CN104496756A - Electrodialysis technology for preparing xylitol by taking viscose fiber squeezed alkali liquid - Google Patents
Electrodialysis technology for preparing xylitol by taking viscose fiber squeezed alkali liquid Download PDFInfo
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- CN104496756A CN104496756A CN201410622134.7A CN201410622134A CN104496756A CN 104496756 A CN104496756 A CN 104496756A CN 201410622134 A CN201410622134 A CN 201410622134A CN 104496756 A CN104496756 A CN 104496756A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/132—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group
- C07C29/136—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH
- C07C29/14—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of a —CHO group
- C07C29/141—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of a —CHO group with hydrogen or hydrogen-containing gases
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
- C13K13/002—Xylose
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Abstract
A provided electrodialysis technology for preparing xylitol by taking viscose fiber squeezed alkali liquid comprises the following concrete steps: A, performing membrane concentration, namely, firstly pre-filtering the squeezed liquid produced from viscose fiber to remove large-particle impurity, processing the penetration liquid by a nanofiltration membrane for cyclic concentration for 2-4 times, sending the final time of the concentrate to an electrodialysis membrane pile, and recovering the alkali liquid in an anode chamber, so as to obtain a concentrate of the squeezed liquid, wherein before each time of the 2-4 times of cyclic concentration by using the nanofiltration membrane, the material liquid is diluted by adding water and then enters the nanofiltration membrane; B, extracting hemicelluloses, namely adding an acid into the concentrate of the squeezed liquid for neutralization, so as to obtain a hemicellulose liquid; C, hydrolyzing, namely, adding diluted sulfuric acid into the hemicellulose liquid to perform hydrolysis reaction; D, purification, namely, filtering the hydrolysis solution with a ceramic membrane, enabling the penetration solution to enter a nanofiltration membrane for desalting, and decoloring the concentrate with active carbon, so as to obtain a purification liquid of xylose; and E, introducing hydrogen into the purification liquid of xylose, so as to perform hydrogenation reaction under the catalytic effect of nickel, so as to obtain xylitol.
Description
Technical field
The present invention relates to Xylitol preparation field, the membrane concentration technique that to be specifically related to viscose fiber pressed liquor be raw material production Xylitol.
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 with viscose fiber press lye as the electrodialysis process of Xylitol prepared by raw material.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:
With viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: concrete technology step is as follows:
A, membrane concentration
The pressed liquor that viscose fiber is produced is first through pre-filtering removing large granular impurity, and last concentrated solution, through concentrated 2-4 time of nanofiltration membrane circulation, is sent into electrodialysis membrane stack by permeate, reclaims the alkali lye of anolyte compartment, is the concentrated solution of pressed liquor; Concentrated 2-4 time of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up.
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid.
C, hydrolysis
In half fine liquid, add dilute sulphuric acid, hydrolysis reaction occurs;
D, purifying
Hydrolyzed solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and concentrated solution, through activated carbon decolorizing, obtains the refined solution of wood sugar;
E, hydrogenation
Pass into hydrogen in the refined solution of wood sugar, hydrogenation occurs in the katalysis of nickel, obtains Xylitol.
Step A of the present invention, the molecular weight cut-off of nanofiltration membrane is 200-400, and alkali is separated from permeate, progressively lowers alkali dense, promotes half fine concentration.
Step A of the present invention, before each nanofiltration membrane, the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume.While ensureing filtration efficiency, little to the damage of nanofiltration membrane.
Preferably, described permeate, containing alkali 200-300g/l, containing half fine 40-80 g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 12-75g/l, containing half fine 40-80g/l; Containing alkali 2-4g/l in the alkali lye of described anolyte compartment, containing half fine 40-80 g/l.Under lowering the dense prerequisite of alkali, ensure the filtration efficiency of film; Be down to minimum by dense for alkali simultaneously, ensure that the purity of half fibre.
Pre-filtering of the present invention refers to, press lye is successively through rotary drum filtration, Plate Filtration and millipore 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 electrodialytic temperature is 15-45 DEG C, and filtration temperature is high, and liquid viscosity is lower, is conducive to filtration efficiency and improves.
Step A of the present invention, the mistake mould difference of nanofiltration membrane is 3-4bar, and electrodialytic mould difference is excessively 0.3-0.8bar.For the feature that viscose glue press lye viscosity is higher, adopt higher pressure reduction to filter, can ensure that half fine concentration in alkali lye reaches processing requirement.
Step A of the present invention, the flow of feed liquid in nanofiltration membrane is 25-40m
3/ h, the flow in electrodialysis process is 5m
3/ h.The surface velocity that bonding props up film is higher, film is not easy contaminated; Ensure the duration of contact of feed liquid and electrodialytic membranes, thus half fibre can be fully separated with alkali.
Step A of the present invention, electrodialysis impressed DC voltage, magnitude of voltage is 220V, and current value is 10A, and current density is little, realizes the maximization of current efficiency.
Step B of the present invention, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.The advantage adding hydrochloric acid is that the molecules of salt amount formed is lower, is conducive to the desalination in later stage.
Step C of the present invention, the concentration of dilute sulphuric acid is 12%, makes pH value be 0.Wood sugar is fully hydrolyzed under this sour condition.
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 wood sugar molecular weight is much larger than 100, effectively can realize being separated of salt and wood sugar.
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 wood sugar.
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 wood sugar.
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.
Beneficial effect of the present invention is:
1, the present invention adopts nanofiltration membrane and electrodialysis membrane stack combination filtering and concentrating half fibre, because the running cost of nanofiltration membrane is lower than electrodialysis, nanofiltration membrane is first adopted repeatedly progressively to drop to certain degree dense for alkali, concentrated half fibre, little to the damage of film, re-use electrodialysis fine to improve concentrated solution half, reduce alkali dense, thus reduce whole production cost and enhance productivity.Nanofiltration and electrodialysis cooperatively interact, and have complementary advantages, and make containing alkali 2-4g/l in final concentrated solution, containing half fine 40-80 g/l, achieve low alkali dense, height half is fine; And process operation efficiency is high, little to the damage of film, cost is low, is adapted to industrialization scale operation.
2, the amount of nanofiltration membrane thin up of the present invention is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn, can realize nanofiltration membrane water 10m excessively per hour
3left and right, ensure that filtration efficiency; Meanwhile, little to the damage of film, the 2-3 that can reach its quality guarantee period work-ing life doubly, reduces cost to a great extent, is adapted to industrialization scale operation.
3, the present invention adds hydrochloric acid neutralization to the concentrated solution obtained, then adopts molecular weight cut-off to be the nanofiltration membrane desalination of 100-200.In hydrochloric acid and the salt generated be sodium-chlor, the molecular weight of sodium-chlor, far below 100, and wood sugar molecular weight is much larger than 100, effectively can realize being separated of salt and wood sugar.Be conducive to the desalination in later stage, further increase the purity of wood sugar.
4, hydrolyzed solution is entered nanofiltration membrane desalination by the present invention, thus have effectively achieved being separated of salt and wood sugar, ensure that the purity of wood sugar, after wood sugar hydrogenation, be converted into 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
With viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, concrete technology step is as follows:
A, membrane concentration
The pressed liquor that viscose fiber is produced is first through pre-filtering removing large granular impurity, and last concentrated solution, through concentrated 2 times of nanofiltration membrane circulation, is sent into electrodialysis membrane stack by permeate, reclaims the alkali lye of anolyte compartment, is the concentrated solution of pressed liquor; Concentrated 2 times of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up;
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid.
C, hydrolysis
In half fine liquid, add dilute sulphuric acid, hydrolysis reaction occurs;
D, purifying
Hydrolyzed solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and concentrated solution, through activated carbon decolorizing, obtains the refined solution of wood sugar;
E, hydrogenation
Pass into hydrogen in the refined solution of wood sugar, hydrogenation occurs in the katalysis of nickel, obtains Xylitol.
Embodiment 2
With viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, concrete technology step is as follows:
A, membrane concentration
The pressed liquor that viscose fiber is produced is first through pre-filtering removing large granular impurity, and last concentrated solution, through concentrated 3 times of nanofiltration membrane circulation, is sent into electrodialysis membrane stack by permeate, reclaims the alkali lye of anolyte compartment, is the concentrated solution of pressed liquor; Concentrated 3 times of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up;
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid.
C, hydrolysis
In half fine liquid, add dilute sulphuric acid, hydrolysis reaction occurs;
D, purifying
Hydrolyzed solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and concentrated solution, through activated carbon decolorizing, obtains the refined solution of wood sugar;
E, hydrogenation
Pass into hydrogen in the refined solution of wood sugar, hydrogenation occurs in the katalysis of nickel, obtains Xylitol.
Embodiment 3
With viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, concrete technology step is as follows:
A, membrane concentration
The pressed liquor that viscose fiber is produced is first through pre-filtering removing large granular impurity, and last concentrated solution, through concentrated 4 times of nanofiltration membrane circulation, is sent into electrodialysis membrane stack by permeate, reclaims the alkali lye of anolyte compartment, is the concentrated solution of pressed liquor; Concentrated 4 times of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up;
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid.
C, hydrolysis
In half fine liquid, add dilute sulphuric acid, hydrolysis reaction occurs;
D, purifying
Hydrolyzed solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and concentrated solution, through activated carbon decolorizing, obtains the refined solution of wood sugar;
E, hydrogenation
Pass into hydrogen in the refined solution of wood sugar, hydrogenation occurs in the katalysis of nickel, 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 nanofiltration membrane is 200.
The nanofiltration membrane circulation of described step A is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
Embodiment 5
The present embodiment is substantially the same manner as Example 2, on this basis:
Described step A, the molecular weight cut-off of nanofiltration membrane is 400.
The nanofiltration membrane circulation of described step A is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
Embodiment 6
The present embodiment is substantially the same manner as Example 3, on this basis:
Described step A, the molecular weight cut-off of nanofiltration membrane is 300.
The nanofiltration membrane circulation of described step A is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
Embodiment 7
The present embodiment is substantially the same manner as Example 1, on this basis:
Described step A, the molecular weight cut-off of nanofiltration membrane is 250.
The nanofiltration membrane circulation of described step A is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
Embodiment 8
The present embodiment is substantially the same manner as Example 4, on this basis:
Described step A, permeate, containing alkali 300g/l, containing half fine 80g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 75g/l, containing half fine 80g/l; Containing alkali 4g/l in the alkali lye of described anolyte compartment, containing half fine 80 g/l.
Embodiment 9
The present embodiment is substantially the same manner as Example 5, on this basis:
Described step A, permeate, containing alkali 260g/l, containing half fine 70g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 32.5g/l, containing half fine 80g/l; Containing alkali 3.5g/l in the alkali lye of described anolyte compartment, containing half fine 70 g/l.
Embodiment 10
The present embodiment is substantially the same manner as Example 6, on this basis:
Described step A, permeate, containing alkali 200g/l, containing half fine 40g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 12.5g/l, containing half fine 40g/l; Containing alkali 2g/l in the alkali lye of described anolyte compartment, containing half fine 40g/l.
Embodiment 11
The present embodiment is substantially the same manner as Example 7, on this basis:
Described step A, permeate, containing alkali 220g/l, containing half fine 60g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 55g/l, containing half fine 60g/l; Containing alkali 3g/l in the alkali lye of described anolyte compartment, containing half fine 60g/l.
Embodiment 12
The present embodiment is substantially the same manner as Example 8, on this basis:
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and millipore filtration removing large granular impurity.
Embodiment 13
The present embodiment is substantially the same manner as Example 9, on this basis:
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and millipore filtration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 40 DEG C, and electrodialytic temperature is 15 DEG C.
Embodiment 14
The present embodiment is substantially the same manner as Example 10, on this basis:
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and millipore filtration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 60 DEG C, and electrodialytic temperature is 45 DEG C.
Described step A, the mistake mould difference of nanofiltration membrane is 4bar, and electrodialytic mould difference is excessively 0.8bar.
Embodiment 15
The present embodiment is substantially the same manner as Example 11, on this basis:
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and millipore filtration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 45 DEG C, and electrodialytic temperature is 20 DEG C.
Described step A, the mistake mould difference of nanofiltration membrane is 3bar, and electrodialytic mould difference is excessively 0.3bar.
Described step A, the flow of feed liquid in nanofiltration membrane is 25m
3/ h, the flow in electrodialysis process is 5m
3/ h.
Embodiment 16
The present embodiment is substantially the same manner as Example 11, on this basis:
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and millipore filtration removing large granular impurity.
Described step A, the temperature of nanofiltration membrane is 55 DEG C, and electrodialytic temperature is 30 DEG C.
Described step A, the mistake mould difference of nanofiltration membrane is 3.6bar, and electrodialytic mould difference is excessively 0.5bar.
Described step A, the flow of feed liquid in nanofiltration membrane is 40m
3/ h, the flow in electrodialysis process is 5m
3/ h.
Described step A, it is 26.8m that the list of nanofiltration membrane props up filtration area
2.
Described step A, electrodialysis impressed DC voltage, magnitude of voltage is 220V, and current value is 10A.
Embodiment 17
The present embodiment is substantially the same manner as Example 8, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Embodiment 18
The present embodiment is substantially the same manner as Example 9, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described step C, the concentration of dilute sulphuric acid is 12%, makes pH value be 0.
Embodiment 19
The present embodiment is substantially the same manner as Example 10, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described step C, the concentration of dilute sulphuric acid is 12%, makes pH value be 0.
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 11, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described step C, the concentration of dilute sulphuric acid is 12%, makes pH value be 0.
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 15, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described step C, the concentration of dilute sulphuric acid is 12%, makes pH value be 0.
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 16, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described step C, the concentration of dilute sulphuric acid is 12%, makes pH value be 0.
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 16, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described step C, the concentration of dilute sulphuric acid is 12%, makes pH value be 0.
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 Xylitol is 8500 μ s/cm, and ignition residue is 4%.
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.
Described step C, the concentration of dilute sulphuric acid is 12%, makes pH value be 0.
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 Xylitol is 9000 μ s/cm, and ignition residue is 5%.
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.
Described step C, the concentration of dilute sulphuric acid is 12%, makes pH value be 0.
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 specific conductivity obtaining Xylitol is 10000 μ s/cm, and ignition residue is 6%.
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.
Described step C, the concentration of dilute sulphuric acid is 12%, makes pH value be 0.
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 specific conductivity obtaining Xylitol is 8000 μ s/cm, and ignition residue is 3%.
Claims (15)
1. with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: concrete technology step is as follows:
A, membrane concentration
The pressed liquor that viscose fiber is produced is first through pre-filtering removing large granular impurity, and last concentrated solution, through concentrated 2-4 time of nanofiltration membrane circulation, is sent into electrodialysis membrane stack by permeate, reclaims the alkali lye of anolyte compartment, is the concentrated solution of pressed liquor; Concentrated 2-4 time of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up;
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid;
C, hydrolysis
In half fine liquid, add dilute sulphuric acid, hydrolysis reaction occurs;
D, purifying
Hydrolyzed solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and concentrated solution, through activated carbon decolorizing, obtains the refined solution of wood sugar;
E, hydrogenation
Pass into hydrogen in the refined solution of wood sugar, hydrogenation occurs in the katalysis of nickel, obtains Xylitol.
2. according to claim 1 with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: described step A, the molecular weight cut-off of nanofiltration membrane is 200-400.
3. according to claim 1 with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: described step A, before each nanofiltration membrane, the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume.
4. according to claim 3 with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: described permeate containing alkali 200-300g/l, containing half fine 40-80 g/l; Containing alkali 2-4g/l in the alkali lye of described anolyte compartment, containing half fine 40-80 g/l.
5. according to claim 1 with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: described step A, the temperature of nanofiltration membrane treatment is 40-60 DEG C, and electrodialytic temperature is 15-45 DEG C.
6. according to claim 1 with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: described step A, the mistake mould difference of nanofiltration membrane is 3-4bar, and electrodialytic to cross mould difference be 0.3-0.8bar.
7. according to claim 1 with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: described step A, the flow of feed liquid in nanofiltration membrane is 25-40m
3/ h, the flow in electrodialysis process is 5m
3/ h.
8. according to claim 1 with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: described step A, electrodialysis impressed DC voltage, magnitude of voltage is 220V, and current value is 10A.
9. according to claim 1 with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: described step B, concentrated solution acid neutralization, refer to and add hydrochloric acid neutralization.
10. according to claim 1 with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: described step C, the concentration of dilute sulphuric acid is 12%, makes pH value be 0.
11. according to claim 1 with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: described D step, the molecular weight cut-off of nanofiltration membrane is 100-200.
12. according to claim 11 with viscose fiber pressed liquor with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: the mistake mould difference of described nanofiltration membrane is 3-4bar, temperature is 30-40 DEG C, and single filtration area is 26.8 m
2.
13. according to claim 1 with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: described D step, the material liquid volume before nanofiltration membrane concentrates be the 10-15 of concentrated solution volume doubly.
14. according to claim 1 with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, 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.
15. according to claim 14 with viscose fiber press lye for the electrodialysis process of Xylitol prepared by raw material, it is characterized in that: described gac is LY-T-ac gac, consumption is 3-5%.
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