CN103352277B - The pretreating process of press lye in viscose production is reclaimed in a kind of diffusion dialysis - Google Patents
The pretreating process of press lye in viscose production is reclaimed in a kind of diffusion dialysis Download PDFInfo
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Abstract
The present invention relates to the pretreating process that press lye in viscose production is reclaimed in a kind of diffusion dialysis, belong to technical field of viscose production.Naoh concentration is 50-200g/L by the present invention, and hemicellulose concentration is the press lye of 20-150g/L is first 1100-1300g/m through the aperture of filter cloth
2flame filter press filtration treatment, then be the ultrafiltration membrance filter process of 20-1000A ° through aperture, reduce large granular impurity concentration, obtain the pretreatment fluid carrying out diffusion dialysis process for cation-exchange membrane.The present invention is directed to the diffusion dialysis technique being applied to and reclaiming viscose press lye, specific preprocess method is adopted to process press lye, enter diffusion dialysis process again, improve the rate of recovery of alkali and hemicellulose in press lye, reduce alkali lye to the damage of diffusion dialysis membranous system, prevent the blocking to diffusion dialysis film, improve service life of film, and ensure that carrying out smoothly of diffusion dialysis and subsequent handling.
Description
Technical field
The present invention relates to the technique of material process in a kind of Chemical Manufacture, more particularly, the present invention relates to the pretreating process that press lye in viscose production is reclaimed in a kind of diffusion dialysis, belong to technical field of viscose production.
Background technology
Production process of viscose fiber in chemical fibre industry, can produce the akaline liquid containing high-enriched organics (based on hemicellulose).If let alone direct discharge, serious environmental pollution will be caused.If adopt this alkali lye of method process of neutralization, a large amount of acid will be consumed, and cause in alkali lye and form a large amount of inorganic salts, therefore the alkali in this alkali lye is reclaimed, and make organic matter wherein become the solid matter that can carry out harmless treatment to be only the processing mode more friendly to environment.
Viscose staple fibre is the cellulose reprocessing product be present in natural products, have water suction moisturizing, smooth nice and cool, ventilative, antistatic, dye the characteristic such as gorgeous.Its production process is with bamboo, wood, cotton, the pulps be rich in obtained by cellulosic plant such as fiber crops are raw material, flood through caustic soda, yellow, and regenerate in acid coagulating bath thus obtain viscose product, flood at caustic soda, the link of squeezing can produce above-mentioned akaline liquid, this akaline liquid is called press lye, be different from the spent lye that other industry produces, its composition is mainly NaOH and hemicellulose, at present effective means are also lacked to the alkali collection in this alkali lye, although adopt Nanofiltering membrane to reclaim alkali in minority field, but still it is low to there is the rate of recovery, the shortcoming that operating cost is high.
Diffusion dialysis utilizes pellicle or perm-selective ion-ex-change membrane, and make the process that the solute in solution is moved to low concentration side by film by high concentration side, this process take concentration difference as power.It is mainly used in organic and abstraction and purification that is inorganic electrolyte.In environmental project, be mainly used in process and the recovery of Suan ﹑ alkali wasteliquid at present.
The beginning of the fifties in 19th century, Englishize scholar T. Graham Sodd method of investing starts the diffusion systematically studying solution, have studied again the characteristic of different solute by pellicle (film that parchment or celloidin etc. are made) subsequently, find that the molecule of some solutes or ion are by the larger colloidal particle then intransitable phenomenon of the pore of pellicle, Graham Sodd method of investing claims this phenomenon to be dialysis.The equipment around this principle made is called dialyzer, is usually used in the purification of the macromolecular compounds such as the concentrated of colloidal solution and the sour ﹑ protein of core.The 1950's, there is the diffusion dialysis device using amberplex as barrier film.
Domesticly just have developed diffusion dialysis film as far back as 1964.But due to the restriction of film preparation technique, the structure of the similar homogeneous phase ionic membrane of the film obtained, as polysulfones quaternary ammonium cavity block S203, DF120 and chlorinated polyvinyl chloride type weak alkaline ionexchange memberanes are all this type of film.
In diffusion dialysis process, the motive force of ion transmission is the concentration difference of film both sides, and the homo-ion repulsion that application Donnan (Donnan) balances and electroneutral maintain correlation theory, realizes the selectively penetrating of ion thus reaches the object of separation.This process is divided into anode membrane diffusion dialysis (recovery as alkali) and cavity block diffusion dialysis (recovery as acid).Wherein cavity block diffusion dialysis technology utilizes anion-exchange membrane to realize acid and being separated of salt to hydrogen ion is different from the selective penetrated property of metal ion, such as the mixed solution of hydrochloric acid and aluminium chloride and water are placed in respectively the both sides of anion-exchange membrane, because the acid of solution side and the concentration of salt are far above water side, the trend of acid and salt oriented water side infiltration, but anion-exchange membrane has selective penetrated property, often kind of ion can not be allowed to pass through with equal opportunity; First anionic membrane skeleton itself is positively charged, have in the solution and attract electronegative ion hydration and repel the characteristic of positively charged ion hydration, therefore under the effect of concentration difference, the chlorion of solution side is attracted and successfully enters the side of water through fenestra road; Simultaneously according to electroneutral requirement, the ion with positive charge also can be carried secretly, but due to H
+hydrated radius smaller, electric charge is less, and aluminum ions ion hydration radius is larger, again with high valence charge, therefore hydrogen ion can be preferential by film, and the acid in such solution will be separated into water inlet side, the hydrionic key by being diffusion dialysis in this process.Amberplex used needs to possess some suitable performances, such as stability in an acidic solution, and high hydrogen ion percent of pass, to high rate of rejection and the low water percent of pass etc. of metal ion.Anode membrane diffusion dialysis process for alkali collection is similar with it.
Abroad, the technical development that acid is reclaimed in diffusion dialysis is comparatively rapid, and wherein representative country is the U.S. and Japan.The Exergy technique company of the U.S. develops a kind of online diffusion dialysis technology newly, and pushes commercial Application to.This technique adopts amberplex process Waste Sulfuric Acid, makes it recycle.System utilizes flowmeter and liquid level gauge to control, and is designed to full-automatic mode, is provided with grid spacer between film, stablizes to keep lamination.The rate of recovery of acid can reach 88%, and metal rejection reaches 95%, and greatly reduce the dialysis liquid measure delivering to Waste Water Treatment, thus reduce the consumption of neutralization chemicals, energy consumption also greatly reduces.
It is CN1450001 that State Intellectual Property Office discloses a publication number in 2003.10.22, the patent of invention that name is called " reclaiming the method for alkali in chemical fibre waste fluid and hemicellulose ", the patent provides a kind of method reclaiming alkali in chemical fibre waste fluid and hemicellulose.Method of the present invention comprises the steps: the pressed liquor containing alkali and hemicellulose to enter membrane separation device through pre-filtering and essence filter, obtain the permeate containing alkali and the concentrate containing hemicellulose, in the permeate obtained, concentration of lye can reach 80-250 grams per liter, in concentrate, final alkali content is 5-30 grams per liter, and hemicellulose level is 100-200 grams per liter.Hemicellulose and alkali lye not only obtain effective abstraction and purification, and technical process is simple, and the hemicellulose in concentrate and the alkali in filter liquor are convenient to be used respectively, not only make use of resource but also protect environment.This technological transformation tradition liquid waste processing mode is adopted to have investment short for return period, high financial profit and the good feature of environmental benefit.The popularization and application of this technology will promote the overall industrial level of chemical fibre industry.
Above-mentioned patent is the recovery adopting conventional membrane filtration technique to carry out alkali lye and hemicellulose, although the press lye in producing viscose has certain recovering effect, still there is the rate of recovery not high, energy consumption is large, cannot online recycling and recycle.
The above all shows that the technology of diffusion dialysis reclamation film has other membrane process and the incomparable advantage of the way of distillation, but current diffusion dialysis is mainly used in acid recovery, and it is little for the diffusion dialysis film of alkali collection, even for the recovery of alkali in alkali lye, also be that other industry alkali lye is reclaimed, the constituent of its recycle object, index parameter differ comparatively large with the akaline liquid that viscose industry produces, the technology that existing diffusion dialysis cannot be reclaimed alkali is directly used in the akaline liquid produced in viscose technique.
It is CN102976450A that State Intellectual Property Office discloses a publication number in 2013.3.20, the patent of invention that name is called " a kind of viscose squeezes the alkali recovery process of waste liquid in producing ", which disclose during a kind of viscose is produced the alkali recovery process squeezing waste liquid, allow squeezing waste liquid and distilled water flow through cation-exchange membrane diffusion dialysis device inner chamber simultaneously, control squeezing waste liquid and the flow velocity of water, to make the squeezing waste liquid that flows out in cation-exchange membrane diffusion dialysis device NaOH content for 15-25g/L.This technique can effectively reclaim alkali in squeezing waste liquid for regenerative ratio, reduce acid consumption, reduce sewage disposal difficulty and reduce energy consumption, the beneficial effect reducing viscose production cost can be brought.
Diffusion dialysis technology is adopted to be applied to the alkali collection of the squeezing waste liquid in viscose production in above-mentioned patent, but the rate of recovery is not high, sodium hydrate content in liquid is after treatment only 15-25g/L, be difficult to direct reuse in viscose glue produce in other need alkali link, cause waste.And squeezing waste liquid is directly entered diffusion dialysis treating apparatus, can cause damage to film, affect carrying out smoothly of whole recovery process.
It is CN102941017A that State Intellectual Property Office discloses a publication number in 2013.2.27, the patent of invention that name is called " a kind of viscose produce in the secondary treatment method of waste alkali liquor ", this patent relates to the secondary treatment method of waste alkali liquor in the production of a kind of viscose, belongs to field of viscose fiber.The present invention will be pretreated through routine, naoh concentration is 70-90g/L, waste alkali liquor and the demineralized water of half fiber content 60-70g/L are delivered to diffusion dialysis membrane stack respectively, carry out diffusion dialysis, described preliminary treatment spent lye and the flow-rate ratio of demineralized water are 1-2:1, be separated by the alkali lye of the alkali lye of low hemicellulose concentration with the fine concentration of height half after diffusion dialysis, the alkali lye of described low hemicellulose concentration is back to production.The invention solves in prior art, waste alkali liquor through once recycling still can produce secondary waste alkali lye, if directly discharged, the problem of considerable damage can be caused environment, provide a kind of processing method of secondary waste alkali lye, pass through diffusion dialysis, the NaOH in waste alkali liquor can be reclaimed to greatest extent, reduce environmental pollution, improve ecological benefits, reduce the cost of environmental protection treatment simultaneously.
The same alkali collection adopting diffusion dialysis technology to be applied to the squeezing waste liquid in viscose production in above-mentioned patent, first waste liquid is carried out conventional preliminary treatment although refer in technical scheme, but still cannot for the press lye in viscose carry out specific cation-exchange membrane diffusion dialysis film reclaim process, can directly affect carrying out smoothly of the recovery of diffusion dialysis film and subsequent treatment and recycling, and the scope of the press lye that can process is narrower, process yield is low.
Summary of the invention
The present invention is intended to solve existing the diffusion dialysis technology Problems existing and the defect that are applied to the press lye reclaimed in viscose production, a kind of diffusion dialysis is provided to reclaim the pretreating process of press lye in viscose production, only for being applied to the cation-exchange membrane diffusion dialysis technique reclaiming viscose press lye, the press lye of specific preprocess method to specific indexes is adopted to process, cation-exchange membrane diffusion dialysis process is entered again after obtaining suitable pretreatment fluid, improve the rate of recovery and the yield of alkali and hemicellulose in press lye, reduce alkali lye to the damage of diffusion dialysis membranous system, improve the service life of film, and ensure carrying out smoothly of diffusion dialysis and subsequent handling.
In order to realize foregoing invention object, concrete technical scheme of the present invention is as follows:
Diffusion dialysis reclaim viscose produce in the pretreating process of press lye, it is characterized in that: be 50-200g/L by naoh concentration, hemicellulose concentration is the press lye of 20-150g/L is first 1100-1300g/m through the aperture of filter cloth
2flame filter press filtration treatment, then be the ultrafiltration membrance filter process of 20-1000A ° through aperture, reduce large granular impurity concentration, obtain the pretreatment fluid carrying out diffusion dialysis process for cation-exchange membrane.
Flame filter press of the present invention and the ultrafiltration membrance filter process naoh concentration controlled in the pretreatment fluid obtained are 50-200g/L, and hemicellulose concentration is 20-150g/L, and large granular impurity concentration is for being less than 1g/L.
Above-mentioned large granular impurity comprises bulky grain dust impurity, bulky grain metal impurities etc.
The of the present invention temperature of press lye control before flame filter press filters is 5-50 DEG C.
The Stress control of flame filter press of the present invention is 0.05-0.5Mpa.
The filter area of flame filter press of the present invention and the ratio of the flow of press lye control as 1m
2: 15-25m
3/ h.
Milipore filter of the present invention adopts Kynoar (PVDF).
The shape in the hole of milipore filter of the present invention is circular.
The Stress control of ultrafiltration of the present invention is 0.1-0.5Mpa.
The Advantageous Effects that the present invention brings:
1, the invention solves existing the diffusion dialysis technology Problems existing and the defect that are applied to the press lye reclaimed in viscose production, for being applied to the diffusion dialysis technique reclaiming viscose press lye, specific preprocess method is adopted to process press lye, obtain the pretreatment fluid of specific indexes, enter cation-exchange membrane diffusion dialysis process again, alkali concn and the wider press lye of hemicellulose concentration range can be applicable to, improve the rate of recovery and the yield of alkali and hemicellulose in press lye, decrease the damage of alkali lye to cation-exchange membrane diffusion dialysis membranous system, prevent the blocking to diffusion dialysis cation-exchange membrane, improve the service life of film, and ensure that carrying out smoothly of diffusion dialysis and subsequent handling.The aperture of flame filter press filter cloth is 1100-1300g/cm
2the aperture of milipore filter is 20-1000A °, the selection in above-mentioned aperture is applicable to process press lye of the present invention, effectively ensure that the service life of filter plant, in addition can the large molecule of effectively catching and other impurity, and press lye can be made or not again equipment or filter material because pressure is excessive along bad with good speed by worry machine, extension device service life, the selection in two kinds of apertures acts synergistically mutually, effectively reduces the large granular impurity concentration in press lye.
2, flame filter press of the present invention and the ultrafiltration membrance filter process naoh concentration controlled in the pretreatment fluid obtained are 50-200g/L, and hemicellulose concentration is 20-150g/L, and other bulky grain concentration are for being less than 1g/L.Also greatly reduce the content of large granular impurity, the index of above-mentioned pretreatment fluid is the entirety of three parameters, obtained by specific pretreatment mode, the combination of three parameters, synergy, the infringement of other materials to film can be reduced, reduce the frequency of film group device cleaning, the service life of extension device, what ensure diffusion dialysis processing procedure and subsequent treatment operation carries out reductions energy consumption smoothly, the Ethylene recov obtained after making diffusion dialysis in addition can efficiently, the recovery separation NaOH of high yield pulp1 and hemicellulose.
3, the of the present invention temperature of press lye control before flame filter press filters is 5-50 DEG C.Before preliminary treatment, temperature adjustment is carried out to press lye, and select this temperature range effectively can increase the speed of molecular motion, make to filter and carry out smoothly, also can reduce the damage of temperature to filter material in cation-exchange membrane diffusion dialysis equipment, the service life of extension device.
4, the Stress control of flame filter press of the present invention is 0.05-0.5Mpa; The aperture of flame filter press filter cloth is 1100-1300g/cm
2; The filter area of flame filter press and the discharge relation of press lye are 1m
2: 15-25m
3/ h.The preferred version that three technological parameters of above-mentioned plate-frame filtering are selected constitutes a parameter system, spent lye can be made or not again equipment or filter material damage because pressure is excessive with good speed by worry machine, effectively retain oarse-grained impurity, small part larger molecular organics and other impurity, and the strainability of flame filter press can be made full use of and ensure that the flux of press lye.
5, milipore filter of the present invention adopts Kynoar (PVDF); The aperture of milipore filter is 20-1000A °; The shape in the hole of described milipore filter is circular; The Stress control of described ultrafiltration is 0.1-0.5Mpa.Above-mentioned technological parameter selection, material selection etc. can make ultrafiltration membrance filter equipment more alkaline-resisting, be applicable to process press lye of the present invention, extend the service life of considering core, equipment, in addition can the large molecule of effectively catching and other impurity, and press lye can be made or not again equipment or filter material because pressure is excessive along bad with good speed by worry machine, extension device service life.
6, above-mentioned plate-frame filtering and ultrafiltration acting in conjunction, form pretreating process of the present invention, the technological parameter of above-mentioned two kinds of filter types is as a complete parameter system, complement each other, alkali concn and the wider press lye of hemicellulose concentration range can be applicable to, the pretreatment fluid obtained through preliminary treatment enters cation-exchange membrane diffusion dialysis again, improve the rate of recovery and the yield of alkali and hemicellulose in press lye, decrease the damage of alkali lye to cation-exchange membrane diffusion dialysis membranous system, prevent the blocking to diffusion dialysis cation-exchange membrane, improve the service life of film, and ensure that carrying out smoothly of diffusion dialysis and subsequent handling.
Accompanying drawing explanation
Fig. 1 is the structural representation of cation-exchange membrane diffusion dialysis device film group device of the present invention;
Reference numeral: 1 is the first clamping plate, 2 be the second clamping plate, 3 for press lye runner interlayer, 4 for absorption liquid runner interlayer, 5 for press lye import, 6 for absorption liquid import, 7 for raffinate outlet, 8 for Ethylene recov outlet, 9 be cation-exchange membrane, 10 be dividing plate.
Detailed description of the invention
embodiment 1
Diffusion dialysis reclaim viscose produce in the pretreating process of press lye, be 50g/L by naoh concentration, hemicellulose concentration is the press lye of 20g/L is first 1100g/m through the aperture of filter cloth
2flame filter press filtration treatment, then be the ultrafiltration membrance filter process of 20A ° through aperture, reduce large granular impurity concentration, obtain the pretreatment fluid carrying out diffusion dialysis process for cation-exchange membrane.
embodiment 2
Diffusion dialysis reclaim viscose produce in the pretreating process of press lye, be 200g/L by naoh concentration, hemicellulose concentration is the press lye of 150g/L is first 1300g/m through the aperture of filter cloth
2flame filter press filtration treatment, then be the ultrafiltration membrance filter process of 1000A ° through aperture, reduce large granular impurity concentration, obtain the pretreatment fluid carrying out diffusion dialysis process for cation-exchange membrane.
embodiment 3
Diffusion dialysis reclaim viscose produce in the pretreating process of press lye, be 125g/L by naoh concentration, hemicellulose concentration is the press lye of 85g/L is first 1200g/m through the aperture of filter cloth
2flame filter press filtration treatment, then be the ultrafiltration membrance filter process of 510A ° through aperture, reduce large granular impurity concentration, obtain the pretreatment fluid carrying out diffusion dialysis process for cation-exchange membrane.
embodiment 4
A pretreating process for press lye in viscose production is reclaimed in diffusion dialysis, is 180g/L by naoh concentration, and hemicellulose concentration is the aperture of the first machine filter cloth after filtration of press lye of 36g/L is 1150g/m
2flame filter press filtration treatment, then be the ultrafiltration membrance filter process of 800A ° through aperture, reduce large granular impurity concentration, obtain the pretreatment fluid carrying out diffusion dialysis process for cation-exchange membrane.
embodiment 5
On the basis of embodiment 1-4, preferred:
Index through the pretreatment fluid that preliminary treatment obtains:
Described flame filter press and the ultrafiltration membrance filter process naoh concentration controlled in the pretreatment fluid obtained are 50g/L, and hemicellulose concentration is 20g/L, and large granular impurity concentration is for being less than 1g/L.
Temperature adjustment process before preliminary treatment:
Described controls to be 5 DEG C by the temperature of press lye before flame filter press filters.
Plate-frame filtering:
The Stress control of described flame filter press is 0.05Mpa.
The filter area of described flame filter press and the ratio of the flow of press lye control as 1m
2: 15m
3/ h.
Ultrafiltration membrance filter:
Described milipore filter adopts Kynoar (PVDF).
The shape in the hole of described milipore filter is circular.
The Stress control of described ultrafiltration is 0.1Mpa.
embodiment 6
On the basis of embodiment 1-4, preferred:
Index through the pretreatment fluid that preliminary treatment obtains:
Described flame filter press and the ultrafiltration membrance filter process naoh concentration controlled in the pretreatment fluid obtained are 200g/L, and hemicellulose concentration is 150g/L, and large granular impurity concentration is for being less than 1g/L.
Temperature adjustment process before preliminary treatment:
Described controls to be 50 DEG C by the temperature of press lye before flame filter press filters.
Plate-frame filtering:
The Stress control of described flame filter press is 0.5Mpa.
Described flame filter press
The filter area of described flame filter press and the ratio of the flow of press lye control as 1m
2: 25m
3/ h.
Ultrafiltration membrance filter:
Described milipore filter adopts Kynoar (PVDF).
The shape in the hole of described milipore filter is circular.
The Stress control of described ultrafiltration is 0.5Mpa.
embodiment 7
On the basis of embodiment 1-4, preferred:
Index through the pretreatment fluid that preliminary treatment obtains:
Described flame filter press and the ultrafiltration membrance filter process naoh concentration controlled in the pretreatment fluid obtained are 125g/L, and hemicellulose concentration is 85g/L, and large granular impurity concentration is for being less than 1g/L.
Temperature adjustment process before preliminary treatment:
Described controls to be 28 DEG C by the temperature of press lye before flame filter press filters.
Plate-frame filtering:
The Stress control of described flame filter press is 0.275Mpa.
The filter area of described flame filter press and the ratio of the flow of press lye control as 1m
2: 20m
3/ h.
Ultrafiltration membrance filter:
Described milipore filter adopts Kynoar (PVDF).
The shape in the hole of described milipore filter is circular.
The Stress control of described ultrafiltration is 0.3Mpa.
embodiment 8
On the basis of embodiment 1-4, preferred:
Index through the pretreatment fluid that preliminary treatment obtains:
Described flame filter press and the ultrafiltration membrance filter process naoh concentration controlled in the pretreatment fluid obtained are 180g/L, and hemicellulose concentration is 36g/L, and large granular impurity concentration is for being less than 1g/L.
Temperature adjustment process before preliminary treatment:
Described controls to be 39 DEG C by the temperature of press lye before flame filter press filters.
Plate-frame filtering:
The Stress control of described flame filter press is 0.4Mpa.
The filter area of described flame filter press and the ratio of the flow of press lye control as 1m
2: 21m
3/ h.
Ultrafiltration membrance filter:
Described milipore filter adopts Kynoar (PVDF).
The shape in the hole of described milipore filter is circular.
The Stress control of described ultrafiltration is 0.21Mpa.
embodiment 9
Diffusion dialysis is carried out by cation-exchange membrane:
The method of press lye in viscose production is reclaimed in a kind of diffusion dialysis, be 50-200g/L by naoh concentration, hemicellulose concentration is that the press lye of 20-150g/L reduces large granular impurity concentration through filtering preliminary treatment, then enter in diffusion dialysis film group device with the demineralized water as absorption liquid, flow in the mode of cross-flow, carry out diffusion dialysis by cation-exchange membrane, be recycled alkali lye; Gauge pressure in described diffusion dialysis process is 0.03-0.08MPa.
The described naoh concentration reduced through filtering preliminary treatment in the press lye of large granular impurity concentration controls as 50-200g/L, and hemicellulose concentration controls as 20-150g/L, and large granular impurity content controls as being less than 1g/L.
Above-mentioned large granular impurity comprises bulky grain dust impurity, bulky grain metal impurities etc.
Described cation-exchange membrane is with the cloth of a kind of or two kinds of cospinning shapes in nylon, polypropylene, polyvinyl chloride, polytetrafluoroethylene (PTFE) for basement membrane, then with the alkaline-resisting cation-exchange membrane that perfluorinated sulfonic acid is filmed with rubbing method.
The thickness of above-mentioned basement membrane is 0.05-2mm.
The aperture of described cation-exchange membrane is 5-10nm.
Width of flow path in described diffusion dialysis film group device is 0.2-1mm.
The flow control of described press lye is 2-20mm/s, and the flow control of described demineralized water is 3-25mm/s.
In described diffusion dialysis film group device, the clearance control often between adjacent two cation-exchange membranes is 0.4-0.9mm.
Naoh concentration in described recovery alkali lye controls as 40-160g/L, and hemicellulose concentration controls as < 10g/L.
embodiment 10
Diffusion dialysis reclaimed after post processing:
The post-processing approach of press lye in viscose production is reclaimed in a kind of diffusion dialysis, be 50-200g/L by naoh concentration, hemicellulose concentration is that the press lye of 20-150g/L reduces large granular impurity concentration through filtering preliminary treatment, again through cation-exchange membrane diffusion dialysis process, the Ethylene recov of low hemicellulose level obtain separation and the raffinate of hemicellulose content carry out post processing; Described post processing is carried out concentrating or diluting post processing by the Ethylene recov of low hemicellulose level, reclaims alkali lye, in being carried out by the raffinate of hemicellulose content and post processing, reclaims hemicellulose.
The described naoh concentration reduced through filtering preliminary treatment in the press lye of large granular impurity concentration controls as 50-200g/L, and hemicellulose concentration controls as 20-150g/L, and the concentration of large granular impurity controls as being less than 1g/L.
Above-mentioned large granular impurity comprises bulky grain dust impurity, bulky grain metal impurities etc.
The naoh concentration that described cation-exchange membrane diffusion dialysis process controls in the Ethylene recov of the low hemicellulose level obtained is 40-160g/L, and hemicellulose concentration is < 10g/L.
The described concentrated post processing carried out low hemicellulose Ethylene recov, the naoh concentration controlled in the alkali lye obtained is 160-420g/L, and hemicellulose concentration is < 10g/L.
The described dilution post processing carried out low hemicellulose Ethylene recov, the naoh concentration controlled in the alkali lye obtained is 0.5-40g/L, and hemicellulose concentration is < 10g/L.
The described concentrated post processing carried out low hemicellulose Ethylene recov is reverse osmosis concentration or distillation and concentration.
Above-mentioned reverse osmosis concentration adopts hollow fiber form membrane module, and the external diameter of doughnut is 50-200 μm, and internal diameter is 25-42 μm.
The Stress control of above-mentioned reverse osmosis concentration is 100-1000psi.
The temperature of above-mentioned reverse osmosis concentration controls as 0-45 DEG C.
The Stress control of above-mentioned distillation and concentration is 0.08-0.2Mpa.
The heating and temperature control of above-mentioned distillation and concentration is 80-120 DEG C.
The condensation temperature of above-mentioned distillation and concentration controls as 0-25 DEG C.
Described dilutes for adding demineralized water in low hemicellulose Ethylene recov the dilution post processing that low hemicellulose Ethylene recov carries out.
The described cation-exchange membrane diffusion dialysis process naoh concentration controlled in the raffinate of the hemicellulose content obtained is 8-15g/L, and hemicellulose concentration is 20-50g/L.
During the described raffinate to hemicellulose content carries out and post processing refer to and adopt the raffinate of acid solution and hemicellulose content to carry out mix and blend, hemicellulose precipitate, and supernatant enters biochemistry pool process, discharge after biochemical treatment is up to standard.
The concentration of above-mentioned acid solution is 0.1-2.5mol/L.
The addition of above-mentioned acid solution is the volume ratio of the raffinate of described acid solution and hemicellulose content is 1:0.5-25.
Above-mentioned acid solution is sulfuric acid solution, hydrochloric acid solution or salpeter solution.
embodiment 11
Preparation method for the cation-exchange membrane of diffusion dialysis:
The selection of A, basement membrane
Select with a kind of cloth in nylon, polypropylene and polyvinyl chloride, or the cloth of any two cospinning shape is basement membrane;
The irradiation activation of B, basement membrane
Activate under the basement membrane of steps A is placed in electron beam irradiation under nitrogen atmosphere, described activation adopts the electron linear accelerator of 10Mev, and irradiation dose controls as 2-20kgy.
C, functional group grafting process
Functional group grafting is carried out through the basement membrane of irradiation activation by step B;
D, sulfonation process
By being catalyst through the basement membrane of grafting with silver sulfate in step C, be that sulfonating agent carries out sulfonation with the concentrated sulfuric acid, then through cooling, be separated, take out obtain of the present invention be applicable to diffusion dialysis reclaim viscose produce in the cation-exchange membrane of press lye.
In step C, described refer to the basement membrane through irradiation activation in step B to be soaked in the mixed solution of styrene, divinylbenzene and benzoyl peroxide carry out functional group grafting by carrying out functional group grafting through the basement membrane of irradiation activation in step B.
The amount ratio of above-mentioned styrene, divinylbenzene and benzoyl peroxide is 70-90:10-20:0.1-1.
In step D, in described sulfonation process, sulfonation temperature is 40-60 DEG C.
In step D, in described sulfonation process, sulfonation time is 5-7 hour.
embodiment 12
As shown in Figure 1, for the film group device of diffusion dialysis:
A kind of film group device being applicable to press lye in the production of diffusion dialysis recovery viscose, comprise the first clamping plate 1, second clamping plate 2, dividing plate 10 and cation-exchange membrane 9, described dividing plate 10 is multiple with cation-exchange membrane 9, and interval is alternately stacked, and compress mutually, described dividing plate 10 is squeezed alkali lye runner interlayer 3 with cation-exchange membrane 9 and absorption liquid runner interlayer 4 clamps, and described press lye runner interlayer 3 and absorption liquid runner interlayer 4 are clamped by the first clamping plate 1 and the second clamping plate 2 again.
Described press lye runner interlayer 3 bottom is provided with press lye import 5, and top is provided with raffinate outlet 7.
Described absorption liquid runner interlayer 4 bottom is provided with absorption liquid import 6, and top is provided with Ethylene recov outlet 8.
Be provided with polytetrafluoroethylene sealing gasket sheet between described dividing plate 10, thickness is 0.1-0.15mm.
In described cation-exchange membrane 9, the distance often between adjacent two cation-exchange membranes 9 is 0.4-0.9mm.
Described cation-exchange membrane 9 is perfluorinated sulfonic acid cation-exchange membrane.
The aperture of described cation-exchange membrane 9 is 5-10nm.
Width of flow path in described press lye runner interlayer 3 and absorption liquid runner interlayer 4 is 0.2-1mm.
Claims (3)
1. diffusion dialysis reclaim viscose produce in the pretreating process of press lye, it is characterized in that: be 180g/L by naoh concentration, hemicellulose concentration is 36g/L, and it is first 1150g/m through the aperture of filter cloth that temperature controls to be the press lye of 39 DEG C
2, Stress control is the flame filter press filtration treatment of 0.4MPa, and the filter area of flame filter press and the ratio of the flow of press lye control as 1m
2: 21m
3/ h, be the ultrafiltration membrance filter process of 800A ° again through aperture, the Stress control of ultrafiltration is 0.21MPa, reduce large granular impurity concentration, obtain carrying out diffusion dialysis process for cation-exchange membrane, naoh concentration is 180g/L, and hemicellulose concentration is 36g/L, and large granular impurity concentration is the pretreatment fluid being less than 1g/L.
2. the pretreating process of press lye in viscose production is reclaimed in a kind of diffusion dialysis according to claim 1, it is characterized in that: described milipore filter adopts Kynoar.
3. the pretreating process of press lye in viscose production is reclaimed in a kind of diffusion dialysis according to claim 1 and 2, it is characterized in that: the shape in the hole of described milipore filter is for circular.
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| CN101851030A (en) * | 2009-03-30 | 2010-10-06 | 广州中科建禹水处理技术有限公司 | Technical method for purifying and reutilizing jean silkete alkali waste liquid by membrane method |
| CN102941017A (en) * | 2012-11-26 | 2013-02-27 | 宜宾海丝特纤维有限责任公司 | Process for secondary treating of waste alkali liquid during production of viscose fibers |
| CN102963994A (en) * | 2012-11-26 | 2013-03-13 | 宜宾海丝特纤维有限责任公司 | Treatment method of waste alkali liquor in production of viscose fibers |
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| CN100567156C (en) * | 2007-02-14 | 2009-12-09 | 湖州东洋水处理设备有限公司 | Adopt ultra-filtration membrane to purify and reclaim the method and apparatus of silking dirt alkali |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101851030A (en) * | 2009-03-30 | 2010-10-06 | 广州中科建禹水处理技术有限公司 | Technical method for purifying and reutilizing jean silkete alkali waste liquid by membrane method |
| CN102941017A (en) * | 2012-11-26 | 2013-02-27 | 宜宾海丝特纤维有限责任公司 | Process for secondary treating of waste alkali liquid during production of viscose fibers |
| CN102963994A (en) * | 2012-11-26 | 2013-03-13 | 宜宾海丝特纤维有限责任公司 | Treatment method of waste alkali liquor in production of viscose fibers |
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