CN102011216B - Method for recycling zinc from spinning plasticizing bath waste liquid - Google Patents
Method for recycling zinc from spinning plasticizing bath waste liquid Download PDFInfo
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- CN102011216B CN102011216B CN201010508852A CN201010508852A CN102011216B CN 102011216 B CN102011216 B CN 102011216B CN 201010508852 A CN201010508852 A CN 201010508852A CN 201010508852 A CN201010508852 A CN 201010508852A CN 102011216 B CN102011216 B CN 102011216B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The invention discloses a method for recycling zinc from spinning plasticizing bath waste liquid. The method comprises the following steps of: (1) adding solution of sodium hydroxide into the plasticizing bath waste liquid during spinning of viscose fiber to react until the pH value is 7.5 to 8.5; (2) standing and demixing the reaction solution and separating the lower layer precipitates out; and (3) adding solution of sulfuric acid into the precipitates to dissolve and recycling in coagulating bath of a spinning step. By the method, the recycling of zinc sulfate is realized, the consumption of chemical raw materials is reduced, the production cost is reduced, and the consumption of lime or alkali during processing with the lime or the alkali in the prior art is avoided; meanwhile, the pollution of the zinc in waste water and waste residues to the environment is avoided; and the method is an environment-friendly, energy-saving and high-benefit production and recycling process.
Description
Technical field
The present invention relates to the cellulose fibre technical field, relate in particular to the recoverying and utilizing method of zinc in a kind of viscose spinning plasticizing-bath waste liquid.
Background technology
Viscose is a kind of important chemical fibre kind; Since suitability for industrialized production; With the premium properties of its product uniqueness and the recyclability of raw material, demonstrate the vitality of vigorous development, but the three wastes problem that is produced in the viscose production is the difficult problem that people constantly explore solution always.Zinc-containing sludge surpasses the solid dangerous waste that 100mg/l belongs to national regulation; Zinc in the mud that present domestic viscose enterprise is produced does not much all reach discharge standard; Exist as solid dangerous waste, become the generality difficult problem of puzzlement viscose enterprise.
The spinning technique flow process of viscose comprises operations such as coagulation forming, plasticizing drawing-off and washing, the coagulating bath of coagulation forming process, or claim acid bath, a bath; Its component is sulfuric acid 100～130g/l, zinc sulfate 7～12g/l, sodium sulphate 280～350g/l; Temperature is at 45～55 ℃, and strand gets into plasticizing-bath behind the coagulating bath coagulation forming, also claims two baths in the production; Component in the plasticizing-bath is brought in mainly being bathed by the strand spontaneous coagulation, and each producer's basis is the process conditions control process separately, and the main component of plasticizing-bath also is sulfuric acid, zinc sulfate, sodium sulphate and water; Sulfuric acid 15～30g/l wherein, zinc sulfate 3～6g/l.The effect of plasticizing-bath is that the tow behind the spinning moulding is concentrated drawing-off under plastifying state, and is powerful to improve strand, simultaneously with tow heating and decomposition in high temperature plasticizing-bath more than 95 ℃, makes carbon disulfide in the tow overflow and reclaim.Because the viscose tow is constantly brought coagulating bath in the plasticizing-bath in the spinning process; Cause the amount of plasticizing-bath constantly to increase; Guarantee the balance of plasticizing-bath total amount and stablizing of technology so need carry out certain discharging; Present domestic viscose industry generally adopts the mode to plasticizing-bath continuous blow-down, after only being used lime or alkali treatment, discharges on the zinc in the plasticizing-bath, and be the main pollution source of zinc in waste water, the waste residue.This has caused in waste residue, the waste water zinc to the pollution of environment on the one hand; On the other hand, because zinc sulfate is a kind of industrial chemicals in the viscose production, caused the waste of raw material; Secondly, increased the consumption and the improvement operating cost of lime in the sewage disposal.
Prepare in the process in viscose stoste; The alkali cellulose squeezing process can produce a large amount of salkali waste, and the concentration of salkali waste is at 160～250g/l, and this part salkali waste part is used for allocating again and utilizes; The part of need draining in addition; The PH that few part is used for Sewage Plant regulates, and the processing of salkali waste also is one of problem of puzzlement viscose enterprise, does not particularly possess the factory of pulp fibers coproduction condition.
Summary of the invention
Technical problem to be solved by this invention is: to the deficiency that prior art exists, a kind of recoverying and utilizing method of avoiding zinc to zinc in the pollution of environment and the spinning plasticizing-bath waste liquid that can reduce production costs is provided.
For solving the problems of the technologies described above, technical scheme of the present invention is:
The recoverying and utilizing method of zinc in a kind of spinning plasticizing-bath waste liquid may further comprise the steps:
(1) add the aqueous slkali reaction in the plasticizing-bath waste liquid that in the viscose spinning, discharges, to pH value be 7.5～8.5;
(2) separate with above-mentioned reaction solution standing demix, and with the lower sediment thing;
(3) in said sediment, add acid solution dissolving fully after, be back to use in the allotment of coagulating bath of spinning step.
In the step (1), the aqueous slkali of said adding is a sodium hydroxide solution.
As a kind of improvement, the aqueous slkali of said adding is that viscose glue prepares the squeezing spent caustic solution that process produces.
The said standing demix time is 5～30 minutes.
The acid solution of said adding is a sulfuric acid solution.
As a kind of improvement, the acid solution of said adding is a spinning coagulation bath.
Can contain aluminum sulfate in the said plasticizing-bath waste liquid.
The plasticizing-bath waste liquid and the sodium hydroxide solution reaction of discharging during the present invention at first produces viscose, NaOH elder generation and sulfuric acid generation neutralization reaction are 7.5～8.5 o'clock at PH then; Generating the zinc hydroxide deposition with zinc sulfate separates out; Through leaving standstill certain hour, zinc hydroxide sediment and solution system stratified sedimentation are separated to lower floor, according to the ambisexuality of zinc hydroxide; Sulfuric acid and the zinc hydroxide sediment generation zinc sulfate that reacts; And the zinc sulfate constituent of coagulating bath just can be back to use in the production, and some viscose enterprises have brought into use the zinc sulfate concentrated solution to carry out the allotment of coagulating bath now; So just can be back to use the circulation mixing system of spinning coagulation bath constantly with elder generation of the zinc sulfate in the plasticizing-bath and alkali, then born again with acid reaction again.
At present, some viscose glue manufacturer is for fear of the pollution of zinc ion to environment, and the coagulating bath component adopts aluminum sulfate to replace zinc sulfate, and the present invention is equally applicable to the recycling to aluminum sulfate to the recycling of zinc sulfate.
Owing to adopted technique scheme, the invention has the beneficial effects as follows:
1, the present invention generates the zinc hydroxide deposition with alkali reaction earlier with the zinc sulfate in the plasticizing-bath waste liquid of discharging; And then become zinc sulfate to be back to use in the spinning coagulation bath with sulfate reduction; Not only realize the recycling of zinc sulfate, reduced the consumption of industrial chemicals, reduced production cost; But also the lime when having avoided using lime or alkali treatment in the prior art or the consumption of alkali have also avoided in waste water, the waste residue zinc to the pollution of environment simultaneously.
2, the present invention uses the salkali waste that squeezing process produces with zinc sulfate in the plasticizing-bath waste liquid and alkali reaction the time;, uses the zinc hydroxide sediment spinning coagulation bath when being dissolved; In removal process, not only do not need industrial chemicals consumption, but also accomplished the treatment of wastes with processes of wastes against one another zinc sulfate; Having solved the emission problem of squeezing salkali waste, is that technology is reclaimed in a kind of environmental protection, production energy-conservation, high benefit.
The specific embodiment
Embodiment 1
(1) in containing the spinning plasticizing-bath waste liquid of sulfuric acid 18g/l, zinc sulfate 3g/l, aluminum sulfate 0.6g/l, add the squeezing spent caustic solution of 170g/l, to pH value be 8.0.
(2) separate with above-mentioned reaction solution standing demix 30min, and with the sediment of lower floor's zinc hydroxide and aluminium hydroxide, the precipitation capacity that records zinc is 96wt%.
(3) sediment with zinc hydroxide and aluminium hydroxide uses sulfur acid 116g/l, after zinc sulfate is the coagulating bath solution dissolving of 7.2g/l, is back to use in the coagulating bath allotment of spinning step.
Embodiment 2
(1) in containing the spinning plasticizing-bath waste liquid of sulfuric acid 18g/l, zinc sulfate 3g/l, add the sodium hydroxide solution of 10wt%, to pH value be 8.2.
(2) separate with above-mentioned reaction solution standing demix 15min, and with lower floor's zinc hydroxide sediment, the precipitation capacity that records zinc is 95wt%.
(3) with after the sulfuric acid solution dissolving of zinc hydroxide sediment with 2mol/l, be back to use in the coagulating bath allotment of spinning step.
Embodiment 3
(1) in containing the spinning plasticizing-bath waste liquid of sulfuric acid 25g/l, zinc sulfate 5g/l, add the squeezing spent caustic solution of 180g/l, to pH value be 8.1.
(2) separate with above-mentioned reaction solution standing demix 20min, and with lower floor's zinc hydroxide sediment, the precipitation capacity that records zinc is 96wt%.
(3) the zinc hydroxide sediment is used sulfur acid 120g/l, after zinc sulfate is the coagulating bath solution dissolving of 9.6g/l, be back to use in the coagulating bath allotment of spinning step.
Claims (5)
1. the recoverying and utilizing method of zinc in the spinning plasticizing-bath waste liquid is characterized in that may further comprise the steps:
(1) add the sodium hydroxide solution reaction in the plasticizing-bath waste liquid in the viscose spinning, to pH value be 7.5～8.5;
(2) separate with above-mentioned reaction solution standing demix, and with the lower sediment thing;
(3) in said sediment, after the dissolving fully of adding sulfuric acid solution, be back to use in the coagulating bath of spinning step.
2. the recoverying and utilizing method of zinc in the spinning plasticizing-bath waste liquid as claimed in claim 1 is characterized in that: in the step (1), add viscose glue in the plasticizing-bath waste liquid in the viscose spinning and prepare the squeezing spent caustic solution reaction that process produces.
3. the recoverying and utilizing method of zinc in the spinning plasticizing-bath waste liquid as claimed in claim 1, it is characterized in that: the said standing demix time is 5～30 minutes.
4. the recoverying and utilizing method of zinc in the spinning plasticizing-bath waste liquid as claimed in claim 1 is characterized in that: in the step (3), the sulfuric acid solution of said adding is a spinning coagulation bath.
5. the recoverying and utilizing method of zinc in the spinning plasticizing-bath waste liquid as claimed in claim 1 is characterized in that: contain aluminum sulfate in the said plasticizing-bath waste liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010508852A CN102011216B (en) | 2010-10-09 | 2010-10-09 | Method for recycling zinc from spinning plasticizing bath waste liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010508852A CN102011216B (en) | 2010-10-09 | 2010-10-09 | Method for recycling zinc from spinning plasticizing bath waste liquid |
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| CN102011216A CN102011216A (en) | 2011-04-13 |
| CN102011216B true CN102011216B (en) | 2012-09-12 |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102311141B (en) * | 2011-04-29 | 2013-01-09 | 冯若愚 | Method for simultaneously preparing zinc hydroxide and sodium chloride by chemical fiber waste residue mud |
| CN102311139B (en) * | 2011-04-29 | 2013-01-09 | 冯若愚 | Method for simultaneously preparing zinc nitrate and sodium chloride by chemical fiber waste residue mud |
| CN102311143A (en) * | 2011-04-29 | 2012-01-11 | 冯若愚 | Method for simultaneously preparing zinc chloride and sodium sulfide by chemical fiber waste residue mud |
| CN102311106A (en) * | 2011-04-29 | 2012-01-11 | 冯若愚 | Method for simultaneously preparing zinc phosphate and sodium chloride by chemical fiber waste residue mud |
| CN102311144B (en) * | 2011-04-29 | 2013-01-09 | 冯若愚 | Method for simultaneously preparing zinc sulfate and sodium chloride by chemical fiber waste residue mud |
| CN102311145B (en) * | 2011-04-29 | 2013-01-30 | 冯若愚 | Method for preparing zinc sulfide and coproducing sodium chloride from chemical fiber waste slag mud |
| CN102409434B (en) * | 2011-09-26 | 2013-09-25 | 宜宾海丝特纤维有限责任公司 | Method for treating secondary waste viscose |
| CN104058539B (en) * | 2014-07-07 | 2016-02-10 | 成都丽雅纤维股份有限公司 | A kind of half fine treatment process based on wastewater from viscose fiber producing |
| CN107902855B (en) * | 2017-11-07 | 2020-10-27 | 宜宾海丝特纤维有限责任公司 | Recovery process of waste zinc ions in viscose fiber production |
| CN111362482B (en) * | 2020-03-06 | 2023-04-18 | 山东默锐环境产业股份有限公司 | Method for recovering zinc chloride in zinc chloride wastewater and zero-discharge treatment of wastewater |
| CN112390281A (en) * | 2020-10-30 | 2021-02-23 | 冉国庆 | Method for recovering zinc oxide from Cellulose Carbamate (CC) fiber coagulation bath and application |
| CN115323516A (en) * | 2020-12-25 | 2022-11-11 | 内蒙古双欣环保材料股份有限公司 | Six-effect evaporation, condensation and recovery device and method for fiber tow washing water |
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2010
- 2010-10-09 CN CN201010508852A patent/CN102011216B/en active Active
Non-Patent Citations (1)
| Title |
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| 丁传伟 等."用碳酸钠法从塑化浴中回收锌".《化纤与纺丝技术》.1984,第1984卷(第2期),全文. |
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| CN102011216A (en) | 2011-04-13 |
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Effective date of registration: 20211227 Address after: 224400 Jiangsu Yancheng Funing high tech Industrial Development Zone Aoyang Avenue Saideli (Yancheng) Fiber Co., Ltd Patentee after: Saideli (Yancheng) Fiber Co.,Ltd. Address before: 224400 Funing Aoyang Technology Co., Ltd., Aoyang Industrial Park, Funing County, Yancheng City, Jiangsu Province Patentee before: FUNING AOYANG TECHNOLOGY CO.,LTD. |