CN104357493A - Method for preparing xylitol from viscose fiber squeezed alkali liquor - Google Patents
Method for preparing xylitol from viscose fiber squeezed alkali liquor Download PDFInfo
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- CN104357493A CN104357493A CN201410622094.6A CN201410622094A CN104357493A CN 104357493 A CN104357493 A CN 104357493A CN 201410622094 A CN201410622094 A CN 201410622094A CN 104357493 A CN104357493 A CN 104357493A
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- xylitol
- viscose fiber
- membrane
- nanofiltration membrane
- concentrated solution
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- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 title claims abstract description 71
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 239000000811 xylitol Substances 0.000 title claims abstract description 71
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 title claims abstract description 71
- 229960002675 xylitol Drugs 0.000 title claims abstract description 71
- 235000010447 xylitol Nutrition 0.000 title claims abstract description 71
- 239000003513 alkali Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000000835 fiber Substances 0.000 title claims abstract description 46
- 229920000297 Rayon Polymers 0.000 title claims abstract description 41
- 239000012528 membrane Substances 0.000 claims abstract description 185
- 239000007788 liquid Substances 0.000 claims abstract description 110
- 238000001728 nano-filtration Methods 0.000 claims abstract description 96
- 239000000919 ceramic Substances 0.000 claims abstract description 69
- 238000001914 filtration Methods 0.000 claims abstract description 56
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000012535 impurity Substances 0.000 claims abstract description 24
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012466 permeate Substances 0.000 claims abstract description 20
- 108090000790 Enzymes Proteins 0.000 claims abstract description 18
- 102000004190 Enzymes Human genes 0.000 claims abstract description 18
- 238000000855 fermentation Methods 0.000 claims abstract description 17
- 230000004151 fermentation Effects 0.000 claims abstract description 17
- 239000012141 concentrate Substances 0.000 claims abstract description 15
- 238000005342 ion exchange Methods 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000001976 enzyme digestion Methods 0.000 claims description 40
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- 238000006386 neutralization reaction Methods 0.000 claims description 35
- 229940088598 enzyme Drugs 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 17
- 241000222122 Candida albicans Species 0.000 claims description 15
- 206010007134 Candida infections Diseases 0.000 claims description 15
- 108010059892 Cellulase Proteins 0.000 claims description 15
- 201000003984 candidiasis Diseases 0.000 claims description 15
- 229940106157 cellulase Drugs 0.000 claims description 15
- 108010059820 Polygalacturonase Proteins 0.000 claims description 14
- 229960003487 xylose Drugs 0.000 claims description 13
- 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 claims description 12
- 238000010612 desalination reaction Methods 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- -1 through ion-exchange Chemical compound 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 5
- 229920002488 Hemicellulose Polymers 0.000 abstract description 19
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 241000222120 Candida <Saccharomycetales> Species 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000011033 desalting Methods 0.000 abstract 1
- 238000007380 fibre production Methods 0.000 abstract 1
- 239000008187 granular material Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 64
- 238000005374 membrane filtration Methods 0.000 description 9
- 150000003839 salts Chemical class 0.000 description 9
- 239000000706 filtrate Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 4
- 235000010980 cellulose Nutrition 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229920001131 Pulp (paper) Polymers 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 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
- 239000002994 raw material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 235000014676 Phragmites communis Nutrition 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 238000001354 calcination Methods 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
- 230000000295 complement effect Effects 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
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003792 electrolyte Substances 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
- 239000008103 glucose Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000002440 hepatic effect Effects 0.000 description 1
- 208000006454 hepatitis Diseases 0.000 description 1
- 231100000283 hepatitis Toxicity 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 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
- 210000002381 plasma Anatomy 0.000 description 1
- 238000004094 preconcentration Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
- C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
- C12P7/18—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic polyhydric
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- Organic Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Biotechnology (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention provides a method for preparing xylitol from viscose fiber squeezed alkali liquor. The method comprises the following specific process steps: (A) carrying out membrane concentration: firstly pre-filtering squeezed alkali liquor for viscose fiber production, so as to remove large-granule impurities, thinning up the permeate with water, then, enabling the thinned permeate to enter a first-stage nano-filtration membrane for treatment, thinning up the obtained first-stage concentrate with water, then, enabling the thinned first-stage concentrate to enter a second-stage nano-filtration membrane for treatment, thinning up the obtained second-stage concentrate with water, and then, enabling the thinned second-stage concentrate to enter a ceramic membrane for treatment, so as to obtain a concentrate, namely the concentrate of the squeezed alkali liquor; (B) extracting hemicellulose: adding acid to neutralize the concentrate of the squeezed alkali liquor, so as to obtain hemicellulose liquid; (C) carrying out enzymolysis: adding a compound enzyme into the hemicellulose liquid, and carrying out enzymolysis reaction, so as to obtain an enzymolysis solution; (D) fermenting: fermenting the enzymolysis solution for 0.5-2 hours at the temperature of 50-60 DEG C in the presence of candida; (E) purifying: carrying out ultrafiltration on fermentation liquor, so as to remove impurities, desalting the permeate with the nano-filtration membrane, so as to obtain a concentrate, namely a purified solution of xylitol, and carrying out ion exchange, activated carbon treatment, concentrated crystallization and separation, thereby obtaining xylitol.
Description
Technical field
The present invention relates to Xylitol 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
The sugariness of Xylitol is equivalent to sucrose, and heat is equivalent to glucose, and Xylitol can adjust glycometabolic exception, is nutrition agent and the therapeutical agent of diabetics.Xylitol has stronger anti-ketoboidies effect, can in order to rescue ketoboidies patient.Xylitol can slow down and produce the speed of lipid acid in blood plasma, but blood sugar can not be made to increase, and is also the hepatic of hepatitis patient.Xylitol Heat stability is good, heats and does not produce chemical reaction together with amino acid, can prepare various preparation, as nutrient drug with amino acid.Xylitol also has special preventing decayed tooth function as food.But Xylitol is one of polyvalent alcohol of price, production cost is too high is the major obstacle promoting its application.Annual agroforestry are produced and all can be produced a large amount of waste material containing hemicellulose (about 20% ~ 40%).The xylose utilizing hydrolysis of hemicellulose to obtain produces Xylitol, not only has good economic benefit, also has important environment protection significance.
With 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.
201210104647.X, the patent of invention that name is called " a kind of utilize in production process of viscose fiber the method for squeezing waste lye and preparing wood sugar ".By membrane filtration prepare hemicellulose solution, the extraction of hemicellulose, hemicellulose hydrolysis, in depickling, pre-concentration, decolouring, ion-exchange and Conventional concentration, crystallization, be separated, drying process obtains wood sugar finished product.This patent adopts industrial alcohol to extract hemicellulose, and cost is high.
Summary of the invention
For above-mentioned technical problem, the invention provides a kind of method that viscose fiber press lye prepares Xylitol.The Xylitol 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 Xylitol, 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, fermentation
Enzymolysis solution at the effect bottom fermentation of candidiasis, 50-60 DEG C of bottom fermentation 0.5-2h;
E, purification
Fermented liquid is through ultrafiltration removal of impurities, and permeate, through nanofiltration membrane desalination, obtains the refined solution that concentrated solution is Xylitol, through ion-exchange, activated carbon treatment, condensing crystal, separation, obtains Xylitol.
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, the salinity in half fine liquid is just low, and can not affect the activity of enzyme, the purity of the finished product Xylitol is high; The concentration of half fibre is high, ensure that the yield of the finished product Xylitol.
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 amount adding candidiasis is 0.5-1%, improves the enzymolysis efficiency of enzyme.
Add wood sugar in the enzymolysis solution of D step of the present invention, add-on is 1-1.5%, can improve the transformation efficiency of wood sugar, make maximize conversion.
E step of the present invention, the aperture of described ultra-filtration membrane is 0.001-0.005 micron, the Xylitol liquid in separate fermentation liquid and enzyme.
Preferably, described enzymolysis solution is 60-80m by the flow of ultra-filtration membrane
3/ h, temperature is 30-40 DEG C, and crossing mould difference is 2-3bar.
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, xylitol molecules amount is greater than 100.Effectively can realize being separated of salt and Xylitol.
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 Xylitol.
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 Xylitol.
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 xylitol molecules amount is much larger than 100, effectively can realize being separated of salt and Xylitol.Be conducive to the desalination in later stage, further increase the purity of Xylitol.
4, fermented liquid is first used Xylitol liquid in ultra-filtration and separation fermented liquid and enzyme by the present invention, ensure product purity, permeate enters nanofiltration membrane desalination again, thus have effectively achieved being separated of salt and Xylitol, the specific conductivity finally obtaining Xylitol 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 Xylitol shared by inorganic salt is only 3-6%; Specific conductivity is the electrolytical degree existed in reaction liquid, and the main electrolyte of Xylitol 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 Xylitol 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 Xylitol, 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, fermentation
Enzymolysis solution at the effect bottom fermentation of candidiasis, 50 DEG C of bottom fermentation 2h;
E, purification
Fermented liquid is through ultrafiltration removal of impurities, and permeate is through nanofiltration membrane desalination, and gained concentrated solution is the refined solution of Xylitol, through ion-exchange, activated carbon treatment, condensing crystal, separation, obtains Xylitol.
Embodiment 2
Viscose fiber press lye prepares a method for Xylitol, 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, fermentation
Enzymolysis solution at the effect bottom fermentation of candidiasis, 60 DEG C of bottom fermentation 0.5h;
E, purification
Fermented liquid is through ultrafiltration removal of impurities, and permeate is through nanofiltration membrane desalination, and gained concentrated solution is the refined solution of Xylitol, through ion-exchange, activated carbon treatment, condensing crystal, separation, obtains Xylitol.
Embodiment 3
Viscose fiber press lye prepares a method for Xylitol, 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, fermentation
Enzymolysis solution at the effect bottom fermentation of candidiasis, 55 DEG C of bottom fermentation 1h;
E, purification
Fermented liquid is through ultrafiltration removal of impurities, and permeate is through nanofiltration membrane desalination, and gained concentrated solution is the refined solution of Xylitol, through ion-exchange, activated carbon treatment, condensing crystal, separation, obtains Xylitol.
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 200, and the molecular weight cut-off of secondary nanofiltration membrane is 300, and ceramic membrane interception molecular weight is 800.
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 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 6
The present embodiment is substantially the same manner as Example 3, 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 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 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 8
The present embodiment is substantially the same manner as Example 5, 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 9
The present embodiment is substantially the same manner as Example 6, 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 10
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 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 11
The present embodiment is substantially the same manner as Example 8, 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 12
The present embodiment is substantially the same manner as Example 9, 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 13
The present embodiment is substantially the same manner as Example 9, 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 14
The present embodiment is substantially the same manner as Example 8, 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 15
The present embodiment is substantially the same manner as Example 8, 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 16
The present embodiment is substantially the same manner as Example 9, 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 17
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.
Embodiment 18
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 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 9, 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 15, 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 16, 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 amount adding candidiasis is 1%.
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 amount adding candidiasis is 0.8%.
Add wood sugar in the enzymolysis solution of described D step, add-on is 1.2%.
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 amount adding candidiasis is 0.5%.
Add wood sugar in the enzymolysis solution of described D step, add-on is 1%.
Described E step, the aperture of described ultra-filtration membrane is 0.001 micron.
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 amount adding candidiasis is 0.6%.
Add wood sugar in the enzymolysis solution of described D step, add-on is 1.5%.
Described E step, the aperture of described ultra-filtration membrane is 0.005 micron.
Enzymolysis solution is 60m by the flow of ultra-filtration membrane
3/ h, temperature is 30 DEG C, and crossing mould difference is 2bar.
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 amount adding candidiasis is 0.7%.
Add wood sugar in the enzymolysis solution of described D step, add-on is 1.3%.
Described E step, the aperture of described ultra-filtration membrane is 0.002 micron.
Enzymolysis solution is 80m by the flow of ultra-filtration membrane
3/ h, temperature is 40 DEG C, and crossing mould difference is 3bar.
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 activated carbon decolorizing of described D step refers to: adjusted to ph is 4, adds gac, at 50 DEG C, adsorb 1h.
The specific conductivity obtaining Xylitol 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 amount adding candidiasis is 0.8%.
Add wood sugar in the enzymolysis solution of described D step, add-on is 1.4%.
Described E step, the aperture of described ultra-filtration membrane is 0.003 micron.
Enzymolysis solution is 70m by the flow of ultra-filtration membrane
3/ h, temperature is 34 DEG C, and crossing mould difference is 2.5bar.
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 activated carbon decolorizing of described D step refers to: adjusted to ph is 5, adds gac, at 60 DEG C, adsorb 0.5h.
The specific conductivity obtaining Xylitol is 9000 μ s/cm, and ignition residue is 5%.
Embodiment 27
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 4.3.
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 amount adding candidiasis is 0.9%.
Add wood sugar in the enzymolysis solution of described D step, add-on is 1.1%.
Described E step, the aperture of described ultra-filtration membrane is 0.002 micron.
Enzymolysis solution is 65m by the flow of ultra-filtration membrane
3/ h, temperature is 32 DEG C, and crossing mould difference is 2.3bar.
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 activated carbon decolorizing of described D step refers to: adjusted to ph is 4.5, adds gac, at 52 DEG C, adsorb 0.6h.
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 Xylitol is 10000 μ s/cm, and ignition residue is 6%.
Embodiment 28
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 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 amount adding candidiasis is 0.5-1%.
Add wood sugar in the enzymolysis solution of described D step, add-on is 1.5%.
Described E step, the aperture of described ultra-filtration membrane is 0.005 micron.
Enzymolysis solution is 75m by the flow of ultra-filtration membrane
3/ h, temperature is 36 DEG C, and crossing mould difference is 2.6bar.
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 activated carbon decolorizing of described D step refers to: adjusted to ph is 4.5, adds gac, at 53 DEG C, adsorb 0.6h.
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 Xylitol is 8000 μ s/cm, and ignition residue is 3%.
Claims (21)
1. viscose fiber press lye prepares a method for Xylitol, 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, fermentation
Enzymolysis solution at the effect bottom fermentation of candidiasis, 50-60 DEG C of bottom fermentation 0.5-2h;
E, purification
Fermented liquid is through ultrafiltration removal of impurities, and permeate is through nanofiltration membrane desalination, and gained concentrated solution is the refined solution of Xylitol, through ion-exchange, activated carbon treatment, condensing crystal, separation, obtains Xylitol.
2. a kind of viscose fiber press lye according to claim 1 prepares the method for Xylitol, it is characterized in that: described step A, 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.
3. a kind of viscose fiber press lye according to claim 1 prepares the method for Xylitol, 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 Xylitol, 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 Xylitol, 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 Xylitol, 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 Xylitol, 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 Xylitol, 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 Xylitol, 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 Xylitol, 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 Xylitol, 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 Xylitol, 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 Xylitol, 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 Xylitol, 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 Xylitol, it is characterized in that: described D step, and the amount adding candidiasis is 0.5-1%.
16. a kind of viscose fiber press lyes according to claim 1 prepare the method for Xylitol, and it is characterized in that: add wood sugar in the enzymolysis solution of described D step, add-on is 1-1.5%.
17. a kind of viscose fiber press lyes according to claim 1 prepare the method for Xylitol, it is characterized in that: described E step, and the aperture of described ultra-filtration membrane is 0.001-0.005 micron.
18. a kind of viscose fiber press lyes according to claim 17 prepare the method for Xylitol, it is characterized in that: enzymolysis solution is 60-80m by the flow of ultra-filtration membrane
3/ h, temperature is 30-40 DEG C, and crossing mould difference is 2-3bar.
19. a kind of viscose fiber press lyes according to claim 1 prepare the method for Xylitol, it is characterized in that: described D step, and the molecular weight cut-off of nanofiltration membrane is 100-200.
20. a kind of viscose fiber press lyes according to claim 19 prepare the method for Xylitol, 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.
21. a kind of viscose fiber press lyes according to claim 1 prepare the method for Xylitol, 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.
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| CN201410622094.6A CN104357493A (en) | 2014-11-07 | 2014-11-07 | Method for preparing xylitol from viscose fiber squeezed alkali liquor |
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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 |
| 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 |
| 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 |
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| 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 |
| 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 |
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