CN102399984A - Method for extracting and recovering zinc from zinc-containing waste water - Google Patents
Method for extracting and recovering zinc from zinc-containing waste water Download PDFInfo
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Abstract
The invention relates to a method for extracting and recovering zinc from zinc-containing waste water. The method comprises the following steps of: (1) adding lime into the zinc-containing waste water, filtering, and thus obtaining primary filtrate; (2) mixing sulfonated kerosene, P204 and sodium hydroxide to obtain a pretreatment extractant; (3) extracting the primary filtrate by using the pretreatment extractant to obtain a load organic phase and raffinate; (4) performing reextraction on the load organic phase by using waste electrolyte to obtain a blank organic phase and reextraction liquid; (5) adding the lime into the raffinate, stirring for causticizing, filtering to remove filter residues, and thus obtaining secondary filtrate; and (6) mixing the secondary filtrate and the blank organic phase for pretreatment, standing, and thus obtaining a pretreatment organic phase and pretreatment waste water, wherein the pretreatment organic phase returns to the step (3) to be recycled, and the pretreatment waste water returns to a main production process to be recycled. The method is efficient and clean, and has a good effect on environmental protection.
Description
Technical field
The present invention relates to a kind of recovery method of zinc, particularly a kind of method that reclaims zinc that from zinc-containing water, extracts.
Background technology
The a large amount of zinc-containing water of each operation meeting output of zinc hydrometallurgy, this comprises the washery slag waste water of leached mud output in the washery slag process, the beneficiation wastewater of output when leached mud carries out the ore dressing processing, the flushing waste water that produces when potroom washing equipment, electrode etc.This type of waste water all contains valuable metal zinc and other foreign ion in various degree, if simple discharging can make valuable element loss and environmental pollution; But adopt common waste water treatment process such as lime to neutralize, be unfavorable for reclaiming zinc again.
The another difficult problem that zinc hydrometallurgy enterprise faces is the contradiction of waste water zero emission and zinc metallurgy system " volumetric expansion "; As for the hot acid leached mud that leaches operation, it is about about 6% after separating, washing, to contain zinc in the slag, and wherein the zinc about half is water-soluble zinc, can it be reclaimed through further washing; But owing to receive the restriction of system bulk expansible, slag washing water is difficult to return main flow, has limited zinciferous further washing and recycling in the hot acid leached mud.
For this reason, develop new treatment process, realize having great practical significance realizing the extraction recovery and the waste water recycling of zinc in the zinc-containing water of zinc hydrometallurgy factory output.
Publication number is the one Chinese patent application of CN01114434.3, discloses a kind of zinc hydrometallurgy method of wastewater treatment, and waste water is through NaOH neutralization and deposition, and liquid-solid separation postprecipitation slag further reclaims zinc, and filtrating is qualified discharge after flocculating settling separates; This method is used the NaOH neutralization precipitation instead, has avoided in the lime neutralization precipitation process zinc with the loss of slag, and is guaranteed to the recovery of zinc.But waste water returns and recycles the lasting accumulation that certainly will cause sodium ion, so this method limited the cyclically utilizing of waste water, has to efflux.
For further realizing the dp that waste water recycling and zinc reclaim adopting solvent extraction method to reclaim zinc and also obtained extensive concern in recent years, typical extraction agent is a di-(2-ethylhexyl)phosphoric acid, and the homemade trade mark is P204; Like application number is the one Chinese patent application of 200710034600.X; Disclose the treatment process of a kind of zinc electrolysis flushing waste water recycle, zinc electrolysis flushing waste water neutralizes through alkali, and zinc is carried in the P204 extraction; Reclaim zinc with the waste electrolyte back extraction; Regeneration organic phase, raffinate are returned and are used or efflux after de-oiling is handled; Its shortcoming is that aqueous phase acidity increases in the P204 extracting zinc process, has suppressed the percentage extraction of zinc in the extraction process; Only when containing zinc concentration in the waste water when low, recovery of extraction just reaches 95%, and when waste water contained zinc 9.72g/L, recovery of extraction was merely 88%; Therefore, the recovery of extraction of zinc is low, particularly when zinc concentration is high, after zinc is carried in extraction, still contains the zinc of a great deal of in the raffinate, has limited the use range of processed waste water; If still need carrying out further neutralization precipitation, the words that waste water effluxes handle.This drawbacks limit the suitability of this method.
In order to improve the recovery of extraction of aqueous phase zinc, also there is the investigator to be employed in the extraction process water is added alkali neutral method, as adopting NaOH, NH
3, NH
4HCO
3Neutralize, the shortcoming that these class methods cause is that sodium or the ammonium radical ion that aqueous phase is brought into can't be discharged, and waste water can't recycle, if adopt the lime neutralization, a large amount of calcium sulfate slags forms the operation that then can seriously hinder extracting operation.
Summary of the invention
Handle the problems referred to above that go up existence to existing zinc-containing water; The present invention provides a kind of method that reclaims zinc that from zinc-containing water, extracts; Employing extracts zinc-containing water through the pretreated P204 of containing organic phase and carries zinc; Improve effect of extracting, waste water returns Production Flow Chart after treatment and uses, and when reducing pollution, improves the cyclic utilization rate of water.
The method that reclaims zinc that from zinc-containing water, extracts of the present invention is carried out according to the following steps:
1, in zinc-containing water, add the lime stirring and neutralize, regulating the pH value is 3 ~ 6; Remove by filter filter residue then, obtain first-time filtrate;
2, sulfonated kerosene is mixed the acquisition organic phase with P204; The blending ratio of sulfonated kerosene and P204 is (1.5 ~ 4) by volume: 1; Adopt NaOH to carry out pre-treatment when organic phase is used for the first time, obtain the pre-treatment organic phase, the consumption of sodium hydroxide is 50 ~ 100g/LP204 during pre-treatment;
3, adopt the pre-treatment organic phase that first-time filtrate is carried out 1 ~ 3 grade of extraction, obtain load organic phases and raffinate; The consumption of pre-treatment organic phase is 0.5 ~ 2 times of first-time filtrate TV;
4, load organic phases is carried out 1 ~ 2 grade of reextraction with waste electrolyte, obtain blank organic phase and strip liquor; The volume ratio of load organic phases and waste electrolyte is (1 ~ 2): 1;
5, in raffinate, add the lime stirring and carry out causticization, filter then and remove filter residue, obtain secondary filtrating; The consumption of lime by the quality of CaO in the lime by 0.9 ~ 1.5 extraordinarily the going into of quality of Zn in the processing zinc-containing water;
6, secondary filtrating is mixed with blank organic phase carry out pre-treatment, leave standstill acquisition pre-treatment organic phase and pretreated waste water then, the pre-treatment organic phase turns back in the step 3 and recycles.
Above-mentioned zinc-containing water is the zinc-containing water that each operation of zinc hydrometallurgy produces, and comprises the washery slag waste water of leached mud output in the washery slag process, the beneficiation wastewater of output when leached mud carries out the ore dressing processing, the flushing waste water that produces when potroom washing equipment, electrode; The zinc content of zinc-containing water is 5 ~ 40g/L.
Above-mentioned pretreated waste water turns back in each operation of zinc hydrometallurgy and uses as new water, and the waste water that forms once more gets in the step 1 and handles as zinc-containing water.
The strip liquor that aforesaid method obtains gets into the leaching operation of zinc hydrometallurgy operation, perhaps gets into the electrodeposition operation after the de-oiling.
When the step 3 in the aforesaid method extracted, the time of every grade of extraction was 3 ~ 5min, left standstill 3 ~ 8min after every grade of extraction.
When the step 4 in the aforesaid method was stripped, the time of every grade of reextraction was 3 ~ 5min, left standstill 3 ~ 8min after every grade of reextraction.
The content of zinc is 0.1 ~ 1.6g/L in the raffinate that step 3 obtains in the aforesaid method, the percentage extraction of zinc >=96%.
Method of the present invention is through P204 is carried out pre-treatment, and is high at the extraction efficiency of extraction process zinc, can obviously reduce the required progression of extraction, reduces the investment of extraction equipment investment and purchase extraction agent; And because the percentage extraction of extraction process zinc is high, it is low that the waste water after the processing contains zinc concentration, is convenient to continue to return former operation and recycles; Overall plan combines to form the closed cycle of organic phase and water with other operations, efficient, the cleaning of method of the present invention also has good effect in environment protection.
Description of drawings
Fig. 1 is the method flow synoptic diagram that zinc is reclaimed in the extraction from zinc-containing water in the embodiment of the invention.
Embodiment
The lime that adopts in the embodiment of the invention, sulfonated kerosene, P204 (di-(2-ethylhexyl)phosphoric acid) and sodium hydroxide are the general industry product.
The waste electrolyte that the waste electrolyte of selecting for use in the embodiment of the invention produces for the zinc hydrometallurgy electrowinning process, sulfur acid 140 ~ 160g/L contains zinc 40 ~ 60g/L.
Embodiment 1
The zinc content of the zinc-containing water that adopts is 5.0g/L;
1, in zinc-containing water, add the lime stirring and neutralize, regulating the pH value is 6; Remove by filter filter residue then, obtain first-time filtrate;
2, sulfonated kerosene, P204 and sodium hydroxide are mixed acquisition pre-treatment organic phase; The blending ratio of sulfonated kerosene and P204 is 4:1 by volume, and the consumption of sodium hydroxide is 50g/LP204;
3, adopt the pre-treatment organic phase that first-time filtrate is carried out 1 grade of extraction, obtain load organic phases and raffinate; The consumption of pre-treatment organic phase is 0.5 times of first-time filtrate TV; The time of extraction is 3min, leaves standstill 3min after the extraction; The average content of zinc is 0.1g/L in the raffinate;
4, load organic phases is carried out 1 grade of reextraction with waste electrolyte, obtain blank organic phase and strip liquor; The volume ratio of load organic phases and waste electrolyte is 1:1; Waste electrolyte sulfur acid 156g/L contains zinc 45g/L; The time of stripping is 5min, leaves standstill 8min after the back extraction;
5, in raffinate, add the lime stirring and carry out causticization, filter then and remove filter residue, obtain secondary filtrating; The consumption of lime by the quality of CaO in the lime by 0.9 extraordinarily the going into of quality of Zn in the processing zinc-containing water;
6, secondary filtrating is mixed with blank organic phase carry out pre-treatment, leave standstill acquisition pre-treatment organic phase and pretreated waste water then, the pre-treatment organic phase turns back in the step 3 and recycles;
Pretreated waste water turns back in each operation of zinc hydrometallurgy and uses as new water, and the waste water that forms once more gets in the step 1 and handles as zinc-containing water;
Strip liquor gets into the leaching operation of zinc hydrometallurgy operation, perhaps gets into the electrodeposition operation after the de-oiling;
The percentage extraction of zinc is 98%.
Embodiment 2
The zinc content of the zinc-containing water that adopts is 18.5g/L;
1, in zinc-containing water, add the lime stirring and neutralize, regulating the pH value is 4.5; Remove by filter filter residue then, obtain first-time filtrate;
2, sulfonated kerosene, P204 and sodium hydroxide are mixed acquisition pre-treatment organic phase; The blending ratio of sulfonated kerosene and P204 is 1.5:1 by volume, and the consumption of sodium hydroxide is 70g/LP204;
3, adopt the pre-treatment organic phase that first-time filtrate is carried out 2 grades of extractions, obtain load organic phases and raffinate; The consumption of pre-treatment organic phase is 1 times of first-time filtrate TV; The time of every grade of extraction is 3min, leaves standstill 5min after every grade of extraction; The average content of zinc is 0.18g/L in the raffinate;
4, load organic phases is carried out 1 grade of reextraction with waste electrolyte, obtain blank organic phase and strip liquor; The volume ratio of load organic phases and waste electrolyte is 1:1; Waste electrolyte sulfur acid 140g/L contains zinc 60g/L; The time of stripping is 5min, leaves standstill 8min after the back extraction;
5, in raffinate, add the lime stirring and carry out causticization, filter then and remove filter residue, obtain secondary filtrating; The consumption of lime by the quality of CaO in the lime by 1.1 extraordinarily the going into of quality of Zn in the processing zinc-containing water;
6, secondary filtrating is mixed with blank organic phase carry out pre-treatment, leave standstill acquisition pre-treatment organic phase and pretreated waste water then, the pre-treatment organic phase turns back in the step 3 and recycles;
Pretreated waste water turns back in each operation of zinc hydrometallurgy and uses as new water, and the waste water that forms once more gets in the step 1 and handles as zinc-containing water;
Strip liquor gets into the leaching operation of zinc hydrometallurgy operation, perhaps gets into the electrodeposition operation after the de-oiling;
The percentage extraction of zinc is 99%.
Embodiment 3
The zinc content of the zinc-containing water that adopts is 30.2g/L;
1, in zinc-containing water, add the lime stirring and neutralize, regulating the pH value is 4; Remove by filter filter residue then, obtain first-time filtrate;
2, sulfonated kerosene, P204 and sodium hydroxide are mixed acquisition pre-treatment organic phase; The blending ratio of sulfonated kerosene and P204 is 3:1 by volume, and the consumption of sodium hydroxide is 80g/LP204;
3, adopt the pre-treatment organic phase that first-time filtrate is carried out 3 grades of extractions, obtain load organic phases and raffinate; The consumption of pre-treatment organic phase is 2 times of first-time filtrate TV; The time of every grade of extraction is 4min, leaves standstill 8min after every grade of extraction; The average content of zinc is 0.6g/L in the raffinate;
4, load organic phases is carried out 2 grades of reextraction with waste electrolyte, obtain blank organic phase and strip liquor; The volume ratio of load organic phases and waste electrolyte is 2:1; Waste electrolyte sulfur acid 160g/L contains zinc 40g/L; The time of every grade of reextraction is 3min, leaves standstill 3min after every grade of back extraction;
5, in raffinate, add the lime stirring and carry out causticization, filter then and remove filter residue, obtain secondary filtrating; The consumption of lime by the quality of CaO in the lime by 1.3 extraordinarily the going into of quality of Zn in the processing zinc-containing water;
6, secondary filtrating is mixed with blank organic phase carry out pre-treatment, leave standstill acquisition pre-treatment organic phase and pretreated waste water then, the pre-treatment organic phase turns back in the step 3 and recycles;
Pretreated waste water turns back in each operation of zinc hydrometallurgy and uses as new water, and the waste water that forms once more gets in the step 1 and handles as zinc-containing water;
Strip liquor gets into the leaching operation of zinc hydrometallurgy operation, perhaps gets into the electrodeposition operation after the de-oiling;
The percentage extraction of zinc is 98%.
Embodiment 4
The zinc content of the zinc-containing water that adopts is 35.4g/L;
1, in zinc-containing water, add the lime stirring and neutralize, regulating the pH value is 4; Remove by filter filter residue then, obtain first-time filtrate;
2, sulfonated kerosene, P204 and sodium hydroxide are mixed acquisition pre-treatment organic phase; The blending ratio of sulfonated kerosene and P204 is 3:1 by volume, and the consumption of sodium hydroxide is 100g/LP204;
3, adopt the pre-treatment organic phase that first-time filtrate is carried out 3 grades of extractions, obtain load organic phases and raffinate; The consumption of pre-treatment organic phase is 2 times of first-time filtrate TV; The time of every grade of extraction is 5min, leaves standstill 8min after every grade of extraction; The average content of zinc is 0.71g/L in the raffinate;
4, load organic phases is carried out 2 grades of reextraction with waste electrolyte, obtain blank organic phase and strip liquor; The volume ratio of load organic phases and waste electrolyte is 2:1; Waste electrolyte sulfur acid 150g/L contains zinc 50g/L; The time of every grade of reextraction is 4min, leaves standstill 6min after every grade of back extraction;
5, in raffinate, add the lime stirring and carry out causticization, filter then and remove filter residue, obtain secondary filtrating; The consumption of lime by the quality of CaO in the lime by 1.5 extraordinarily the going into of quality of Zn in the processing zinc-containing water;
6, secondary filtrating is mixed with blank organic phase carry out pre-treatment, leave standstill acquisition pre-treatment organic phase and pretreated waste water then, the pre-treatment organic phase turns back in the step 3 and recycles;
Pretreated waste water turns back in each operation of zinc hydrometallurgy and uses as new water, and the waste water that forms once more gets in the step 1 and handles as zinc-containing water;
Strip liquor gets into the leaching operation of zinc hydrometallurgy operation, perhaps gets into the electrodeposition operation after the de-oiling;
The percentage extraction of zinc is 98%.
Embodiment 5
The zinc content of the zinc-containing water that adopts is 40g/L;
1, in zinc-containing water, add the lime stirring and neutralize, regulating the pH value is 3; Remove by filter filter residue then, obtain first-time filtrate;
2, sulfonated kerosene, P204 and sodium hydroxide are mixed acquisition pre-treatment organic phase; The blending ratio of sulfonated kerosene and P204 is 3:1 by volume, and the consumption of sodium hydroxide is 80g/LP204;
3, adopt the pre-treatment organic phase that first-time filtrate is carried out 1 grade of extraction, obtain load organic phases and raffinate; The consumption of pre-treatment organic phase is 1.5 times of first-time filtrate TV; The time of extraction is 5min, leaves standstill 8min after the extraction; The average content of zinc is 1.6g/L in the raffinate;
4, load organic phases is carried out 2 grades of reextraction with waste electrolyte, obtain blank organic phase and strip liquor; The volume ratio of load organic phases and waste electrolyte is 1.5:1; Waste electrolyte sulfur acid 155g/L contains zinc 48g/L; The time of every grade of reextraction is 4min, leaves standstill 6min after the back extraction;
5, in raffinate, add the lime stirring and carry out causticization, filter then and remove filter residue, obtain secondary filtrating; The consumption of lime by the quality of CaO in the lime by 1.1 extraordinarily the going into of quality of Zn in the processing zinc-containing water;
6, secondary filtrating is mixed with blank organic phase carry out pre-treatment, leave standstill acquisition pre-treatment organic phase and pretreated waste water then, the pre-treatment organic phase turns back in the step 3 and recycles;
Pretreated waste water turns back in each operation of zinc hydrometallurgy and uses as new water, and the waste water that forms once more gets in the step 1 and handles as zinc-containing water;
Strip liquor gets into the leaching operation of zinc hydrometallurgy operation, perhaps gets into the electrodeposition operation after the de-oiling;
The percentage extraction of zinc is 96%.
Claims (4)
1. one kind extracts the method that reclaims zinc from zinc-containing water, it is characterized in that carrying out according to the following steps:
(1) in zinc-containing water, add the lime stirring and neutralize, regulating the pH value is 3 ~ 6, removes by filter filter residue then, obtains first-time filtrate;
(2) sulfonated kerosene is mixed the acquisition organic phase with P204; The blending ratio of sulfonated kerosene and P204 is (1.5 ~ 4) by volume: 1; Adopt NaOH to carry out pre-treatment when organic phase is used for the first time, obtain the pre-treatment organic phase, the consumption of sodium hydroxide is 50 ~ 100g/LP204 during pre-treatment;
(3) adopt the pre-treatment organic phase that first-time filtrate is carried out 1 ~ 3 grade of extraction, obtain load organic phases and raffinate; The consumption of pre-treatment organic phase is 0.5 ~ 2 times of first-time filtrate TV;
(4) load organic phases is carried out 1 ~ 2 grade of reextraction with waste electrolyte, obtain blank organic phase and strip liquor; The volume ratio of load organic phases and waste electrolyte is (1 ~ 2): 1;
(5) in raffinate, add the lime stirring and carry out causticization, filter then and remove filter residue, obtain secondary filtrating; The mass ratio that the consumption of lime is pressed CaO and the Zn in the zinc-containing water that handles in the lime is (0.9 ~ 1.5): 1;
(6) secondary filtrating is mixed with blank organic phase carry out pre-treatment, leave standstill acquisition pre-treatment organic phase and pretreated waste water then, the pre-treatment organic phase turns back in the step 3 and recycles;
Described strip liquor gets into the leaching operation of zinc hydrometallurgy operation, perhaps gets into the electrodeposition operation after the de-oiling; Described pretreated waste water is used as new water.
2. a kind of method that reclaims zinc that from zinc-containing water, extracts according to claim 1, the zinc content that it is characterized in that described zinc-containing water is 5 ~ 40g/L
A kind of method that reclaims zinc that from zinc-containing water, extracts according to claim 1 is characterized in that step (3) when extracting, and the time of every grade of extraction is 3 ~ 5min, leaves standstill 3 ~ 8min after every grade of extraction.
3. a kind of method that reclaims zinc that from zinc-containing water, extracts according to claim 1 is characterized in that step (4) when stripping, and the time of every grade of reextraction is 3 ~ 5min, leaves standstill 3 ~ 8min after every grade of reextraction.
4. a kind of method that reclaims zinc that from zinc-containing water, extracts according to claim 1, the content that it is characterized in that zinc in the described raffinate is 0.1 ~ 1.6g/L, the percentage extraction of zinc >=96%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103146918A (en) * | 2013-03-29 | 2013-06-12 | 云南金鼎锌业有限公司 | Process for directly producing electrolytic zinc from zinc extraction liquid |
| WO2014154160A1 (en) * | 2013-03-27 | 2014-10-02 | 云南祥云飞龙再生科技股份有限公司 | Hydrometallurgical process for recovering lead from lead sulfate |
| CN104451146A (en) * | 2014-11-04 | 2015-03-25 | 云南祥云飞龙再生科技股份有限公司 | Method for recycling zinc from chloride system |
| CN104531995A (en) * | 2014-12-22 | 2015-04-22 | 昆明冶金研究院 | Method for extracting zinc from low-grade zinc-containing material leaching liquid |
| CN105779763A (en) * | 2016-05-27 | 2016-07-20 | 赤峰中色锌业有限公司 | Method for extracting zinc from high-cadmium zinc-contained mineral separation tailing water and preparing electric zinc |
| CN105838886A (en) * | 2016-05-27 | 2016-08-10 | 赤峰中色锌业有限公司 | Method for extracting and recycling zinc from beneficiation tailing water of lead silver residues of zinc hydrometallurgy |
| 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 |
| CN108033589A (en) * | 2017-10-28 | 2018-05-15 | 株洲冶炼集团股份有限公司 | The method that a kind of waste acid removal of impurities in acid making system recycles |
| 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 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2014154160A1 (en) * | 2013-03-27 | 2014-10-02 | 云南祥云飞龙再生科技股份有限公司 | Hydrometallurgical process for recovering lead from lead sulfate |
| CN103146918A (en) * | 2013-03-29 | 2013-06-12 | 云南金鼎锌业有限公司 | Process for directly producing electrolytic zinc from zinc extraction liquid |
| CN104451146A (en) * | 2014-11-04 | 2015-03-25 | 云南祥云飞龙再生科技股份有限公司 | Method for recycling zinc from chloride system |
| CN104531995A (en) * | 2014-12-22 | 2015-04-22 | 昆明冶金研究院 | Method for extracting zinc from low-grade zinc-containing material leaching liquid |
| CN104531995B (en) * | 2014-12-22 | 2017-06-16 | 昆明冶金研究院 | The method of extracting zinc from low-grade material containing zinc leachate |
| CN105779763A (en) * | 2016-05-27 | 2016-07-20 | 赤峰中色锌业有限公司 | Method for extracting zinc from high-cadmium zinc-contained mineral separation tailing water and preparing electric zinc |
| CN105838886A (en) * | 2016-05-27 | 2016-08-10 | 赤峰中色锌业有限公司 | Method for extracting and recycling zinc from beneficiation tailing water of lead silver residues of zinc hydrometallurgy |
| 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 |
| CN108033589A (en) * | 2017-10-28 | 2018-05-15 | 株洲冶炼集团股份有限公司 | The method that a kind of waste acid removal of impurities in acid making system recycles |
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Application publication date: 20120404 |