CN104387506A - Membrane concentration process for extracting hemicellulose by using viscose fiber extruded liquid as raw material - Google Patents

Membrane concentration process for extracting hemicellulose by using viscose fiber extruded liquid as raw material Download PDF

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Publication number
CN104387506A
CN104387506A CN201410622171.8A CN201410622171A CN104387506A CN 104387506 A CN104387506 A CN 104387506A CN 201410622171 A CN201410622171 A CN 201410622171A CN 104387506 A CN104387506 A CN 104387506A
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China
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membrane
viscose fiber
raw material
liquid
concentrated solution
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Inventor
邓传东
冯涛
孙毅
唐孝兵
莫世清
周林
罗红梅
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Yibin Grace Group Co Ltd
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YIBIN YATAI BIOTECHNOLOGY Co Ltd
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Abstract

The invention provides a membrane concentration process for extracting hemicellulose by using a viscose fiber extruded liquid as a raw material. The membrane concentration process is characterized by comprising the following steps: prefiltering a squeezing alkali liquid produced from viscose fiber so as to remove large-granular impurities, performing micro-filtration membrane treatment, circulating and concentrating permeate for 2-4 times by using a nano filtering membrane, adding water to dilute the last concentrated liquid, feeding the diluted liquid into a ceramic membrane for filtration, and adding acid to neutralize the concentrated liquid, thereby obtaining a half-fiber liquid, wherein the nano filtering membrane is adopted to circulate and concentrate the permeate for 2-4 times, and water is added to dilute the liquid and the diluted liquid is fed into the nano filtering membrane before being filtered each time. The obtained half-fiber liquid is low in alkali concentration, low in salt content, high in half-fiber purity, high in process operation efficiency and applicable to large-scale production.

Description

With viscose fiber pressed liquor for raw material extracts half fine membrane concentration technique
Technical field
The invention belongs to the recycling field of viscose fiber, be specifically related to a kind of with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre.
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.
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 the technique that a kind of press lye produced with viscose fiber is raw material extraction half fibre.The alkali obtaining half fine liquid is dense low, and salinity is low, and half fine purity is high.
For achieving the above object, the present invention adopts following technical scheme:
With viscose fiber pressed liquor for raw material extracts half fine membrane concentration technique, it is characterized in that: the press lye produced by viscose fiber is first through pre-filtering removing large granular impurity, enter microfiltration membrane process, permeate is through concentrated 2-4 time of nanofiltration membrane circulation, send after last concentrated solution thin up into ceramic membrane filter, the concentrated solution acid neutralization obtained, obtains half fine liquid; Concentrated 2-4 time of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up.
First through microfiltration membrane and nanofiltration membrane, efficiency is higher than ceramic membrane, first with the macro-molecular protein in micro-filtrate membrane filtration removal alkali lye and bacterium, nanofiltration membrane is adopted repeatedly progressively to drop to certain degree dense for alkali again, 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.
Microfiltration membrane aperture of the present invention is 5 microns, and the molecular weight cut-off of described nanofiltration membrane is 200-400, and the molecular weight cut-off of ceramic membrane is 800-1500.
Micro-filtrate membrane filtration amount is large, is conducive to improving filtration efficiency; The molecular weight cut-off of 200-400, makes alkali separate from permeate, progressively lowers alkali dense, promotes half fine concentration, retain a part of monose simultaneously; The molecular weight cut-off of ceramic membrane is 800-1500, can retain half fibre, improve the purity of product.
Described nanofiltration membrane circulation is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.While ensureing filtration efficiency, little to the damage of nanofiltration membrane.
Preferably, described permeate, containing alkali 200-300g/l, containing half fine 40-80 g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 12-75g/l, containing half fine 40-80g/l.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 filters and Plate Filtration removing large granular impurity through rotary drum successively.Make press lye not containing the solid impurity of more than 5 microns, protection film is not below damaged by solid impurity.
The temperature of micro-filtration of the present invention is 40-50 DEG C, and the temperature of nanofiltration membrane treatment is 40-60 DEG C, and the temperature of ceramic membrane process 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 micro-filtration of the present invention is 1-2bar, and the mistake mould difference of nanofiltration membrane is 3-4bar, and the mistake mould difference of ceramic membrane is 5-6bar.For the feature that viscose glue press lye viscosity is higher, adopt higher pressure reduction to filter, can ensure that half fine concentration in alkali lye reaches processing requirement.
Feed liquid of the present invention is 20-40 m at the flow of microfiltration membrane 3/ h, the flow 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 1m that the list of described microfiltration membrane props up filtration area 2, it is 26.8m that the list of nanofiltration membrane props up filtration area 2, it is 0.6m that the list of ceramic membrane props up filtration area 2, single film has larger filtration area under the prerequisite taking less space.
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, except the salinity of low 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 microfiltration membrane, nanofiltration membrane and ceramic membrane to combine filtering and concentrating half fibre, because the filtration efficiency of micro-filtration and nanofiltration is higher than ceramic membrane, first with the macro-molecular protein in micro-filtrate membrane filtration removal alkali lye and bacterium, nanofiltration membrane is adopted repeatedly progressively to drop to certain degree dense for alkali again, concentrated half fibre, little to the damage of 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.Microfiltration membrane, 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
With viscose fiber pressed liquor for raw material extracts half fine membrane concentration technique, the press lye that viscose fiber is produced is first through pre-filtering removing large granular impurity, enter microfiltration membrane process, permeate is through concentrated 2 times of nanofiltration membrane circulation, send after last concentrated solution thin up into ceramic membrane filter, the concentrated solution acid neutralization obtained, obtains half fine liquid; Concentrated 2 times of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up.
Embodiment 2
With viscose fiber pressed liquor for raw material extracts half fine membrane concentration technique, the press lye that viscose fiber is produced is first through pre-filtering removing large granular impurity, enter microfiltration membrane process, permeate is through concentrated 3 times of nanofiltration membrane circulation, send after last concentrated solution thin up into ceramic membrane filter, the concentrated solution acid neutralization obtained, obtains half fine liquid; Concentrated 3 times of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up.
Embodiment 3
With viscose fiber pressed liquor for raw material extracts half fine membrane concentration technique, the press lye that viscose fiber is produced is first through pre-filtering removing large granular impurity, enter microfiltration membrane process, permeate is through concentrated 4 times of nanofiltration membrane circulation, send after last concentrated solution thin up into ceramic membrane filter, the concentrated solution acid neutralization obtained, obtains half fine liquid; Concentrated 4 times of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up.
Embodiment 4
The present embodiment is substantially the same manner as Example 1, on this basis:
Described microfiltration membrane aperture is 5 microns, and the molecular weight cut-off of nanofiltration membrane is 200, and the molecular weight cut-off of ceramic membrane is 800.
Described nanofiltration membrane circulation is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
Embodiment 5
The present embodiment is substantially the same manner as Example 2, on this basis:
Described microfiltration membrane aperture is 5 microns, and the molecular weight cut-off of nanofiltration membrane is 400, and the molecular weight cut-off of ceramic membrane is 1500.
Described nanofiltration membrane circulation is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
Embodiment 6
The present embodiment is substantially the same manner as Example 3, on this basis:
Described microfiltration membrane aperture is 5 microns, and the molecular weight cut-off of nanofiltration membrane is 300, and the molecular weight cut-off of ceramic membrane is 1000.
Described nanofiltration membrane circulation is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
Embodiment 7
The present embodiment is substantially the same manner as Example 1, on this basis:
Described microfiltration membrane aperture is 5 microns, and the molecular weight cut-off of nanofiltration membrane is 250, and the molecular weight cut-off of ceramic membrane is 900.
Described nanofiltration membrane circulation is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
Embodiment 8
The present embodiment is substantially the same manner as Example 4, on this basis:
Described permeate, containing alkali 300g/l, containing half fine 80g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 75g/l, containing half fine 80g/l.
Embodiment 9
The present embodiment is substantially the same manner as Example 5, on this basis:
Described permeate, containing alkali 260g/l, containing half fine 70g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 32.5g/l, containing half fine 80g/l.
Embodiment 10
The present embodiment is substantially the same manner as Example 6, on this basis:
Described permeate, containing alkali 200g/l, containing half fine 40g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 12.5g/l, containing half fine 40g/l.
Embodiment 11
The present embodiment is substantially the same manner as Example 7, on this basis:
Described permeate, containing alkali 220g/l, containing half fine 60g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 55g/l, containing half fine 60g/l.
Embodiment 12
The present embodiment is substantially the same manner as Example 8, 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.
Embodiment 13
The present embodiment is substantially the same manner as Example 9, 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 filters and Plate Filtration removing large granular impurity through rotary drum successively.
The temperature of described micro-filtration is 40 DEG C, and the temperature of nanofiltration membrane is 40 DEG C, and the temperature of ceramic membrane filter is 60 DEG C.
Embodiment 14
The present embodiment is substantially the same manner as Example 10, 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 50g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
The temperature of described micro-filtration is 50 DEG C, and the temperature of nanofiltration membrane is 60 DEG C, and the temperature of ceramic membrane filter is 80 DEG C.
The mistake mould difference of described micro-filtration is 1bar, and the mistake mould difference of nanofiltration membrane is 4bar, and the mistake mould difference of ceramic membrane is 6bar.
Embodiment 15
The present embodiment is substantially the same manner as Example 11, 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 60g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
The temperature of described micro-filtration is 45 DEG C, and the temperature of nanofiltration membrane is 45 DEG C, and the temperature of ceramic membrane filter is 65 DEG C.
The mistake mould difference of described micro-filtration is 2bar, and the mistake mould difference of nanofiltration membrane is 3bar, and the mistake mould difference of ceramic membrane is 5bar.
Described feed liquid is 20m at the flow of microfiltration membrane 3/ h, the flow in nanofiltration membrane is 25m 3/ h, the flow in ceramic membrane is 200m 3/ h.
Embodiment 16
The present embodiment is substantially the same manner as Example 11, 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 70g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
The temperature of described micro-filtration is 46 DEG C, and the temperature of nanofiltration membrane is 55 DEG C, and the temperature of ceramic membrane filter is 75 DEG C.
The mistake mould difference of described micro-filtration is 1.5bar, and the mistake mould difference of nanofiltration membrane is 3.6bar, and the mistake mould difference of ceramic membrane is 5.6bar.
Described feed liquid is 40m at the flow of microfiltration membrane 3/ h, the flow in nanofiltration membrane is 40m 3/ h, the flow in ceramic membrane is 250m 3/ h.
It is 1m that the list of described microfiltration membrane props up filtration area 2, it is 26.8m that the list of nanofiltration membrane props up filtration area 2, it is 0.6m that the list of ceramic membrane props up filtration area 2.
Embodiment 17
The present embodiment is substantially the same manner as Example 11, 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 3.8g/l in the concentrated solution of described ceramic membrane filter, containing half fine 65g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
The temperature of described micro-filtration is 42 DEG C, and the temperature of nanofiltration membrane is 55 DEG C, and the temperature of ceramic membrane filter is 72 DEG C.
The mistake mould difference of described micro-filtration is 1.2bar, and the mistake mould difference of nanofiltration membrane is 3.6bar, and the mistake mould difference of ceramic membrane is 5.2bar.
Described feed liquid is 30m at the flow of microfiltration membrane 3/ h, the flow in nanofiltration membrane is 30m 3/ h, the flow in ceramic membrane is 220m 3/ h.
It is 1m that the list of described microfiltration membrane props up filtration area 2, it is 26.8m that the list of nanofiltration membrane props up filtration area 2, it is 0.6m that the list of ceramic membrane props up filtration area 2.
Described concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization.
Embodiment 18
The present embodiment is substantially the same manner as Example 11, 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 70g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
The temperature of described micro-filtration is 48 DEG C, and the temperature of nanofiltration membrane is 55 DEG C, and the temperature of ceramic membrane filter is 66 DEG C.
The mistake mould difference of described micro-filtration is 1.6bar, and the mistake mould difference of nanofiltration membrane is 3bar, and the mistake mould difference of ceramic membrane is 5bar.
Described feed liquid is 25m at the flow of microfiltration membrane 3/ h, the flow in nanofiltration membrane is 30m 3/ h, the flow in ceramic membrane is 225m 3/ h.
It is 1m that the list of described microfiltration membrane props up filtration area 2, it is 26.8m that the list of nanofiltration membrane props up filtration area 2, it is 0.6m that the list of ceramic membrane props up filtration area 2.
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 19
The present embodiment is substantially the same manner as Example 11, 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 65g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
The temperature of described micro-filtration is 42 DEG C, and the temperature of nanofiltration membrane is 46 DEG C, and the temperature of ceramic membrane filter is 68 DEG C.
The mistake mould difference of described micro-filtration is 1.6bar, and the mistake mould difference of nanofiltration membrane is 4bar, and the mistake mould difference of ceramic membrane is 5.5bar.
Described feed liquid is 35m at the flow of microfiltration membrane 3/ h, the flow in nanofiltration membrane is 28m 3/ h, the flow in ceramic membrane is 230m 3/ h.
It is 1m that the list of described microfiltration membrane props up filtration area 2, it is 26.8m that the list of nanofiltration membrane props up filtration area 2, it is 0.6m that the list of ceramic membrane props up filtration area 2.
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 20
The present embodiment is substantially the same manner as Example 11, 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 50g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
The temperature of described micro-filtration is 45 DEG C, and the temperature of nanofiltration membrane is 52 DEG C, and the temperature of ceramic membrane filter is 65 DEG C.
The mistake mould difference of described micro-filtration is 1.5bar, and the mistake mould difference of nanofiltration membrane is 3.2bar, and the mistake mould difference of ceramic membrane is 5.6bar.
Described feed liquid is 30m at the flow of microfiltration membrane 3/ h, the flow in nanofiltration membrane is 32m 3/ h, the flow in ceramic membrane is 220m 3/ h.
It is 1m that the list of described microfiltration membrane props up filtration area 2, it is 26.8m that the list of nanofiltration membrane props up filtration area 2, it is 0.6m that the list of ceramic membrane props up filtration area 2.
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 21
The present embodiment is substantially the same manner as Example 11, 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 41g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
The temperature of described micro-filtration is 49 DEG C, and the temperature of nanofiltration membrane is 42 DEG C, and the temperature of ceramic membrane filter is 65 DEG C.
The mistake mould difference of described micro-filtration is 1.3bar, and the mistake mould difference of nanofiltration membrane is 3.2bar, and the mistake mould difference of ceramic membrane is 5.2bar.
Described feed liquid is 22m at the flow of microfiltration membrane 3/ h, the flow in nanofiltration membrane is 28m 3/ h, the flow in ceramic membrane is 215m 3/ h.
It is 1m that the list of described microfiltration membrane props up filtration area 2, it is 26.8m that the list of nanofiltration membrane props up filtration area 2, it is 0.6m that the list of ceramic membrane props up filtration area 2.
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 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 22
The present embodiment is substantially the same manner as Example 11, 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 52g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
The temperature of described micro-filtration is 48 DEG C, and the temperature of nanofiltration membrane is 48 DEG C, and the temperature of ceramic membrane filter is 62 DEG C.
The mistake mould difference of described micro-filtration is 1.8bar, and the mistake mould difference of nanofiltration membrane is 3bar, and the mistake mould difference of ceramic membrane is 5.2bar.
Described feed liquid is 30m at the flow of microfiltration membrane 3/ h, the flow in nanofiltration membrane is 32m 3/ h, the flow in ceramic membrane is 230m 3/ h.
It is 1m that the list of described microfiltration membrane props up filtration area 2, it is 26.8m that the list of nanofiltration membrane props up filtration area 2, it is 0.6m that the list of ceramic membrane props up filtration area 2.
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 3.3bar, and temperature is 35 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 23
The present embodiment is substantially the same manner as Example 10, 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 63 g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
The temperature of described micro-filtration is 42 DEG C, and the temperature of nanofiltration membrane is 55 DEG C, and the temperature of ceramic membrane filter is 75 DEG C.
The mistake mould difference of described micro-filtration is 1.2bar, and the mistake mould difference of nanofiltration membrane is 3bar, and the mistake mould difference of ceramic membrane is 5bar.
Described feed liquid is 25m at the flow of microfiltration membrane 3/ h, the flow in nanofiltration membrane is 36m 3/ h, the flow in ceramic membrane is 225m 3/ h.
It is 1m that the list of described microfiltration membrane props up filtration area 2, it is 26.8m that the list of nanofiltration membrane props up filtration area 2, it is 0.6m that the list of ceramic membrane props up filtration area 2.
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 130.
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 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 24
The present embodiment is substantially the same manner as Example 9, 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 65 g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
The temperature of described micro-filtration is 46 DEG C, and the temperature of nanofiltration membrane is 55 DEG C, and the temperature of ceramic membrane filter is 70 DEG C.
The mistake mould difference of described micro-filtration is 1.6bar, and the mistake mould difference of nanofiltration membrane is 3.6bar, and the mistake mould difference of ceramic membrane is 5.5bar.
Described feed liquid is 26m at the flow of microfiltration membrane 3/ h, the flow in nanofiltration membrane is 35m 3/ h, the flow in ceramic membrane is 235m 3/ h.
It is 1m that the list of described microfiltration membrane props up filtration area 2, it is 26.8m that the list of nanofiltration membrane props up filtration area 2, it is 0.6m that the list of ceramic membrane props up filtration area 2.
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 155.
The mistake mould difference of described nanofiltration membrane is 3.8bar, 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 4%.
Embodiment 25
The present embodiment is substantially the same manner as Example 11, 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 78g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
The temperature of described micro-filtration is 42 DEG C, and the temperature of nanofiltration membrane is 42 DEG C, and the temperature of ceramic membrane filter is 65 DEG C.
The mistake mould difference of described micro-filtration is 1.5bar, and the mistake mould difference of nanofiltration membrane is 3bar, and the mistake mould difference of ceramic membrane is 5bar.
Described feed liquid is 26m at the flow of microfiltration membrane 3/ h, the flow in nanofiltration membrane is 28m 3/ h, the flow in ceramic membrane is 205m 3/ h.
It is 1m that the list of described microfiltration membrane props up filtration area 2, it is 26.8m that the list of nanofiltration membrane props up filtration area 2, it is 0.6m that the list of ceramic membrane props up filtration area 2.
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 4bar, and temperature is 32 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 9500 μ s/cm, and ignition residue is 5%.

Claims (17)

1. with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre, it is characterized in that: the press lye that viscose fiber is produced is first through pre-filtering removing large granular impurity, enter microfiltration membrane process, permeate is through concentrated 2-4 time of nanofiltration membrane circulation, send after last concentrated solution thin up into ceramic membrane filter, the concentrated solution acid neutralization obtained, obtains half fine liquid; Concentrated 2-4 time of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up.
2. according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre, it is characterized in that: described microfiltration membrane aperture is 5 microns, the molecular weight cut-off of nanofiltration membrane is 200-400, and the molecular weight cut-off of ceramic membrane is 800-1500.
3. according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre, it is characterized in that: described nanofiltration membrane circulation is concentrated, the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
4. according to claim 3 with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre, it is characterized in that: described permeate contains alkali 200-300g/l, containing half fine 40-80 g/l, after nanofiltration membrane circulation is concentrated, obtain concentrated solution containing alkali 12-75g/l, containing half fine 40-80g/l.
5. according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre, 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. according to claim 5 with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre, it is characterized in that: containing alkali 2-4g/l in the concentrated solution of described ceramic membrane filter, containing half fine 40-80 g/l.
7. according to claim 1ly extract half fine membrane concentration technique with viscose fiber pressed liquor for raw material, it is characterized in that: described pre-filtering refers to, pressed liquor to filter and Plate Filtration removes large granular impurity through rotary drum successively.
8. according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre, it is characterized in that: the temperature of described micro-filtration is 40-50 DEG C, the temperature of nanofiltration membrane treatment is 40-60 DEG C, and the temperature of ceramic membrane process is 60-80 DEG C.
9. according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre, it is characterized in that: the mistake mould difference of described micro-filtration is 1-2bar, and the mistake mould difference of nanofiltration membrane is 3-4bar, and the mistake mould difference of ceramic membrane is 5-6bar.
10. according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre, it is characterized in that: described feed liquid is 20-40m at the flow of microfiltration membrane 3/ h, the flow in nanofiltration membrane is 25-40m 3/ h, the flow in ceramic membrane is 200-250m 3/ h.
11. is according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre, it is characterized in that: it is 1m that the list of described microfiltration membrane props up filtration area 2, it is 26.8m that the list of nanofiltration membrane props up filtration area 2, it is 0.6m that the list of ceramic membrane props up filtration area 2.
12. according to claim 1ly extract half fine membrane concentration technique with viscose fiber pressed liquor for raw material, it is characterized in that: described concentrated solution acid neutralization, refer to and add hydrochloric acid neutralization.
13. according to claim 12ly extract half fine membrane concentration technique with viscose fiber pressed liquor for raw material, it is characterized in that: described to add in hydrochloric acid and after, concentrated solution, again through nanofiltration membrane desalination, obtains half fine liquid.
14. is according to claim 13 with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre, it is characterized in that: the molecular weight cut-off of described nanofiltration membrane is 100-200.
15. is according to claim 13 with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre, it is characterized in that: the mistake mould difference of described nanofiltration membrane is 3-4bar, and temperature is 30-40 DEG C, and single filtration area is 26.8 m 2.
16. is according to claim 13 with the membrane concentration technique of viscose fiber pressed liquor for raw material extraction half fibre, it is characterized in that: the material liquid volume before described nanofiltration membrane concentrates is 10-15 times of concentrated solution volume.
17. according to claim 13ly extract half fine membrane concentration technique with viscose fiber pressed liquor for raw material, it is characterized in that: described in obtain half fine liquid specific conductivity be 8000-10000 μ s/cm, ignition residue is 3-6%.
CN201410622171.8A 2014-11-07 2014-11-07 Membrane concentration process for extracting hemicellulose by using viscose fiber extruded liquid as raw material Pending CN104387506A (en)

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CN111661967A (en) * 2020-05-21 2020-09-15 莱特莱德(北京)环境技术股份有限公司 System and method for recovering alkali in viscose fiber production squeezing waste liquid by using double-membrane method

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CN102643935A (en) * 2012-04-11 2012-08-22 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
CN103349909A (en) * 2013-07-24 2013-10-16 宜宾海丝特纤维有限责任公司 Post-processing method for squeezed alkali liquid in diffusion dialysis recycling viscose manufacture
CN103572635A (en) * 2013-05-28 2014-02-12 上海凯鑫分离技术有限公司 Processing and recovering process of chemical fiber pulp cellulose alkali pressed liquor

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CN102643935A (en) * 2012-04-11 2012-08-22 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
CN103572635A (en) * 2013-05-28 2014-02-12 上海凯鑫分离技术有限公司 Processing and recovering process of chemical fiber pulp cellulose alkali pressed liquor
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Publication number Priority date Publication date Assignee Title
CN111661967A (en) * 2020-05-21 2020-09-15 莱特莱德(北京)环境技术股份有限公司 System and method for recovering alkali in viscose fiber production squeezing waste liquid by using double-membrane method

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