Biomass Fractionation 2

Chemical engineering of biobased products
SCIENCE
PASSION
TECHNOLOGY
Chemical engineering of
biobased products
Biomass fractionation (2)

Marlene Kienberger
October 2023
2
Summary last week Hemicellulose
• Bioeconomy / Circular economy

• Biorefinery
• Biomass
• Fractionation technologies Cellulose Lignin
• Overview Extractives, ash
• Comminution
10/16/2023
3
Goals of biomass fractionation
deconstruct LCB create digestible solids
increase surface
modifying & high
area and
polymerization & sugar yields after
porosity
cellulose crystallinity hydrolysis
recovery of
avoid formation of low demand of post-
hemicellulose & lignin
fermantation inhibitors treatment
for co-products
minimal energy,
chemicals, water &
low-cost reactors
10/16/2023
Overview pre-treatment and fractionation processes

Physical Chemical Physico-chemical Biological
Milling Acid processes Autohydrolysis/ Brown-, white-

Liquid hot water and soft-rot
fungi
Grinding Alkaline Steam explosion
processes
Ultrasound Wet Oxidation Sub- and
supercritical fluids
Extrusion Organosolv
Irradiation Ozonolysis
(microwaves, ɣ-
irradiation)
Ionic liquids
Inorganic salts
Carvalheiro, F., Duarte, L.C., Bogel-Lukasik, R., Moniz, P. (2013) Boletim de Biotecnologia., Série 2 (3)
5
Comminution – Stress and Energy Demand
Design Principle – Reduction ratio nr
• Achieved grade in a comminution process
• Defined as the quotient of the characteristic grain size dF before and dPr after
comminution:
dF
𝑛𝑟 = −
dPr
• The finer the comminution, the larger the reduction ratio becomes
• Coarse grinding: nr between 2 and 10
• Fine grinding: nr up to 50
• All crushers have limited reduction ratio
• Number of stages is guided by the size of the feed and requested product
10/16/2023
Design principle – Energy

6
• Use of phenomenological correlations for prediction of comminution work E [kJ·kg-1]

𝑑(𝐸) 𝐾
• Application of simple power function: =−
𝑑(𝑑) 𝑑𝑛
Exponent n varied in 3 different, widely accepted models (integrated forms):
𝑑𝐹
Kick’s law, n=1 𝐸 = 𝐾𝐾 ∙ 𝑙𝑛 Rittinger
𝑑𝑃𝑟 Kick
E [kJ·kg]
Bond
1 1
Bond’s theory, n=1.5 𝐸 = 𝐾𝐵 ∙ 0.5 −
𝑑𝑃𝑟 𝑑𝐹 0.5
1 1
Rittinger’s theory, n=2 𝐸 = 𝐾𝑅 ∙ −
𝑑𝑃𝑟 𝑑𝐹 dPr [m]
General applicability mostly for milling/crushing of hard and brittle materials like minerals
and single-grain-stressing
10/16/2023
7
Example Comminution
Problem description
In lab scale experiments, the energy consumption of a discontinuous mixer grinder for wet soy bean grinding
should be evaluated.
During grinding, the following data on particle size, grinding duration and energy consumption were
generated (Wet grinding characteristics of soybean for soymilk extraction. Vishwanathan, K.H., Singh, V. and
Subramanian, R., Journal of Food Engineering 106 (2011) 28-34). The initial mean particle size of soaked
soy beans was 5345 µm.
Determine which of the three mathematical laws gives the best description of the documented grinding
process
1 1 Grinding Particle Specific energy
 Rittinger’s theory, n=2 𝐸 = 𝐾𝑅 ∙ − time size consumption
𝑑𝑃𝑟 𝑑𝐹
𝑑𝐹 [min] [µm] [kJ·kg-1]
 Kick’s law, n=1 𝐸 = 𝐾𝐾 ∙ 𝑙𝑛 1 364 51.4
𝑑𝑃𝑟
1 1 3 232 180
 Bond’s theory, n=1.5 𝐸 = 𝐾𝐵 ∙ 0.5 −
𝑑𝑃𝑟 𝑑𝐹 0.5 5 182 231.4
8 167 300
10/16/2023
Comminution – equipment summary

8
Jaw crusher Roller mill Edge runner Ball mill Cutting mill Toothed disk
(Kollergang) mill
Material http://www.hoeflinger.de/
properties uploads/pics/003_55.jpg
Prior to friction
Brittle
Tough
Elastic
Coarse
After friction
Medium
Fine
10/16/2023
Comminution – equipment summary

9
Hammer mill Impeller Pin mill Jet mill TASK: What type of mill would
breaker
you use for
Minerals, where the final particle
size is to be coarse
Material
properties soaked soy beans, where the final
Brittle particle size is to be medium-
small
Prior to
friction
Tough
yeast cells
Elastic Sugar crystals
Coarse
Wood trunks for papermaking to
chips
After friction
Medium Wood chips to fibers, e.g. for

pellet production
Fine Deaglomeration of fine ceramic
Video pin mill: Video jet mill: pigments to even finer powder
https://www.youtube.com/watch?v=m3W8gYB0UUE https://www.youtube.com/watch?v=qlLwDw4mk1o
10/16/2023
10
Some equipment in operation
Top: Impact crusher

Bottom: Hammer mill
Jaw crusher
https://www.kleemann.info/en/technologies/crushing-technology/
Ball mill
10/16/2023
11
Free impact vs constraint impact
Free impact Constrained impact
Ensure grinding Carry out chemical transformations
Destruction of the cell
Destruction of the supramolecular structure
Increase the reactivity
Increase the solubility of some compounds
New direction
Preparation of intermediate products of mechanical treatment => mechanocomposites
• high area of contact between the particles of component phases
• high reactivity
Destruction of plant raw material with separation:
into wood and nonwood regions
10/16/2023
12
Grinding and energy
• One of the most widespread and energy-consuming processes
• It is among the top five processes consuming the largest amount of energy
• Up to 2% of energy generated in the world is consumed in grinding processes
• For plant raw material processing, the equipment for mechanical preparation can
account for up to 15% of the capital costs and consume ~10% of the energy necessary
for the biotechnological industry in general
• Energy consumed differ by a factor of several units depending on
• the choice of equipment and
• the parameters of operation
• Most used equipment for plant material: knife mills and hammer mills
10/16/2023
13
Grinding in comparison
Plant material Inorganic material
Heterogeneous Comparably homogeneous
Structured ad cell wall Not structured
Presence of unstable organic compounds Consists no unstable compounds
10/16/2023
Equipment – Ball Mill Design – as an example

Design option for ball mill with separate chambers
Biotechnological Products
• Also cell cultures consist of particles
• Microbial cells produce proteins, enzymes and a variety of metabolites
• Bacteria or yeasts are common production organisms
• Cells are about 1-10 µm in diameter
• Extracellular versus intracellular products
A comparison of size
https://microbiologyinfo.com/different-size-shape-and-arrangement-of-bacterial-cells/
Cell Disruption
Most valuable products naturally occur intracellular,
recovery by
 Genetic engineering for transport across cell wall
or
 Disruption of cells
Knowledge of cell wall necessary Structures of bacterial cell walls
http://simbac.gatech.edu/wordpress/wp-
Difference between bacteria and yeasts content/uploads/2013/04/cellwall-1.png
Structure of yeast cell wall

https://www.researchgate.net/figure/Structure-of-yeast-cell-
wall_fig1_318196547
Criteria for Cell Disruption

Product Quality
No degradation of (complex) products
High degree of product access
Sterile apparatus
No product contamination
Productivity
Easy separation of desired product and cell debris
Low energy demand
Low time demand
Low cost
Cell sediment after centrifugation of cell culture.
https://imgbin.com/png/7PRkQZUx/pichia-pastoris-
centrifugation-cell-milk-bioreactor-png
Cell disruption
alternatives
• Detergents
Mechanical Non-mechanical
• Ultrasonication
• Decompression
• Hughes press
• Lytic enzymes Solid shear Physical Chemical
• Chelating agents
• X-press
• High-pressure homogenizer
• Antibiotics
• French press
• Thermolysis
• Chaotropes
• Microfluidizer
Liquid shear
Osmotic shock
• Ball mill
• Autolysis Enzymatic
• Solvents
Cell disruption
alternatives
Mechanical Non-mechanical
Solid shear Physical Chemical
Ball mill,
Thermolysis, Antibiotics,
Hughes press,
Decompression, Chelating agents,
X-press
Osmotic shock Solvents, Chaotropes,
Detergents
Liquid shear
Enzymatic
Ultrasonication,
High-pressure
homogenizer, Lytic enzymes
Microfluidizer Autolysis
French press
Cell Disruption with Bead Mills

Bead loading and bead diameter influence heating and power consumption
Optimal bead loading = 80 - 85%
0.1 – 0.15 mm  disruption of bacteria In which diameter do you expect the
0.25 – 0.27  disruption of yeasts grinding balls to be?
Industrial machines
0.4 – 0.6 mm  easier separation of the beads
Why do we need a cooling jacket?

Cell Disruption - High-Pressure Homogenizer

Liquid shear applied
Efficiency mainly determined by
• Operating pressure
• Number of passes
• Suspension temperature
• Homogenizer valve design Acceleration from
Important machine for dairy production 3 m/s to 300 m/s
• Milk fat globule disruption

• Size control
First valve is operated at 15 MPa  splitting of large fat globules
Second stage splits small fat globules  pressure: 55 – 200 MPa
 Similar pressures for disruption of microbial cells
Bacterial cell culture before (a) and after one (b), two (c) or three (d) passes through a high pressure homogenizer at 135 Mpa.
Dean Bury, (2000) Growth and disruption of Lactobacillus delbrueckii ssp. biilgaricuî for lactose hydrolysis applications.
Non-Mechanical Treatment
Physical disruption
Decompression using sub or supercritical gas in the cells
Osmotic shock
Chemical permeabilization
Can be accomplished e.g. by antibiotics, chelating agents, detergents, solvents,…
Enzymatic disruption
Lysis: Enzymatic, specific and gentle, but expensive
Combination of lysozyme and EDTA  disruption of lipopolysaccharide layer (gram neg.
bacteria)  attack the peptidoglycan structure
Sieving and Sieving Analysis

Most common and easiest method for particle size analysis or separation of particles
based on their size and shape
Sieving area
Other techniques for particle
size analysis
 Ultrasonic extinction
 Optical techniques like image analysis,
light scattering
Measurement range: 20 μm to 125 mm
Sieve tray: http://www.aimsizer.com/index.html
Sieve area: e.g. wire mesh,
perforated metal plate Mesh size
Undersized fraction: “fines” Coarse
material
Feed
residue on sieve: “coarse” fraction
Fine material
Sieving Analysis
Difference between two consecutive sieve mesh widths = grain class or grain class width Δd
Associated load = fraction
Analysis can be performed with a single sieve or a set of sieves
 By hand or sieving machine
 Dry or wet
 With or without sieve motion
=> Compute a particle size distribution
Sieving Analysis – Particle Size Distribution

1. Define particle size classes
2. Determine amount of particles within each class experimentally
3. Calculate particle size distribution:
 Frequency distribution q3 (density diagram)
 Cumulative particle size distribution Q3 (cumulative density diagram)
𝑑𝑛
𝑄3 𝑑 = න 𝑞3 𝑑 𝑑(𝑑) 𝑞3 𝑑𝑚𝑖 = 𝑑𝑄3 𝑑𝑚𝑖 /𝑑(𝑑)
0
∆𝑚𝑖 ∆𝑄3,𝑖
For discrete data: ∆𝑄3,𝑖 = 𝑄3 (𝑑) = ෍ ∆𝑄3 𝑖 𝑞3,𝑖 =
𝑚𝑡𝑜𝑡𝑎𝑙 ∆𝑑𝑖
Sieving Analysis – Example 1

A size distribution analysis is performed using a screener with a total feed of 12.00 g of
polydisperse silica sand. The largest particle has a diameter of
mesh size
1.25 mm. The mass of the residue on each mesh size is shown below: [mm]
coarse fraction [g]
0.250 2.3933
0.400 1.7019
The sieving tower has six screens 0.500 2.0077
with the following mesh widths: du [mm] do [mm] 0.630 1.9563
0 0.250 0.800 1.2820
0.250 0.4 1.000 0.5897
0.4 0.5
0.5 0.63 Total Feed /g 12.0000
0.63 0.8
0.8 1
1 1.25
Determine the size distribution (Q3 and q3) and draw the density diagram and the cumulative
distribution diagram
∆𝑚𝑖 ∆𝑄3,𝑖
∆𝑄3,𝑖 = 𝑄3 (𝑑) = ෍ ∆𝑄3 𝑖 𝑞3,𝑖 =
𝑚𝑡𝑜𝑡𝑎𝑙 ∆𝑑𝑖
Sieving Analysis – Example 1 q3 (dm) density diagramm

1,6
i du do dm Δd Δm ΔQ3 Q3 q3 1,4
1,2
1 0 0.250
1
q3 [m-1]
0,8
2 0.250 0.4 0,6
0,4
3 0.4 0.5 0,2
0
4 0.5 0.63 0 0,2 0,4 0,6 0,8 1 1,2
dm (mm)
5 0.63 0.8
6 0.8 1
i du do dm Δd Δm ΔQ3 Q3 q3 Q3 (do)
1 7 0 1 1.25
0.250 0.125 0.250 2.069 0.172 0.172 0.689 1
0,9
0,8
2 0.250 0.4 0.325 0.150 2.393 0.199 0.372 1.330 0,7
0,6
Q3 []
3 0.4 0.5 0.45 0.100 1.702 0.142 0.514 1.418 0,5
cummulative
0,4
4 0.5 0.63 0.565 0.130 2.008 0.167 0.681 1.287 0,3
0,2
distribution diagramm
0,1
5 0.63 0.8 0.715 0.170 1.956 0.163 0.844 0.959 0
0,0 0,2 0,4 0,6 0,8 1,0 1,2 1,4
6 0.8 1 0.9 0.200 1.282 0.107 0.951 0.534 do (mm)
7 1 1.25 1.125 0.250 0.590 0.049 1.000 0.197

Sieve Types Characterization of amplitude and frequency in

an oscillatory sieving machine
fixed grates • High amplitude  particles are thrown higher
and further
• Particles large  high amplitude
β • Particles small  small amplitudes and high
wet sieving
frequency
oscillatory sieve
roller screen β
Videolink: https://www.youtube.com/watch?v=LydDIcKusr0 Spiral sieve: https://www.youtube.com/watch?v=rWls8Kpz5bU Classifying sieve: https://www.youtube.com/watch?v=gRn30EzUsB8

Design Principles for Vibrating Sieves

Minimum length Lmin of a continuous sieving machine
𝑁𝑝 = 𝑛 ∗ 𝑡𝑟𝑒𝑠 Np… number of collision events between particle and sieve
n… frequency of screen motion [s-1]
𝐿
𝑡𝑟𝑒𝑠 = tres… mean residence time [s]
𝑣𝑝
L… length of screen [m]
vp… mean particle velocity along screen [m·s-1]
𝑣𝑝 ∗𝑁𝑝
𝐿𝑚𝑖𝑛 = Lmin… minimum length of continuous sieving apparatus [m]
𝑛
Screen number
𝑎 𝑟 ∗ ω2 𝑎
𝐾= 𝑔
= 𝑔
→ K𝑣 = 𝑔𝑣 r… amplitude of oscillator [m]
𝑣
ω… angular velocity of oscillator [rad·s-1]
a… centrifugal (centripetal) acceleration [m·s-2]
g… gravitational constant [m·s-2]
Kv… screen number, ratio of centrifugal- and gravitational acceleration perpendicular to the screen
Design Principles for Vibrating Sieves – Screen Number
av
α+β
α
a
β
gv
g
Screen number Kv for a linear oscillator

𝑎 ∗ sin(𝛼 + 𝛽)
𝐾𝑣 =
𝑔 ∗ cos 𝛽
Screen number Kv for a circular oscillator
𝑎
𝐾𝑣 =
𝑔 ∗ cos 𝛽
Design Principles for Vibrating Sieves – Screen Number
Kv Motion Sieving effect
<1 no transport (slipping) small sieving effect, plugging
1 … 1.5 little motion of particles slow, sub-optimal sieving
gentle sieving, for easy to sieve

1.6 … 1.8 flat trajectory
materials
moderately steep gentle sieving, hard to sieve
2.1 … 2.3
trajectory materials
hard to sieve materials, high
3.0 … 3.5 steep trajectory
amount of fine fraction
very sharp sieving, loosening of
3.3-4.0 (up to 8.0) very steep trajectory
the particle bed
Design Principles for Vibrating Sieves – Throughput

• Numerous factors influencing throughput
• Based on lab- or small-scale experiments
• Based on tabulated or plotted empirical factors/correlations
gives rough estimate of total or undersized (fines) throughput
• No generally accepted values, examples can be found in “Handbuch der mechanischen
Verfahrenstechnik” (puplished by Heinrich Schubert)
The equation for volume throughput 𝑉ሶ [m3·h-1] reads
𝑉ሶ = 𝑉𝐴ሶ ∙ 𝐴 ∙ ෑ 𝑘𝑖
• theoretical area specific throughput 𝑉𝐴ሶ [m3·m-2·h-1]

• sieving area A [m2]
• correction factors 𝑘𝑖 []
Design Principles for Vibrating Sieves – Limitations

Plugging of the sieves:
Vibration of the sieve (movement, frequency)
Screen characteristics (mesh size, geometry, material)
Use of sieving supports (e.g. rubber balls)
Condition of the feed material (sticky or wet particles)
Pro´s and Con´s vibrating sieve

+ Standard equipment (maintenance)
https://www.allgaier-
+ Simple construction group.com/sites/default/files/downloads/en/allgaier_apt

_sat_trumblerscreeningmachines_en.pdf
- Higher safety standards (high forces due to motion)

- Plugging of mesh


fungi
processes
(microwaves, ɣ-
irradiation)
Ionic liquids
Inorganic salts
35
Extrusion
Developed for mixing of plastics
Today actively used for processing of plant material
• Mechanical treatment not accompanied with grinding
• Main working part = archimedes screw(s)
• Material strongly interacts with the walls => friction
• Plastic deformation
• Hole at the end – sharp pressure drop
• Equipment heated to several hundreds degrees
• Humidity of plant material plays a major role
• Boiling of water – condition sclose to autoclave => vapor explosion
What is in summary the principle of biomass

pretreatment using extrusion? 10/16/2023
36
Extrusion
is a combination of
Pros
• Heating, mixing and shearing
No chemicals
• strong plastic deformation
Treatment of particels of several 10 mm
• short-time autoclave treatment
High water content
• vapor explosion treatment
 formation of mechanocomposites, mass
transfer inside solid particles, and
Cons
chemical reactions
High mechanical load
leads to High energy demand
• disruption of lignocellulose structure,

defibrillation and shortening of fibres
10/16/2023
37
Extrusion - examples
Feedstocks Extrusion Sugar yield
conditions
Physical Corn stover, corn cobs, 40-180ºC Glucose: 41%-95% Xylose:
swichgrass, Douglas-fir 25%-79%
Acid Rice straw, pine sawdust, MSW 60-230ºC Glucose: 41%-60% Xylose: 84%
Alkali Wheat straw, corn stover, 55-180ºC Glucose: 87%-92% Xylose:

swichgrass 36-82%
Alkali combined Wheat straw, corn stover, Room-140ºC Glucose: 88%-92% Xylan removal: 95%
treatment* swichgrass, bagasse, prairie Lignin removal: 87%
cordgrass
*Alkali+Ionic liquids; Alkali+organic solvent; Alkali+steam explosion; Alkali+LHW
 Can be operated at mild temperatures

 Can produce appreciable sugar yields
Adpt. Zheng, J & Rehmann, L. (2014) Int. J. Mol. Sci. 2014, 15, 18967-1898
10/16/2023
38
Energy irradiation methods
novel form of biomass pretreatment using
• electron beam
• gamma ray
• pulsed electrical field
• microwave and ultrasound
Pretreatment mechanisms differ with applied process
Technologies are often often combined with chemical and/or biological pretreatment
In which region are the wave

lengths for the radiation
mechnism named?
http://son.nasa.gov/tass/content/electrospectrum.htm
10/16/2023
39
Gamma ray irradiation
• high-energy ionizing radiation, electromagnetic spectrum that penetrates most materials
• commonly applied in radiotherapy or in medical apparatus sterilization
• decrease intra and intermolecular order of cellulose - breakdown of hydrogen bonds
• energy transferred by collision of radiation - ionization
• biomass component undergo scission – formation of various short and long-lived
radicals
• fragments with low degree polymerization generated from the process increases
• alteration of biomass structure - providing access for subsequent process
10/16/2023
40
Take home messages
• Physical biomass fractionation – a need
• Subdevision in physical, chemical, physical-chemical and biological pretreatment
• physical partial covered by mechanical unit operations already - recap
• Example cell discruption – an overview
• Example diary industry – high pressure homogenizer
• Caluclation example
• Comminution – soy beans
• Particel sieze distribution – silica sand
• You may practice at home vibration sieves – example provided
10/16/2023
SCIENCE
PASSION
TECHNOLOGY
biobased products
Biomass fractionation (2)

Marlene Kienberger
October 2023
42
Summary last week
• Physical biomass fractionation – a need
• Subdevision in physical, chemical, physical-chemical and biological pretreatment
• physical partial covered by mechanical unit operations already - recap
• Example cell discruption – an overview
• Example diary industry – high pressure homogenizer
• Caluclation example
• Comminution – soy beans
• Particel sieze distribution – silica sand
• First insight into irradiation
10/16/2023


fungi
processes
(microwaves, ɣ-
irradiation) Today
Ionic liquids
Inorganic salts
44
Electron beam irradiation
• widely used for changing the properties of polymers
• the most important characteristics: electron energy and
average beam power
• industrially classified according to their energy ranges
• biomass is exposed to a highly charged stream electron Source: https://www.nhv.jp/en/eb/
• electron is emitted by electron beam gun and accelerated by accelerator

• electron energy can be controlled and modulated by varying the irradiation dose
• Induces a chain–cleavage mechanism by depolymerizing the polymeric material
• high energy electrons emitted travel into
biomass – energy transfer into the material
• heating process initiates chemical and
thermal reactions Experimental set-up for electron beam
irradiation
10/16/2023
45
Microwave treatment
Function principle
• electromagnetic waves - frequency range 0.3-300 GHz
• affect the material thermally and non-thermally
• heating of material by interaction of molecules with electromagnetic field
• non-thermally – microwaves lead to physical, chemical and biological reactions
• microwaves are generally used in association with chemicals
• alkali reagents are highly effective
• combination of microwaves with mechanical processes
Effects of microwave treatment
• increased lignin removal
• increased efficiency to remove hemicellulose
• reduction of cellulose cristallinity
10/16/2023
46
Microwave treatment - examples
Feedstock Assisted Aim Reference

treatments
Maize bran No, water only Production of Rose and Inglett
arabinoxylooligosaccharides (2009)
Sugarcane Yes, acid Enzymatic hydrolysis Moretii et al.

bagasse (2014)
Sugarcane Yes, acid Hemicellulose hydrolysis to Bian et al.
bagasse produce xylooligosaccharides (2014)
Swichgrass Yes, Alkali Enzymatic hydrolysis Hu and Wen

Li et al (2016) Biores. Technol. 199, 34–41
(2008)
Tea residues No, water only Phenolic compounds Tsubaki et al.
(2010)
10/16/2023
47
Ultrasound treatment or Ultrasonication
Equipment: probe-type ultrasonication or ultrasonic bath
Function principle
• pressure waves travel through the liquid
• rarefaction create cavities (bubbles)
• bubbles expand and contract with rarefaction and contraction
• large bubbles than float to the surface are subjected to coalescence or collapse
Status quo
Ultrasonication pretreatment of biomass and
• It has been performed on a great variety of lignocellulosic biomass biofibre mechanisms
• generally used in combination with chemicals

• temperature ~50ºC
• employed for extracting hemis, cellulose and lignin
• Enhancement of cellulose saccharification
10/16/2023
48
Ultrasonication - Examples
Feed stream Ultrasonic configuration Chemical Benefit
Sugar cane bagasse 20 kHz Sulfuric acid 26 g/L sugar
50-200 W Corresponds to 94.9% theoretical
xield
Corncob for xylan 20 kHz Sulfuric acid Increase of xylan yield by 14.7%, time
extraction 1000 W reduction from 24 h to 45 min
Delignification of 20 kHz Ethanol, methanol 96%delignification, >75%
poplar wood 1000 W dioxane hemicellulose removal
25°C, 30 min
Sugar cane bagasse 24 kHz NaOH Increase of hemicellulose yield by a
400 W factor of 1.5
30-50°C, 5-50 min
Deligification of waste 20 kHz NaOH Increased delignification by a factor of
newspaper 100 W 2, significantly reduced treatment time,
70 min from 7h to 70 min
Rice straw 28 kHz Ionic liquids 19.5% increased sugar yield
300 W Cholin hydroxyde
10/16/2023
49
Reactor configuration and operation
Reactor configuration
• Ultrasonic horn
• Ultrasonic bath
• Flow reactors
Operation parameter https://en.wikipedia.org/wiki/Ultras
onic_horn#/media/File:Full-
wave_Barbell_Horn.jpg
• ultrasonic frequency
typically 10-100 kHz
• intensity of ultrasonic irradiation
• temperature
• ultrasound treatment time
Ultrasonic flow reactor

DOI: 10.1080/19443994.2015.1051128
10/16/2023
50
Comparison conventionell vs. Ultrasound assistat treatment
Enzymatic hydrolysis of delignified newspaper
Typically combined with solvents or acids => higher yield among others with respect to
fermentable sugars.
10/16/2023
51
Comparison
Pros and Gamma ray Electron beam Ultrasound Microwave
cons
 Significant No temperature control Mild temperatures Increased yield
improvement in needed Enhancement of Reduced
terms of possible No neutralization step cellulose hemicellulose
cost reduction needed saccharification cristallinity
opportunities and
absence of any
reduced toxicity
byproducts
More research Exclusively used to Apparatus design Apparatus –
needed enhance the enzymatic Energy input scale up
hydrolysis of
lignocellulose
not been commercially
successful yet
10/16/2023


fungi
processes
(microwaves, ɣ-
irradiation)
Ionic liquids
Inorganic salts
53
Guest talk
Adrian Drescher
10/16/2023
54
Pulsed electric energy on biomaterials
Pulsed electric fields:
• Between plate elcttodes, relatively homogeneous electrical field
• Effect primarily related to loss of membrane barrier
High-voltage electrical discharge
Impacts on
• Damage of cells
• Mechanical fragmentation
• Elevation of temperature
10/16/2023
55
Pulsed electric energy on biomaterials
Impact is primarily related to loss of membrane barrier => electroporation
Degree of electroporation depends on
• the electrical potential (0.5-1.5V) => electrical potential is proportional to cell radius
• larger cells are damaged before smaller ones
• material properties such as size of the cells, electrical conductivity
• amplitude of pulse or electircal field strength and shape
• duration Plant damage Microbial
• number of repeats inactivation
• interval between pulses Electrical 500-1000 V/cm 20-50 kV/cm
field strength
Typically applied under non-thermal conditions
duration 10-4-10-1 sec 10-5-10-4 sec
Pulsed electrical field treatment may display
synergistiv effects
10/16/2023
56
High voltage electrical discharge
Mechanism: electroporation thermal and mechanical stress
Pulse shape represents dumping oscillations
High voltage electrical discharge can accompany
• electrical breakdown
• propagation of streamer
• bubble formation
• cavitations
• light emission
• localized regions with high pressure
• formation of shockwaves and acoustic waves
Large quantity of radical species and oszone can be formed => provoke fragmentation of
suspended soldi particles
10/16/2023
57
Examples
Raw materials examples:
Fruits, vegetables, eggs, tea, mushrooms, yeast, microalgae, pomace, seeds, peels,
kernels, husks of grapes, marcs, oil-cakes, stems, sawdust, leaves, and wood bark energy
crops, and municipal wastes, vine shoots, leaves, debris,
Pulsed electric energy assisted applications
…..are used for
drying, diffusion, pressing, osmotic treatment, freezing, lyophilization
Giancarlo Dessì
…..they allow for

enhanced pressing yield of juices, extraction yield of sucrose, inulin, proteins,
phenolics, and many other high-added substance
© http://lifesarmiento.eu/ 10/16/2023
58
Questions and comments?
10/16/2023
59
Additional tasks
Task slide 6
Integrate the power funktion for the three different exponents. Integrate from dF to dPr
Vibrating sieves
Vibration sieves (see next two slides)
10/16/2023
Example Sieving
For classification of dried soy beans, a circular motion vibratory machine should be used. The
following specifications are valid for the considered batch of soy beans:
Density ρp = 0.753 g·cm-3
Size distribution:
d0 /mm 7.5 6.35 4.75 3.0
Required throughput: m= 2.5 t/h
∆Q3 0.6736 0.2981 0.0217 0.0066
Screen plate specifications
Sieve hole sizing w x w’: 4.75 x 20 mm (slotted sieve)
Number of openings in the screen plate N = 3·103 holes/m2
Percentage of total lower grains (undersize content) in
the screen overflow: 3 %
Sieve area: A = 2 m2
Determine if the required throughput can be achieved with the specified sieve.
Chemical engineering
Mesh width or holeof biobased
diameter products
[mm] 3 6 – 14 > 40
61 𝒎𝟑 𝑤 𝑤 𝑤
𝑽ሶ 𝑨 4 ∙ log 24 ∙ log 51 ∙ log
𝒎𝟐 ∙ 𝒉 0.08 1.74 9.15
Correction factor k1: influence of the fraction d < w/2 in the feed
Particle fraction < w/2 [w-%] 0 10 20 30 40 50 60 70 80 90
k1 0.44 0.55 0.70 0.80 1.0 1.2 1.4 1.8 2.2 3.0
Correction factor k2: influence of the fraction of undersized grains from the feed in the sieve underflow
Fraction of undersized grains in sieve 70 80 85 90 95

underflow [w-%]
k2 2.25 1.75 1.5 1.25 1.0
Correction factor k3: influence of the sieve hole dimensions
Dimensions w' < 2w 2w<w’<4w 4w<w’<25w w’>25w
k3 1.15 1.75 1.5 1.25
Multi-deck sieves First (highest) deck 2nd deck 3rd deck
k4 1 0.9 0.8
Influence of open sieve area 𝐴𝑜𝑝𝑒𝑛
k5 𝑘5 =
𝐴𝑡𝑜𝑡𝑎𝑙
Wet sieving with spray water
Mesh width w ≤0.8 1.6 3.2 5 8 9.5 13 20 25 50
[mm]
k6 1.25 3.0 3.5 3.5 3.0 2.5 1.75 1.35 1.25 1.0
SCIENCE
PASSION
TECHNOLOGY
biobased products
Biomass Fractionation Technologies (2)

Marlene Kienberger
October 2023

Biomass Fractionation 2

Uploaded by

Document Information

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Biomass Fractionation 2

Uploaded by

Copyright:

Available Formats

Chemical engineering of biobased products

Biomass fractionation (2)

• Bioeconomy / Circular economy

• Overview Extractives, ash

Overview pre-treatment and fractionation processes

Milling Acid processes Autohydrolysis/ Brown-, white-

Design principle – Energy

• Use of phenomenological correlations for prediction of comminution work E [kJ·kg-1]

Comminution – equipment summary

Comminution – equipment summary

Medium Wood chips to fibers, e.g. for

Top: Impact crusher

Structured ad cell wall Not structured

Presence of unstable organic compounds Consists no unstable compounds

Equipment – Ball Mill Design – as an example

Difference between bacteria and yeasts content/uploads/2013/04/cellwall-1.png

Structure of yeast cell wall

Criteria for Cell Disruption

Solid shear Physical Chemical

Cell Disruption with Bead Mills

Why do we need a cooling jacket?

Cell Disruption - High-Pressure Homogenizer

• Milk fat globule disruption

Sieving and Sieving Analysis

Sieving Analysis – Particle Size Distribution

Sieving Analysis – Example 1

Sieving Analysis – Example 1 q3 (dm) density diagramm

7 1 1.25 1.125 0.250 0.590 0.049 1.000 0.197

Sieve Types Characterization of amplitude and frequency in

Videolink: https://www.youtube.com/watch?v=LydDIcKusr0 Spiral sieve: https://www.youtube.com/watch?v=rWls8Kpz5bU Classifying sieve: https://www.youtube.com/watch?v=gRn30EzUsB8

Design Principles for Vibrating Sieves

Design Principles for Vibrating Sieves – Screen Number

Screen number Kv for a linear oscillator

Design Principles for Vibrating Sieves – Screen Number

Kv Motion Sieving effect

<1 no transport (slipping) small sieving effect, plugging

1 … 1.5 little motion of particles slow, sub-optimal sieving

gentle sieving, for easy to sieve

Design Principles for Vibrating Sieves – Throughput

The equation for volume throughput 𝑉ሶ [m3·h-1] reads

• theoretical area specific throughput 𝑉𝐴ሶ [m3·m-2·h-1]

Design Principles for Vibrating Sieves – Limitations

Pro´s and Con´s vibrating sieve

+ Simple construction group.com/sites/default/files/downloads/en/allgaier_apt

- Higher safety standards (high forces due to motion)

Overview pre-treatment and fractionation processes

Milling Acid processes Autohydrolysis/ Brown-, white-

What is in summary the principle of biomass

leads to High energy demand

• disruption of lignocellulose structure,

Alkali Wheat straw, corn stover, 55-180ºC Glucose: 87%-92% Xylose:

*Alkali+Ionic liquids; Alkali+organic solvent; Alkali+steam explosion; Alkali+LHW

 Can be operated at mild temperatures

In which region are the wave

Biomass fractionation (2)

Overview pre-treatment and fractionation processes

Milling Acid processes Autohydrolysis/ Brown-, white-

• electron is emitted by electron beam gun and accelerated by accelerator

Feedstock Assisted Aim Reference

Sugarcane Yes, acid Enzymatic hydrolysis Moretii et al.

Swichgrass Yes, Alkali Enzymatic hydrolysis Hu and Wen

• generally used in combination with chemicals

Ultrasonic flow reactor

Overview pre-treatment and fractionation processes