CN104496756B - The electrodialysis process of xylitol is prepared with viscose rayon press lye for raw material - Google Patents
The electrodialysis process of xylitol is prepared with viscose rayon press lye for raw material Download PDFInfo
- Publication number
- CN104496756B CN104496756B CN201410622134.7A CN201410622134A CN104496756B CN 104496756 B CN104496756 B CN 104496756B CN 201410622134 A CN201410622134 A CN 201410622134A CN 104496756 B CN104496756 B CN 104496756B
- Authority
- CN
- China
- Prior art keywords
- membrane
- viscose rayon
- concentrated solution
- xylitol
- raw material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides a kind of electrodialysis process preparing xylitol with viscose rayon press lye for raw material, concrete technology step is as follows: A, membrance concentration, the pressed liquor that viscose rayon produces first removes large granular impurity through pre-filtering, permeate is through NF membrane circulation concentration 2-4 time, last concentrated solution is sent into electrodialysis membrane stack, reclaim the alkali liquor of anode chamber, be the concentrated solution of pressed liquor；Described NF membrane circulation concentration 2-4 time, before filtering, feed liquid all enters NF membrane after dilute every time；B, extraction half fibre, neutralize the concentrated solution acid adding of press lye, obtains half fine liquid。C, hydrolysis, add dilute sulfuric acid in half fine liquid, hydrolysis occur；D, purification, hydrolyzed solution is through ceramic membrane filter, and permeate enters NF membrane desalination, and concentrated solution, through activated carbon decolorizing, obtains the refined solution of xylose；E, hydrogenation, pass into hydrogen in the refined solution of xylose, hydrogenation occurs in the catalytic action of nickel, obtains xylitol。
Description
Technical field
The present invention relates to xylitol preparation field, be specifically related to the membrance concentration technique being raw material production xylitol with viscose rayon pressed liquor。
Background technology
The sugariness of xylitol is equivalent to sucrose, and heat is equivalent to glucose, and xylitol can adjust glycometabolic exception, is nutrient and the therapeutic agent of diabetes patient。Xylitol has stronger anti-ketoboidies effect, may be used to rescue ketoboidies patient。Xylitol can slow down and produce the speed of fatty acid in blood plasma, but blood glucose will not be made to increase, and is also the hepatic of hepatitis patient。Xylitol Heat stability is good, heats together with aminoacid and does not produce chemical reaction, it is possible to prepare various preparations with aminoacid, as nutrient drug。Xylitol also has special preventing decayed tooth function as food。But xylitol is one of polyhydric alcohol of price, production cost is too high is the major obstacle promoting its application。Annual agriculture and forestry produce and all can produce a large amount of waste material containing hemicellulose (about 20% ~ 40%)。Utilize the xylose that hydrolysis of hemicellulose obtains to produce xylitol, not only there is good economic benefit, also have important environment protection significance。
With chemical pulp plant celluloses such as () wood pulp, cotton pulp, straw pulp, reed pulps for the production process of viscose fiber of raw material, adopting alkali liquor that cellulose processes (dipping, squeezing) is the first step manufacturing viscose rayon。Hemicellulose concentration is high, cellulose viscose manufacturing technique and end product quality are produced extremely disadvantageous impact, therefore must in impregnation technology with alkali liquor by hemicellulose dissolution, the cellulose of high intensity could be obtained, so the substantial amounts of high concentration alkali pressed liquor rich in hemicellulose can be produced in above process。
Alkali pressed liquor is mainly composed of sodium hydroxide and hemicellulose。Hemicellulose is therefrom separated by processing method many employings nanofiltration of existing press lye, obtains comparatively pure alkali liquor。Through the alkali liquor that purification can direct reuse in technique, but NF membrane is only capable of part alkali is realized reuse, the hemicellulose in its trapped fluid still contains substantial amounts of alkali in the concentrated solution that obtains after concentration。This part feed liquid is used for neutralizing technique as salkali waste at present, and hemicellulose enters wastewater treatment, or adopts calcination to reclaim sodium hydroxide, and hemicellulose is burned。From above existing technique it can be seen that hemicellulose is not fully used。
201210104647.X, name is called the patent of invention of " a kind of utilize the spent lye method of preparing xylose of squeezing in production process of viscose fiber "。By membrane filtration prepare hemicellulose solution, the extraction of hemicellulose, hemicellulose hydrolysis, neutralize deacidification, pre-concentration, decolouring, ion exchange and Conventional concentration, crystallization, separation, drying process obtain xylose 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 the electrodialysis process preparing xylitol with viscose rayon press lye for raw material。The xylitol salinity obtained is low, and purity is high, and process operation efficiency is high, is adapted to large-scale production。
For achieving the above object, the present invention adopts the following technical scheme that:
The electrodialysis process of xylitol is prepared with viscose rayon press lye for raw material, it is characterised in that: concrete technology step is as follows:
A, membrance concentration
The pressed liquor that viscose rayon produces first removes large granular impurity through pre-filtering, and last concentrated solution, through NF membrane circulation concentration 2-4 time, is sent into electrodialysis membrane stack, reclaimed the alkali liquor of anode chamber, be the concentrated solution of pressed liquor by permeate；Described NF membrane circulation concentration 2-4 time, before filtering, feed liquid all enters NF membrane after dilute every time。
B, extraction half fibre
The concentrated solution acid adding of press lye is neutralized, obtains half fine liquid。
C, hydrolysis
Half fine liquid adds dilute sulfuric acid, hydrolysis occurs；
D, purification
Hydrolyzed solution is through ceramic membrane filter, and permeate enters NF membrane desalination, and concentrated solution, through activated carbon decolorizing, obtains the refined solution of xylose；
E, hydrogenation
The refined solution of xylose passes into hydrogen, the catalytic action of nickel occurs hydrogenation, obtains xylitol。
Step A of the present invention, the molecular cut off of NF membrane is 200-400, makes alkali separate from permeate, progressively lowers alkali dense, promotes half fine concentration。
Step A of the present invention, before each nanofiltration membrane, 1 times that amount is material liquid volume of dilute, the concentrated solution volume being filtrated to get is identical with material liquid volume。While ensureing filter efficiency, the damage of NF membrane is little。
Preferably, described permeate is containing alkali 200-300g/l, containing half fine 40-80g/l, after NF membrane circulation concentration, obtains concentrated solution containing alkali 12-75g/l, containing half fine 40-80g/l；Containing alkali 2-4g/l in the alkali liquor of described anode chamber, containing half fine 40-80g/l。Lower under the premise that alkali is dense, it is ensured that the filter efficiency of film；Simultaneously by dense for alkali be down to minimum, it is ensured that half fine purity。
Pre-filtering of the present invention refers to, press lye sequentially passes through rotary drum filtration, plate-and-frame filtration and microporous filter and removes large granular impurity。Pre-filtering is to make press lye without the solid impurity of more than 5 microns, protects film below not 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 relatively low, is conducive to filter efficiency to improve。
Step A of the present invention, the mistake mould difference of NF membrane is 3-4bar, and electrodialytic mould difference of crossing is 0.3-0.8bar。For the feature that viscose glue press lye viscosity is higher, higher pressure reduction is adopted to be filtered, it is ensured that half fine concentration in alkali liquor reaches technological requirement。
Step A of the present invention, feed liquid flow in NF membrane is 25-40m3/ h, the flow in electrodialytic process is 5m3/ h。Ensure that the surface velocity of single film is higher, make film be not easy contaminated；Half fibre ensures the time of contact of feed liquid and electrodialytic membranes, so that can be sufficiently separated with alkali。
Step A of the present invention, electrodialysis impressed DC voltage, magnitude of voltage is 220V, and current value is 10A, and electric current density is little, it is achieved the maximization of current efficiency。
Step B of the present invention, concentrated solution acid adding neutralizes, and refers to addition hydrochloric acid and neutralizes。The advantage adding hydrochloric acid is that the molecules of salt amount formed is relatively low, is conducive to the desalination in later stage。
Step C of the present invention, the concentration of dilute sulfuric acid is 12%, and making pH value is 0。Xylose is fully hydrolyzed when this acid。
D step of the present invention, the molecular cut off of described NF membrane is 100-200。Owing to adopting hydrochloric acid to neutralize, the salt of generation is sodium chloride, and the molecular weight of sodium chloride is smaller, and far below 100, and xylose molecular weight is much larger than 100, it is possible to be effectively realized the separation of salt and xylose。
Preferably, described NF membrane desalination, crossing mould difference is 3-4bar, and temperature is 30-40 DEG C, and single filter area is 26.8m2, adapt to the change of low catching molecular, it is ensured that the separation of salt and xylose。
Preferably, 10-15 times that material liquid volume is concentrated solution volume before the concentration of described NF membrane, advantageously reduce the salt content in xylose。
The decolouring of D step of the present invention refers to: adjustment pH value is 4-5, adds activated carbon, adsorbs 0.5-1h at 50-60 DEG C。
Preferably, described activated carbon is LY-T-ac activated carbon, and consumption is 3-5%。The decolorizing effect of sugar liquid is best, and percent of decolourization is 70%, and the loss rate of sugar is minimum。
The beneficial effects of the present invention is:
1, the present invention adopts NF membrane and electrodialysis membrane stack combination filtering and concentrating half fine, owing to the operating cost of NF membrane is lower than electrodialysis, nanofiltration membrane is first adopted repeatedly progressively to drop to certain degree dense for alkali, concentration half is fine, the damage of film is little, re-use electrodialysis fine to improve concentrated solution half, reduce alkali dense, thus reducing the cost of whole production and improving production efficiency。Nanofiltration and electrodialysis cooperate, and have complementary advantages, make containing alkali 2-4g/l in final concentrated solution, containing half fine 40-80g/l, it is achieved that low alkali is dense, high partly fine；And process operation efficiency is high, the damage of film is little, and cost is low, is adapted to industrialization large-scale production。
2,1 times that amount is material liquid volume of the nanofiltration membrane dilute of the present invention, the concentrated solution volume being every time filtrated to get is identical with material liquid volume, it may be achieved NF membrane crosses water 10m per hour3Left and right, it is ensured that filter efficiency；Meanwhile, the damage of film is little, service life can reach 2-3 times of its quality guarantee period, largely reduces cost, is adapted to industrialization large-scale production。
3, the concentrated solution obtained is added hydrochloric acid neutralization then the NF membrane desalination adopting molecular cut off to be 100-200 by the present invention。In hydrochloric acid, the salt with generation is sodium chloride, and the molecular weight of sodium chloride, far below 100, and xylose molecular weight is much larger than 100, it is possible to be effectively realized the separation of salt and xylose。Be conducive to the desalination in later stage, further increase the purity of xylose。
4, hydrolyzed solution is entered NF membrane desalination by the present invention, thus have effectively achieved the separation of salt and xylose, it is ensured that the purity of xylose, is converted into xylitol after xylose hydrogenation, and the electrical conductivity finally giving xylitol is 8000-10000 μ s/cm, and ignition residue is 3-6%。Ignition residue is the direct indicator weighing inorganic salt, describes in xylitol the mass fraction shared by inorganic salt and is only 3-6%；Electrical conductivity is the electrolytical degree existed in reaction liquid, and the main electrolyte of xylitol is exactly inorganic salts, thus this index can also reflect salinity in product number。Low conductivity and ignition residue describe and adopt the xylitol salinity that the inventive method obtains low, high purity more than 85%。
Detailed description of the invention
Below in conjunction with detailed description of the invention, the essentiality content of the present invention is described in further detail。
Embodiment 1
Prepare the electrodialysis process of xylitol with viscose rayon press lye for raw material, concrete technology step is as follows:
A, membrance concentration
The pressed liquor that viscose rayon produces first removes large granular impurity through pre-filtering, and last concentrated solution, through NF membrane circulation concentration 2 times, is sent into electrodialysis membrane stack, reclaimed the alkali liquor of anode chamber, be the concentrated solution of pressed liquor by permeate；Described NF membrane circulation concentration 2 times, before filtering, feed liquid all enters NF membrane after dilute every time；
B, extraction half fibre
The concentrated solution acid adding of press lye is neutralized, obtains half fine liquid。
C, hydrolysis
Half fine liquid adds dilute sulfuric acid, hydrolysis occurs；
D, purification
Hydrolyzed solution is through ceramic membrane filter, and permeate enters NF membrane desalination, and concentrated solution, through activated carbon decolorizing, obtains the refined solution of xylose；
E, hydrogenation
The refined solution of xylose passes into hydrogen, the catalytic action of nickel occurs hydrogenation, obtains xylitol。
Embodiment 2
Prepare the electrodialysis process of xylitol with viscose rayon press lye for raw material, concrete technology step is as follows:
A, membrance concentration
The pressed liquor that viscose rayon produces first removes large granular impurity through pre-filtering, and last concentrated solution, through NF membrane circulation concentration 3 times, is sent into electrodialysis membrane stack, reclaimed the alkali liquor of anode chamber, be the concentrated solution of pressed liquor by permeate；Described NF membrane circulation concentration 3 times, before filtering, feed liquid all enters NF membrane after dilute every time；
B, extraction half fibre
The concentrated solution acid adding of press lye is neutralized, obtains half fine liquid。
C, hydrolysis
Half fine liquid adds dilute sulfuric acid, hydrolysis occurs；
D, purification
Hydrolyzed solution is through ceramic membrane filter, and permeate enters NF membrane desalination, and concentrated solution, through activated carbon decolorizing, obtains the refined solution of xylose；
E, hydrogenation
The refined solution of xylose passes into hydrogen, the catalytic action of nickel occurs hydrogenation, obtains xylitol。
Embodiment 3
Prepare the electrodialysis process of xylitol with viscose rayon press lye for raw material, concrete technology step is as follows:
A, membrance concentration
The pressed liquor that viscose rayon produces first removes large granular impurity through pre-filtering, and last concentrated solution, through NF membrane circulation concentration 4 times, is sent into electrodialysis membrane stack, reclaimed the alkali liquor of anode chamber, be the concentrated solution of pressed liquor by permeate；Described NF membrane circulation concentration 4 times, before filtering, feed liquid all enters NF membrane after dilute every time；
B, extraction half fibre
The concentrated solution acid adding of press lye is neutralized, obtains half fine liquid。
C, hydrolysis
Half fine liquid adds dilute sulfuric acid, hydrolysis occurs；
D, purification
Hydrolyzed solution is through ceramic membrane filter, and permeate enters NF membrane desalination, and concentrated solution, through activated carbon decolorizing, obtains the refined solution of xylose；
E, hydrogenation
The refined solution of xylose passes into hydrogen, the catalytic action of nickel occurs hydrogenation, obtains xylitol。
Embodiment 4
The present embodiment is substantially the same manner as Example 1, on this basis:
Described step A, the molecular cut off of NF membrane is 200。
The NF membrane circulation concentration of described step A, 1 times that amount is material liquid volume of dilute, the concentrated solution volume being every time filtrated to get is identical with material liquid volume。
Embodiment 5
The present embodiment is substantially the same manner as Example 2, on this basis:
Described step A, the molecular cut off of NF membrane is 400。
The NF membrane circulation concentration of described step A, 1 times that amount is material liquid volume of dilute, the concentrated solution volume being every time filtrated to get is identical with material liquid volume。
Embodiment 6
The present embodiment is substantially the same manner as Example 3, on this basis:
Described step A, the molecular cut off of NF membrane is 300。
The NF membrane circulation concentration of described step A, 1 times that amount is material liquid volume of dilute, the concentrated solution volume being every time filtrated to get is identical with material liquid volume。
Embodiment 7
The present embodiment is substantially the same manner as Example 1, on this basis:
Described step A, the molecular cut off of NF membrane is 250。
The NF membrane circulation concentration of described step A, 1 times that amount is material liquid volume of dilute, the concentrated solution volume being every time filtrated to get is identical with material liquid volume。
Embodiment 8
The present embodiment is substantially the same manner as Example 4, on this basis:
Described step A, permeate is containing alkali 300g/l, containing half fine 80g/l, after NF membrane circulation concentration, obtains concentrated solution containing alkali 75g/l, containing half fine 80g/l；Containing alkali 4g/l in the alkali liquor of described anode chamber, containing half fine 80g/l。
Embodiment 9
The present embodiment is substantially the same manner as Example 5, on this basis:
Described step A, permeate is containing alkali 260g/l, containing half fine 70g/l, after NF membrane circulation concentration, obtains concentrated solution containing alkali 32.5g/l, containing half fine 80g/l；Containing alkali 3.5g/l in the alkali liquor of described anode chamber, containing half fine 70g/l。
Embodiment 10
The present embodiment is substantially the same manner as Example 6, on this basis:
Described step A, permeate is containing alkali 200g/l, containing half fine 40g/l, after NF membrane circulation concentration, obtains concentrated solution containing alkali 12.5g/l, containing half fine 40g/l；Containing alkali 2g/l in the alkali liquor of described anode chamber, 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 is containing alkali 220g/l, containing half fine 60g/l, after NF membrane circulation concentration, obtains concentrated solution containing alkali 55g/l, containing half fine 60g/l；Containing alkali 3g/l in the alkali liquor of described anode chamber, 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 sequentially passes through rotary drum filtration, plate-and-frame filtration and microporous filter and removes 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 sequentially passes through rotary drum filtration, plate-and-frame filtration and microporous filter and removes 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 sequentially passes through rotary drum filtration, plate-and-frame filtration and microporous filter and removes 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 NF membrane is 4bar, and electrodialytic mould difference of crossing is 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 sequentially passes through rotary drum filtration, plate-and-frame filtration and microporous filter and removes 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 NF membrane is 3bar, and electrodialytic mould difference of crossing is 0.3bar。
Described step A, feed liquid flow in NF membrane is 25m3/ h, the flow in electrodialytic process is 5m3/h。
Embodiment 16
The present embodiment is substantially the same manner as Example 11, on this basis:
Described pre-filtering refers to, pressed liquor sequentially passes through rotary drum filtration, plate-and-frame filtration and microporous filter and removes 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 NF membrane is 3.6bar, and electrodialytic mould difference of crossing is 0.5bar。
Described step A, feed liquid flow in NF membrane is 40m3/ h, the flow in electrodialytic process is 5m3/h。
Described step A, it is 26.8m that the list of NF membrane props up filter area2。
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 adding neutralizes, and refers to addition hydrochloric acid and neutralizes。
Embodiment 18
The present embodiment is substantially the same manner as Example 9, on this basis:
Described step B, concentrated solution acid adding neutralizes, and refers to addition hydrochloric acid and neutralizes。
Described step C, the concentration of dilute sulfuric acid is 12%, and making pH value is 0。
Embodiment 19
The present embodiment is substantially the same manner as Example 10, on this basis:
Described step B, concentrated solution acid adding neutralizes, and refers to addition hydrochloric acid and neutralizes。
Described step C, the concentration of dilute sulfuric acid is 12%, and making pH value is 0。
Described D step, the molecular 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 adding neutralizes, and refers to addition hydrochloric acid and neutralizes。
Described step C, the concentration of dilute sulfuric acid is 12%, and making pH value is 0。
Described D step, the molecular cut off of ceramic membrane is 1500。
Described D step, the molecular cut off of NF 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 adding neutralizes, and refers to addition hydrochloric acid and neutralizes。
Described step C, the concentration of dilute sulfuric acid is 12%, and making pH value is 0。
Described D step, the molecular cut off of ceramic membrane is 1000。
Described D step, the molecular cut off of NF membrane is 100。
The mistake mould difference of described NF membrane is 3bar, and temperature is 30 DEG C, and single filter area is 26.8m2。
Embodiment 22
The present embodiment is substantially the same manner as Example 16, on this basis:
Described step B, concentrated solution acid adding neutralizes, and refers to addition hydrochloric acid and neutralizes。
Described step C, the concentration of dilute sulfuric acid is 12%, and making pH value is 0。
Described D step, the molecular cut off of ceramic membrane is 900。
Described D step, the molecular cut off of NF membrane is 120。
The mistake mould difference of described NF membrane is 4bar, and temperature is 40 DEG C, and single filter area is 26.8m2。
Described D step, material liquid volume is concentrated solution volume 10 times before NF membrane concentration。
Embodiment 23
The present embodiment is substantially the same manner as Example 16, on this basis:
Described step B, concentrated solution acid adding neutralizes, and refers to addition hydrochloric acid and neutralizes。
Described step C, the concentration of dilute sulfuric acid is 12%, and making pH value is 0。
Described D step, the molecular cut off of ceramic membrane is 950。
Described D step, the molecular cut off of NF membrane is 150。
The mistake mould difference of described NF membrane is 3.5bar, and temperature is 32 DEG C, and single filter area is 26.8m2。
Described D step, material liquid volume is concentrated solution volume 15 times before NF membrane concentration。
The decolouring of described D step refers to: adjusting pH value is 4, adds activated carbon, adsorbs 1h at 50 DEG C。
The electrical 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 adding neutralizes, and refers to addition hydrochloric acid and neutralizes。
Described step C, the concentration of dilute sulfuric acid is 12%, and making pH value is 0。
Described D step, the molecular cut off of ceramic membrane is 1200。
Described D step, the molecular cut off of NF membrane is 180。
The mistake mould difference of described NF membrane is 3.6bar, and temperature is 35 DEG C, and single filter area is 26.8m2。
Described D step, material liquid volume is concentrated solution volume 12 times before NF membrane concentration。
The decolouring of described D step refers to: adjusting pH value is 5, adds activated carbon, adsorbs 0.5h at 60 DEG C。
Described activated carbon is LY-T-ac activated carbon, and consumption is 3%。
The electrical 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 adding neutralizes, and refers to addition hydrochloric acid and neutralizes。
Described step C, the concentration of dilute sulfuric acid is 12%, and making pH value is 0。
Described D step, the molecular cut off of ceramic membrane is 800。
Described D step, the molecular cut off of NF membrane is 105。
The mistake mould difference of described NF membrane is 3.6bar, and temperature is 36 DEG C, and single filter area is 26.8m2。
Described D step, material liquid volume is concentrated solution volume 13 times before NF membrane concentration。
The decolouring of described D step refers to: adjusting pH value is 4.5, adds activated carbon, adsorbs 0.6h at 52 DEG C。
Described activated carbon is LY-T-ac activated carbon, and consumption is 5%。
The electrical 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 adding neutralizes, and refers to addition hydrochloric acid and neutralizes。
Described step C, the concentration of dilute sulfuric acid is 12%, and making pH value is 0。
Described D step, the molecular cut off of ceramic membrane is 1000。
Described D step, the molecular cut off of NF membrane is 120。
The mistake mould difference of described NF membrane is 3bar, and temperature is 32 DEG C, and single filter area is 26.8m2。
Described D step, material liquid volume is concentrated solution volume 12 times before NF membrane concentration。
The decolouring of described D step refers to: adjusting pH value is 4.5, adds activated carbon, adsorbs 0.6h at 53 DEG C。
Described activated carbon is LY-T-ac activated carbon, and consumption is 4%。
The electrical conductivity obtaining xylitol is 8000 μ s/cm, and ignition residue is 3%。
Claims (11)
1. the electrodialysis process of xylitol is prepared with viscose rayon press lye for raw material, it is characterised in that: concrete technology step is as follows:
A, membrance concentration
The pressed liquor that viscose rayon produces first removes large granular impurity through pre-filtering, and last concentrated solution, through NF membrane circulation concentration 2-4 time, is sent into electrodialysis membrane stack, reclaimed the alkali liquor of anode chamber, be the concentrated solution of pressed liquor by permeate；Described NF membrane circulation concentration 2-4 time, before filtering, feed liquid all enters NF membrane after dilute every time；
Described permeate is containing alkali 200-300g/l, containing half fine 40-80g/l；Containing alkali 2-4g/l in the alkali liquor of described anode chamber, containing half fine 40-80g/l；
B, extraction half fibre
The concentrated solution of press lye adds hydrochloric acid neutralize, obtain half fine liquid；
C, hydrolysis
Half fine liquid adds dilute sulfuric acid, hydrolysis occurs；
The concentration of dilute sulfuric acid is 12%, and making pH value is 0；
D, purification
Hydrolyzed solution is through ceramic membrane filter, and permeate enters NF membrane desalination, and concentrated solution, through activated carbon decolorizing, obtains the refined solution of xylose；The molecular cut off of NF membrane is 100-200, and the molecular cut off of ceramic membrane is 800-1500；
E, hydrogenation
The refined solution of xylose passes into hydrogen, the catalytic action of nickel occurs hydrogenation, obtains xylitol。
2. the electrodialysis process preparing xylitol with viscose rayon press lye for raw material according to claim 1, it is characterised in that: described step A, the molecular cut off of NF membrane is 200-400。
3. the electrodialysis process preparing xylitol with viscose rayon press lye for raw material according to claim 1, it is characterized in that: described step A, before each nanofiltration membrane, 1 times that amount is material liquid volume of dilute, the concentrated solution volume being filtrated to get is identical with material liquid volume。
4. the electrodialysis process preparing xylitol with viscose rayon press lye for raw material according to claim 1, it is characterised in that: described step A, the temperature of nanofiltration membrane treatment is 40-60 DEG C, and electrodialytic temperature is 15-45 DEG C。
5. the electrodialysis process preparing xylitol with viscose rayon press lye for raw material according to claim 1, it is characterised in that: described step A, the mistake mould difference of NF membrane is 3-4bar, and electrodialytic mould difference of crossing is 0.3-0.8bar。
6. the electrodialysis process preparing xylitol with viscose rayon press lye for raw material according to claim 1, it is characterised in that: described step A, feed liquid flow in NF membrane is 25-40m3/ h, the flow in electrodialytic process is 5m3/h。
7. the electrodialysis process preparing xylitol with viscose rayon press lye for raw material according to claim 1, it is characterised in that: described step A, electrodialysis impressed DC voltage, magnitude of voltage is 220V, and current value is 10A。
8. the electrodialysis process preparing xylitol with viscose rayon press lye for raw material according to claim 1, it is characterised in that: described D step, the mistake mould difference of NF membrane is 3-4bar, and temperature is 30-40 DEG C, and single filter area is 26.8m2。
9. the electrodialysis process preparing xylitol with viscose rayon press lye for raw material according to claim 1, it is characterised in that: described D step, 10-15 times that material liquid volume is concentrated solution volume before NF membrane concentration。
10. the electrodialysis process preparing xylitol with viscose rayon press lye for raw material according to claim 1, it is characterised in that: the decolouring of described D step refers to: adjustment pH value is 4-5, adds activated carbon, adsorbs 0.5-1h at 50-60 DEG C。
11. the electrodialysis process preparing xylitol with viscose rayon press lye for raw material according to claim 10, it is characterised in that: described activated carbon is LY-T-ac activated carbon, and consumption is 3-5%。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410622134.7A CN104496756B (en) | 2014-11-07 | 2014-11-07 | The electrodialysis process of xylitol is prepared with viscose rayon press lye for raw material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410622134.7A CN104496756B (en) | 2014-11-07 | 2014-11-07 | The electrodialysis process of xylitol is prepared with viscose rayon press lye for raw material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104496756A CN104496756A (en) | 2015-04-08 |
| CN104496756B true CN104496756B (en) | 2016-06-22 |
Family
ID=52938232
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410622134.7A Active CN104496756B (en) | 2014-11-07 | 2014-11-07 | The electrodialysis process of xylitol is prepared with viscose rayon press lye for raw material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104496756B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106237859B (en) * | 2015-06-12 | 2019-11-22 | 上海凯鑫分离技术股份有限公司 | The alkali recovery process of alkali pressed liquor in production process of viscose fiber |
| CN106242101B (en) * | 2015-06-12 | 2019-11-22 | 上海凯鑫分离技术股份有限公司 | The processing recovery process of alkali pressed liquor in production process of viscose fiber |
| CN106222313A (en) * | 2016-08-26 | 2016-12-14 | 唐山三友集团兴达化纤有限公司 | A kind of method utilizing the waste liquid produced in viscose staple fiber production process to prepare food stage xylose |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101028996A (en) * | 2006-02-27 | 2007-09-05 | 吴玉华 | Production of xylosic alcohol from corncob |
| CN101723799A (en) * | 2008-10-14 | 2010-06-09 | 安素梅 | Method for making xylitol by corn cob |
| CN101665523B (en) * | 2009-09-30 | 2015-09-30 | 济南圣泉唐和唐生物科技有限公司 | The production method of L-arabinose and D-xylose pref |
| EP2402454A1 (en) * | 2010-06-30 | 2012-01-04 | Süd-Chemie AG | Cellobiose production from biomass |
| CN102452898B (en) * | 2010-10-26 | 2013-11-13 | 施冬梅 | Method for producing crystalline xylitol by using membrane technology and indirect electroreduction method |
| CN102643935B (en) * | 2012-04-11 | 2013-08-07 | 宜宾丝丽雅股份有限公司 | Method for preparing xylose by using squeezed waste alkali liquor in viscose fiber production process |
| CN103409565B (en) * | 2013-07-26 | 2015-04-22 | 山东福田药业有限公司 | Preparation technology of xylose |
| CN103657419A (en) * | 2013-12-06 | 2014-03-26 | 南京工业大学 | Process for recovering alkali by double-membrane separation method in chemical fiber production |
| CN104099431B (en) * | 2014-08-01 | 2015-05-13 | 沈阳新华环境工程有限公司 | Method for extracting xylose from viscoce chemical fiber squeezed alkali liquor |
-
2014
- 2014-11-07 CN CN201410622134.7A patent/CN104496756B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104496756A (en) | 2015-04-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103409565B (en) | Preparation technology of xylose | |
| CN104311391B (en) | Membrane concentration process for producing xylitol by using viscose fiber squeezed liquid as raw material | |
| CN102320641B (en) | Resource utilization method for saponification waste water producing epoxypropane by chlorohydrination process | |
| CN106397630B (en) | A method of Sodium Hyaluronate is extracted using membrane separation technique | |
| CN103388198B (en) | A kind of bipolar membrane electrodialysis method is produced the method for soda acid from viscose rayon sodium sulphate waste liquid | |
| CN106242101B (en) | The processing recovery process of alkali pressed liquor in production process of viscose fiber | |
| CN102676707A (en) | Efficient and energy-saving xylose producing process | |
| CN104496756B (en) | The electrodialysis process of xylitol is prepared with viscose rayon press lye for raw material | |
| CN105969916A (en) | Method for preparing xylose by taking squeezed alkali liquid obtained in production of viscose as raw material | |
| CN109439695B (en) | Method for co-producing xylooligosaccharide, xylose and xylitol by industrial waste | |
| CN104357513A (en) | Electrodialysis process for preparing food-grade xylo-oligosaccharide from viscose fiber squeezed alkali liquor | |
| CN106555014A (en) | A kind of technique that xylose is prepared as raw material with viscose rayon press lye | |
| CN106191325A (en) | The technique that a kind of press lye produced with viscose rayon prepares xylose for raw material | |
| CN112679559B (en) | Method for separating and purifying xylose by electrodialysis combined flocculation technology | |
| CN104404104A (en) | Method for preparing food-grade xylo-oligosaccharide from viscose fiber squeezed alkali solution | |
| CN104402676A (en) | Membrane filtration technology for preparing xylitol from viscose fiber squeezed alkali solution | |
| CN104357493A (en) | Method for preparing xylitol from viscose fiber squeezed alkali liquor | |
| CN103724459B (en) | The method of the clear utilization of wastewater resource of a kind of glue | |
| CN104311706A (en) | Electrodialysis technology for exacting semi fibers by using viscose fiber pressed alkali liquor as raw materials | |
| CN104311704A (en) | Membrane filter technology for exacting semi fibers by using viscose fiber pressed alkali liquor as raw materials | |
| CN103343403B (en) | Viscose sodium sulfate waste liquor acid and alkali recycling technology by virtue of bipolar membrane electrodialysis method | |
| CN103386254B (en) | Cleaning method for bipolar-membrane electrodialysis membrane group device for preparing acid/base from sodium sulfate waste liquid | |
| CN104357492A (en) | Membrane concentration process for preparing xylitol from viscose production pressed liquor | |
| CN105420313A (en) | Method for preparing feed-grade xylo-oligosaccharide through viscose squeezed alkali liquid | |
| CN104357494A (en) | Process for producing xylitol from viscose fiber squeezed alkali liquor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |