CN100473617C - Treatment method for recycling zinc electrolysis washing wastewater - Google Patents
Treatment method for recycling zinc electrolysis washing wastewater Download PDFInfo
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- CN100473617C CN100473617C CNB200710034600XA CN200710034600A CN100473617C CN 100473617 C CN100473617 C CN 100473617C CN B200710034600X A CNB200710034600X A CN B200710034600XA CN 200710034600 A CN200710034600 A CN 200710034600A CN 100473617 C CN100473617 C CN 100473617C
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Abstract
A treatment method for recycling zinc electrolysis washing wastewater mainly comprises the following steps: 1. neutralization/filtration: electrolyzing and washing zinc with alkali to adjust the pH value of the wastewater to 3-6, and filtering to remove residues; 2. and extraction: by selecting P204The neutralized wastewater clear liquor is mixed with an organic phase for extraction, so that zinc in a water phase is transferred into the organic phase, and raffinate is returned to an electrolysis process as washing water directly or after deoiling treatment; 3. back extraction: using spent electrolyte or sulfuric acid pairsCarrying out back extraction on the zinc-rich organic phase to ensure that the zinc in the organic phase is transferred into the water phase again and the organic phase is recycled; 4. deoiling: and adsorbing and deoiling the back extracted liquid by using active carbon, and electrolyzing the deoiled liquid to precipitate zinc or returning the liquid to a leaching system to be used as a leaching agent. The method effectively recovers the zinc in the wastewater, realizes the recycling of the wastewater, has simple process flow and low operation cost, can be well connected with the existing zinc hydrometallurgy system, and is widely suitable for the treatment of zinc electrolytic washing wastewater of various zinc hydrometallurgy plants.
Description
Technical field: the invention belongs to the electrolytic non-ferrous metal technical field of waste water processing, be specifically related to the treatment process of a kind of zinc electrolysis flushing waste water recycle.
Background technology: zinc hydrometallurgy factory can produce the many flushing waste waters of quantity in electrolysis zinc metallurgy process.According to statistics, certain produces the zinc hydrometallurgy factory of 300,000 tons of electric zinc per year, and the annual electrolysis flushing waste water that produces reaches 200,000 m
3, contain zinc 5～15g/l in the waste water, Mnl～2g/l, H
2SO
410～30g/l, other foreign matter contents are very little, use if it is directly returned wet zinc-making system, can cause system bulk to expand, and normal operation is produced in influence.Therefore, at present spelter works all directly drains into the plant effluent total system with this waste water, adopts the method for milk of lime neutralization precipitation to handle, and processed waste water effluxes, and the zinc in the waste water then enters in the gypsum tailings that neutralization precipitation obtains.Because in and the quantity of slag is big, zinc content is low, can't economical and effective reclaim zinc wherein, thereby caused the waste of zinc metal and water resources, and the cost for wastewater treatment height.
Summary of the invention: the object of the invention is to provide a kind of can make the recycle of zinc electrolysis flushing waste water, the treatment process of the zinc in again can efficient recovery waste water.
Technical scheme of the present invention is: adopt the zinc in the solvent extraction enriching and recovering waste water, and realize the reuse of waste water, this method comprises the steps:
1. neutralization/sedimentation and filtration: according to the acidity and the foreign matter content situation of zinc electrolysis flushing waste water, making flushing waste water pH value with the alkali neutralization is 3～6, and then, mistake filters to remove solid slag wherein, as does not have solid slag, then need not filter.
2. extraction: select two-2-ethylhexyl phosphoric acid P for use
204Make extraction agent, kerosene is made thinner, and both are mixed into extracted organic phase, the back waste water clear liquor that will neutralize mixes with organic phase and extracts, make the zinc of aqueous phase change organic phase over to, raffinate returns the electrowinning process use as wash-down water directly or after further de-oiling is handled.
3. back extraction: the rich zinc organic phase that abovementioned steps obtains is carried out back extraction with waste electrolyte or sulfuric acid, makes the zinc in the organic phase change water again over to, the organic phase reusable edible.
4. de-oiling: liquid removes wherein the extraction agent and the kerosene of trace with charcoal absorption after the back extraction, and solution send electrowinning process to sink zinc after the de-oiling, or returns the leaching system and use as leaching agent.
Neutralization can be sodium hydroxide (NaOH), potassium hydroxide (KOH), the yellow soda ash (Na of solid or solution with alkali
2CO
3) and lime in one or more combination.
Use P
204In kerosene liquid when extraction,, kerosene can be No. 200 kerosene, No. 260 kerosene or sulfonated kerosene, P in the extracted organic phase
204Percentage concentration is 15～40%; Extraction conditions: organic phase and water are in a ratio of 1:2～2:1,1～5 minute extraction time, and 10～40 ℃ of temperature, settling time is more than 2 minutes, raffinate pH value 0.5～4.0.
When the acidity of raffinate and foreign matter content are low, directly return as wash-down water and use,, then need after de-oiling, alkali neutralizing treatment, just can return use with oil, when impurity metal ion content is high as acidity.
When doing reverse-extraction agent with waste electrolyte or sulfuric acid, the reverse-extraction agent sulfuric acid concentration is 150～250g/l, zinc concentration 40～60g/l in the waste electrolyte, the back extraction condition: organic phase and water are in a ratio of 5:1～15:1,2～6 minutes back extraction time, 10～45 ℃ of temperature, settling time is more than 2 minutes, organic phase reusable edible after the back extraction contains zinc less than 1g/l in the circulation organic phase.
The charcoal absorption method is all adopted in liquid and raffinate de-oiling after the back extraction, and activated carbon dosage is 2～10g/l, and the de-oiling temperature is 10～80 ℃, handles back aqueous phase organic concentration less than 1ppm.
After the de-oiling after the back extraction liquid whereabouts decide by wherein zinc and foreign matter content height, if zinc content 〉=75g/l, foreign matter content reaches the new liquid requirement of electrolysis, then directly zinc is sunk in electrolysis; If zinc content＜70g/l, foreign matter content exceeds new liquid requirement, then returns the leaching system as leaching agent.
Along with the carrying out of process, after work for some time, can accumulation Fe in the organic phase
3+, the circulation organic phase can be used 6mol/l salt acid elution removal Fe wherein
3+Impurity.
Compared with prior art, the invention has the advantages that: (1) efficient recovery resource, eliminate and reduced environmental pollution, realized the recycle of waste water.(2) can finely be connected with existing wet zinc-making system, materials such as flushing waste water, waste electrolyte, raffinate, organic extractant recycle in whole technology, both guaranteed the host system volumetric balance, flushing waste water recycle treatment system has stronger handiness again.(3) technology is simple, simple to operate and cost is low, and comprehensive benefit is remarkable, can be widely used in the processing of each zinc hydrometallurgy factory zinc electrolysis flushing waste water.
Description of drawings: Fig. 1 is a process flow diagram of the present invention.
Embodiment:
Embodiment 1: the zinc electrolysis wastewater contains Zn15g/l, H
2SO
420g/l with the NaOH neutralization, regulates pH to 5.0, carries out extracting and enriching zinc then, and concrete extraction conditions is: P
204Make extraction agent, 200
#Kerosene is made thinner, and both volume ratios are P
204: kerosene=40%:60%, extraction phase be than 1.4:1,30 ℃ of extraction temperature, and mixing time 3 minutes, settling time is 5 minutes, 3 grades of extraction progression, control extraction equilibrium pH value about 1.5, recovery of extraction 90%.
Raffinate contains Zn1.2g/l, after the employing 2g/l charcoal absorption de-oiling, returns and does the flushing waste water use.
Rich zinc organic phase contains the about 9g/l of zinc, with containing Zn44.15g/l, H
2SO
4The waste electrolyte back extraction of 187g/l, the back extraction condition is: organic phase and water be than 5:1,30 ℃ of back extraction temperature, mixing time 5 minutes, settling time 10 minutes, 3 grades of back extraction progression, liquid contains Zn90g/l, H approximately after the back extraction
2SO
4140g/l, the zinc back extraction rate of recovery 99%.
Liquid is after 2g/l charcoal absorption de-oiling after the back extraction, and the aqueous phase organic concentration is reduced to below the 1ppm, and the heavy zinc of electrolysis then is at 500A/m
2Electrolysis is 24 hours under the current density, and current efficiency is greater than 90%, and cathode zinc quality reaches the requirement of No. 0 zinc of Zn 〉=99.995%, impurity summation≤0.0050%.
Example 2: the zinc electrolysis wastewater contains Zn10.65g/l, H
2SO
430g/l uses in the lime and adjusting pH to 5.0, filters then, and clear liquid carries out extracting and enriching zinc, and concrete extraction conditions is: P
204Make extraction agent, 200
#Kerosene is made thinner, and both volume ratios are P
204: kerosene=40%:60%, extraction phase be than 1.2/1,30 ℃ of extraction temperature, and mixing time 3 minutes, settling time is 5 minutes, 3 grades of extraction progression, recovery of extraction 92%.
Raffinate contains Zn0.4g/l, and pH value 1.2 after the employing 2g/l charcoal absorption de-oiling, is returned and done the flushing waste water use.
Rich zinc organic phase contains the about 8.5g/l of zinc, with containing Zn44.15g/l, H
2SO
4The waste electrolyte back extraction of 187g/l, the back extraction condition is: organic phase/water compares 6/1,30 ℃ of back extraction temperature, mixing time 5 minutes, settling time 10 minutes, 3 grades of back extraction progression, liquid contains Zn95g/l, H approximately after the back extraction
2SO
4130g/l, the zinc back extraction rate of recovery is greater than 99%.
The liquid aftertreatment is with embodiment 1 after the back extraction, and the heavy zinc of electrolysis then is at 500A/m
2Electrolysis is 24 hours under the current density, and current efficiency is greater than 90%, and cathode zinc quality reaches the requirement of No. 0 zinc of Zn 〉=99.995%, impurity summation≤0.0050%.
Example 3: the zinc electrolysis wastewater contains Zn7.65g/l, H
2SO
430g/l uses in the lime and adjusting pH to 5.0, filters then, and clear liquid carries out extracting and enriching zinc, and concrete extraction conditions is: P
204Make extraction agent, 260
#Kerosene is made thinner, and both volume ratios are P
204: kerosene=40%:60%, extraction phase be than 1/1,25 ℃ of extraction temperature, and mixing time 3 minutes, settling time is 5 minutes, 3 grades of extraction progression, recovery of extraction 95%.
Raffinate contains Zn0.2g/l, and pH value 2.0 after the employing 2g/l charcoal absorption de-oiling, is returned and done the flushing waste water use.
Rich zinc organic phase contains the about 7.5g/l of zinc, with containing Zn44.15g/l, H
2SO
4The waste electrolyte back extraction of 187g/l, the back extraction condition is: organic phase/water compares 8/1,30 ℃ of back extraction temperature, mixing time 5 minutes, settling time 10 minutes, 3 grades of back extraction progression, liquid contains Zn104g/l, H approximately after the back extraction
2SO
4127g/l, the zinc back extraction rate of recovery is greater than 99%.
Liquid is handled with embodiment 1 after the back extraction.
Example 4: the zinc electrolysis wastewater contains Zn9.72g/l, H
2SO
415g/l with the KOH neutralization, regulates pH to pH〉4.0, carry out extracting and enriching zinc then, concrete extraction conditions is: P
204Make extraction agent, 200
#Kerosene is made thinner, and both volume ratios are P
204: kerosene=40%:60%, extraction phase be than 1.2/1,30 ℃ of extraction temperature, and mixing time 3 minutes, settling time is 5 minutes, 3 grades of extraction progression, extraction terminal point acidity H
2SO
412.37g/l, recovery of extraction 88%.
Raffinate contains Zn1.13g/l, adopts 2g/l charcoal absorption de-oiling, returns then and does the flushing waste water use.
Rich zinc organic phase contains the about 7g/l of zinc, uses H
2SO
4The sulfuric acid back extraction of 187g/l, the back extraction condition is: organic phase/water compares 5/1,30 ℃ of back extraction temperature, mixing time 5 minutes, settling time 10 minutes, 3 grades of back extraction progression, liquid contains Zn34.5g/l, H after the back extraction
2SO
4143g/l, the zinc back extraction rate of recovery 99%.
Liquid is after 2g/l charcoal absorption de-oiling after the back extraction, and the aqueous phase organic concentration is reduced to below the lppm, returns the leaching system then and does the leaching agent use.
Example 5: the zinc electrolysis wastewater contains Zn7.65g/l, H
2SO
415g/l with the KOH neutralization, regulates pH to pH〉4.0, carry out extracting and enriching zinc then, concrete extraction conditions is: P
204Make extraction agent, 200
#Kerosene is made thinner, and both volume ratios are P
204: kerosene=30%:70%, extraction phase be than 1/1,30 ℃ of extraction temperature, and mixing time 3 minutes, settling time is 8 minutes, 2 grades of extraction progression, control extraction equilibrium pH value about 3.0, recovery of extraction 90%.
Raffinate contains Zn0.1g/l, adopts 2g/l charcoal absorption de-oiling, returns then and does the flushing waste water use.
Rich zinc organic phase contains the about 7.5g/l of zinc, uses H
2SO
4The sulfuric acid back extraction of 187g/l, the back extraction condition is: organic phase/water compares 8/1,30 ℃ of back extraction temperature, mixing time 5 minutes, settling time 10 minutes, 3 grades of back extraction progression, liquid contains Zn60g/l, H after the back extraction
2SO
4125g/l, the zinc back extraction rate of recovery 99%.
Liquid is after 2g/l charcoal absorption de-oiling after the back extraction, and the aqueous phase organic concentration is reduced to below the 1ppm, returns the leaching system then and does the leaching agent use.
Example 6: the zinc electrolysis wastewater contains Zn5.0g/l, H
2SO
430g/l with the lime neutralization, regulates pH to 4.0, filters then, and clear liquid carries out extracting and enriching zinc, and concrete extraction conditions is: P
204Make extraction agent, 200
#Kerosene is made thinner, and both volume ratios are P
204: kerosene=25%:75%, extraction phase be than 1/1,30 ℃ of extraction temperature, and mixing time 2 minutes, settling time is 5 minutes, 2 grades of extraction progression, recovery of extraction is greater than 95%.
Raffinate contains Zn 0.1g/l, and pH value 3.0 after the employing 2g/l charcoal absorption de-oiling, is returned and done the flushing waste water use.
Rich zinc organic phase contains the about 5g/l of zinc, uses 180g/l H
2SO
4The sulfuric acid back extraction, the back extraction condition is: organic phase/water compares 10/1,25 ℃ of back extraction temperature, mixing time 5 minutes, settling time 10 minutes, 2 grades of back extraction progression, liquid contains Zn50g/l, H approximately after the back extraction
2SO
4130g/l, the zinc back extraction rate of recovery 99%.
Liquid is after 2g/l charcoal absorption de-oiling after the back extraction, and the aqueous phase organic concentration is reduced to below the 1ppm, returns the leaching system then and does the leaching agent use.
Example 7: zinc electrolysis flushing waste water contains Zn5.2g/l, H
2SO
415g/l uses Na
2CO
3PH to 4.0 is regulated in neutralization, carries out extracting and enriching zinc then, and concrete extraction conditions is: P
204Make extraction agent, 260
#Kerosene is made thinner, and both volume ratios are P
204: kerosene=20%:80%, extraction phase be than 1/1,35 ℃ of extraction temperature, and mixing time 3 minutes, settling time is 5 minutes, 2 grades of extraction progression, the rate of recovery is greater than 95%.
Raffinate contains Zn 0.2g/l, and pH value 3.0 after the employing 2g/l charcoal absorption de-oiling, is returned and done the flushing waste water use.
Rich zinc organic phase contains the about 5g/l of zinc, uses 180g/l H
2SO
4The sulfuric acid back extraction, the back extraction condition is: organic phase/water compares 8/1,30 ℃ of back extraction temperature, mixing time 5 minutes, settling time 10 minutes, 3 grades of back extraction progression, liquid contains Zn40g/l, H approximately after the back extraction
2SO
4140g/l, the zinc back extraction rate of recovery 99%.
Liquid is after 2g/l charcoal absorption de-oiling after the back extraction, and the aqueous phase organic concentration is reduced to below the 1ppm, returns the leaching system then and does the leaching agent use.
Claims (6)
1. zinc electrolysis flushing waste water recycle treatment process, it is characterized in that: this method comprises the steps: (1) neutralization/filtration: it is 3～6 that zinc electrolysis flushing waste water is neutralized to the pH value with alkali, filter and remove residue; (2) extraction: with two-2-ethylhexyl phosphoric acid P
204Make extraction agent and kerosene is mixed into organic phase, the back waste water clear liquor that will neutralize mixes with organic phase and extracts, and makes the zinc of aqueous phase change organic phase over to, and raffinate returns and does the use of zinc electrolysis wash-down water directly or after the de-oiling processing; (3) back extraction: do reverse-extraction agent with sulfuric acid or waste electrolyte,, make the zinc in the organic phase change water again over to, the organic phase recycle to the rich zinc organic phase back extraction that preceding step obtains; (4) de-oiling: with gac to back extraction after the liquid de-oiling, solution send the heavy zinc of electrolysis or returns the leaching system as leaching agent after the de-oiling.
2. zinc electrolysis flushing waste water recycle treatment process according to claim 1 is characterized in that: neutralization is one or more combination in sodium hydroxide, potassium hydroxide, yellow soda ash and the lime with alkali.
3. zinc electrolysis flushing waste water recycle treatment process according to claim 1, it is characterized in that: extraction conditions is: extractant concentration P in the extracted organic phase
20415～40%, organic phase and water are in a ratio of 1:2～2:1,10～40 ℃ of temperature, and 1～5 minute extraction time, settling time is greater than 2 minutes, raffinate pH value 0.5～4.0.
4. zinc electrolysis flushing waste water recycle treatment process according to claim 1, it is characterized in that: during rich zinc organic phase back extraction, reverse-extraction agent sulfuric acid concentration 150～250g/l, zinc concentration 40～60g/l in the waste electrolyte, the back extraction condition: organic phase and water be than 5:1～15:1,2～6 minutes time, 10～45 ℃ of temperature, settling time contained zinc less than 1g/l in the circulation organic phase greater than 2 minutes after the back extraction.
5. according to the described zinc electrolysis of claim 1 flushing waste water recycle treatment process, it is characterized in that: the de-oiling condition: activated carbon dosage is 2～10g/l, and the de-oiling temperature is 10～80 ℃, handles back aqueous phase organic concentration less than 1ppm.
6. according to the described zinc electrolysis of claim 1 flushing waste water recycle treatment process, it is characterized in that: solution zinc content 〉=75g/l after the de-oiling, foreign matter content reaches the new liquid requirement of electrolysis, the heavy zinc of then direct electrolysis, if zinc content＜70g/l, foreign matter content exceeds new liquid requirement, then returns the leaching system as leaching agent.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101886170B (en) * | 2010-06-29 | 2012-05-30 | 白银先达科技服务有限责任公司 | Production process for isolating fluorine and chlorine by acid extraction during electrolytic zinc production |
| CN102399984A (en) * | 2011-12-16 | 2012-04-04 | 东北大学 | Method for extracting and recovering zinc from zinc-containing waste water |
| CN102583598A (en) * | 2012-03-19 | 2012-07-18 | 赤峰中色锌业有限公司 | Cycle production method for recovering zinc from beneficiation wastewater of high leaching slag |
| CN102600980A (en) * | 2012-03-19 | 2012-07-25 | 赤峰中色锌业有限公司 | Recycling method for mineral processing waste water with high leaching residue content in zinc hydrometallurgy |
| CN105858779B (en) * | 2016-04-15 | 2018-11-27 | 江南大学 | A method of by recycling metal in low-concentration heavy metal ions waste water |
| CN106630313A (en) * | 2016-12-16 | 2017-05-10 | 江苏永葆环保科技股份有限公司 | Reduction circulation process method for recycling zinc elements in iron-containing waste acid |
| CN108314200A (en) * | 2017-01-17 | 2018-07-24 | 云南祥云飞龙再生科技股份有限公司 | A kind of recovery processing technique of Mn-bearing waste water |
| CN108751445B (en) * | 2018-06-01 | 2021-06-01 | 武汉钢铁有限公司 | Method for preparing circulating cooling water quality stabilizer by using zinc-containing wastewater and application thereof |
| CN109354252A (en) * | 2018-11-27 | 2019-02-19 | 来宾华锡冶炼有限公司 | A kind of processing method of Sewage from Sulphuric Acid Plants |
| CN113023799B (en) * | 2021-03-02 | 2022-10-28 | 江西金晖锂电材料股份有限公司 | Waste lithium battery electrolyte wastewater recovery processing device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4401531A (en) * | 1981-07-24 | 1983-08-30 | Daniel Martin San Lorenzo | Process for the production of electrolytic zinc or high purity zinc salts from secondary zinc raw-materials |
| CN1384063A (en) * | 2001-04-29 | 2002-12-11 | 曾智勇 | Effluent treating process for wet zinc smelting |
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2007
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4401531A (en) * | 1981-07-24 | 1983-08-30 | Daniel Martin San Lorenzo | Process for the production of electrolytic zinc or high purity zinc salts from secondary zinc raw-materials |
| CN1384063A (en) * | 2001-04-29 | 2002-12-11 | 曾智勇 | Effluent treating process for wet zinc smelting |
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