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Caustic Recovery Test Report
Caustic Recovery Test Report
Preliminary tests for design of a Caustic Recovery Pilot Plant for Kamal
Ltd.
Pakistan
Test Report
SCI-Pak
Contents
Introduction ............................................................................... 3
Process Description.................................................................................... 3
Target ......................................................................................................... 3
Problem Statement .................................................................................... 3
Tests ........................................................................................... 5
Colours present in washing effluent .......................................................... 5
Indigo (Vat Blue CI Reduced Vat Blue1).................................................................... 5
Properties ......................................................................................................................... 6
Challenge.................................................................................... 7
Procedure ................................................................................................... 8
Filtration ................................................................................................................ 8
Outlook ..................................................................................... 14
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Introduction
In textile processing plants, Denim fabric is treated with caustic soda in a
mercerization process and then washed to remove un-treated caustic soda.
Process Description
The industrial client is a denim manufacturing unit in Karachi, Pakistan. The client
process description is that fresh caustic soda, used in the mercerization process, is in
the concentration of 25-30 B. After the mercerization, the fabric is washed to
remove the residual caustic at a flow of 120 litre/min and a temperature of 65C.
The washing effluent contains 4-5 B caustic soda with contamination of:
1. Indigo colour,
2. Sulphur colours (Black, Yellow Brown) and
3. Sizing material (Maize starch, PVA, Acrylic and wax).
Target
The target is to recover & reuse Caustic Soda from the spent washes. Normally, no
denim manufacturer in Pakistan recovers caustic soda due to the contaminations
mentioned in the section above. However there is great saving potential that exists in
this option. The industrial company is interested to get a solution for this problem,
and wants to become Pilot Project under SCI-PAK.
The target is to recover caustic from 7200 litre per hour 4-5 B effluent. The quality
requirement for process is that the recovered caustic solution must be colourless,
as the fresh solution of caustic used for mercerization must always be colourless.
Problem Statement
To recover Caustic Soda from denim fabric mercerization waste liquor. The spent
liquor contains 4-5 B (see Figure 1) caustic soda at a flow rate of 7,200 liters per
hour.
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In the above context, the sample was collected from the client. The sample was
bluish-dark in colour (see Figure 2). The sample was filtered and the resultant colour
is yellowish (Figure 3), which makes it unusable.
No chemical analysis had been performed on the solution yet.
In this aspect, technical assistance was required for modifications in the design of
the Caustic Recovery process, for further purification of the liquor, in order to get a
colourless solution.
PH-value of the washing effluent
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Figure 4: Washing effluent (left) and filtered effluent (right) as obtained from Kamal
Tests
In order to determine the right membrane for separating the colors present in the
washing effluent, first the chemical build-up of these colors had to be known.
Colours present in washing effluent
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Properties
Indigo is a dark blue crystalline powder that sublimes at 390392 C. It is insoluble
in water, alcohol, or ether but soluble in DMSO, chloroform, nitrobenzene, and
concentrated sulfuric acid.
Chemical Build-up
Chemical Formula:
C16H10N2O2
Molar Mass:
262.27 g/mol
Appearance:
Density:
1.199 g/cm3
Melting point:
390392 C
Solubility in water:
insoluble at 20 C
CI Sulphur Black 1
Properties
Sulphur black is an important class of dye for the coloration of cellulosic, being in
existence for nearly a hundred years.
The good fastness properties, cost effectiveness & ease of applicability under
different processing conditions (semi-continuous and continuous) make it one of the
most popular dyestuffs.
Chemical Build-up
Chemical Formula:
C6H4N2O5
Molar Mass:
184.11 g/mol
Density:
1.87 g/cm3
Boiling point:
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Chemical analysis
The samples, collected from Kamal were first subjected to a number of tests:
pH-value
Redox potential
electrical conductivity
The results can be found in the following table:
Parameter
Unit
Raw
Caustic
pH
12.88
Temperature C
23
Redox
mV
-338
Electrical
mS/cm 360
Conductivity
Filtered
Caustic
12.68
23.1
-333
327
400 500
Da Filtrate
13.08
21.2
-357
407
200
Da
Filtrate
13.14
21.22
-357
339
Table 4: results from chemical analysis of the samples collected from Kamal
Challenge
The idea was to use a two step membrane process to remove the colors from the
washing effluent. For this purpose, membranes had to be found, which are resistant
to high pH-values, since the pH of the washing effluent is between 13.2 and 13.5.
Two membranes where finally identified as pH-resistant:
Membrane
pH-range
molecular weight cut-off (MWCO)
[Dalton]
Maximum operating pressure [bar]
Processing Temperature [C]
Producer
1
1-14
400-500
2
0-14
200
40
5-95
Microdyn
Nadir
35
0-70
Koch
Membranes
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Procedure
The samples collected from Kamal were filtered, using membranes obtained from the
producers mentioned in Table 5. The apparatus used was a small-scale test
membrane system.
Filtration
400-500 Dalton cut-off size Membrane (Microdyn Nadir)
Testing Conditions:
Operating pressure
Membrane dfferential pressure
U
Volume flow of caustic soda over membrane
Membran Area
Test Temperatur
Flow velocity over Membrane
Kinematic viscosity of water (22C)
hydraulic Pipe diameter
Reynolds Number
35
3
1000
1,0E-05
1,710E-03
22
0,67
9,5650E-07
0,00375
2614
bar
bar
1/min
m/s
m
C
m/s
m/s
m
transition
Table 6: Testing Conditions of the first filtration step (MWCO 400-500 Da)
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Figure 6: Permeate of the 400-500 Da filtration (left) and the filter sample obtained
from Kamal (right)
The permeate of the 400-500 Dalton Nano-filtration showed a lighter colouring than
the sample collected from Kamal (see Figure 6).
The permeate was further used in the next filtration step, using the 200 Dalton
Nano-filtration membrane from Koch Membranes.
Testing Conditions:
Operating pressure
Membrane dfferential pressure
U
Volume flow of caustic soda over membrane
Membran Area
Test Temperatur
Flow velocity over Membrane
Kinematic viscosity of water (22C)
hydraulic Pipe diameter
Reynolds Number
35
3
1000
1,0E-05
1,710E-03
22
0,67
9,5650E-07
0,00375
2614
bar
bar
1/min
m/s
m
C
m/s
m/s
m
transition
Table 7: Testing Conditions of the first filtration step (MWCO 200 Da)
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Colouration [m-1]
430nm 545nm 610nm
Raw
9,61
3,18
1,94
Filtrate
8,39
2,09
1,29
400 500 Da 4,02
0,906
0,490
200 Da
2,68
0,608
0,403
0
0
0
11
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The dialysis process is applied for the recovery of free acids or bases from spent
treatment bath solutions in surface finishing and textile processes. The spent bath
solution is separated in a chamber in counter-current flow and via an ion exchange
membrane and is then routed to a second chamber through which water flows. The
free acid or base is able to permeate while the salts are retained. Depending on the
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process design, up to 95% of the free acid and up to 80% of the base can be
recovered in this way and returned to the production process.
New membranes, which have high chemical and thermal resistance, have been
developed for use in acid dialysis, thus allowing troublesome process solutions to be
treated also. When applied at industrial level, these membranes can be easily
cleaned because of their improved resistance to oxidation as well as their high
chlorine tolerance.
New membrane modules combined with highly permeable membranes have been
developed to reduce investment costs.
Alternative 2
The third option would be a combination of a micro- and/or nano-filtration process
and a diffusion dialysis/electro-dialysis process.
Hybrid processes combining diffusion-/electro- dialysis and/or micro-/nano-filtration
have been developed for operations with a low salt concentration and high volume
flows, hence reducing investment costs effectively. Typical applications for this hybrid
process can be found in acid as well as base recovery.
Figure 10: Possible Set-up of the pilot plant for Kamal Ltd.
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Outlook
In order to find the optimum solution for recovering the caustic soda at Kamal Ltd.,
additional tests are necessary.
These tests could be done by TTZ, which would require additional samples of about
200-300 l of spent wash.
Alternatively, service providers/producers of the envisioned processes/equipment
could be contacted, in order to undertake tests and install the pilot plant at Kamal
Limited. Either way, these service providers/producers would have to be contacted at
one point, to install the pilot plant at Kamal Limited.
Following is a table of the most promising service providers/producers, who are able
to undertake further pilot tests and install the pilot plant:
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Service
Provider/
Producer
Microdyn Nadir
GmbH
Koch Membrane
Systems
OSMO Membrane
Systems GmbH
Process, Equipment
Reverse osmosis
Nanofiltration
Ultrafiltration
Microfiltration
Electro dialysis
Diffusion dialysis
Services
Contact
www.microdyn-nadir.de
info@microdyn-nadir.de
+49 (0) 611 - 962 6001
www.kochmembrane.com
farrel2m@kochind.com
hatchl@kochind.com
www.osmo-membrane.de
info@osmo-membrane.de
General manager: Dipl.Ing. Christian Steine
DEUKUM GmbH
Documentation
Start-up
After sales service and spare parts supply
Elektrodialysis
Membranelektrolysis
Diffusiondialysis
Pilot plants
www.deukum.de
info@deukum.de
HANS-JRGEN RAPP
Dr. Ing.
Verfahrenstechnik
Geschftsfhrer
+49 (0)70 22 / 47 06 95
FuMA-Tech
GmbH
Electrodialysis
Bipolar membrane
technology
Membrane electrolysis
Diffusion dialysis
Reverse osmosis
Nanofiltration
Ultrafiltration
Microfiltration
www.fumatech.com
office@fumatech.de
Yervant Bohdjalian
(Membrane Technology)
T: +49 6894 9265-23
Dr. Karl Danz
(Components & Plant
Engineering)
T: +49 7042 97024-23
WAG-Freiburg
GmbH
Piping diagrams
Process development
Controll-system design
Software-services
Ingeneering services
Pilot-plants
Experimental projects
Table 8: Service providers/producers for pilot plant tests, design and set-up
www.wag-freiburg.de
info@wag-freiburg.de
+49 (0)7668 / 95 20 74
(sales)
+49 (0)7668 / 95 20 75
(service)