CN104404104A - Method for preparing food-grade xylo-oligosaccharide from viscose fiber squeezed alkali solution - Google Patents
Method for preparing food-grade xylo-oligosaccharide from viscose fiber squeezed alkali solution Download PDFInfo
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- CN104404104A CN104404104A CN201410622092.7A CN201410622092A CN104404104A CN 104404104 A CN104404104 A CN 104404104A CN 201410622092 A CN201410622092 A CN 201410622092A CN 104404104 A CN104404104 A CN 104404104A
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- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 title claims abstract description 68
- 239000003513 alkali Substances 0.000 title claims abstract description 47
- 239000000835 fiber Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 43
- 229920000297 Rayon Polymers 0.000 title claims abstract description 36
- 239000012528 membrane Substances 0.000 claims abstract description 180
- 239000000919 ceramic Substances 0.000 claims abstract description 82
- 238000001914 filtration Methods 0.000 claims abstract description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012141 concentrate Substances 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 18
- 239000012535 impurity Substances 0.000 claims abstract description 18
- 108090000790 Enzymes Proteins 0.000 claims abstract description 14
- 102000004190 Enzymes Human genes 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005516 engineering process Methods 0.000 claims abstract description 6
- 238000005342 ion exchange Methods 0.000 claims abstract description 5
- 238000000746 purification Methods 0.000 claims abstract description 5
- 238000001704 evaporation Methods 0.000 claims abstract description 4
- 238000000605 extraction Methods 0.000 claims abstract description 4
- 239000011347 resin Substances 0.000 claims abstract description 4
- 229920005989 resin Polymers 0.000 claims abstract description 4
- 238000001728 nano-filtration Methods 0.000 claims description 91
- 239000007788 liquid Substances 0.000 claims description 89
- 238000006243 chemical reaction Methods 0.000 claims description 38
- 238000001976 enzyme digestion Methods 0.000 claims description 38
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- 238000006386 neutralization reaction Methods 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 17
- 108010059892 Cellulase Proteins 0.000 claims description 15
- 229940106157 cellulase Drugs 0.000 claims description 15
- 108010059820 Polygalacturonase Proteins 0.000 claims description 14
- 229940088598 enzyme Drugs 0.000 claims description 13
- 239000012466 permeate Substances 0.000 claims description 13
- 238000010612 desalination reaction Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 238000001179 sorption measurement Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 abstract description 12
- 150000003839 salts Chemical class 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 230000002255 enzymatic effect Effects 0.000 abstract 2
- 230000007071 enzymatic hydrolysis Effects 0.000 abstract 2
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 abstract 2
- 239000000413 hydrolysate Substances 0.000 abstract 2
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 239000002131 composite material Substances 0.000 abstract 1
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 238000007865 diluting Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 46
- 229920002488 Hemicellulose Polymers 0.000 description 10
- 238000005374 membrane filtration Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 5
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 4
- 235000010980 cellulose Nutrition 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 3
- JCSJTDYCNQHPRJ-UHFFFAOYSA-N 20-hydroxyecdysone 2,3-acetonide Natural products OC1C(O)C(O)COC1OC1C(O)C(O)C(OC2C(C(O)C(O)OC2)O)OC1 JCSJTDYCNQHPRJ-UHFFFAOYSA-N 0.000 description 2
- 241000186000 Bifidobacterium Species 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 229920001131 Pulp (paper) Polymers 0.000 description 2
- SRBFZHDQGSBBOR-LECHCGJUSA-N alpha-D-xylose Chemical compound O[C@@H]1CO[C@H](O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-LECHCGJUSA-N 0.000 description 2
- JCSJTDYCNQHPRJ-FDVJSPBESA-N beta-D-Xylp-(1->4)-beta-D-Xylp-(1->4)-D-Xylp Chemical compound O[C@@H]1[C@@H](O)[C@H](O)CO[C@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O)C(O)OC2)O)OC1 JCSJTDYCNQHPRJ-FDVJSPBESA-N 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011112 process operation Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 150000003740 xylobioses Chemical group 0.000 description 2
- 229960003487 xylose Drugs 0.000 description 2
- ABKNGTPZXRUSOI-UHFFFAOYSA-N xylotriose Natural products OCC(OC1OCC(OC2OCC(O)C(O)C2O)C(O)C1O)C(O)C(O)C=O ABKNGTPZXRUSOI-UHFFFAOYSA-N 0.000 description 2
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- AYRXSINWFIIFAE-SCLMCMATSA-N Isomaltose Natural products OC[C@H]1O[C@H](OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O)[C@@H](O)[C@@H](O)[C@@H]1O AYRXSINWFIIFAE-SCLMCMATSA-N 0.000 description 1
- 235000014676 Phragmites communis Nutrition 0.000 description 1
- JVZHSOSUTPAVII-UHFFFAOYSA-N Xylotetraose Natural products OCC(OC1OCC(OC2OCC(OC3OCC(O)C(O)C3O)C(O)C2O)C(O)C1O)C(O)C(O)C=O JVZHSOSUTPAVII-UHFFFAOYSA-N 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
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- 235000013361 beverage Nutrition 0.000 description 1
- 238000002306 biochemical method Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- -1 far below 100 Chemical compound 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- DLRVVLDZNNYCBX-RTPHMHGBSA-N isomaltose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)C(O)O1 DLRVVLDZNNYCBX-RTPHMHGBSA-N 0.000 description 1
- 230000008720 membrane thickening Effects 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
- 229920001221 xylan Polymers 0.000 description 1
- 150000004823 xylans Chemical class 0.000 description 1
Landscapes
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides a method for preparing food-grade xylo-oligosaccharide from a viscose fiber squeezed alkali solution. The technology comprises the following steps: step A, membrane condensation: pre-filtering the squeezed alkali solution, which is generated during the production process of viscose fibers, to remove the large particle impurities, adding water into the filtrate to dilute the filtrate, then processing the diluted filtrate by a primary nano-filter membrane so as to obtain primary concentrate, adding water to dilute the primary concentrate, then processing the diluted primary concentrate by a secondary nano-filter membrane so as to obtain the secondary concentrate, diluting the secondary concentrate by water, then processing the diluted secondary concentrate by a ceramic membrane so as to obtain the concentrate namely the concentrate of squeezed alkali solution; step B, semi-fiber extraction: adding acid into the obtained concentrate to neutralize the alkali solution so as to obtain a semi-fiber solution; step C, enzymatic hydrolysis: adding composite enzymes into the semi-fiber solution to carry out enzymatic hydrolysis so as to obtain enzymatic hydrolysate; step D, purification: filtering the enzymatic hydrolysate by a ceramic membrane, then filtering the filtrate by a nano-filter membrane to remove the salts, decoloring the obtained concentrate by active carbon, then making the concentrate go through a resin column to carry out ion exchange so as to obtain a purified xylo-oligosaccharide solution, and finally evaporating and drying the solution so as to obtain food-grade xylo-oligosaccharide.
Description
Technical field
The present invention relates to xylo-oligosaccharide preparation field, be specifically related to a kind of with the technique 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 a kind of method that viscose fiber press lye prepares 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:
Viscose fiber press lye prepares a method for food-grade xylooligosaccharide, it is characterized in that: concrete technology step is as follows:
A, membrane concentration
The press lye that viscose fiber is produced is first through pre-filtering removing large granular impurity, permeate is after thin up, enter one-level nanofiltration membrane treatment, secondary nanofiltration membrane treatment is entered after gained primary concentration liquid thin up, enter ceramic membrane process after gained secondary concentration liquid thin up, gained concentrated solution is the concentrated solution of press lye;
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 one-level nanofiltration membrane is 200-300, and the molecular weight cut-off of secondary nanofiltration membrane is 300-400, and ceramic membrane interception molecular weight is 800-1500.
The molecular weight cut-off of 200-300, makes alkali separate from permeate; Slightly improve molecular weight cut-off to 300-400, progressively lower alkali dense, and allow certain half fine through, reduce because half finely blocks the nanofiltration membrane damage caused; The molecular weight cut-off of ceramic membrane is 800-1500, can retain half fibre, improve the purity of product.
Step A of the present invention, before one-level nanofiltration membrane and secondary nanofiltration membrane, the amount of thin up is 1 times of stock liquid volume, and the volume of gained concentrated solution is identical with stock liquid volume.While ensureing filtration efficiency, little to the damage of nanofiltration membrane.
Preferably, described permeate contains alkali 200-300g/l, containing half fine 40-80 g/l; Primary concentration liquid contains alkali 100-150g/l, containing half fine 40-80 g/l; Secondary concentration liquid contains alkali 50-75g/l, containing half fine 40-80g/l.Under lowering the dense prerequisite of alkali, ensure the filtration efficiency of film.
Step A of the present invention, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.While ensureing filtration efficiency, little to the damage of ceramic membrane.
Preferably, containing alkali 2-4g/l in the concentrated solution of described ceramic membrane filter, containing half fine 40-80 g/l.Be down to minimum by dense for alkali, 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, micro-filtrate membrane filtration 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 ceramic membrane filter is 60-80 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 ceramic membrane is 5-6bar.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 ceramic membrane is 200-250m
3/ h.The surface velocity that bonding props up film is higher, film is not easy contaminated.
Step A of the present invention, it is 26.8m that the list of nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic 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 ceramic membrane combination filtering and concentrating half fibre, because the filtration efficiency of nanofiltration membrane is higher than ceramic membrane, first adopts multistage nanofiltration membrane that alkali concn is progressively dropped to certain degree; Slightly improve molecular weight cut-off concentrated half fine simultaneously, allow certain half fine through, reduce the damage to film, then adopt ceramic membrane filter; The feed liquid that ceramic membrane is applicable to filter the dense height of later stage low alkali half fine is run, and is the powerful guarantee that low alkali is dense.Nanofiltration membrane and ceramic membrane 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.
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; Ceramic membrane filter, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.This technique can realize nanofiltration membrane water 10m excessively per hour
3left and right, ceramic membrane is per hour crosses water 45m
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
Viscose fiber press lye prepares a method for food-grade xylooligosaccharide, and concrete technology step is as follows:
A, membrane concentration
The press lye that viscose fiber is produced is first through pre-filtering removing large granular impurity, permeate is after thin up, enter one-level nanofiltration membrane treatment, secondary nanofiltration membrane treatment is entered after gained primary concentration liquid thin up, enter ceramic membrane process after gained secondary concentration liquid thin up, gained concentrated solution is the concentrated solution of press lye;
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
The present embodiment is substantially the same manner as Example 1, on this basis:
Described step A, the molecular weight cut-off of one-level nanofiltration membrane is 200, and the molecular weight cut-off of secondary nanofiltration membrane is 300, and ceramic membrane interception molecular weight is 800.
Embodiment 3
The present embodiment is substantially the same manner as Example 1, on this basis:
Described step A, the molecular weight cut-off of one-level nanofiltration membrane is 300, and the molecular weight cut-off of secondary nanofiltration membrane is 400, and ceramic membrane interception molecular weight is 1500.
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 one-level nanofiltration membrane is 250, and the molecular weight cut-off of secondary nanofiltration membrane is 350, and ceramic membrane interception molecular weight is 1000.
Embodiment 5
The present embodiment is substantially the same manner as Example 2, on this basis:
Described step A, before one-level nanofiltration membrane and secondary nanofiltration membrane, the amount of thin up is respectively 1 times of stock liquid volume, and the volume of gained concentrated solution is identical with stock liquid volume respectively.
Described step A, permeate contains alkali 200g/l, containing half fine 40g/l; Primary concentration liquid contains alkali 100g/l, containing half fine 40g/l; Secondary concentration liquid contains alkali 50g/l, containing half fine 40g/l.
Embodiment 6
The present embodiment is substantially the same manner as Example 3, on this basis:
Described step A, before one-level nanofiltration membrane and secondary nanofiltration membrane, the amount of thin up is respectively 1 times of stock liquid volume, and the volume of gained concentrated solution is identical with stock liquid volume respectively.
Described step A, permeate contains alkali 300g/l, containing half fine 80 g/l; Primary concentration liquid contains alkali 150g/l, containing half fine 80 g/l; Secondary concentration liquid contains alkali 75g/l, containing half fine 80g/l.
Embodiment 7
The present embodiment is substantially the same manner as Example 4, on this basis:
Described step A, before one-level nanofiltration membrane and secondary nanofiltration membrane, the amount of thin up is respectively 1 times of stock liquid volume, and the volume of gained concentrated solution is identical with stock liquid volume respectively.
Described step A, permeate contains alkali 280g/l, containing half fine 70g/l; Primary concentration liquid contains alkali 140g/l, containing half fine 70g/l; Secondary concentration liquid contains alkali 70g/l, containing half fine 70g/l.
Embodiment 8
The present embodiment is substantially the same manner as Example 5, on this basis:
The ceramic membrane filter of described step A, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
Described step A, containing alkali 2g/l in the concentrated solution of ceramic membrane filter, containing half fine 40g/l.
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and micro-filtrate membrane filtration removing large granular impurity.
Embodiment 9
The present embodiment is substantially the same manner as Example 7, on this basis:
The ceramic membrane filter of described step A, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
Described step A, containing alkali 4g/l in the concentrated solution of ceramic membrane filter, containing half fine 80 g/l.
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and micro-filtrate membrane filtration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 40-60 DEG C, and the temperature of ceramic membrane filter is 60-80 DEG C.
Embodiment 10
The present embodiment is substantially the same manner as Example 6, on this basis:
The ceramic membrane filter of described step A, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
Described step A, containing alkali 3g/l in the concentrated solution of ceramic membrane filter, containing half fine 60g/l.
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and micro-filtrate membrane filtration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 40 DEG C, and the temperature of ceramic membrane filter is 60 DEG C.
Embodiment 11
The present embodiment is substantially the same manner as Example 6, on this basis:
The ceramic membrane filter of described step A, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
Described step A, containing alkali 2.5g/l in the concentrated solution of ceramic membrane filter, containing half fine 55g/l.
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and micro-filtrate membrane filtration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 60 DEG C, and the temperature of ceramic membrane filter is 80 DEG C.
Described step A, the mistake mould difference of nanofiltration membrane is 4bar, and the mistake mould difference of ceramic membrane is 6bar.
Embodiment 12
The present embodiment is substantially the same manner as Example 5, on this basis:
The ceramic membrane filter of described step A, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
Described step A, containing alkali 3.5g/l in the concentrated solution of ceramic membrane filter, containing half fine 45 g/l.
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and micro-filtrate membrane filtration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 50 DEG C, and the temperature of ceramic membrane filter is 70 DEG C.
Described step A, the mistake mould difference of nanofiltration membrane is 3bar, and the mistake mould difference of ceramic membrane is 5bar.
Described step A, the flow of feed liquid in nanofiltration membrane is 25m
3/ h, the flow in ceramic membrane is 200m
3/ h.
Embodiment 13
The present embodiment is substantially the same manner as Example 5, on this basis:
The ceramic membrane filter of described step A, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
Described step A, containing alkali 3.7g/l in the concentrated solution of ceramic membrane filter, containing half fine 65g/l.
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and micro-filtrate membrane filtration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 45 DEG C, and the temperature of ceramic membrane filter is 65 DEG C.
Described step A, the mistake mould difference of nanofiltration membrane is 3.2bar, and the mistake mould difference of ceramic membrane is 5.2bar.
Described step A, the flow of feed liquid in nanofiltration membrane is 40m
3/ h, the flow in ceramic membrane is 250m
3/ h.
Described step A, it is 26.8m that the list of nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Embodiment 14
The present embodiment is substantially the same manner as Example 5, on this basis:
The ceramic membrane filter of described step A, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
Described step A, containing alkali 3.2g/l in the concentrated solution of ceramic membrane filter, containing half fine 75g/l.
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and micro-filtrate membrane filtration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 55 DEG C, and the temperature of ceramic membrane filter is 75 DEG C.
Described step A, the mistake mould difference of nanofiltration membrane is 3.5bar, and the mistake mould difference of ceramic membrane is 5.2bar.
Described step A, the flow of feed liquid in nanofiltration membrane is 30m
3/ h, the flow in ceramic membrane is 220m
3/ h.
Described step A, it is 26.8m that the list of nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Embodiment 15
The present embodiment is substantially the same manner as Example 4, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.
Embodiment 16
The present embodiment is substantially the same manner as Example 5, 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 17
The present embodiment is substantially the same manner as Example 6, 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 18
The present embodiment is substantially the same manner as Example 7, 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 19
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 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 20
The present embodiment is substantially the same manner as Example 13, 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 21
The present embodiment is substantially the same manner as Example 14, 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 22
The present embodiment is substantially the same manner as Example 14, 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 23
The present embodiment is substantially the same manner as Example 14, 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 24
The present embodiment is substantially the same manner as Example 14, 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 25
The present embodiment is substantially the same manner as Example 14, 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 26
The present embodiment is substantially the same manner as Example 14, 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 (21)
1. viscose fiber press lye prepares a method for food-grade xylooligosaccharide, it is characterized in that: concrete technology step is as follows:
A, membrane concentration
The press lye that viscose fiber is produced is first through pre-filtering removing large granular impurity, permeate is after thin up, enter one-level nanofiltration membrane treatment, secondary nanofiltration membrane treatment is entered after gained primary concentration liquid thin up, enter ceramic membrane process after gained secondary concentration liquid thin up, gained concentrated solution is the concentrated solution of press lye;
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. a kind of viscose fiber press lye according to claim 1 prepares the method for food-grade xylooligosaccharide, it is characterized in that: described step A, the molecular weight cut-off of one-level nanofiltration membrane is 200-300, the molecular weight cut-off of secondary nanofiltration membrane is 300-400, and ceramic membrane interception molecular weight is 800-1500.
3. a kind of viscose fiber press lye according to claim 1 prepares the method for food-grade xylooligosaccharide, it is characterized in that: described step A, before one-level nanofiltration membrane and secondary nanofiltration membrane, the amount of thin up is 1 times of stock liquid volume, and the volume of gained concentrated solution is identical with stock liquid volume.
4. a kind of viscose fiber press lye according to claim 3 prepares the method for food-grade xylooligosaccharide, it is characterized in that: described permeate contains alkali 200-300g/l, containing half fine 40-80 g/l; Primary concentration liquid contains alkali 100-150g/l, containing half fine 40-80 g/l; Secondary concentration liquid contains alkali 50-75g/l, containing half fine 40-80g/l.
5. a kind of viscose fiber press lye according to claim 1 prepares the method for food-grade xylooligosaccharide, it is characterized in that: described step A, feed liquid first enters ceramic membrane device through thin up, add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
6. a kind of viscose fiber press lye according to claim 5 prepares the method for food-grade xylooligosaccharide, it is characterized in that: containing alkali 2-4g/l in the concentrated solution of described ceramic membrane filter, containing half fine 40-80 g/l.
7. a kind of viscose fiber press lye according to claim 1 prepares the method for food-grade xylooligosaccharide, it is characterized in that: described step A, and the temperature of nanofiltration membrane is 40-60 DEG C, and the temperature of ceramic membrane filter is 60-80 DEG C.
8. a kind of viscose fiber press lye according to claim 1 prepares the method for food-grade xylooligosaccharide, it is characterized in that: described step A, and the mistake mould difference of nanofiltration membrane is 3-4bar, and the mistake mould difference of ceramic membrane is 5-6bar.
9. a kind of viscose fiber press lye according to claim 1 prepares the method for food-grade xylooligosaccharide, it is characterized in that: described step A, and the flow of feed liquid in nanofiltration membrane is 25-40m
3/ h, the flow in ceramic membrane is 200-250m
3/ h.
10. a kind of viscose fiber press lye according to claim 1 prepares the method for food-grade xylooligosaccharide, it is characterized in that: described step A, and it is 26.8m that the list of nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
11. a kind of viscose fiber press lyes according to claim 1 prepare the method for 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.
12. a kind of viscose fiber press lyes according to claim 1 prepare the method for food-grade xylooligosaccharide, and it is characterized in that: described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
13. a kind of viscose fiber press lyes according to claim 12 prepare the method for 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.
14. a kind of viscose fiber press lyes according to claim 12 prepare the method for food-grade xylooligosaccharide, it is characterized in that: the enzyme concentration of described enzyme digestion reaction is 0.5-1.5%.
15. a kind of viscose fiber press lyes according to claim 1 prepare the method for food-grade xylooligosaccharide, it is characterized in that: described D step, and the molecular weight cut-off of ceramic membrane is 800-1500.
16. a kind of viscose fiber press lyes according to claim 1 prepare the method for food-grade xylooligosaccharide, it is characterized in that: described D step, and the molecular weight cut-off of nanofiltration membrane is 100-200.
17. a kind of viscose fiber press lyes according to claim 16 prepare the method for 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.
18. a kind of viscose fiber press lyes according to claim 1 prepare the method for 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.
19. a kind of viscose fiber press lyes according to claim 1 prepare the method for 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.
20. a kind of viscose fiber press lyes according to claim 19 prepare the method for food-grade xylooligosaccharide, and it is characterized in that: described gac is LY-T-ac gac, consumption is 3-5%.
21. a kind of viscose fiber press lyes according to claim 1 prepare the method for 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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Cited By (4)
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| CN105420313A (en) * | 2015-12-15 | 2016-03-23 | 宜宾雅泰生物科技有限公司 | Method for preparing feed-grade xylo-oligosaccharide through viscose squeezed alkali liquid |
| CN105420312A (en) * | 2015-12-15 | 2016-03-23 | 宜宾雅泰生物科技有限公司 | Method for preparing food-grade xylo-oligosaccharide through viscose squeezed alkali liquid |
| CN105420292A (en) * | 2015-12-15 | 2016-03-23 | 宜宾雅泰生物科技有限公司 | Method for preparing xylitol through viscose squeezed alkali liquid |
| CN107628712A (en) * | 2017-11-10 | 2018-01-26 | 哈尔滨美森食品制造有限公司 | A kind of purifying treatment method of hickory nut waste water |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420313A (en) * | 2015-12-15 | 2016-03-23 | 宜宾雅泰生物科技有限公司 | Method for preparing feed-grade xylo-oligosaccharide through viscose squeezed alkali liquid |
| CN105420312A (en) * | 2015-12-15 | 2016-03-23 | 宜宾雅泰生物科技有限公司 | Method for preparing food-grade xylo-oligosaccharide through viscose squeezed alkali liquid |
| CN105420292A (en) * | 2015-12-15 | 2016-03-23 | 宜宾雅泰生物科技有限公司 | Method for preparing xylitol through viscose squeezed alkali liquid |
| CN107628712A (en) * | 2017-11-10 | 2018-01-26 | 哈尔滨美森食品制造有限公司 | A kind of purifying treatment method of hickory nut waste water |
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