CN103351064A - Millipore filtration pretreatment technology for recovery of electrodialysis alkali from pressed liquor in production of viscose fiber - Google Patents
Millipore filtration pretreatment technology for recovery of electrodialysis alkali from pressed liquor in production of viscose fiber Download PDFInfo
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- CN103351064A CN103351064A CN2013103117775A CN201310311777A CN103351064A CN 103351064 A CN103351064 A CN 103351064A CN 2013103117775 A CN2013103117775 A CN 2013103117775A CN 201310311777 A CN201310311777 A CN 201310311777A CN 103351064 A CN103351064 A CN 103351064A
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- viscose fiber
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Abstract
The invention provides a millipore filtration pretreatment technology for recovery of electrodialysis alkali from pressed liquor in production of a viscose fiber. The millipore filtration pretreatment technology is characterized in that large-grained impurities are filtered from the pressed liquor with the NaOH content of 50-200g/L by a sheet frame filter, then the pressed liquor enters a millipore filter through a pump, and dilute alkali is obtained for subsequent electrodialysis treatment. The technology is used for pretreating the waste alkali and allows indices of the waste alkali to be applicable to a subsequent electrodialysis alkali recovery technology according to the characteristic that the viscose fiber produces the high-concentration waste alkali containing hemicellulose during pressing, so that the viscosity of the waste liquid is reduced, the energy consumption is effectively reduced, and the permeation efficiency and the operation stability are improved.
Description
Technical field
The invention belongs to the Waste recovery technical field in the viscose fiber production, be specifically related to the millipore filtration pretreatment technology that a kind of pressed liquor electrodialysis alkali that is applicable in the viscose fiber production reclaims.
Background technology
Viscose fiber is the man-made fiber that utilizes process the chemistry such as the macromolecular material wood pulp contain natural cellulose, cotton pulp and mechanical means to process.Viscose fiber is the kind that approaches the most with the natural fiber clothes performance in the chemical fibre, have soft, moisture absorption is breathed freely, it is elegant to overhang, bright-coloured, the antistatic characteristics such as textile process that are easy to of dyeing, yet being to come from the sky to be better than natural regenerated cellulose fibre, is one of important materials of textile industry raw material.China has about 40 of viscose fiber enterprise 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.
Need a large amount of industrial chemicals in the production process of viscose fiber, can produce a large amount of waste water, these waste water contain sulfuric acid, zinc sulfate, dithiocarbonic anhydride, Mierocrystalline cellulose, dissolved organic matter etc., all environment are produced very large harm, are one of primary pollution source of textile industry.
In production process of viscose fiber, need to by dipping method the hemicellulose in the raw material be dissolved out with alkaline solution, otherwise can produce extremely adverse influence to production technique and final product quality.Therefore, when producing viscose fiber, the press lye treating plant need to be set in process procedure, from the steeping lye system, separate a certain amount of hemicellulose.And can produce the high density salkali waste contain hemicellulose in the expressing process, and for reducing production costs, reducing alkaline consumption, each chemical fiber factory mainly adopts dialysis technique to separate half fibre to carry out recycle of alkali liquor at present.But dialysis technique reclaims the alkali lye inefficiency, and water consumption is large, and takies larger floor area of building, progressively eliminates.The electrodialysis alkali recovery technology that develops rapidly in recent years is expected to replace dialysis technique and carries out recycle of alkali liquor, improves the quality of products and the waste water utilization rate.
201210486339.8, name is called the application for a patent for invention of " secondary treatment method of discarded alkali lye in a kind of viscose fiber production ", this patent will be through conventional pretreated, naoh concentration is 70 ~ 90g/L, discarded alkali lye and the de-mineralized water of half fibre content, 60 ~ 70g/L are delivered to respectively the millipore filtration membrane stack, carry out millipore filtration, the throughput ratio of described pre-treatment waste lye and de-mineralized water is 1 ~ 2:1, the alkali lye that will hang down hemicellulose concentration after the millipore filtration separates with the alkali lye of height half fine concentration, and the alkali lye of described low hemicellulose concentration is back to production.This patent adopts the method for millipore filtration that discarded alkali lye in the viscose fiber production is reclaimed, before millipore filtration, adopt ordinary method that waste lye is carried out pre-treatment, still, reclaim waste lye by electrodialytic method at present, in viscose fiber production, also be not widely used, because the chemical ingredients in the viscose fiber waste lye is different from general black liquor, uses conventional pretreated alkali lye, can not satisfy electrodialytic technical requirements, the result who processes is undesirable, and alkali recovery is not high.
03116938.4, name is called the patent of invention of " alkali in the recovery chemical fibre waste fluid and the method for hemicellulose ", a kind of alkali in the chemical fibre waste fluid and method of hemicellulose of reclaiming is provided, comprise the steps: that the pressed liquor that will contain alkali and hemicellulose enters membrane separation unit through pre-filtering and smart filter, acquisition contains seeing through liquid and containing the concentrated solution of hemicellulose of alkali, what obtain can reach 80 ~ 250 grams per liters through concentration of lye in the liquid, final alkali content is 5 ~ 30 grams per liters in the concentrated solution, and hemicellulose level is 100 ~ 200 grams per liters.This patent does not take into full account the singularity of the chemical ingredients in the 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, the millipore filtration pretreatment technology that pressed liquor electrodialysis alkali reclaims in a kind of viscose fiber production has been proposed, in expressing process, produce the characteristic of the high density salkali waste that contains hemicellulose according to viscose fiber, first salkali waste is carried out pre-treatment, make the index of waste lye be applicable to follow-up electrodialysis alkali recovery process, thereby reduce the viscosity of waste liquid, effectively reduce energy consumption, improve infiltration efficient, stable.
For achieving the above object, the present invention adopts following technical scheme:
The millipore filtration pretreatment technology that pressed liquor electrodialysis alkali reclaimed during viscose fiber was produced, it is characterized in that: NaOH content is that the pressed liquor of 50 ~ 200g/L filters out oarse-grained impurity by flame filter press first, enter millipore filter by pump again, obtain sig water and be used for follow-up electrodialysis process.
Pressed liquor naoh concentration after pretreatment is 50 ~ 200g/L, and half fibre content is 20 ~ 150g/L.
The density of filter cloth is 1100 ~ 1300g/m in the described flame filter press
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 that the filter cloth duct from being blocked by the particle of microorganism, and can simultaneously, the flintiness of filter cake be reduced the filtrate that obtains at the very start clarifying, and voidage increases, and helps to improve filtering velocity.
The diatomaceous thickness in described filter cloth surface is 2mm.
The service temperature of described millipore filter is 20 ~ 40 ℃, and pressure is 0.1 ~ 0.5Mpa.
The membrane pore size of described millipore filter is 0.1 ~ 0.2 μ m.
Described millipore filter, when the Pressure Drop of pressed liquor by filter core greater than 0.08Mpa, namely filter core is cleaned.
Beneficial effect of the present invention is:
1, the present invention produces the characteristic of the high density salkali waste that contains hemicellulose in expressing process according to viscose fiber production, adopt the pretreatment technology of flame filter press-millipore filtration, make the index of pressed liquor be applicable to follow-up electrodialysis alkali recovery process, thereby reduce the viscosity of waste liquid, effectively reduce energy consumption, improve infiltration efficient, stable.
2, owing to can produce the high density salkali waste that contains hemicellulose in the production process of viscose fiber, according to this characteristic, the present invention has selected the special process parameter system of optimizing, first by the suspended substance in the flame filter press removal pressed liquor, by millipore filtration waste lye being carried out initial filter again, is 50 ~ 200g/L thereby make the pressed liquor naoh concentration, and half fibre content is 20 ~ 150g/L, satisfy the electrodialysis requirement, can reclaim better alkali lye.
3, the present invention smears diatomite on the filter cloth surface of flame filter press, can prevent that the filter cloth duct from being blocked by the particle of microorganism, and can simultaneously, the flintiness of filter cake be reduced the filtrate that obtains at the very start clarifying, and voidage increases, and helps to improve filtering velocity.
4, the present invention controls the Pressure Drop of pressed liquor by the millipore filter filter core greater than 0.08Mpa, namely filter core is cleaned, because the Mierocrystalline cellulose in the pressed liquor easily stops up filter core, should carry out slightly in advance, when Pressure Drop during greater than 0.08Mpa, just should clean filter core, otherwise filter core is difficult for cleaning up, can makes if things go on like this filtrate 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 that pressed liquor electrodialysis alkali reclaimed during viscose fiber was produced: NaOH content is that the pressed liquor of 165g/L filters out oarse-grained impurity by flame filter press first, enter millipore filter by pump again, obtain sig water and be used for follow-up electrodialysis process.
Embodiment 2
The millipore filtration pretreatment technology that pressed liquor electrodialysis alkali reclaimed during viscose fiber was produced: NaOH content is that the pressed liquor of 50g/L filters out oarse-grained impurity by flame filter press first, enter millipore filter by pump again, obtain sig water and be used 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 that pressed liquor electrodialysis alkali reclaimed during viscose fiber was produced: NaOH content is that the pressed liquor of 200g/L filters out oarse-grained impurity by flame filter press first, enter millipore filter by pump again, obtain sig water and be used for follow-up electrodialysis process.
Pressed liquor naoh concentration after pretreatment is 200g/L, and half fibre content is 150g/L.
Embodiment 4
Present embodiment is substantially the same manner as Example 3, on this basis:
The density of filter cloth is 1100g/m in the described flame filter press
2
Pressed liquor naoh concentration after pretreatment is 120g/L, and half fibre content is 80g/L.
Embodiment 5
Present embodiment is substantially the same manner as Example 3, on this basis:
The density of filter cloth is 1300g/m in the described flame filter press
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
Present embodiment is substantially the same manner as Example 3, on this basis:
The density of filter cloth is 1200g/m in the described flame filter press
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
Present embodiment is substantially the same manner as Example 3, on this basis:
The density of filter cloth is 1150g/m in the described flame filter press
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
Present embodiment is substantially the same manner as Example 7, on this basis:
The service temperature of described millipore filter is 20 ℃, and pressure is 0.1Mpa.
Pressed liquor naoh concentration after pretreatment is 151g/L, and half fibre content is 35g/L.
Embodiment 9
Present embodiment is substantially the same manner as Example 7, on this basis:
The service temperature of described millipore filter is 40 ℃, and pressure is 0.5Mpa.
The membrane pore size of described millipore filter is 0.1 μ m.
Pressed liquor naoh concentration after pretreatment is 175g/L, and half fibre content is 32g/L.
Embodiment 10
Present embodiment is substantially the same manner as Example 7, on this basis:
The service temperature of described millipore filter is 30 ℃, and pressure is 0.2Mpa.
The membrane pore size of described millipore filter is 0.15 μ m.
Described millipore filter, when the Pressure Drop of pressed liquor by filter core greater than 0.08Mpa, namely filter core is cleaned.
Pressed liquor naoh concentration after pretreatment is 182g/L, and half fibre content is 45g/L.
Embodiment 11
Present embodiment is substantially the same manner as Example 7, on this basis:
The service temperature of described millipore filter is 25 ℃, and pressure is 0.12Mpa.
The membrane pore size of described millipore filter is 0.16 μ m.
Described millipore filter, when the Pressure Drop of pressed liquor by filter core greater than 0.08Mpa, namely filter core is cleaned.
Pressed liquor naoh concentration after pretreatment is 165g/L, and half fibre content is 56g/L.
Embodiment 12
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 be delivered to the electrodialysis film group device, carry out electrodialysis and reclaim alkali lye.
Described waste lye and de-mineralized water enter the electrodialysis film group device in the mode of cross-flow.
Recovery concentration of lye after electrodialysis is 281g/L, contains half fine 8.5g/L, and the recycle of alkali liquor rate is 85%.
Embodiment 13
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 be delivered to the electrodialysis film group device, carry out electrodialysis and reclaim alkali lye.
Described waste lye and de-mineralized water enter the electrodialysis film group device in the mode of cross-flow.
Described electrodialytic temperature is 28 ℃.
The gauge pressure of described pump is 0.06Mpa.
Flux of alkaline liquor is 700L/h, and the de-mineralized water flow is 500L/h.
Described electrodialysis impressed DC voltage, magnitude of voltage are 40V, and current value is 92A, and interelectrode distance is 10cm.
The enrichment alkali that the electrodialysis cathode compartment obtains is recycled, and the anolyte compartment contains the waste liquid acid neutralization of hemicellulose, and the Precipitation hemicellulose filters, and obtains hemicellulose as fermentation raw material.
Acid neutralization to pH value is 5.
Described acid is that concentration is the sulfuric acid of 0.15mol/L.
In the described electrodialysis process, the concentration of lye of anolyte compartment's waste liquid is 8g/L.
Describedly separate out filtrate behind the hemicellulose through reverse osmosis, obtain de-mineralized water and recycle.
Described film group device uses is many to anion and cation exchange membrane pair, and the distance between the anion and cation exchange membrane is 0.13mm.
Recovery concentration of lye after electrodialysis is 305g/L, contains half fine 6.3g/L, and the recycle of alkali liquor rate is 88%.
Embodiment 14
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 be delivered to the diffusion dialysis film group device, the waste lye that flows 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 the diffusion dialysis film group device in the mode of cross-flow.
Recovery concentration of lye after electrodialysis is 254g/L, contains half fine 8.3g/L, and the recycle of alkali liquor rate is 87%.
Embodiment 15
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 be delivered to the diffusion dialysis film group device, the waste lye that flows 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 the diffusion dialysis film group device in the mode of cross-flow.
The temperature of described technological operation is 32 ℃.
The gauge pressure of described pump is 0.06Mpa.
In the described diffusion dialysis process, the waste lye flow is 80L/h, and the flow of de-mineralized water is 60L/h.
In the described electrodialysis process, flux of alkaline liquor is 550L/h, and the de-mineralized water flow is 300L/h.
The described sig water concentration that obtains after diffusion dialysis is 250g/L.
Described electrodialysis impressed DC voltage, magnitude of voltage are 40V, and current value is 92A, and interelectrode distance is 10cm, is conducive to promote dialysis efficiency.
Described electrodialytic anolyte compartment obtains containing the waste liquid acid neutralization of hemicellulose, and the Precipitation hemicellulose filters, and obtains hemicellulose as fermentation raw material;
Acid neutralization to pH value is 3.
Described acid is that concentration is the sulfuric acid of 2.5mol/L.
In the described electrodialysis process, the concentration of lye of holding anode chamber waste liquid is 15g/L.
Describedly separate out filtrate behind the hemicellulose through ultrafiltration, obtain de-mineralized water and recycle.
What described diffusion dialysis film group device used is many cationic exchange membranes, and the distance between the cationic exchange membrane is 0.6mm.
Described electrodialysis film group device uses is many to anion and cation exchange membrane pair, between the anion and cation exchange membrane apart from 0.15mm.
Recovery concentration of lye after electrodialysis is 298g/L, contains half fine 5.6g/L, and the recycle of alkali liquor rate is 92%.
Claims (9)
1. the millipore filtration pretreatment technology that the pressed liquor electrodialysis alkali during viscose fiber is produced reclaims, it is characterized in that: NaOH content is that the pressed liquor of 50 ~ 200g/L filters out oarse-grained impurity by flame filter press first, enter millipore filter by pump again, obtain sig water and be used for follow-up electrodialysis process.
2. the millipore filtration pretreatment technology that the pressed liquor electrodialysis alkali during viscose fiber according to claim 1 is produced reclaims, it is characterized in that: pressed liquor naoh concentration after pretreatment is 50 ~ 200g/L, half fibre content is 20 ~ 150g/L.
3. the millipore filtration pretreatment technology that the pressed liquor electrodialysis alkali during viscose fiber according to claim 1 is produced reclaims, it is characterized in that: the density of filter cloth is 1100 ~ 1300g/m in the described flame filter press
2
4. the millipore filtration pretreatment technology that the pressed liquor electrodialysis alkali during viscose fiber according to claim 1 is produced reclaims, it is characterized in that: the working pressure of described flame filter press is 0.05-0.5Mpa, flow is 20m
3/ (h*m
2).
5. the millipore filtration pretreatment technology that the pressed liquor electrodialysis alkali during viscose fiber according to claim 1 is produced reclaims, it is characterized in that: the filter cloth surface of described flame filter press scribbles diatomite.
6. the millipore filtration pretreatment technology that the pressed liquor electrodialysis alkali during viscose fiber according to claim 6 is produced reclaims is characterized in that: the diatomaceous thickness in described filter cloth surface is 2mm.
7. the millipore filtration pretreatment technology that the pressed liquor electrodialysis alkali during viscose fiber according to claim 1 is produced reclaims, it is characterized in that: the service temperature of described millipore filter is 20 ~ 40 ℃, pressure is 0.1 ~ 0.5Mpa.
8. the millipore filtration pretreatment technology that the pressed liquor electrodialysis alkali during viscose fiber according to claim 1 is produced reclaims, it is characterized in that: the membrane pore size of described millipore filter is 0.1 ~ 0.2 μ m.
9. the millipore filtration pretreatment technology that the pressed liquor electrodialysis alkali during viscose fiber according to claim 1 is produced reclaims is characterized in that: described millipore filter, when the Pressure Drop of pressed liquor by filter core greater than 0.08Mpa, namely filter core is cleaned.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107812401A (en) * | 2017-11-20 | 2018-03-20 | 宜宾丝丽雅股份有限公司 | A kind of pretreating process for viscose rayon spent lye |
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| CN103351064B (en) | 2015-08-19 |
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