22/04/2021

Aplikasi Teknologi Membran

pada Produksi Kecap

Dr. Faleh Setia Budi, ST, MT

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Agenda
• Introduction
• Membrane Selection
• Optimization of process parameters
• Membrane fouling and Regeneration

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Introduction
Proses Pembuatan Kecap
Kedelai

Fermentasi Koji

Fermentasi Garam

Refining

Kecap

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Introduction (lanjutan…)
Proses Pembuatan Kecap

Sterilization
T: 113 C - 117 C

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Introduction

Application of membrane technology in soy sauce

processing include
• Clarification and sterilization of soy sauce by MF
and UF
• Desalination and decoloration of soy sauce by NF.

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Intorduction
Characteristic of soy sauce product
• AN and SSESC at a maximal level
• the viable count as low as possible in soy sauce
Characteristic of raw soy sauce
Parameter Komposisi
AN (g/L) 9.3
NaCl (g/L) 188
Total acidity (g/L) 19.1
Reducing sugar (g/L) 51.6
Absorbance (at 760 nm) 0.545
Sediment (yes or no) Yes
SSESC (g/L) 236
Viable count (cfu/mL) 6300
AN : Amino Nitrogen
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SSESC : Soluble Solids Excluding Sodium Chloride

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MF AND UF FOR STERILIZATION AND CLARIFICATION OF

SOY SAUCE

 Membrane Selection
Ceramic membrane or Polymeric membrane : 0.2 - 0.5 μm

Cost High lower

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MF AND UF FOR STERILIZATION AND CLARIFICATION

o 0.2-μm ceramic membrane :
o four ceramic tubular MF membranes (Tien and Chiang, 1992)
 did not alter the general composition of soy sauce
 significantly reduced turbidity and count of aerobic
microorganisms
 gave the highest permeate flux
 99% of bacteria removal (reduced from 3200 to 30 cfu/mL)
 flux decline was much faster for membranes with large pore
size due to more severe fouling
o hollow fiber MF membrane (polyphthalazinone ether sulfone
ketone /PPESK)
o pore size of the membrane was 0.2 μm (Tian et al. 2007)
 complete removal of bacteria
 slight flux decline in the 30-h operation (flux decreased from
27 L/m2 h to 24 L/m2 h)
o MF of soy sauce by polysulfone membranes with pore sizes of 0.1
 flux (41.77 L/m2 h) and complete removal of microbes

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MF AND UF FOR STERILIZATION AND CLARIFICATION OF

SOY SAUCE
Membrane Selection
Ceramic membrane or Polymeric membrane

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MF AND UF FOR STERILIZATION AND CLARIFICATION OF

SOY SAUCE
• The hollow fiber membrane module was widely used for refining,
• the outside-in mode was considered to be more suitable, though the
inside-out mode was also adopted

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MF AND UF FOR STERILIZATION AND CLARIFICATION OF

SOY SAUCE

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Optimization of Process Parameters

Process parameters significantly affected process efficiency and

product quality .
• property and composition of soy sauce,
• transmembrane pressure (TMP) or permeate flux,
• shear rate or cross-flow velocity,

π = 𝑀𝑅𝑇

1. efficiency of process was affected by feed composition.

• increasing total solids concentration would enhance
concentration polarization and decrease the flux (Li et al.
2007)
• close correlation between the permeation flux and the total
nitrogen (TN) concentration of the raw soy sauce for
agitated disk membrane module (Matsushitak et al. 2002)
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Concentration Polarization
- The nearly complete rejection of solute by the membrane
leads to a higher concentration at the membrane surface than
in the bulk solution.

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Optimization of Process Parameters

2. increase in TMP, permeate flux increases as long as the flux is
below the limiting flux.
• MF inorganic membrane 0.2 μm.
the initial flux decline became larger with an increase in TMP, and
after a 30-min operation, the flux at 0.24 MPa was less than that at
0.22 MPa.
• TMP at 0.07 MPa was optimal (using a hollow fiber MF
membrane made from PPESK)
• TMP was at 0.28 MPa (a ceramic tubular MF membrane)
• TMP higher than the shred hold would not increase permeate flux,
but would increase the deposition of particle, resulting in more
pore blocking and compressing the cake, leading to a serious flux
decline

Pi  Po
P   Pp
2
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Optimization of Process Parameters

3. Increasing temperature leads to the increase in permeate flux
• However, the increase in temperature solute, solubility may
increase, and precipitation may form when the temperature
goes down.
• In determining processing temperature, permeate flux, energy
consumption, heat resistance of the membrane, and product
quality should be taken into account.

4. Increasing the shear rate (the stirring speed for stirred cell and
the cross-flow velocity (CFV) for cross-flow filtration enhance
the permeate flux and reduce the fouling rate (in UF and MF ).
• Resistance (overall filtration and concentration polarization
layer) in cross-flow MF α-Al2O3 membrane 0.2 μm
decreased with an increase in CFV from 0.29 to 0.58 m/s
• increasing CFV would increase permeate flux and decrease
concentration polarization.
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Increasing the shear rate

to reduce fouling

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Industrial Application of Soy Sauce Ultrafiltration

UF membrane system for soy

sauce processing

a soy sauce manufacturing plant in South China

• two-stage UF membrane system.
• Each with 2 parallel membrane housings individually equipped with 3
spiral-wound UF elements
• use 12 spiral wound UF elements, (total membrane area of 360 m2)
• distributed in 4 cylindrical membrane housings
• Pore size of membrane : 150-kDa MWCO
• Membrane Material : PVDF
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Spiral wound module

Spiral wound module in housing

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Industrial Application of Soy Sauce UF

• Raw soy sauce was prefiltered by a filter cloth (200 mesh) and
then was subjected to a two-stage UF.
• Average permeate flux of around 14 L/m2 h,
• the production capacity of refined soy sauce is around 5 m3/h.

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REVERSE OSMOSIS AND NANOFILTRATION FOR

DESALINATION AND DECOLORATION OF SOY SAUCE
In Japan
1. Akiko et al. proposed to use a low-pressure RO membrane
2. There are also researcher which employ a two-step NF
• NF1 having 5 - 25% of salt rejection to obtain permeate liquid,
• then concentrating the permeate liquid with NF2 having at least
60% salt rejection.

In Chinese
• Use two-step NF process
• First NF membrane to reduce the salt
• Permeate liquid from first NF was concentrated by NF membrane
having high amino acids rejection and around 50% rejection of
NaCl

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REVERSE OSMOSIS AND NANOFILTRATION FOR

DESALINATION AND DECOLORATION OF SOY SAUCE

Primary Retentate Secondary Retentate

(Low-Salt Soy Sauce) (Light Color Soy Sauce)

Feed
(Row Soy Sauce) NF1 NF2
Primary Secondary
Permeate Permeate
(Processing Water)
NF1: NF2:
5 - 25% salt rejection 60% salt rejection

Schematic diagram of two-stage NF process for desalination

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REVERSE OSMOSIS AND NANOFILTRATION FOR

DESALINATION AND DECOLORATION OF SOY SAUCE

1. Performance of Different Membranes

• membrane with high rejection of organic Desirable for
solutes (e.g., amino acids, polysaccharides, industrial
etc.) application
• high flux but low rejection of monovalent of soy sauce
ions desalination

Rentetate (high amino

acid, saccharide)

Permeate (high NaCl)

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REVERSE OSMOSIS AND NANOFILTRATION FOR

DESALINATION AND DECOLORATION OF SOY SAUCE
• suitability of 4 commercial NF membranes for desalination:
NF-, NF90, NF270, and Desal-5 DL.
NF90 was not suitable for desalination (high rejection of NaCl).
• removal of AN and SSESC was in this order:
NF-,NF270,Desal-5 DL.
Desal-5 DL was also excluded (high loss of AN and SSESC)
o Loss of AN (18.57%) & SSESC (3.98%) NF- < NF270 (18.81%
and 4.87%)
o NF270 had lower TMP at constant flux or higher flux at
constant TMP when compared with NF-
o NF270 membrane : the most suitable one (have high
nutritional component retention, high salt transmission, and
relatively high permeate flux)

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REVERSE OSMOSIS AND NANOFILTRATION FOR

DESALINATION AND DECOLORATION OF SOY SAUCE
2. Effect of Operating Conditions
• raw soy sauce: high concentration of salt and other soluble solids.
• It is necessary to dilute the raw soy sauce

a. Concentration
• Increase of dilution factor (DF), salt removal and AN loss
increased, while SSESC remains more or less constant
• low DF: less water consumption, less processing time, and higher
nutrient (e.g., AN) retention

desalination constant flux using concentration mode with

• increasing permeate flux,
• TMP increased,
• the loss of SSESC and AN decreased,
• while salt removal was more or less constant
π = 𝑀𝑅𝑇
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REVERSE OSMOSIS AND NANOFILTRATION FOR

DESALINATION AND DECOLORATION OF SOY SAUCE
b. Temperature
increasing temperature, →
• the loss of SSESC and AN increased,
• The removal of NaCl slightly decreased
• the TMP also decreased
increasing temperature →
decrease the viscosity and
Increase solute diffusivity,
thus lessening concentration polarization.
increasing temperature → severer membrane fouling.
due to the denaturation of some biologically active substances
(proteins and polypeptides)

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MEMBRANE FOULING AND REGENERATION

Membrane Fouling
major limitation of MF and UF : permeate flux decline
(due to concentration polarization and membrane fouling).
increase in nominal pore size → total resistance (Rt) increased
→concentration polarization resistance (Rcp) increased
→cake resistance (Rc) decrease
→internal fouling resistance (Rif) decreased

Rcp and Rc could be affected by system hydrodynamics,

fouling control : enhancing the turbulence in the membrane
modules through operating condition control
and membrane module design.

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Membrane Fouling

Fouling

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MEMBRANE FOULING AND REGENERATION

Regeneration
Cleaning of membrane can be accomplished by
• physically removing the foulants from the membranes (e.g.,
backflushing, mechanical scrubbing)
• using chemical cleaning agents (e.g., acids, alkalis, surfactants,
and enzymes) to remove or decompose the foulants.

Cleaning solutions composed of

• mineral acids, sodium hexametaphosphate, polyacrylates, and
EDTA (suitable for salt precipitates and mineral scalants),
• caustics based on NaOH and/or NaClO (for removing fats and
proteins)
• Enzyme cleaners are used to remove protein and other types of
biofoulants in specific instances main components of the foulants
(protein, ash, cell debris, and other suspended solids)

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MEMBRANE FOULING AND REGENERATION

Regeneration
Different cleaning methods for MF and UF membrane
• hot water (100oC) backflushing → membrane flux recovery > 96%
• caustic cleaning (NaOH solution at pH 9-10) could restore
membrane flux completely.

fouled ceramic membrane MF was regenerated by a four-step

cleaning i.e.
1. Water rinsing for 30 min at 20 ± 3oC
2. Cleansing with 1.5 wt% NaOH for 40 min at 40 ± 3oC
3. Cleansing with 0.15 mol/L HNO3 for 40 min at 40 ± 3oC,
and
4. finally water rinsing again until neutrality

• Fouled UF polysulfone membrane was regenerated by

trypsin solution and NaOH solution and proposed a two
step cleaning protocol

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MEMBRANE FOULING AND REGENERATION

Regeneration of fouled NF membrane
• could not use caustic cleaning (0.1% (w/v) NaOH solution) or by
soaking overnight
• homemade composite cleaning agent (alkali, surfactant, &
enzyme) 0.3% (w/v) could recover the water permeability

• Multiple interactions with the foulants (solubilization, dispersion,

hydrolysis, and decomposition) would favor the regeneration of
the fouled NF membrane, and composite cleaning formulation
would be preferred.

For sterilizing the NF system,

• perform a thorough washing with 1% (w/v) NaHSO3 solution
every week to ensure the product was free of bacteria,
• a monthly washing with 2% (w/v) citric acid solution to remove
inorganic salt precipitates.

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TERIMA KASIH

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