CN103351064B - The millipore filtration pretreatment technology of pressed liquor electrodialysis alkali collection produced by viscose fiber - Google Patents
The millipore filtration pretreatment technology of pressed liquor electrodialysis alkali collection produced by viscose fiber Download PDFInfo
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- CN103351064B CN103351064B CN201310311777.5A CN201310311777A CN103351064B CN 103351064 B CN103351064 B CN 103351064B CN 201310311777 A CN201310311777 A CN 201310311777A CN 103351064 B CN103351064 B CN 103351064B
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Abstract
The present invention proposes the millipore filtration pretreatment technology of pressed liquor electrodialysis alkali collection in the production of a kind of viscose fiber, it is characterized in that: NaOH content is that the pressed liquor of 50 ~ 200g/L first filters out oarse-grained impurity by flame filter press, enter millipore filter by pump again, obtain sig water for follow-up electrodialysis process.The present invention produces the characteristic of the high density salkali waste containing hemicellulose according to viscose fiber in expressing process, first pre-treatment is carried out to salkali waste, the index of waste lye is made to be applicable to follow-up electrodialysis alkali recovery process, thus reduce the viscosity of waste liquid, effective reduction energy consumption, improves osmotic efficiency, stable.
Description
Technical field
The invention belongs to the Waste recovery technical field in viscose fiber production, be specifically related to a kind of millipore filtration pretreatment technology of the pressed liquor electrodialysis alkali collection be applicable in viscose fiber production.
Background technology
Viscose fiber is the man-made fiber utilizing macromolecular material wood pulp, cotton pulp etc. containing natural cellulose to process through chemistry and mechanical means.Viscose fiber is kind the most close with natural fiber clothes performance in chemical fibre, have soft, moisture absorption is breathed freely, it is elegant to overhang, bright, be antistaticly comparatively easy to the features such as textile process, being come from sky but be better than natural regenerated cellulose fibre, is one of important materials of textile industry raw material.China has viscose fiber enterprise about 40 at present, and except production common viscose fiber (long filament, staple fibre) and high-tenacity fibre, the viscose fiber of high wet modulus fibrid and special property also has production.
A large amount of industrial chemicals is needed in production process of viscose fiber, a large amount of waste water can be produced, these waste water contain sulfuric acid, zinc sulfate, dithiocarbonic anhydride, Mierocrystalline cellulose, dissolved organic matter etc., and all producing very large harm to environment, is one of primary pollution source of textile industry.
In production process of viscose fiber, need by dipping method, the hemicellulose in raw material to be dissolved out with alkaline solution, otherwise extremely adverse influence can be produced to production technique and final product quality.Therefore, when producing viscose fiber, needing in process procedure, arrange press lye treating plant, from steeping lye system, separating a certain amount of hemicellulose.And the high density salkali waste that can produce in expressing process containing hemicellulose, for reducing production cost, reduce alkaline consumption, current each chemical fiber factory mainly adopts dialysis technique to be separated half fibre to carry out recycle of alkali liquor.But dialysis technique reclaims alkali lye inefficiency, and water consumption is large, and takies larger floor area of building, progressively eliminates.The electrodialysis alkali recovery technology developed rapidly is in recent years expected to replace dialysis technique and carries out recycle of alkali liquor, improves the quality of products and waste water utilization rate.
201210486339.8, the application for a patent for invention that name is called " a kind of viscose fiber produce in the secondary treatment method of waste alkali liquor ", this patent will be pretreated through routine, naoh concentration is 70 ~ 90g/L, waste alkali liquor and the de-mineralized water of half fibre content 60 ~ 70g/L are delivered to millipore filtration membrane stack respectively, carry out millipore filtration, described pre-treatment waste lye and the throughput ratio of de-mineralized 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 millipore filtration, the alkali lye of described low hemicellulose concentration is back to production.During this patent adopts the method for millipore filtration to produce viscose fiber, waste alkali liquor reclaims, before millipore filtration, ordinary method is adopted to carry out pre-treatment to waste lye, but, reclaim waste lye by electrodialytic method at present, also be not widely used in viscose fiber is produced, because the chemical composition in viscose fiber waste lye is different from general black liquor, use conventional pretreated alkali lye, electrodialytic technical requirements can not be met, the result of process is undesirable, and alkali recovery is not high.
03116938.4, the patent of invention that name is called " alkali in recovery chemical fibre waste fluid and the method for hemicellulose ", provide a kind of method reclaiming alkali in chemical fibre waste fluid and hemicellulose, the pressed liquor containing alkali and hemicellulose is comprised the steps: to enter membrane separation unit through pre-filtering and essence filter, obtain the permeate containing alkali and the concentrated solution containing hemicellulose, in the permeate obtained, concentration of lye can reach 80 ~ 250 grams per liters, in concentrated solution, final alkali content is 5 ~ 30 grams per liters, and hemicellulose level is 100 ~ 200 grams per liters.This patent does not take into full account the singularity of the chemical composition in viscose fiber waste lye equally, uses the alkali recovery of the further membrane sepn of conventional pretreated alkali lye low.
Summary of the invention
The present invention is directed to above-mentioned technical problem, propose the millipore filtration pretreatment technology of pressed liquor electrodialysis alkali collection in the production of a kind of viscose fiber, in expressing process, the characteristic of the high density salkali waste containing hemicellulose is produced according to viscose fiber, first pre-treatment is carried out to salkali waste, the index of waste lye is made to be applicable to follow-up electrodialysis alkali recovery process, thus reduce the viscosity of waste liquid, effectively reduce energy consumption, improve osmotic efficiency, stable.
For achieving the above object, the present invention adopts following technical scheme:
The millipore filtration pretreatment technology of pressed liquor electrodialysis alkali collection in viscose fiber production, it is characterized in that: NaOH content is that the pressed liquor of 50 ~ 200g/L first filters out oarse-grained impurity by flame filter press, enter millipore filter by pump again, obtain sig water for follow-up electrodialysis process.
Pressed liquor naoh concentration after pretreatment is 50 ~ 200g/L, and half fibre content is 20 ~ 150g/L.
In described flame filter press, the density of filter cloth is 1100 ~ 1300g/m
2.
The working pressure of described flame filter press is 0.05-0.5Mpa, and flow is 20m
3/ (h*m
2).
The filter cloth surface of described flame filter press scribbles diatomite, can prevent filter cloth duct from being blocked by the particle of microorganism, and can the filtrate obtaining at the very start clarifying, and meanwhile, the flintiness of filter cake is reduced, voidage increases, and contributes to improving filtering velocity.
The diatomaceous thickness of described filter cloth surface is 2mm.
The service temperature of described millipore filter is 20 ~ 40 DEG C, and pressure is 0.1 ~ 0.5Mpa.
The membrane pore size of described millipore filter is 0.1 ~ 0.2 μm.
Described millipore filter, when pressed liquor is greater than 0.08Mpa by the Pressure Drop of filter core, namely cleans filter core.
Beneficial effect of the present invention is:
1, the present invention produces the characteristic producing the high density salkali waste containing hemicellulose in expressing process according to viscose fiber, adopt the pretreatment technology of flame filter press-millipore filtration, the index of pressed liquor is made to be applicable to follow-up electrodialysis alkali recovery process, thus reduce the viscosity of waste liquid, effective reduction energy consumption, improves osmotic efficiency, stable.
2, due to the high density salkali waste containing hemicellulose can be produced in production process of viscose fiber, according to this characteristic, the present invention have selected the special process parameter system of optimization, first remove the suspended substance in pressed liquor by flame filter press, carry out initial filter by millipore filtration to waste lye again, thus make pressed liquor naoh concentration be 50 ~ 200g/L, half fibre content is 20 ~ 150g/L, meet electrodialysis requirement, alkali lye can be reclaimed better.
3, the present invention smears diatomite at the filter cloth surface of flame filter press, can prevent filter cloth duct from being blocked by the particle of microorganism, and can the filtrate obtaining at the very start clarifying, and meanwhile, the flintiness of filter cake is reduced, voidage increases, and contributes to improving filtering velocity.
4, the present invention controls pressed liquor and is greater than 0.08Mpa by the Pressure Drop of millipore filter filter core, namely filter core is cleaned, because the Mierocrystalline cellulose in pressed liquor easily blocks filter core, should carry out slightly in advance, when Pressure Drop is greater than 0.08Mpa, just should clean filter core, otherwise filter core not easily cleans up, filtrate can be made if things go on like this to produce caking.
Embodiment
Below in conjunction with embodiment, essentiality content of the present invention is described in further detail.
Embodiment 1
The millipore filtration pretreatment technology of pressed liquor electrodialysis alkali collection in viscose fiber production: NaOH content is that the pressed liquor of 165g/L first filters out oarse-grained impurity by flame filter press, enter millipore filter by pump again, obtain sig water for follow-up electrodialysis process.
Embodiment 2
The millipore filtration pretreatment technology of pressed liquor electrodialysis alkali collection in viscose fiber production: NaOH content is that the pressed liquor of 50g/L first filters out oarse-grained impurity by flame filter press, enter millipore filter by pump again, obtain sig water for follow-up electrodialysis process.
Pressed liquor naoh concentration after pretreatment is 50g/L, and half fibre content is 20g/L.
Embodiment 3
The millipore filtration pretreatment technology of pressed liquor electrodialysis alkali collection in viscose fiber production: NaOH content is that the pressed liquor of 200g/L first filters out oarse-grained impurity by flame filter press, enter millipore filter by pump again, obtain sig water for follow-up electrodialysis process.
Pressed liquor naoh concentration after pretreatment is 200g/L, and half fibre content is 150g/L.
Embodiment 4
The present embodiment is substantially the same manner as Example 3, on this basis:
In described flame filter press, the density of filter cloth is 1100g/m
2.
Pressed liquor naoh concentration after pretreatment is 120g/L, and half fibre content is 80g/L.
Embodiment 5
The present embodiment is substantially the same manner as Example 3, on this basis:
In described flame filter press, the density of filter cloth is 1300g/m
2.
The working pressure of described flame filter press is 0.05Mpa, and flow is 20m
3/ (h*m
2).
Pressed liquor naoh concentration after pretreatment is 150g/L, and half fibre content is 85g/L.
Embodiment 6
The present embodiment is substantially the same manner as Example 3, on this basis:
In described flame filter press, the density of filter cloth is 1200g/m
2.
The working pressure of described flame filter press is 0.5Mpa, and flow is 20m
3/ (h*m
2).
The filter cloth surface of described flame filter press scribbles diatomite.
Pressed liquor naoh concentration after pretreatment is 156g/L, and half fibre content is 23g/L.
Embodiment 7
The present embodiment is substantially the same manner as Example 3, on this basis:
In described flame filter press, the density of filter cloth is 1150g/m
2.
The working pressure of described flame filter press is 0.2Mpa, and flow is 20m
3/ (h*m
2).
The filter cloth surface of described flame filter press scribbles diatomite.
Diatomaceous thickness is 2mm.
Pressed liquor naoh concentration after pretreatment is 160g/L, and half fibre content is 36g/L.
Embodiment 8
The present embodiment is substantially the same manner as Example 7, on this basis:
The service temperature of described millipore filter is 20 DEG C, and pressure is 0.1Mpa.
Pressed liquor naoh concentration after pretreatment is 151g/L, and half fibre content is 35g/L.
Embodiment 9
The present embodiment is substantially the same manner as Example 7, on this basis:
The service temperature of described millipore filter is 40 DEG C, and pressure is 0.5Mpa.
The membrane pore size of described millipore filter is 0.1 μm.
Pressed liquor naoh concentration after pretreatment is 175g/L, and half fibre content is 32g/L.
Embodiment 10
The present embodiment is substantially the same manner as Example 7, on this basis:
The service temperature of described millipore filter is 30 DEG C, and pressure is 0.2Mpa.
The membrane pore size of described millipore filter is 0.15 μm.
Described millipore filter, when pressed liquor is greater than 0.08Mpa by the Pressure Drop of filter core, namely cleans filter core.
Pressed liquor naoh concentration after pretreatment is 182g/L, and half fibre content is 45g/L.
Embodiment 11
The present embodiment is substantially the same manner as Example 7, on this basis:
The service temperature of described millipore filter is 25 DEG C, and pressure is 0.12Mpa.
The membrane pore size of described millipore filter is 0.16 μm.
Described millipore filter, when pressed liquor is greater than 0.08Mpa by the Pressure Drop of filter core, namely cleans filter core.
Pressed liquor naoh concentration after pretreatment is 165g/L, and half fibre content is 56g/L.
Embodiment 12
The present embodiment is substantially the same manner as Example 11, on this basis:
Waste lye after pretreatment and de-mineralized water are entered membrane module by the throughput ratio of 1.6:1 by pump and is delivered to electrodialysis film group device, carry out electrodialysis and reclaim alkali lye.
Described waste lye and de-mineralized water enter electrodialysis film group device in the mode of cross-flow.
Recovery concentration of lye after electrodialysis is 281g/L, and containing half fine 8.5g/L, recycle of alkali liquor rate is 85%.
Embodiment 13
The present embodiment is substantially the same manner as Example 11, on this basis:
Waste lye after pretreatment and de-mineralized water are entered membrane module by the throughput ratio of 1.5:1 by pump and is delivered to electrodialysis film group device, carry out electrodialysis and reclaim alkali lye.
Described waste lye and de-mineralized water enter electrodialysis film group device in the mode of cross-flow.
Described electrodialytic temperature is 28 DEG C.
The gauge pressure of described pump is 0.06Mpa.
Flux of alkaline liquor is 700L/h, and de-mineralized water flow is 500L/h.
Described electrodialysis impressed DC voltage, magnitude of voltage is 40V, and current value is 92A, and interelectrode distance is 10cm.
The enrichment alkali collection obtained by electrodialysis cathode compartment utilizes, and anolyte compartment is containing the waste liquid acid neutralization of hemicellulose, and Precipitation hemicellulose, filters, obtain hemicellulose as fermentation raw material.
Acid neutralization to pH value is 5.
The sulfuric acid of described acid to be concentration be 0.15mol/L.
In described electrodialysis process, the concentration of lye of anolyte compartment's waste liquid is 8g/L.
Filtrate after described precipitation hemicellulose, through reverse osmosis, obtains de-mineralized water and recycles.
Described film group device uses multipair anion and cation exchange membrane pair, and the distance between anion and cation exchange membrane is 0.13mm.
Recovery concentration of lye after electrodialysis is 305g/L, and containing half fine 6.3g/L, recycle of alkali liquor rate is 88%.
Embodiment 14
The present embodiment is substantially the same manner as Example 11, on this basis:
Waste lye after pretreatment and de-mineralized water are entered membrane module by the throughput ratio of 1:1 by pump and is delivered to diffusion dialysis film group device, the waste lye flowed out is by electrodialytic anolyte compartment, sig water by cathode compartment, reclaims the enrichment alkali that cathode compartment obtains as electrolytic solution.
Described waste lye and de-mineralized water enter diffusion dialysis film group device in the mode of cross-flow.
Recovery concentration of lye after electrodialysis is 254g/L, and containing half fine 8.3g/L, recycle of alkali liquor rate is 87%.
Embodiment 15
The present embodiment is substantially the same manner as Example 11, on this basis:
Waste lye after pretreatment and de-mineralized water are entered membrane module by the throughput ratio of 2:1 by pump and is delivered to diffusion dialysis film group device, the waste lye flowed out is by electrodialytic anolyte compartment, sig water by cathode compartment, reclaims the enrichment alkali that cathode compartment obtains as electrolytic solution.
Described waste lye and de-mineralized water enter diffusion dialysis film group device in the mode of cross-flow.
The temperature of described technological operation is 32 DEG C.
The gauge pressure of described pump is 0.06Mpa.
In described diffusion dialysis process, waste lye flow is 80L/h, and the flow of de-mineralized water is 60L/h.
In described electrodialysis process, flux of alkaline liquor is 550L/h, and de-mineralized water flow is 300L/h.
The described sig water concentration obtained after diffusion dialysis is 250g/L.
Described electrodialysis impressed DC voltage, magnitude of voltage is 40V, and current value is 92A, and interelectrode distance is 10cm, is conducive to promoting dialysis efficiency.
Described electrodialytic anolyte compartment obtains the waste liquid acid neutralization containing hemicellulose, Precipitation hemicellulose, filters, obtains hemicellulose as fermentation raw material;
Acid neutralization to pH value is 3.
The sulfuric acid of described acid to be concentration be 2.5mol/L.
In described electrodialysis process, the concentration of lye of holding anode room waste liquid is 15g/L.
Filtrate after described precipitation hemicellulose, through ultrafiltration, obtains de-mineralized water and recycles.
Described diffusion dialysis film group device uses multiple cationic exchange membranes, and the distance between cationic exchange membrane is 0.6mm.
Described electrodialysis film group device uses multipair anion and cation exchange membrane pair, the distance 0.15mm between anion and cation exchange membrane.
Recovery concentration of lye after electrodialysis is 298g/L, and containing half fine 5.6g/L, recycle of alkali liquor rate is 92%.
Claims (1)
1. the millipore filtration pretreatment technology of the pressed liquor electrodialysis alkali collection in viscose fiber production, it is characterized in that: NaOH content is that the pressed liquor of 200g/L first filters out oarse-grained impurity by flame filter press, enter millipore filter by pump again, obtain sig water for follow-up electrodialysis process;
Pressed liquor naoh concentration after pretreatment is 160-200g/L, and half fibre content is 36-150g/L;
In described flame filter press, the density of filter cloth is 1150g/m
2;
The working pressure of described flame filter press is 0.2Mpa, and flow is 20m
3/ (h*m
2);
The filter cloth surface of described flame filter press scribbles diatomite, and diatomaceous thickness is 2mm;
The service temperature of described millipore filter is 25 DEG C, and pressure is 0.12Mpa;
The membrane pore size of described millipore filter is 0.16 μm;
Described millipore filter, when pressed liquor is greater than 0.08Mpa by the Pressure Drop of filter core, namely cleans filter core;
Waste lye after pretreatment and de-mineralized water are entered membrane module by the throughput ratio of 2:1 by pump and is delivered to diffusion dialysis film group device, the waste lye flowed out is by electrodialytic anolyte compartment, sig water by cathode compartment, reclaims the enrichment alkali that cathode compartment obtains as electrolytic solution;
Described waste lye and de-mineralized water enter diffusion dialysis film group device in the mode of cross-flow;
The temperature of described technological operation is 32 DEG C;
The gauge pressure of described pump is 0.06Mpa;
In described diffusion dialysis process, waste lye flow is 80L/h, and the flow of de-mineralized water is 60L/h;
In described electrodialysis process, flux of alkaline liquor is 550L/h, and de-mineralized water flow is 300L/h;
The described sig water concentration obtained after diffusion dialysis is 250g/L;
Described electrodialysis impressed DC voltage, magnitude of voltage is 40V, and current value is 92A, and interelectrode distance is 10cm;
Described electrodialytic anolyte compartment obtains the waste liquid acid neutralization containing hemicellulose, Precipitation hemicellulose, filters, obtains hemicellulose as fermentation raw material;
Acid neutralization to pH value is 3;
The sulfuric acid of described acid to be concentration be 2.5mol/L;
In described electrodialysis process, the concentration of lye of holding anode room waste liquid is 15g/L;
Filtrate after described precipitation hemicellulose, through ultrafiltration, obtains de-mineralized water and recycles;
Described diffusion dialysis film group device uses multiple cationic exchange membranes, and the distance between cationic exchange membrane is 0.6mm;
Described electrodialysis film group device uses multipair anion and cation exchange membrane pair, the distance 0.15mm between anion and cation exchange membrane;
Recovery concentration of lye after electrodialysis is 298g/L, and containing half fine 5.6g/L, recycle of alkali liquor rate is 92%.
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