CN104311702A - Method for extracting hemicellulose from viscose squeezing alkali liquor - Google Patents
Method for extracting hemicellulose from viscose squeezing alkali liquor Download PDFInfo
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- CN104311702A CN104311702A CN201410622026.XA CN201410622026A CN104311702A CN 104311702 A CN104311702 A CN 104311702A CN 201410622026 A CN201410622026 A CN 201410622026A CN 104311702 A CN104311702 A CN 104311702A
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- nanofiltration membrane
- membrane
- ceramic membrane
- viscose fiber
- concentrated solution
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- 239000003513 alkali Substances 0.000 title claims abstract description 67
- 229920002488 Hemicellulose Polymers 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 47
- 229920000297 Rayon Polymers 0.000 title claims abstract description 36
- 239000012528 membrane Substances 0.000 claims abstract description 262
- 238000001728 nano-filtration Methods 0.000 claims abstract description 131
- 239000000919 ceramic Substances 0.000 claims abstract description 129
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 30
- 239000012535 impurity Substances 0.000 claims abstract description 24
- 239000002253 acid Substances 0.000 claims abstract description 20
- 239000012466 permeate Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims description 154
- 238000001914 filtration Methods 0.000 claims description 102
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 50
- 239000000835 fiber Substances 0.000 claims description 38
- 239000000463 material Substances 0.000 claims description 25
- 239000000706 filtrate Substances 0.000 claims description 17
- 238000005374 membrane filtration Methods 0.000 claims description 17
- 238000010612 desalination reaction Methods 0.000 claims description 16
- 239000012141 concentrate Substances 0.000 claims description 7
- 238000010790 dilution Methods 0.000 abstract description 4
- 239000012895 dilution Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 72
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 46
- 150000003839 salts Chemical class 0.000 description 9
- 239000007787 solid Substances 0.000 description 5
- 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
- 239000002699 waste material Substances 0.000 description 4
- 229920003043 Cellulose fiber Polymers 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000007380 fibre production Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000004627 regenerated cellulose Substances 0.000 description 3
- 229920001131 Pulp (paper) Polymers 0.000 description 2
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 description 2
- 238000011112 process operation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- 239000000811 xylitol Substances 0.000 description 2
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 2
- 229960002675 xylitol Drugs 0.000 description 2
- 235000010447 xylitol Nutrition 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 235000014676 Phragmites communis Nutrition 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000010902 straw Substances 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
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides a method for extracting hemicellulose from a viscose squeezing alkali liquor. The method is characterized in that the squeezing alkali liquor for viscose production is pre-filtered for removal of large-particle impurities; a permeate is added with water for dilution, and then the diluted permeate enters a primary nanofiltration membrane for treatment; an obtained primary concentrated liquor is added with water for dilution, and then the diluted primary concentrated liquor enters a secondary nanofiltration membrane for treatment; an obtained secondary concentrated liquor is added with water for dilution, and then the diluted secondary concentrated liquor enters a ceramic membrane for treatment; the concentrated liquor is added with an acid for neutralization, so as to obtain a hemicellulose liquor. The obtained hemicellulose liquor has low alkali concentration, low salinity and high hemicellulose purity; the process has high operating efficiency, so as to be applicable for large-scale production.
Description
Technical field
The invention belongs to the recycling field that viscose fiber is produced, be specifically related to a kind of method extracting hemicellulose from viscose fiber press lye.
Background technology
Hemicellulose is the natural polymer that the whole world extensively exists,, Greenhouse effect day by day exhausted at the energy are day by day serious, the exploitation of biomass are more and more subject to the attention of the mankind, but also there is many difficult points at present, the comprehensive utilization of hemicellulose is all the more so, hemicellulose is due to the shortcoming of himself, and as easily degraded, difficult separation etc., its utility value is often easily ignored by people.
At chemical pulp plant celluloses such as () wood pulp, cotton pulp, straw pulp, reed pulps in the production process of viscose fiber of raw material, adopting alkali lye to process (dipping, squeezing) to Mierocrystalline cellulose is the first step manufacturing viscose fiber.Hemicellulose concentration is high, extremely adverse influence is produced to cellulose viscose manufacturing technique and final product quality, therefore must in impregnation technology with alkali lye by hemicellulose stripping, the Mierocrystalline cellulose of high strength could be obtained, so a large amount of high concentration alkali pressed liquors being rich in hemicellulose can be produced in above process.
Main component in alkali pressed liquor is sodium hydroxide and hemicellulose.Hemicellulose is therefrom separated by treatment process many employings nanofiltration of existing press lye, obtains comparatively pure alkali lye.Through purification alkali lye can direct reuse in technique, but part alkali only can be realized reuse by nanofiltration membrane, still containing a large amount of alkali in the concentrated solution that the hemicellulose in its trapped fluid obtains after concentrated.During at present this part feed liquid is used for as salkali waste and technique, hemicellulose enters wastewater treatment, or adopts calcination to reclaim sodium hydroxide, and hemicellulose is burned.From above existing technique, hemicellulose is not fully used.
As 201410091864.9, the application for a patent for invention that name is called " extracting the fine method of regenerated cellulose fibre steeping fluid half and half fine application ", the fine method of centrifugal extraction regenerated cellulose fibre steeping fluid half is added with membrane concentration, concrete steps comprise: obtaining containing alkali concn by pressed liquor through three dilutions and three membrane concentration is 26.5 grams per liters, and half fine concentration is the concentrated solution of 65 grams per liters; Concentrated solution whizzer is carried again, obtains half fine solid.Half fine solid is used for the allotment acid bath of regenerated cellulose fibre production acid bath workshop, and half fibre is spray-dried to be produced for Xylitol.The alkali concn of this patent is also higher, forms the salinity of higher concentration after neutralization of the acids, makes half fine purity low; And the yield that half fine solid is extracted in employing centrifugation is low.
201310515214.8, name is called the application for a patent for invention of " method extracting hemicellulose from vegetable fibre ", vegetable fibre is dissolved with the alkaline solution that massfraction is 5% ~ 15%, then large granular impurity is removed through squeezing the alkali lye obtained through conventional pre-filtering method, again alkali lye is entered ceramic membrane device by pump and carry out cross flow filter, by the concentrated solution acid neutralization obtained, collect the hemicellulose of precipitation and dry, obtaining hemicellulose; Described alkali lye after pre-filtering contains alkali 50 ~ 100g/l, containing hemicellulose 40 ~ 60g/l.This patent does not carry out desalination to the fine liquid of half after acid adding, and salt concentration is higher, and half fine purity is still lower.
201310593785.3, the application for a patent for invention that name is called " a kind of viscose fiber produces the extraction of hemicellulose in waste liquid and quaternised modified method ", its extracting method is carry out separation and Extraction with membrane sepn to the hemicellulose in viscose fiber production waste liquid and alkali lye, and concentrated solution is for containing alkali hemicellulose; Method of modifying is contain alkali hemicellulose for raw material with what extract in viscose fiber production waste liquid, and 2,3-epoxypropyltrimethylchloride chloride is etherifying agent, obtains quaternary ammonium hemicellulose after direct etherificate.It is little that the film list that this patent adopts props up filtration area, and operational efficiency is low, and running cost is high, is unfavorable for scale operation.
Summary of the invention
For above-mentioned technical problem, the invention provides a kind of method extracting hemicellulose from viscose fiber press lye.The alkali of obtain half fine liquid is dense low, and salinity is low, and half fine 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:
A kind of method extracting hemicellulose from viscose fiber press lye, it is characterized in that: 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, concentrated solution acid neutralization after gained secondary concentration liquid thin up, obtain half fine liquid.
The filtration efficiency of nanofiltration membrane is higher than ceramic membrane, nanofiltration membrane is first adopted repeatedly progressively to drop to certain degree dense for alkali, concentrated half fibre, little to the damage of film, adopt ceramic membrane filter again, the feed liquid that ceramic membrane is applicable to filter the dense height of later stage low alkali half fine is run, and be the powerful guarantee that low alkali is dense, and the efficiency of filtering is high.
The molecular weight cut-off of one-level nanofiltration membrane of the present invention 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.
Before described 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.
Described 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.While ensureing filtration efficiency, little to the damage of ceramic membrane.
Preferably, containing alkali 2-4g/l in the concentrated solution of described ceramic membrane filter, containing half fine 40-80 g/l.Be down to minimum by dense for alkali, ensure that the purity of half fibre.
Pre-filtering of the present invention refers to, press lye is successively through rotary drum filtration, Plate Filtration, micro-filtrate membrane filtration removing large granular impurity.Pre-filtering makes press lye not containing the solid impurity of more than 5 microns, and protection film is not below damaged by solid impurity.
The temperature of nanofiltration membrane of the present invention 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.
The mistake mould difference of nanofiltration membrane of the present invention 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.
The flow of feed liquid of the present invention 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.
It is 26.8m that the list of nanofiltration membrane of the present invention 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.
Described concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, and the advantage adding hydrochloric acid is that the molecules of salt amount formed is lower, is conducive to the desalination in later stage.
Preferably, described to add in hydrochloric acid and after, concentrated solution, again through nanofiltration membrane desalination, obtains half fine liquid, and the salinity of removing half fine liquid, improves half fine purity further.
Preferably, 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 half fine molecular weight is much larger than 100, effectively can realize salt and half fine being separated.
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, ensure salt and half fine being separated.
Preferably, the material liquid volume before described nanofiltration membrane concentrates is 10-15 times of concentrated solution volume, is conducive to the salt content in reduction by half fibre.
After nanofiltration membrane desalination, the specific conductivity obtaining half fine liquid is 8000-10000 μ s/cm, and ignition residue is 3-6%.
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; In filtration procedure, 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, 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; 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 half fine molecular weight is much larger than 100, effectively can realize being separated of salt and half fibre.Be conducive to the desalination in later stage, further increase the purity of half fine liquid.
4, the inventive method obtains the specific conductivity of half fine liquid is 8000-10000 μ s/cm, and ignition residue is 3-6%, and ignition residue is the direct indicator weighing inorganic salt, and the massfraction described in half fine liquid shared by inorganic salt is only 3-6%; Specific conductivity is the electrolytical degree existed in reaction liquid, and the main electrolyte of half fine liquid 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 half fine liquid salinity adopting the inventive method to obtain, and can be directly used in and prepare the byproduct such as xylo-oligosaccharide and Xylitol, the product purity obtained is up to more than 85%.
Embodiment
Below in conjunction with embodiment, essentiality content of the present invention is described in further detail.
Embodiment 1
A kind of method extracting hemicellulose from viscose fiber press lye, 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, concentrated solution acid neutralization after gained secondary concentration liquid thin up, obtain half fine liquid.
Embodiment 2
The present embodiment is substantially the same manner as Example 1, on this basis:
The molecular weight cut-off of described one-level nanofiltration membrane is 200, and the molecular weight cut-off of secondary nanofiltration membrane is 300, and ceramic membrane interception molecular weight is 800.
Embodiment 3
The present embodiment is substantially the same manner as Example 1, on this basis:
The molecular weight cut-off of described one-level nanofiltration membrane is 300, and the molecular weight cut-off of secondary nanofiltration membrane is 400, and ceramic membrane interception molecular weight is 1500.
Embodiment 4
The present embodiment is substantially the same manner as Example 1, on this basis:
The molecular weight cut-off of described one-level nanofiltration membrane is 250, and the molecular weight cut-off of secondary nanofiltration membrane is 350, and ceramic membrane interception molecular weight is 1000.
Embodiment 5
The present embodiment is substantially the same manner as Example 2, on this basis:
Before described 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 permeate contains alkali 200g/l, containing half fine 40g/l; Primary concentration liquid contains alkali 100g/l, containing half fine 40g/l; Secondary concentration liquid contains alkali 50g/l, containing half fine 40g/l.
Embodiment 6
The present embodiment is substantially the same manner as Example 3, on this basis:
Before described 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 permeate contains alkali 300g/l, containing half fine 80 g/l; Primary concentration liquid contains alkali 150g/l, containing half fine 80 g/l; Secondary concentration liquid contains alkali 75g/l, containing half fine 80g/l.
Embodiment 7
The present embodiment is substantially the same manner as Example 4, on this basis:
Before described 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 permeate contains alkali 280g/l, containing half fine 70g/l; Primary concentration liquid contains alkali 140g/l, containing half fine 70g/l; Secondary concentration liquid contains alkali 70g/l, containing half fine 70g/l.
Embodiment 8
The present embodiment is substantially the same manner as Example 5, on this basis:
Described 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.
Containing alkali 2g/l in the concentrated solution of described ceramic membrane filter, containing half fine 40g/l.
Described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and micro-filtrate membrane filtration removing large granular impurity.
Embodiment 9
The present embodiment is substantially the same manner as Example 7, on this basis:
Described 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.
Containing alkali 4g/l in the concentrated solution of described 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.
The temperature of described nanofiltration membrane is 40-60 DEG C, and the temperature of ceramic membrane filter is 60-80 DEG C.
Embodiment 10
The present embodiment is substantially the same manner as Example 6, on this basis:
Described 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.
Containing alkali 3g/l in the concentrated solution of described 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.
The temperature of described nanofiltration membrane is 40 DEG C, and the temperature of ceramic membrane filter is 60 DEG C.
Embodiment 11
The present embodiment is substantially the same manner as Example 6, on this basis:
Described 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.
Containing alkali 2.5g/l in the concentrated solution of described 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.
The temperature of described nanofiltration membrane is 60 DEG C, and the temperature of ceramic membrane filter is 80 DEG C.
The mistake mould difference of described nanofiltration membrane is 4bar, and the mistake mould difference of ceramic membrane is 6bar.
Embodiment 12
The present embodiment is substantially the same manner as Example 5, on this basis:
Described 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.
Containing alkali 3.5g/l in the concentrated solution of described 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.
The temperature of described nanofiltration membrane is 50 DEG C, and the temperature of ceramic membrane filter is 70 DEG C.
The mistake mould difference of described nanofiltration membrane is 3bar, and the mistake mould difference of ceramic membrane is 5bar.
The flow of described feed liquid in nanofiltration membrane is 25m
3/ h, the flow in ceramic membrane is 200m
3/ h.
Embodiment 13
The present embodiment is substantially the same manner as Example 5, on this basis:
Described 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.
Containing alkali 3.7g/l in the concentrated solution of described 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.
The temperature of described nanofiltration membrane is 45 DEG C, and the temperature of ceramic membrane filter is 65 DEG C.
The mistake mould difference of described nanofiltration membrane is 3.2bar, and the mistake mould difference of ceramic membrane is 5.2bar.
The flow of described feed liquid in nanofiltration membrane is 40m
3/ h, the flow in ceramic membrane is 250m
3/ h.
It is 26.8m that the list of described nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Embodiment 14
The present embodiment is substantially the same manner as Example 5, on this basis:
Described 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.
Containing alkali 3.2g/l in the concentrated solution of described 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.
The temperature of described nanofiltration membrane is 55 DEG C, and the temperature of ceramic membrane filter is 75 DEG C.
The mistake mould difference of described nanofiltration membrane is 3.5bar, and the mistake mould difference of ceramic membrane is 5.2bar.
The flow of described feed liquid in nanofiltration membrane is 30m
3/ h, the flow in ceramic membrane is 220m
3/ h.
It is 26.8m that the list of described nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Described concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Embodiment 15
The present embodiment is substantially the same manner as Example 5, on this basis:
Described 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.
Containing alkali 2.8g/l in the concentrated solution of described 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.
The temperature of described nanofiltration membrane is 52 DEG C, and the temperature of ceramic membrane filter is 60 DEG C.
The mistake mould difference of described nanofiltration membrane is 3.8bar, and the mistake mould difference of ceramic membrane is 5.3bar.
The flow of described feed liquid in nanofiltration membrane is 32m
3/ h, the flow in ceramic membrane is 230m
3/ h.
It is 26.8m that the list of described nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Described concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described to add in hydrochloric acid and after, concentrated solution, again through nanofiltration membrane desalination, obtains half fine liquid.
Embodiment 16
The present embodiment is substantially the same manner as Example 6, on this basis:
Described 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.
Containing alkali 2.6g/l in the concentrated solution of described ceramic membrane filter, containing half 66g/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.
The temperature of described nanofiltration membrane is 55 DEG C, and the temperature of ceramic membrane filter is 65 DEG C.
The mistake mould difference of described nanofiltration membrane is 3.6bar, and the mistake mould difference of ceramic membrane is 5.8bar.
The flow of described feed liquid in nanofiltration membrane is 35m
3/ h, the flow in ceramic membrane is 210m
3/ h.
It is 26.8m that the list of described nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Described concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described to add in hydrochloric acid and after, concentrated solution, again through nanofiltration membrane desalination, obtains half fine liquid.
The molecular weight cut-off of described nanofiltration membrane is 100.
Embodiment 17
The present embodiment is substantially the same manner as Example 7, on this basis:
Described 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.
Containing alkali 2.6g/l in the concentrated solution of described 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.
The temperature of described nanofiltration membrane is 46 DEG C, and the temperature of ceramic membrane filter is 62 DEG C.
The mistake mould difference of described nanofiltration membrane is 3.6bar, and the mistake mould difference of ceramic membrane is 5.3bar.
The flow of described feed liquid in nanofiltration membrane is 32m
3/ h, the flow in ceramic membrane is 240m
3/ h.
It is 26.8m that the list of described nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Described concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described to add in hydrochloric acid and after, concentrated solution, again through nanofiltration membrane desalination, obtains half fine liquid.
The molecular weight cut-off of described nanofiltration membrane is 200.
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.
Embodiment 18
The present embodiment is substantially the same manner as Example 5, on this basis:
Described 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.
Containing alkali 3g/l in the concentrated solution of described 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.
The temperature of described nanofiltration membrane is 56 DEG C, and the temperature of ceramic membrane filter is 65 DEG C.
The mistake mould difference of described nanofiltration membrane is 3.2bar, and the mistake mould difference of ceramic membrane is 5.3bar.
The flow of described feed liquid in nanofiltration membrane is 28m
3/ h, the flow in ceramic membrane is 225m
3/ h.
It is 26.8m that the list of described nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Described concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described to add in hydrochloric acid and after, concentrated solution, again through nanofiltration membrane desalination, obtains half fine liquid.
The molecular weight cut-off of described nanofiltration membrane is 150.
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.
Material liquid volume before described nanofiltration membrane concentrates is 10 times of concentrated solution volume.
Embodiment 19
The present embodiment is substantially the same manner as Example 5, on this basis:
Described 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.
Containing alkali 3.2g/l in the concentrated solution of described ceramic membrane filter, containing half fine 76g/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.
The temperature of described nanofiltration membrane is 55 DEG C, and the temperature of ceramic membrane filter is 65 DEG C.
The mistake mould difference of described nanofiltration membrane is 3.3bar, and the mistake mould difference of ceramic membrane is 5.2bar.
The flow of described feed liquid in nanofiltration membrane is 28m
3/ h, the flow in ceramic membrane is 235m
3/ h.
It is 26.8m that the list of described nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Described concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described to add in hydrochloric acid and after, concentrated solution, again through nanofiltration membrane desalination, obtains half fine liquid.
The molecular weight cut-off of described nanofiltration membrane is 120.
The mistake mould difference of described nanofiltration membrane is 3.2bar, and temperature is 32 DEG C, and single filtration area is 26.8 m
2.
Material liquid volume before described nanofiltration membrane concentrates is 15 times of concentrated solution volume.
The described specific conductivity obtaining half fine liquid is 8000 μ s/cm, and ignition residue is 3%.
Embodiment 20
The present embodiment is substantially the same manner as Example 5, on this basis:
Described 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.
Containing alkali 3.6g/l in the concentrated solution of described ceramic membrane filter, containing half fine 72g/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.
The temperature of described nanofiltration membrane is 55 DEG C, and the temperature of ceramic membrane filter is 68 DEG C.
The mistake mould difference of described nanofiltration membrane is 3.6bar, and the mistake mould difference of ceramic membrane is 5.6bar.
The flow of described feed liquid in nanofiltration membrane is 35m
3/ h, the flow in ceramic membrane is 220m
3/ h.
It is 26.8m that the list of described nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Described concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described to add in hydrochloric acid and after, concentrated solution, again through nanofiltration membrane desalination, obtains half fine liquid.
The molecular weight cut-off of described nanofiltration membrane is 160.
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.
Material liquid volume before described nanofiltration membrane concentrates is 12 times of concentrated solution volume.
The described specific conductivity obtaining half fine liquid is 10000 μ s/cm, and ignition residue is 6%.
Embodiment 21
The present embodiment is substantially the same manner as Example 6, on this basis:
Described 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.
Containing alkali 3.2g/l in the concentrated solution of described ceramic membrane filter, containing half fine 70g/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.
The temperature of described nanofiltration membrane is 45 DEG C, and the temperature of ceramic membrane filter is 65 DEG C.
The mistake mould difference of described nanofiltration membrane is 3.5bar, and the mistake mould difference of ceramic membrane is 5bar.
The flow of described feed liquid in nanofiltration membrane is 26m
3/ h, the flow in ceramic membrane is 240m
3/ h.
It is 26.8m that the list of described nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Described concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described to add in hydrochloric acid and after, concentrated solution, again through nanofiltration membrane desalination, obtains half fine liquid.
The molecular weight cut-off of described nanofiltration membrane is 180.
The mistake mould difference of described nanofiltration membrane is 4bar, and temperature is 36 DEG C, and single filtration area is 26.8 m
2.
Material liquid volume before described nanofiltration membrane concentrates is 13 times of concentrated solution volume.
The described specific conductivity obtaining half fine liquid is 9000 μ s/cm, and ignition residue is 5%.
Embodiment 22
The present embodiment is substantially the same manner as Example 5, on this basis:
Described 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.
Containing alkali 3g/l in the concentrated solution of described 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.
The temperature of described nanofiltration membrane is 50 DEG C, and the temperature of ceramic membrane filter is 75 DEG C.
The mistake mould difference of described nanofiltration membrane is 3.5bar, and the mistake mould difference of ceramic membrane is 5.5bar.
The flow of described feed liquid in nanofiltration membrane is 28m
3/ h, the flow in ceramic membrane is 215m
3/ h.
It is 26.8m that the list of described nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Described concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Described to add in hydrochloric acid and after, concentrated solution, again through nanofiltration membrane desalination, obtains half fine liquid.
The molecular weight cut-off of described nanofiltration membrane is 180.
The mistake mould difference of described nanofiltration membrane is 3.6bar, and temperature is 38 DEG C, and single filtration area is 26.8 m
2.
Material liquid volume before described nanofiltration membrane concentrates is 11 times of concentrated solution volume.
The described specific conductivity obtaining half fine liquid is 8500 μ s/cm, and ignition residue is 4%.
Claims (17)
1. one kind is extracted the method for hemicellulose from viscose fiber press lye, it is characterized in that: 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, concentrated solution acid neutralization after gained secondary concentration liquid thin up, obtain half fine liquid.
2. a kind of method extracting hemicellulose from viscose fiber press lye according to claim 1, it is characterized in that: the molecular weight cut-off of described one-level nanofiltration membrane is 200-300, the molecular weight cut-off of secondary nanofiltration membrane is 300-400, and ceramic membrane interception molecular weight is 800-1500.
3. a kind of method extracting hemicellulose from viscose fiber press lye according to claim 1, it is characterized in that: before described 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.
4. a kind of method extracting hemicellulose from viscose fiber press lye according to claim 3, 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 method extracting hemicellulose from viscose fiber press lye according to claim 1, it is characterized in that: described ceramic membrane filter, 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 method extracting hemicellulose from viscose fiber press lye according to claim 5, 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 method extracting hemicellulose from viscose fiber press lye according to claim 1, is characterized in that: described pre-filtering refers to, pressed liquor is successively through rotary drum filtration, Plate Filtration and micro-filtrate membrane filtration removing large granular impurity.
8. a kind of method extracting hemicellulose from viscose fiber press lye according to claim 1, is characterized in that: the temperature of described nanofiltration membrane is 40-60 DEG C, and the temperature of ceramic membrane filter is 60-80 DEG C.
9. a kind of method extracting hemicellulose from viscose fiber press lye according to claim 1, is characterized in that: the mistake mould difference of described nanofiltration membrane is 3-4bar, and the mistake mould difference of ceramic membrane is 5-6bar.
10. a kind of method extracting hemicellulose from viscose fiber press lye according to claim 1, is characterized in that: the flow of described feed liquid in nanofiltration membrane is 25-40m
3/ h, the flow in ceramic membrane is 200-250m
3/ h.
11. a kind of methods extracting hemicellulose from viscose fiber press lye according to claim 1, is characterized in that: it is 26.8m that the list of described nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
12. a kind of methods extracting hemicellulose from viscose fiber press lye according to claim 1, is characterized in that: described concentrated solution acid neutralization, refer to and add hydrochloric acid neutralization.
13. a kind of methods extracting hemicellulose from viscose fiber press lye according to claim 12, is characterized in that: described to add in hydrochloric acid and after, concentrated solution, again through nanofiltration membrane desalination, obtains half fine liquid.
14. a kind of methods extracting hemicellulose from viscose fiber press lye according to claim 13, is characterized in that: the molecular weight cut-off of described nanofiltration membrane is 100-200.
15. a kind of methods extracting hemicellulose from viscose fiber press lye according to claim 13, 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.
16. a kind of methods extracting hemicellulose from viscose fiber press lye according to claim 13, is characterized in that: the material liquid volume before described nanofiltration membrane concentrates is 10-15 times of concentrated solution volume.
17. a kind of methods extracting hemicellulose from viscose fiber press lye according to claim 13, is characterized in that: described in obtain half fine liquid specific conductivity be 8000-10000 μ s/cm, ignition residue is 3-6%.
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Cited By (5)
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| CN105601765A (en) * | 2015-12-23 | 2016-05-25 | 中国科学院过程工程研究所 | Device for desalting hemicellulose extract |
| CN105969916A (en) * | 2016-07-20 | 2016-09-28 | 宜宾雅泰生物科技有限公司 | Method for preparing xylose by taking squeezed alkali liquid obtained in production of viscose as raw material |
| CN106243248A (en) * | 2016-08-23 | 2016-12-21 | 南京工业大学 | A kind of viscose rayon reclaims the method for alkaline extraction hemicellulose in producing |
| CN109554948A (en) * | 2018-11-28 | 2019-04-02 | 宜宾丝丽雅股份有限公司 | A kind of lye multistage recovery process |
| CN109912730A (en) * | 2019-03-19 | 2019-06-21 | 阿拉尔市富丽达纤维有限公司 | The recyclable device and recovery method of hemicellulose in a kind of concentration lye |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105601765A (en) * | 2015-12-23 | 2016-05-25 | 中国科学院过程工程研究所 | Device for desalting hemicellulose extract |
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| CN106243248A (en) * | 2016-08-23 | 2016-12-21 | 南京工业大学 | A kind of viscose rayon reclaims the method for alkaline extraction hemicellulose in producing |
| CN109554948A (en) * | 2018-11-28 | 2019-04-02 | 宜宾丝丽雅股份有限公司 | A kind of lye multistage recovery process |
| CN109554948B (en) * | 2018-11-28 | 2021-01-01 | 宜宾丝丽雅股份有限公司 | Multistage alkali liquor recovery process |
| CN109912730A (en) * | 2019-03-19 | 2019-06-21 | 阿拉尔市富丽达纤维有限公司 | The recyclable device and recovery method of hemicellulose in a kind of concentration lye |
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