CN104450828A - Membrane filtration process for producing food-grade xylooligosaccharide by taking viscose fiber pressing alkali liquor as raw material - Google Patents
Membrane filtration process for producing food-grade xylooligosaccharide by taking viscose fiber pressing alkali liquor as raw material Download PDFInfo
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Abstract
The invention provides a membrane filtration process for producing food-grade xylooligosaccharide by taking viscose fiber pressing alkali liquor as a raw material. The membrane filtration process particularly comprises the following process steps of: A, membrane concentration: firstly pre-filtering pressed liquor produced through a viscose fiber to remove large-granular impurities, circularly concentrating permeating liquid for 2-4 times through a nanofiltration membrane, and introducing a last-time concentrated solution into a diffusion dialysis cation exchange membrane stack to obtain a concentrated solution, namely a concentrated solution of the pressed liquor, in the processes of circularly concentrating for 2-4 times through the nanofiltration membrane, feed liquid is diluted by adding water and then enters the nanofiltration membrane before being filtered every time; B, hemicellulose extraction: neutralizing the concentration solution of the pressing alkali liquor by adding acid to obtain hemicellulose liquid; C, enzymolysis: adding a complex enzyme to the hemicellulose liquid for carrying out enzymolysis reaction to obtain enzymolysis liquid; D, purification: filtering the enzymolysis liquid through a ceramic membrane, introducing the permeating liquid into the nanofiltration membrane for desalination, decoloring the obtained concentration solution through active carbon, carrying out resin-ion exchange to obtain purifying liquid of xylooligosaccharide, and evaporating and drying to obtain the food-grade xylooligosaccharide.
Description
Technical field
The present invention relates to xylo-oligosaccharide preparation field, be specifically related to the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide.
Background technology
Xylo-oligosaccharide, also known as wood oligose, is the general name of the IMO be combined into β-Isosorbide-5-Nitrae-glycosidic link by 2-7 wood sugar.Effective constituent is xylo-bioses, xylotriose, Xylotetrose, wooden pentasaccharides etc., wherein based on xylo-bioses and xylotriose.Have unique advantage compared with soybean oligosaccharide, oligofructose, oligomeric isomaltose etc. that xylo-oligosaccharide is used with usual people, it optionally can promote the proliferation activity of intestinal bifidobacteria, and its bifidobacterium factor functional is 10-20 times of other polymerization carbohydrate.Xylo-oligosaccharide is considered to desirable protective foods sweeting agent because of advantages such as its significant bifidus bacillus multiplication capacity, decomposition difficult to digest, low carious tooth, effectively intake are few, and its acidproof heat-proof also makes it be applied to the industries such as medicine, beverage, fodder additives simultaneously.
Xylo-oligosaccharide, to be rich in the plant of xylan for raw material, is produced by biochemical method.The production of current xylo-oligosaccharide is raw material mainly with corn cob, and complex manufacturing, cost is higher.And at chemical pulp plant celluloses such as () wood pulp, cotton pulp, straw pulp, reed pulps in the production process of viscose fiber of raw material, adopting alkali lye to process (dipping, squeezing) to Mierocrystalline cellulose is the first step manufacturing viscose fiber.Hemicellulose concentration is high, extremely adverse influence is produced to cellulose viscose manufacturing technique and final product quality, therefore must in impregnation technology with alkali lye by hemicellulose stripping, the Mierocrystalline cellulose of high strength could be obtained, so a large amount of high concentration alkali pressed liquors being rich in hemicellulose can be produced in above process.
Main component in alkali pressed liquor is sodium hydroxide and hemicellulose.Hemicellulose is therefrom separated by treatment process many employings nanofiltration of existing press lye, obtains comparatively pure alkali lye.Through purification alkali lye can direct reuse in technique, but part alkali only can be realized reuse by nanofiltration membrane, still containing a large amount of alkali in the concentrated solution that the hemicellulose in its trapped fluid obtains after concentrated.During at present this part feed liquid is used for as salkali waste and technique, hemicellulose enters wastewater treatment, or adopts calcination to reclaim sodium hydroxide, and hemicellulose is burned.From above existing technique, hemicellulose is not fully used.
Document " the membrane separation concentration technical study of xylo-oligosaccharide " (" foodstuffs industry ", 09 phase in 2012), pilot plant test device is adopted to carry out pilot plant test to the separation of lower concentration xylo-oligosaccharide solution is concentrated, the effect of the polyamide-based nanofiltration of comparative studies and reverse osmosis two kinds of membrane techniquies, determines the optimised process operational condition that nanofiltration membrane separation concentrates xylo-oligosaccharide solution.This technique nanofiltration membrane thickening temperature is low, and membrane filtration efficiency is lower, is unsuitable for industrialization scale operation.
Summary of the invention
For above-mentioned technical problem, the invention provides with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide.The xylo-oligosaccharide salinity obtained is low, and purity is high, and process operation efficiency is high, is adapted to scale operation.
For achieving the above object, the present invention adopts following technical scheme:
With the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: concrete technology step is as follows:
A, membrane concentration
The pressed liquor that viscose fiber is produced is first through pre-filtering removing large granular impurity, and permeate is through concentrated 2-4 time of nanofiltration membrane circulation, and last concentrated solution enters diffusion dialysis cationic exchange membrane stack, and gained concentrated solution is the concentrated solution of pressed liquor; Concentrated 2-4 time of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up.
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid.
C, enzymolysis
In half fine liquid, add prozyme, enzyme digestion reaction occurs and obtains enzymolysis solution;
D, purification
Enzymolysis solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and gained concentrated solution is through activated carbon decolorizing, and resin ion obtains the refined solution of xylo-oligosaccharide after exchanging, then obtains xylo-oligosaccharide through evaporation, oven dry.
The xylo-oligosaccharide that preparation method of the present invention obtains meets the industry standard QBT 2984-2008 of food-grade xylooligosaccharide.
Step A of the present invention, the molecular weight cut-off of nanofiltration membrane is 200-400, and alkali is separated from permeate, progressively lowers alkali dense, promotes half fine concentration.
Step A of the present invention, the film that diffusion dialysis uses is multiple cationic exchange membranes, and the distance between cationic exchange membrane is 0.4-0.9mm, prevents the blocking to diffusion dialysis film.
Step A of the present invention, before each nanofiltration membrane, the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume.While ensureing filtration efficiency, little to the damage of nanofiltration membrane.
Preferably, described permeate, containing alkali 200-300g/l, containing half fine 40-80 g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 12-75g/l, containing half fine 40-80g/l; Containing alkali 2-4g/l in described diffusion dialysis concentrated solution, containing half fine 40-80g/l.Under lowering the dense prerequisite of alkali, ensure the filtration efficiency of film; Be down to minimum by dense for alkali simultaneously, ensure that the purity of half fibre.
Pre-filtering of the present invention refers to, press lye is successively through rotary drum filtration, Plate Filtration and ultrafiltration removing large granular impurity.Pre-filtering makes press lye not containing the solid impurity of more than 5 microns, and protection film is not below damaged by solid impurity.
Step A of the present invention, the temperature of nanofiltration membrane is 40-60 DEG C, and the temperature of diffusion dialysis is 15-45 DEG C, and filtration temperature is high, and liquid viscosity is lower, is conducive to filtration efficiency and improves.
Step A of the present invention, the mistake mould difference of nanofiltration membrane is 3-4bar, and the mistake mould difference of diffusion dialysis is 0.3-0.8bar.For the feature that viscose glue press lye viscosity is higher, adopt higher pressure reduction to filter, can ensure that half fine concentration in alkali lye reaches processing requirement.
Step A of the present invention, the flow of feed liquid in nanofiltration membrane is 25-40m
3/ h, the flow in diffusion dialysis is 2-20mm/s.The surface velocity that bonding props up film is higher, film is not easy contaminated; Ensure the duration of contact of feed liquid and electrodialytic membranes, thus half fibre can be fully separated with alkali.
Step A of the present invention, it is 26.8m that the list of nanofiltration membrane props up filtration area
2,it is a membrane stack 50m that the list of diffusion dialysis cationic exchange membrane props up filtration area
2, single film has larger filtration area under the prerequisite taking less space.
Step B of the present invention, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4-5.The advantage adding hydrochloric acid is that the molecules of salt amount formed is lower, and be conducive to the desalination in later stage, pH value is 4-5, adapts to the pH value requirement of enzymolysis.
Step C of the present invention, prozyme is zytase, cellulase and polygalacturonase, can improve sugared associative key susceptibility to enzymic hydrolysis after adding appropriate cellulase and pectin in zytase.
Preferably, the ratio of described zytase, cellulase and polygalacturonase is 3:2:1, and adopt the prozyme of this ratio to carry out degrading and can make the maximum production of xylo-oligosaccharide, the percent hydrolysis of hemicellulose is up to more than 95%.
Preferably, the enzymolysis time of described enzyme digestion reaction is 0.5-2h, and temperature is 50-60 DEG C, and the pH value of enzyme digestion reaction is 4-5, and under this condition, the activity of enzyme is the highest.
Preferably, the enzyme concentration of described enzyme digestion reaction is 0.5-1.5%, and now the catalytic effect of enzyme is best.
D step of the present invention, the molecular weight cut-off of ceramic membrane is 800-1500, and separating oligomeric wood sugar and undegradable half fibre, ensure product purity.
D step of the present invention, the molecular weight cut-off of described nanofiltration membrane is 100-200.Owing to adopting hydrochloric acid neutralization, the salt of generation is sodium-chlor, and the molecular weight of sodium-chlor is smaller, and far below 100, and xylo-oligosaccharide molecular weight is much larger than 100, effectively can realize being separated of salt and xylo-oligosaccharide.
Preferably, described nanofiltration membrane desalination, crossing mould difference is 3-4bar, and temperature is 30-40 DEG C, and single filtration area is 26.8 m
2, adapt to the change of low catching molecular, guarantee salt is separated with xylo-oligosaccharide.
Preferably, the material liquid volume before described nanofiltration membrane concentrates is 10-15 times of concentrated solution volume, is conducive to reducing the salt content in xylo-oligosaccharide.
The decolouring of D step of the present invention refers to: adjusted to ph is 4-5, adds gac, at 50-60 DEG C, adsorb 0.5-1h.
Preferably, described gac is LY-T-ac gac, and consumption is 3-5%.Best to the decolorizing effect of liquid glucose, percent of decolourization is 70%, and the rate of loss of sugar is minimum.
The ion-exchange of D step of the present invention refers to: concentrated solution first by positive post, then falls charged impurity by cloudy post exchange adsorption, and ratio of desalinization is 60-70%, and the purity obtaining xylo-oligosaccharide refined solution is 60-70%, thus has ensured the purity of product.
Membrane concentration technique of the present invention obtains the water content < 5% of xylo-oligosaccharide, pH=4-5, ash content < 0.3%, ignition residue 3-6%, dry-matter > 75%, transmittance > 70%, specific conductivity is 8000-10000 μ s/cm.
Beneficial effect of the present invention is:
1, the present invention adopts nanofiltration membrane and diffusion dialysis membrane stack combination filtering and concentrating half fibre, because the running cost of nanofiltration membrane is lower than diffusion dialysis, nanofiltration membrane is first adopted repeatedly progressively to drop to certain degree dense for alkali, concentrated half fibre, little to the damage of film, re-use diffusion dialysis fine to improve concentrated solution half, reduce alkali dense, thus reduce whole production cost and enhance productivity.Nanofiltration and diffusion dialysis cooperatively interact, and have complementary advantages, and make containing alkali 2-4g/l in final concentrated solution, containing half fine 40-80 g/l, achieve low alkali dense, height half is fine; And process operation efficiency is high, little to the damage of film, cost is low, is adapted to industrialization scale operation.
2, the amount of nanofiltration membrane thin up of the present invention is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn, can realize nanofiltration membrane water 10m excessively per hour
3left and right, ensure that filtration efficiency; Meanwhile, little to the damage of film, the 2-3 that can reach its quality guarantee period work-ing life doubly, reduces cost to a great extent, is adapted to industrialization scale operation.
3, the present invention adds hydrochloric acid neutralization to the concentrated solution obtained, then adopts molecular weight cut-off to be the nanofiltration membrane desalination of 100-200.In hydrochloric acid and the salt generated be sodium-chlor, the molecular weight of sodium-chlor, far below 100, and xylo-oligosaccharide molecular weight is much larger than 100, effectively can realize being separated of salt and xylo-oligosaccharide.Be conducive to the desalination in later stage, further increase the purity of xylo-oligosaccharide.
4, enzymolysis solution is first used ceramic membrane separation xylo-oligosaccharide and undegradable half fibre by the present invention, ensure product purity, permeate enters nanofiltration membrane desalination again, thus have effectively achieved being separated of salt and xylo-oligosaccharide, the specific conductivity finally obtaining xylo-oligosaccharide is 8000-10000 μ s/cm, and ignition residue is 3-6%.Ignition residue is the direct indicator weighing inorganic salt, and the massfraction described in xylo-oligosaccharide shared by inorganic salt is only 3-6%; Specific conductivity is the electrolytical degree existed in reaction liquid, and the main electrolyte of xylo-oligosaccharide is exactly inorganic salts, so this index also can reflect the number of salinity in product.It is low that low conductivity and ignition residue describe the xylo-oligosaccharide salinity adopting the inventive method to obtain, high purity more than 85%.
Embodiment
Below in conjunction with embodiment, essentiality content of the present invention is described in further detail.
Embodiment 1
With the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, concrete technology step is as follows:
A, membrane concentration
The pressed liquor that viscose fiber is produced is first through pre-filtering removing large granular impurity, and permeate is through concentrated 2 times of nanofiltration membrane circulation, and last concentrated solution enters diffusion dialysis cationic exchange membrane stack, and gained concentrated solution is the concentrated solution of pressed liquor; Concentrated 2 times of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up;
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid.
C, enzymolysis
In half fine liquid, add prozyme, enzyme digestion reaction occurs and obtains enzymolysis solution;
D, purification
Enzymolysis solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and gained concentrated solution is through activated carbon decolorizing, and resin ion obtains the refined solution of xylo-oligosaccharide after exchanging, then obtains food-grade xylooligosaccharide through evaporation, oven dry.
Embodiment 2
With the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, concrete technology step is as follows:
A, membrane concentration
The pressed liquor that viscose fiber is produced is first through pre-filtering removing large granular impurity, and permeate is through concentrated 3 times of nanofiltration membrane circulation, and last concentrated solution enters diffusion dialysis cationic exchange membrane stack, and gained concentrated solution is the concentrated solution of pressed liquor; Concentrated 3 times of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up;
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid.
C, enzymolysis
In half fine liquid, add prozyme, enzyme digestion reaction occurs and obtains enzymolysis solution;
D, purification
Enzymolysis solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and gained concentrated solution is through activated carbon decolorizing, and resin ion obtains the refined solution of xylo-oligosaccharide after exchanging, then obtains food-grade xylooligosaccharide through evaporation, oven dry.
Embodiment 3
With the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, concrete technology step is as follows:
A, membrane concentration
The pressed liquor that viscose fiber is produced is first through pre-filtering removing large granular impurity, and permeate is through concentrated 4 times of nanofiltration membrane circulation, and last concentrated solution enters diffusion dialysis cationic exchange membrane stack, and gained concentrated solution is the concentrated solution of pressed liquor; Concentrated 4 times of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up;
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid.
C, enzymolysis
In half fine liquid, add prozyme, enzyme digestion reaction occurs and obtains enzymolysis solution;
D, purification
Enzymolysis solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and gained concentrated solution is through activated carbon decolorizing, and resin ion obtains the refined solution of xylo-oligosaccharide after exchanging, then obtains food-grade xylooligosaccharide through evaporation, oven dry.
Embodiment 4
The present embodiment is substantially the same manner as Example 1, on this basis:
Described step A, the molecular weight cut-off of nanofiltration membrane is 200.
The nanofiltration membrane circulation of described step A is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
The film that described diffusion dialysis uses is multiple cationic exchange membranes, and the distance between cationic exchange membrane is 0.4mm.
Embodiment 5
The present embodiment is substantially the same manner as Example 2, on this basis:
Described step A, the molecular weight cut-off of nanofiltration membrane is 400.
The nanofiltration membrane circulation of described step A is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
The film that described diffusion dialysis uses is multiple cationic exchange membranes, and the distance between cationic exchange membrane is 0.9mm.
Embodiment 6
The present embodiment is substantially the same manner as Example 3, on this basis:
Described step A, the molecular weight cut-off of nanofiltration membrane is 300.
The nanofiltration membrane circulation of described step A is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
The film that described diffusion dialysis uses is multiple cationic exchange membranes, and the distance between cationic exchange membrane is 0.5mm.
Embodiment 7
The present embodiment is substantially the same manner as Example 1, on this basis:
Described step A, the molecular weight cut-off of nanofiltration membrane is 250.
The nanofiltration membrane circulation of described step A is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
The film that described diffusion dialysis uses is multiple cationic exchange membranes, and the distance between cationic exchange membrane is 0.6mm.
Embodiment 8
The present embodiment is substantially the same manner as Example 4, on this basis:
Described step A, described permeate, containing alkali 300g/l, containing half fine 80g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 75g/l, containing half fine 80g/l; Containing alkali 4g/l in described diffusion dialysis concentrated solution, containing half fine 80g/l.
Embodiment 9
The present embodiment is substantially the same manner as Example 5, on this basis:
Described step A, described permeate, containing alkali 260g/l, containing half fine 70g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 32.5g/l, containing half fine 80g/l; Containing alkali 3.5g/l in described diffusion dialysis concentrated solution, containing half fine 70g/l.
Embodiment 10
The present embodiment is substantially the same manner as Example 6, on this basis:
Described step A, described permeate, containing alkali 200g/l, containing half fine 40g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 12.5g/l, containing half fine 40g/l; Containing alkali 2g/l in described diffusion dialysis concentrated solution, containing half fine 40g/l.
Embodiment 11
The present embodiment is substantially the same manner as Example 7, on this basis:
Described step A, described permeate, containing alkali 220g/l, containing half fine 60g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 55g/l, containing half fine 60g/l; Containing alkali 3g/l in described diffusion dialysis concentrated solution, containing half fine 60g/l.
Embodiment 12
The present embodiment is substantially the same manner as Example 8, on this basis:
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and ultrafiltration removing large granular impurity.
Embodiment 13
The present embodiment is substantially the same manner as Example 9, on this basis:
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and ultrafiltration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 40 DEG C, and the temperature of diffusion dialysis is 15 DEG C.
Embodiment 14
The present embodiment is substantially the same manner as Example 10, on this basis:
Pre-filtering refer to, pressed liquor successively through rotary drum filter, Plate Filtration and ultrafiltration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 60 DEG C, and the temperature of diffusion dialysis is 45 DEG C.
Described step A, the mistake mould difference of nanofiltration membrane is 4bar, and the mistake mould difference of diffusion dialysis is 0.8bar.
Embodiment 15
The present embodiment is substantially the same manner as Example 11, on this basis:
Described step A, pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and ultrafiltration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 45 DEG C, and the temperature of diffusion dialysis is 20 DEG C.
Described step A, the mistake mould difference of nanofiltration membrane is 3bar, and the mistake mould difference of diffusion dialysis is 0.3bar.
Described step A, the flow of feed liquid in nanofiltration membrane is 25m
3/ h, the flow in diffusion dialysis process is 2mm/s.
Embodiment 16
The present embodiment is substantially the same manner as Example 11, on this basis:
Described step A, pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and ultrafiltration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 55 DEG C, and the temperature of diffusion dialysis is 30 DEG C.
Described step A, the mistake mould difference of nanofiltration membrane is 3.6bar, and the mistake mould difference of diffusion dialysis is 0.5bar.
Described step A, the flow of feed liquid in nanofiltration membrane is 40m
3/ h, the flow in diffusion dialysis process is 20mm/s.
Described step A, it is 26.8m that the list of nanofiltration membrane props up filtration area
2, it is a membrane stack 50m that the list of diffusion dialysis cationic exchange membrane props up filtration area
2.
Embodiment 17
The present embodiment is substantially the same manner as Example 8, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.
Embodiment 18
The present embodiment is substantially the same manner as Example 9, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 5.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
Embodiment 19
The present embodiment is substantially the same manner as Example 10, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.5.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 0.5h, and temperature is 60 DEG C, and the pH value of enzyme digestion reaction is 4.5.
Embodiment 20
The present embodiment is substantially the same manner as Example 11, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.6.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 2h, and temperature is 50 DEG C, and the pH value of enzyme digestion reaction is 4.6.
The enzyme concentration of described enzyme digestion reaction is 0.5%.
Embodiment 21
The present embodiment is substantially the same manner as Example 15, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value 4.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 1h, and temperature is 52 DEG C, and the pH value of enzyme digestion reaction is 4.
The enzyme concentration of described enzyme digestion reaction is 1.5%.
Described D step, the molecular weight cut-off of ceramic membrane is 800.
Embodiment 22
The present embodiment is substantially the same manner as Example 16, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 5.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 1.5h, and temperature is 55 DEG C, and the pH value of enzyme digestion reaction is 5.
The enzyme concentration of described enzyme digestion reaction is 1%.
Described D step, the molecular weight cut-off of ceramic membrane is 1500.
Described D step, the molecular weight cut-off of nanofiltration membrane is 200.
Embodiment 23
The present embodiment is substantially the same manner as Example 16, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.2.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 0.6h, and temperature is 52 DEG C, and the pH value of enzyme digestion reaction is 4.2.
The enzyme concentration of described enzyme digestion reaction is 0.6%.
Described D step, the molecular weight cut-off of ceramic membrane is 1000.
Described D step, the molecular weight cut-off of nanofiltration membrane is 100.
The mistake mould difference of described nanofiltration membrane is 3bar, and temperature is 30 DEG C, and single filtration area is 26.8 m
2.
Embodiment 24
The present embodiment is substantially the same manner as Example 16, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.5.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 1.5h, and temperature is 58 DEG C, and the pH value of enzyme digestion reaction is 4.5.
The enzyme concentration of described enzyme digestion reaction is 0.8%.
Described D step, the molecular weight cut-off of ceramic membrane is 900.
Described D step, the molecular weight cut-off of nanofiltration membrane is 120.
The mistake mould difference of described nanofiltration membrane is 4bar, and temperature is 40 DEG C, and single filtration area is 26.8 m
2.
Described D step, the material liquid volume before nanofiltration membrane concentrates is 10 times of concentrated solution volume.
Embodiment 25
The present embodiment is substantially the same manner as Example 16, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 0.7h, and temperature is 52 DEG C, and the pH value of enzyme digestion reaction is 4.
The enzyme concentration of described enzyme digestion reaction is 0.8%.
Described D step, the molecular weight cut-off of ceramic membrane is 950.
Described D step, the molecular weight cut-off of nanofiltration membrane is 150.
The mistake mould difference of described nanofiltration membrane is 3.5bar, and temperature is 32 DEG C, and single filtration area is 26.8 m
2.
Described D step, the material liquid volume before nanofiltration membrane concentrates is 15 times of concentrated solution volume.
The decolouring of described D step refers to: adjusted to ph is 4, adds gac, at 50 DEG C, adsorb 1h.
The specific conductivity obtaining xylo-oligosaccharide is 8500 μ s/cm, and ignition residue is 4%.
Embodiment 26
The present embodiment is substantially the same manner as Example 16, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 5.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 2h, and temperature is 56 DEG C, and the pH value of enzyme digestion reaction is 5.
The enzyme concentration of described enzyme digestion reaction is 1.2%.
Described D step, the molecular weight cut-off of ceramic membrane is 1200.
Described D step, the molecular weight cut-off of nanofiltration membrane is 180.
The mistake mould difference of described nanofiltration membrane is 3.6bar, and temperature is 35 DEG C, and single filtration area is 26.8 m
2.
Described D step, the material liquid volume before nanofiltration membrane concentrates is 12 times of concentrated solution volume.
The decolouring of described D step refers to: adjusted to ph is 5, adds gac, at 60 DEG C, adsorb 0.5h.
Described gac is LY-T-ac gac, and consumption is 3%.
The specific conductivity obtaining xylo-oligosaccharide is 9000 μ s/cm, and ignition residue is 5%.
Embodiment 27
The present embodiment is substantially the same manner as Example 16, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.3.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 0.9h, and temperature is 53 DEG C, and the pH value of enzyme digestion reaction is 4.3.
The enzyme concentration of described enzyme digestion reaction is 1.1%.
Described D step, the molecular weight cut-off of ceramic membrane is 800.
Described D step, the molecular weight cut-off of nanofiltration membrane is 105.
The mistake mould difference of described nanofiltration membrane is 3.6bar, and temperature is 36 DEG C, and single filtration area is 26.8 m
2.
Described D step, the material liquid volume before nanofiltration membrane concentrates is 13 times of concentrated solution volume.
The decolouring of described D step refers to: adjusted to ph is 4.5, adds gac, at 52 DEG C, adsorb 0.6h.
Described gac is LY-T-ac gac, and consumption is 5%.
The ion-exchange of described D step refers to: concentrated solution first by positive post, then falls charged impurity by cloudy post exchange adsorption.
The specific conductivity obtaining xylo-oligosaccharide is 10000 μ s/cm, and ignition residue is 6%.
Embodiment 28
The present embodiment is substantially the same manner as Example 16, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.5.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 1.5h, and temperature is 56 DEG C, and the pH value of enzyme digestion reaction is 4.5.
The enzyme concentration of described enzyme digestion reaction is 0.8%.
Described D step, the molecular weight cut-off of ceramic membrane is 1000.
Described D step, the molecular weight cut-off of nanofiltration membrane is 120.
The mistake mould difference of described nanofiltration membrane is 3bar, and temperature is 32 DEG C, and single filtration area is 26.8 m
2.
Described D step, the material liquid volume before nanofiltration membrane concentrates is 12 times of concentrated solution volume.
The decolouring of described D step refers to: adjusted to ph is 4.5, adds gac, at 53 DEG C, adsorb 0.6h.
Described gac is LY-T-ac gac, and consumption is 4%.
The ion-exchange of described D step refers to: concentrated solution first by positive post, then falls charged impurity by cloudy post exchange adsorption.
The specific conductivity obtaining xylo-oligosaccharide is 8000 μ s/cm, and ignition residue is 3%.
Claims (20)
1. with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: concrete technology step is as follows:
A, membrane concentration
The pressed liquor that viscose fiber is produced is first through pre-filtering removing large granular impurity, and permeate is through concentrated 2-4 time of nanofiltration membrane circulation, and last concentrated solution enters diffusion dialysis cationic exchange membrane stack, and gained concentrated solution is the concentrated solution of pressed liquor; Concentrated 2-4 time of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up;
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid;
C, enzymolysis
In half fine liquid, add prozyme, enzyme digestion reaction occurs and obtains enzymolysis solution;
D, purification
Enzymolysis solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and gained concentrated solution is through activated carbon decolorizing, and resin ion obtains the refined solution of xylo-oligosaccharide after exchanging, then obtains food-grade xylooligosaccharide through evaporation, oven dry.
2. according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: described step A, the molecular weight cut-off of nanofiltration membrane is 200-400.
3. according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: described step A, before each nanofiltration membrane, the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume.
4. according to claim 3 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: described permeate is containing alkali 200-300g/l, containing half fine 40-80 g/l, after nanofiltration membrane circulation is concentrated, obtain concentrated solution containing alkali 12-75g/l, containing half fine 40-80g/l; Containing alkali 2-4g/l in described diffusion dialysis concentrated solution, containing half fine 40-80g/l.
5. according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: described step A, the film that diffusion dialysis uses is multiple cationic exchange membranes, and the distance between cationic exchange membrane is 0.4-0.9mm.
6. according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: described step A, the temperature of nanofiltration membrane treatment is 40-60 DEG C, and the temperature of diffusion dialysis is 15-45 DEG C.
7. according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: described step A, the mistake mould difference of nanofiltration membrane is 3-4bar, and the mistake mould difference of diffusion dialysis is 0.3-0.8bar.
8. according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: described step A, the flow of feed liquid in nanofiltration membrane is 25-40m
3/ h, the flow in diffusion dialysis process is 2-20mm/s.
9. according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: described step A, it is 26.8m that the list of nanofiltration membrane props up filtration area
2,it is a membrane stack 50m that the list of diffusion dialysis cationic exchange membrane props up filtration area
2.
10. according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: described step B, concentrated solution acid neutralization, refer to and add hydrochloric acid neutralization, make pH value be 4-5.
11. is according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, and it is characterized in that: described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
12. is according to claim 11 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: the enzymolysis time of described enzyme digestion reaction is 0.5-2h, and temperature is 50-60 DEG C, and the pH value of enzyme digestion reaction is 4-5.
13. is according to claim 11 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: the enzyme concentration of described enzyme digestion reaction is 0.5-1.5%.
14. is according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: described D step, and the molecular weight cut-off of ceramic membrane is 800-1500.
15. is according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: described D step, and the molecular weight cut-off of nanofiltration membrane is 100-200.
16. is according to claim 15 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: the mistake mould difference of described nanofiltration membrane is 3-4bar, and temperature is 30-40 DEG C, and single filtration area is 26.8 m
2.
17. is according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: described D step, and the material liquid volume before nanofiltration membrane concentrates is 10-15 times of concentrated solution volume.
18. is according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: the decolouring of described D step refers to: adjusted to ph is 4-5, adds gac, at 50-60 DEG C, adsorb 0.5-1h.
19. is according to claim 18 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, and it is characterized in that: described gac is LY-T-ac gac, consumption is 3-5%.
20. is according to claim 1 with the membrane filtration process of viscose fiber press lye for raw material production food-grade xylooligosaccharide, it is characterized in that: the ion-exchange of described D step refers to: concentrated solution first by positive post, then falls charged impurity by cloudy post exchange adsorption.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1556110A (en) * | 2004-01-05 | 2004-12-22 | 江南大学 | Production method of high purity oligoxylose |
| CN101484632A (en) * | 2006-05-10 | 2009-07-15 | 连津格股份公司 | Process for producing a pulp |
| CN104099431A (en) * | 2014-08-01 | 2014-10-15 | 沈阳新华环境工程有限公司 | Method for extracting xylose from viscoce chemical fiber squeezed alkali liquor |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1556110A (en) * | 2004-01-05 | 2004-12-22 | 江南大学 | Production method of high purity oligoxylose |
| CN101484632A (en) * | 2006-05-10 | 2009-07-15 | 连津格股份公司 | Process for producing a pulp |
| CN104099431A (en) * | 2014-08-01 | 2014-10-15 | 沈阳新华环境工程有限公司 | Method for extracting xylose from viscoce chemical fiber squeezed alkali liquor |
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