CN105692989A - A comprehensive utilization process for viscose fiber acidic waste water - Google Patents
A comprehensive utilization process for viscose fiber acidic waste water Download PDFInfo
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- CN105692989A CN105692989A CN201410707183.0A CN201410707183A CN105692989A CN 105692989 A CN105692989 A CN 105692989A CN 201410707183 A CN201410707183 A CN 201410707183A CN 105692989 A CN105692989 A CN 105692989A
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Abstract
A comprehensive utilization process for viscose fiber acidic waste water is disclosed. The process includes A) filtering the viscose fiber acidic waste through a filter to remove suspended solids in the waste water, and conveying to filtrate to treatment of the next step, B) feeding the filtrate into a first-grade electrodialysis system to obtain first-grade thick water and first-grade fresh water, subjecting the first-grade fresh water to biochemical treatment and discharging the treated first-grade fresh water or further treating the first-grade fresh water, and conveying the first-grade thick water to the next step, and C) feeding the first-grade thick water obtained through electrodialysis to a multi-effect evaporator, concentrating, feeding into a crystallizing pot, and crystallizing to obtain sodium sulfate crystals, wherein crystallization mother liquor is concentrated sulfuric acid, contains sodium sulfate and zinc sulfate, and can be directly adopted as concentrated sulfuric acid and reused into a coagulating bath. The process adopts a combined technique adopting the electrodialysis as a core, recovers sulfuric acid, the zinc sulfate, the sodium sulfate and water, overcomes the difficulty of zinc discharging and the difficulty of solid wastes, and achieves comprehensive utilization of resources.
Description
Technical field
The present invention relates to three-protection design, particularly relate to the comprehensive utilization process of a kind of viscose fiber acid waste water。
Background technology
Viscose rayon is the regenerated celulose fibre made for raw material with natural fiber。Viscose fiber production process produces substantial amounts of waste water。These waste water mainly contain sulphuric acid, zinc sulfate, sodium sulfate, Carbon bisulfide, hydrogen sulfide, the Organic substance of dissolving, float etc., is one of the primary pollution source of textile industry, environment is brought very big harm。
Acid waste water occurs mainly with spinning workshop, acid station and postprocessing working procedures。Including washing spinning-drawing machine water, acid station washing filter draining, washing a water and post treatment acid wash water。Additionally, clean evaporation equipment, crystallizer also produce a certain amount of acid waste water。Acid waste water mainly contains sulphuric acid, sodium sulfate, zinc sulfate etc., its pH value: 1-2, COD:300-1000mg/L, Zn2+: 50-70mg/L。The major pollutants matter of acid waste water is sulphuric acid, zinc sulfate and sodium sulfate。Wherein sulphuric acid and sulphuric acid zinc concentration are higher。Difficulty of governance is bigger。
Current viscose acid waste water process in many and alkaline waste water and after, then adopt Physiochemical and biochemical two stages for the treatment of。General acid waste water mix with alkaline waste water after about pH2.5, remove after volatile material through stripping, adopt lime cream to regulate pH to 10-11, zinc ion is precipitated, clear liquid adopts Wastewater Treated by Activated Sludge Process, and through sedimentation, draining realizes qualified discharge。But owing to the optimal pH of zinc ion precipitation is narrower, it is incomplete that lime cream adds reaction in process, or throwing amount is improper, can cause zinc ion precipitation not exclusively, cause that subsequent biochemical water outlet is not up to standard。This technique is brought substantial amounts of reluctant containing zinc solid waste simultaneously, and causes the substantial amounts of wasting of resources。Therefore find and can solve an above-mentioned difficult problem, can realize again the technical scheme of resource reclaim be viscose industry in the urgent need to。
Summary of the invention
The purpose of the present invention, it is simply that in order to solve above-mentioned prior art Problems existing, it is provided that the comprehensive utilization process of a kind of viscose fiber acid waste water。
In order to achieve the above object, present invention employs techniques below scheme: the comprehensive utilization process of a kind of viscose fiber acid waste water, it is characterised in that comprise the following steps:
A, pretreatment
Being filtered by filter by viscose fiber acid waste water, remove the float in waste water, filtered solution enters next step and processes；
B, electrodialysis
Filtered solution importing one-level electrodialysis system, obtains the dense water of one-level and one-level fresh water, one-level fresh water discharges after biochemical treatment, or is further processed；The dense water of one-level enters next step and processes；
C, condensing crystallizing
After dense for electrodialysis gained one-level water imports multi-effect evaporator concentration, sending into crystallizer crystallization, obtain sulfate crystal, crystalline mother solution is concentrated sulphuric acid, and containing sodium sulfate and zinc sulfate, can be back to use in coagulating bath directly as concentrated sulphuric acid。
The method being further processed described in step B is, by one-level fresh water then through NF membrane or reverse osmosis membrane processing, the filtrate obtained is pure process water, can direct reuse；Concentrated solution imports two grades of electrodialysis systems, obtains two grades of dense water and two grades of fresh water, and two grades of dense water import multi-effect evaporator and reclaim sulphuric acid, sodium sulfate and zinc sulfate further, and two grades of fresh water discharge after biochemical treatment。
Described pretreatment also includes through heat exchanger, viscose fiber acid waste water is reduced the temperature to≤40 DEG C, and this heat exchanger is placed on before filter or after filter。
Filter described in step A adopts microfilter, and pore size filter is 0.02 micron-20 microns, and filter method is dead-end filtration or cross flow filter。
Filter described in step A adopts ultrafiltration membrane filter or microporous filtration, and pore size filter is 0.02-1 μm, and filter method is dead-end filtration or cross flow filter。
Described cross flow filter film surface velocity controls at 1～6 meter per second, and operation Stress control is at 0.1～1MPa, and operation temperature controls at 1～90 DEG C。
Described cross flow filter film surface velocity controls at 2～5 meter per seconds, and operation Stress control is at 0.2～0.8MPa, and operation temperature controls at 5～70 DEG C。
The pole hydromining of described one-level electrodialysis system or two grades of electrodialysis systems is with 0.5%～1.0% aqueous sodium persulfate solution, or the dense water through electrodialysis purification；Initial dense tank adopts tap water or softening water or pure water。
The mode that described one-level electrodialysis system or two grades of electrodialysis systems adopt multi-machine parallel connection or multimachine series connection or multi-machine parallel connection series connection to combine, to improve the mesohalobic concentration of dense water。
Described NF membrane rejection >=96% to magnesium sulfate, operation temperature controls at 10-50 DEG C, and operation Stress control is at 1-5Mpa。
Described reverse osmosis membrane is to the rejection of sodium chloride more than 98%, and operation Stress control is at 1～5Mpa, and operation temperature controls at 1～40 DEG C。
The comprehensive utilization process of viscose fiber acid waste water of the present invention adopts electrodialytic technique to be the group technology of core, achieve the recovery of sulphuric acid, zinc sulfate, sodium sulfate and water, solve a difficult problem for zinc discharge and a difficult problem for solid waste, it is achieved that the comprehensive utilization of resource。
Water is processed by pretreatment, allows to meet electrodialytic feed needs。Electrodialysis realizes acid and salt and produces the separating organic matters of COD, realizes the initial concentration of acid and salt simultaneously。Acid and salt through electrodialysis initial concentration is concentrated by evaporation and concentration further, crystallization, obtains sulfate crystal, it is achieved the reuse of sodium sulfate。Sulphuric acid and zinc sulfate are stayed in crystalline mother solution, are back to use in coagulating bath, it is achieved the reuse of sulphuric acid and zinc sulfate。
Electrodialysis system involved in the present invention includes being become galvanic power supply, delivery pump and electrodialyzer from alternating current。The critical piece of electrodialyzer is anion exchange membrane (abbreviation cavity block), cation exchange membrane (abbreviation anode membrane), dividing plate and electrode。The passage that compartment is liquid stream process that dividing plate is constituted。The compartment of material process is desalting chamber, and the compartment of dense water process is enriched chamber。Namely the salinity of material is removed, at dense hydroecium, salinity is concentrated simultaneously。Usual cavity block, anode membrane and dense water and diluted gasket are alternately arranged, and plus pair of electrodes just one electrodialyzer of composition。
The thin film that ion is had selective penetrated property that ion exchange membrane is made up of macromolecular material。Main point cation exchange membrane (CM is called for short anode membrane) and two kinds of anion exchange membrane (AM is called for short cavity block)。Anode membrane is owing to film body fixed base is with negatively charged ions, optional through cation；Cavity block is owing to film body fixed base is with positive charge ion, optional through anion。Anode membrane passes through cation, and cavity block is called the selective penetrated property of film through the performance of anion。
The most basic working cell of electrodialyzer is called film pair。One film is to constituting a diluting compartment and an enriched chamber。Under the effect of DC electric field, utilizing the selective penetrated property of ion exchange membrane, cation permeable anode membrane, anion-permeable cavity block, the ion of desalting chamber migrates to enriched chamber, and the ion of enriched chamber cannot migrate to desalting chamber due to the selective penetrated property of film。The salt concentration of such diluting compartment is gradually lowered, and the salt concentration of adjacent enriched chamber gradually rises accordingly。
In order to ensure the stable operation of electrodialysis system and increase the service life, water inlet is had strict demand by it。Viscose is washed a waste water and is mainly contained: sulphuric acid, sodium sulfate, zinc sulfate, elemental sulfur, fiber, saccharide etc., in yellow turbid solution。Wherein suspension content is high, it is difficult to meet electrodialytic inflow requirement。Without suitable pretreatment, it is impossible to ensure electrodialysis system continuous and steady operation。
This technique adopt Millipore filtration techniques or ultra filtration technology carry out pretreatment。Float in pretreatment, waste water, as the insoluble substance such as fiber, elemental sulfur is removed, filtered solution enters electrodialysis system。
Waste water and clear liquid through pretreatment enters electrodialysis system。Waste water is divided into two parts: dense water and fresh water。Wherein salinity includes sodium sulfate, zinc sulfate, sulphuric acid etc. and enters dense water end (W.E.), it is achieved with separating of COD, realize concentration simultaneously。And acid and zinc sulfate, sodium sulfate are removed in fresh water end, PH raises, this waste water without neutralizing, dezincification, biochemical system can be directly entered and process, it is achieved qualified discharge。And the dense water of dense water end (W.E.), owing to COD is removed the overwhelming majority, and through initial concentration。This dense water enters vaporizer and is evaporated concentration, obtains sulfate crystal。Crystalline mother solution is concentrated sulphuric acid, and containing a certain amount of sodium sulfate and zinc sulfate, can be back to use in coagulating bath directly as concentrated sulphuric acid。Sulphuric acid and zinc sulfate is made to be recycled utilization。
Adopting above-mentioned technique, without the discharge of solid waste, sodium sulfate, sulphuric acid, zinc sulfate obtain reuse, and water realizes qualified discharge。
The above-mentioned fresh water through one-level electrodialysis process, then through NF membrane or reverse osmosis membrane processing, obtains pure process water, it is achieved Water circulation。Concentrated solution is through two grades of electrodialysis process, and dense water enters vaporizer and reclaims sulphuric acid and sodium sulfate and zinc sulfate further。Two grades of electrodialytic fresh water enter biochemical treatment。Thus further increase the response rate of sulphuric acid, sodium sulfate, zinc sulfate, decrease discharge, realize the recovery of water simultaneously。
Detailed description of the invention
100M3Washing a water, its electrical conductivity is 20-70ms/cm, sulfuric acid content 5-10g/L, TDS1-6%, sodium sulphate content 15-65g/L, zinc sulfate content 400-1000mg/L, COD400-4000。By being pumped into heat exchanger, temperature being reduced to less than 40 degrees Celsius, input microfilter or ultrafiltration or micro-filtration filter, and remove float, are stored in tank。This filtrate is pumped up into one-level electrodialysis system。Through one-level electrodialysis system, obtain fresh water, its electrical conductivity≤3ms/cm。Sodium sulfate removes more than 95%, and sulphuric acid removes more than 90%。This fresh water enters biochemical system and processes, qualified discharge。In dense water, sodium sulfate concentration reaches 10%, sulphuric acid 2%。The highest can reach 20% sodium sulfate。Dope, after concentrating with the multi-effect evaporator of heat pump assembly, enters crystallizer crystallization, obtains sulfate crystal and concentrated sulphuric acid。Sulfate crystal is as commodity selling。Due to the interference of organics removal in crystallization process, obtain the good anhydrous sodium sulfate of quality。Mother solution after separating sodium sulfate is mainly concentrated sulphuric acid and zinc sulfate, is back to use in acid bath。Whole technique realizes closed cycle。
Improve the implementation process of technique: the electrodialytic fresh water 100M of above-mentioned one-level3, electrical conductivity≤3ms/cm, NF membrane or counter-infiltration system is entered through pump。Under the driving of pressure, water passes through film, obtains permeate, and the part through film is not concentrated solution。Permeate is back in technique。Nanofiltration and reverse osmosis produced water rate 70-90%。The concentrated solution of nanofiltration or reverse osmosis enters two grades of electrodialysis。
Embodiment 1
Washing 80-95 degree Celsius of a water, through plate type heat exchanger, water temperature is dropped to 40 degrees Celsius, enter 5 micrometer Millipore filters through pump, filtrate is placed in tank。Clear liquid through microfilter is entered fresh-water tank in electrodialysis system by transport pump from tank, and pole tank adds 0.5% sodium sulfate。Dense tank adds softening water。Open the circulating pump of fresh-water tank, dense tank, pole tank, control pressure≤0.1Mpa, control the thin water pressure height 0.005MPa of dense water pressure。Operation temperature 40 degrees Celsius。Opening commutator, under the driving of electricity, the sodium sulfate in fresh-water tank, zinc sulfate, sulphuric acid enter dense water side, and dilute side COD is trapped, and salt is separated。When the electrical conductivity of fresh-water tank is lower than 2000us/cm, fresh water discharges。Add the new clear liquid through microfilter, repeat aforesaid operations。In fresh-water tank, liquid electric conductivity is lower than 2000us/cm。Discharge fresh water。Repeating 3 times, dense water reaches salt content 10%。Fresh water electrical conductivity 2000us/cm, COD4000。This fresh water enters biochemical system and processes, and water realizes qualified discharge。
Dense water enters after evaporating with multi-effect evaporator, and liquid enters crystallizer and concentrates further, centrifugal, obtains sulfate crystal, dry, and temperature obtains anhydrous sodium sulfate crystallization。Crystalline mother solution is concentrated sulphuric acid and zinc sulfate。It is back to use in acid bath。
Embodiment 2:
The electrodialytic fresh water of one-level in embodiment 1, electrical conductivity 3000us/cm, COD4000, enter counter-infiltration system。Operation pressure 1.5MPa, operation temperature is less than 40 degrees Celsius。It is purified water。In water, electrical conductivity is less than 100us/cm。Water Sproading rate 80%。Reverse osmosis concentrated water, electrical conductivity 15000us/cm, COD19000, enter two grades of electrodialysis process。Two grades of electrodialysis pole water, dense water all adopt the dense water of one-level electrodialysis。Two grades of electrodialysis fresh water, its COD is about 20000mg/L, electrical conductivity 2000us/cm, enters biochemical treatment of wastewater。Dense water salt content 10%, sends into multi-effect evaporator。
Embodiment 3:
The electrodialytic fresh water of one-level in embodiment 1, electrical conductivity 2000us/cm, COD4000, enter nanofiltration system。Operation pressure 1.5MPa, operation temperature is less than 40 degrees Celsius。It is purified water。In water, electrical conductivity is less than 60us/cm。Water Sproading rate 80%。Nanofiltration concentrated solution, electrical conductivity 9300us/cm, COD18000, enter two grades of electrodialysis process。Two grades of electrodialysis pole water, dense water all adopt the dense water of one-level electrodialysis。Two grades of electrodialysis fresh water, its COD is about 20000mg/L, electrical conductivity 2000us/cm, enters biochemical treatment of wastewater, it is achieved qualified discharge。Dense water salt content 10%, sends into multi-effect evaporator。
Embodiment 4:
Washing 80-95 degree Celsius of a water, through pipe heat exchanger, water temperature is dropped to 40 degrees Celsius, enter microfiltration membrane system, pore size filter 0.1 micron through pump, operate pressure 0.5-0.6MPa, running temperature 40 degrees Celsius, filtrate is placed in tank。Filtrate is pumped up in electrodialysis system。
Claims (11)
1. the comprehensive utilization process of a viscose fiber acid waste water, it is characterised in that comprise the following steps:
A, pretreatment
Being filtered by filter by viscose fiber acid waste water, remove the float in waste water, filtered solution enters next step and processes；
B, electrodialysis
Filtered solution importing one-level electrodialysis system, obtains the dense water of one-level and one-level fresh water, one-level fresh water discharges after biochemical treatment, or is further processed；The dense water of one-level enters next step and processes；
C, condensing crystallizing
After dense for electrodialysis gained one-level water imports multi-effect evaporator concentration, sending into crystallizer crystallization, obtain sulfate crystal, crystalline mother solution is concentrated sulphuric acid, and containing sodium sulfate and zinc sulfate, can be back to use in coagulating bath directly as concentrated sulphuric acid。
2. the comprehensive utilization process of viscose fiber acid waste water according to claim 1, it is characterized in that, the method being further processed described in step B is, by one-level fresh water then through NF membrane or reverse osmosis membrane processing, the filtrate obtained is pure process water, can direct reuse；Concentrated solution imports two grades of electrodialysis systems, obtains two grades of dense water and two grades of fresh water, and two grades of dense water import multi-effect evaporator and reclaim sulphuric acid, sodium sulfate and zinc sulfate further, and two grades of fresh water discharge after biochemical treatment。
3. the comprehensive utilization process of viscose fiber acid waste water according to claim 1, it is characterised in that: described pretreatment also includes through heat exchanger, viscose fiber acid waste water is reduced the temperature to≤40 DEG C, and this heat exchanger is placed on before filter or after filter。
4. the comprehensive utilization process of viscose fiber acid waste water according to claim 1, it is characterised in that: filter described in step A adopts microfilter, and pore size filter is 0.02 micron-20 microns, and filter method is dead-end filtration or cross flow filter。
5. the comprehensive utilization process of viscose fiber acid waste water according to claim 1, it is characterized in that: filter described in step A adopts ultrafiltration membrane filter or microporous filtration, pore size filter is 0.02-1 μm, and filter method is dead-end filtration or cross flow filter。
6. the comprehensive utilization process of viscose fiber acid waste water according to claim 5, it is characterised in that: described cross flow filter film surface velocity controls at 1～6 meter per second, and operation Stress control is at 0.1～1MPa, and operation temperature controls at 1～90 DEG C。
7. the comprehensive utilization process of viscose fiber acid waste water according to claim 5, it is characterised in that: described cross flow filter film surface velocity controls at 2～5 meter per seconds, and operation Stress control is at 0.2～0.8MPa, and operation temperature controls at 5～70 DEG C。
8. the comprehensive utilization process of viscose fiber acid waste water according to claim 1 and 2, it is characterized in that: the pole hydromining of described one-level electrodialysis system or two grades of electrodialysis systems 0.5%～1.0% aqueous sodium persulfate solution, or the dense water through electrodialysis purification；Initial dense tank adopts tap water or softening water or pure water。
9. the comprehensive utilization process of viscose fiber acid waste water according to claim 1 and 2, it is characterized in that: the mode that described one-level electrodialysis system or two grades of electrodialysis systems adopt multi-machine parallel connection or multimachine series connection or multi-machine parallel connection series connection to combine, to improve the mesohalobic concentration of dense water。
10. the comprehensive utilization process of viscose fiber acid waste water according to claim 2, it is characterised in that: described NF membrane rejection >=96% to magnesium sulfate, operation temperature controls at 10-50 DEG C, and operation Stress control is at 1-5Mpa。
11. the comprehensive utilization process of viscose fiber acid waste water according to claim 2, it is characterised in that: described reverse osmosis membrane is to the rejection of sodium chloride more than 98%, and operation Stress control is at 1～5Mpa, and operation temperature controls at 1～40 DEG C。
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| CN107324577A (en) * | 2017-08-17 | 2017-11-07 | 长兴上拓环境科技有限公司 | A kind of epoxy resin production waste-water recycling treatment process |
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| CN107686204A (en) * | 2017-09-27 | 2018-02-13 | 唐山三友集团兴达化纤有限公司 | A kind of method of heat integration during processing viscose rayon acid waste water |
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| CN114075003A (en) * | 2020-08-18 | 2022-02-22 | 中石化南京化工研究院有限公司 | Method for recycling copper and zinc in catalyst production wastewater |
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| CN109293112B (en) * | 2018-10-17 | 2021-07-16 | 新疆中泰纺织集团有限公司 | Treatment method for recycling viscose fiber acid wastewater |
| CN109231603A (en) * | 2018-11-21 | 2019-01-18 | 江苏南大环保科技有限公司 | The method and device of cooperative disposal acid waste liquid in cellulose viscose manufacturing technique |
| CN114075003A (en) * | 2020-08-18 | 2022-02-22 | 中石化南京化工研究院有限公司 | Method for recycling copper and zinc in catalyst production wastewater |
| CN115198038A (en) * | 2021-04-08 | 2022-10-18 | 四川雅华生物有限公司 | Process for recovering electrodialysis sugar-containing wastewater from semi-fiber xylose production |
| CN115198038B (en) * | 2021-04-08 | 2023-09-19 | 四川雅华生物有限公司 | Process for recycling semi-fiber xylose-making electrodialysis sugar-containing wastewater |
| CN114212935A (en) * | 2021-11-30 | 2022-03-22 | 武汉新奇华清膜分离技术工程有限公司 | Zero-emission device and method for recycling high-quality sodium sulfate from lead-containing wastewater |
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