to enhance the content and fill in any gaps

Outcomes:
 Task Team Presentations
- Shared understanding; the
research for the final roadmap
 Comments and Feedback

1:30– 1:50pm Plenary Session: How Ideas Become Solutions (David Turpin)

 Review of next steps for creating the roadmap Outcomes:


- Enthusiasm for continuing the
work. Clarity of purpose and roles
 Presentation/discussion of next steps for moving toward
implementation
1:50– 2:00pm Close (Co-Leads)

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