CN102071318A - Purification method of zinc sulfate leaching liquid - Google Patents
Purification method of zinc sulfate leaching liquid Download PDFInfo
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- CN102071318A CN102071318A CN2011100298464A CN201110029846A CN102071318A CN 102071318 A CN102071318 A CN 102071318A CN 2011100298464 A CN2011100298464 A CN 2011100298464A CN 201110029846 A CN201110029846 A CN 201110029846A CN 102071318 A CN102071318 A CN 102071318A
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Abstract
The invention provides a purification method of zinc sulfate leaching liquid. The purification method comprises the following steps: adding the zinc sulfate leaching liquid into a purification container; leading the inside of the purification container to be under the non-oxidizing atmosphere, and adding zinc powder into the zinc sulfate leaching liquid while stirring so as to precipitate impurity metals, thereby obtaining liquid after precipitation; and carrying out solid-liquid separation on the liquid after precipitation so as to obtain zinc sulfate purification liquid and solids containing impurity precipitates. The purification method at least has one of the following advantages: high purification speed, high purification efficiency and low energy consumption.
Description
Technical field
The present invention relates to field of metallurgy.Particularly, the present invention relates to the purifying method of zinc sulfate leach liquor.
Background technology
Main in the world at present by adopting wet processing to produce zinc.No matter be that traditional roasting-leaching-electrodeposition method zinc metallurgy or zinc sulfide ore directly leaches-electrodeposition method zinc metallurgy, all comprise and leach operation (being generally sulfuric acid leaches), output zinc sulfate leach liquor, and simultaneously some foreign metals for example copper, cadmium, cobalt, nickel etc. also will enter in the infusion solution.Thereby, before the zinc sulfate leach liquor is carried out subsequent disposal such as electrolysis, need purify the zinc sulfate leach liquor.
Therefore, need a kind of method that the zinc sulfate leach liquor is purified in the field of metallurgy at present.
Summary of the invention
The present invention is intended to solve at least one of technical problem that exists in the prior art.For this reason, one object of the present invention is to propose a kind of zinc sulfate purification of leaching liquor method, and it has one of following advantage at least: purification efficiency height, good purification and energy consumption are low.
Zinc sulfate purification of leaching liquor method according to the embodiment of the invention comprises:
A) described zinc sulfate leach liquor is joined in the purifying vessel;
B) make in the described purifying vessel and be under the nonoxidizing atmosphere, in described zinc sulfate leach liquor, add zinc powder while stirring, obtain post precipitation liquid with the precipitated impurities metal; And
C) described post precipitation liquid is carried out solid-liquid separation, obtain zinc sulfate scavenging solution and impure precipitated solid.
In addition, according to embodiments of the invention, can also have following additional technical feature:
According to one embodiment of present invention, the described solution of zinc sulfate sulphuric leachate that is zinc ore.
According to one embodiment of present invention, described foreign metal is be selected from copper, cobalt, cadmium and nickel at least a.
According to one embodiment of present invention, it further comprises: D) reclaim described foreign metal from described impure precipitated solid.
According to one embodiment of present invention, at step B) described in nonoxidizing atmosphere be nitrogen atmosphere, and pressure is 0.2-0.6MPa.
According to one embodiment of present invention, based on the content of zinc sulfate leach liquor foreign metal, institute's addition is 60-110 a times of described foreign metal content.
According to one embodiment of present invention, at step B) in stirring velocity be 250-350rpm.
According to one embodiment of present invention, it further comprises by electro-deposition method and prepares metallic zinc.
Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage are from obviously and easily understanding becoming the description of embodiment in conjunction with following accompanying drawing, wherein:
Fig. 1 is the schema according to the purifying method of the zinc sulfate leach liquor of the embodiment of the invention.
Fig. 2 is the schema of the purifying method of zinc sulfate leach liquor according to another embodiment of the present invention.
Fig. 3 is the schema according to the purifying method of the zinc sulfate leach liquor of further embodiment of this invention.
Embodiment
Describe embodiments of the invention below in detail, the example of described embodiment is shown in the drawings, and wherein identical from start to finish or similar label is represented identical or similar elements or the element with identical or similar functions.Below by the embodiment that is described with reference to the drawings is exemplary, only is used to explain the present invention, and can not be interpreted as limitation of the present invention.
A kind of purifying method of zinc sulfate leach liquor is provided according to embodiments of the invention in one aspect of the invention.With reference to figure 1, this method comprises implements the following step successively:
Step 100: zinc sulfate leach liquor to be clean is joined in the purifying vessel.
Step 200: add zinc powder while stirring in purifying vessel, so that the replacement(metathesis)reaction of zinc powder and impurities element takes place in purifying vessel, thereby making that the impurities element forms in the zinc sulfate leach liquor precipitates, and obtains post precipitation liquid.In this step, keep being in nonoxidizing atmosphere in the purifying vessel.
Step 300: post precipitation liquid is carried out solid-liquid separation, obtain zinc sulfate scavenging solution and impure precipitated solid.
According to the purifying method of above-mentioned zinc sulfate leach liquor, can realize purifying treatment expeditiously to the zinc sulfate leach liquor.
In leaching method, at first pending zinc sulfate leach liquor is joined in the purifying vessel (step 100) according to the zinc sulfate leach liquor of the embodiment of the invention.According to embodiments of the invention, the mode that the zinc sulfate leach liquor is joined in the purifying vessel is not particularly limited.According to concrete example of the present invention, be pumped in the purifying vessel by force (forcing) pump.Thus, can will be added in the purifying vessel in the zinc sulfate leach liquor effectively.Broad understanding should be done in the term that is adopted " zinc sulfate leach liquor " in the present invention, and it can be any solution of zinc sulfate that needs purifying treatment that contains impurity metallic elements.In embodiments of the invention, the zinc sulfate leach liquor can be the leaching zinc sulfate leach liquor that operation produced in the wet processing zinc metallurgy process, and then the impurity metallic elements that is wherein contained is be selected from copper, cobalt, cadmium and nickel at least a.Thus, with reference to figure 2, in concrete example of the present invention, comprise that further the zinc sulfate scavenging solution that the purifying zinc sulfate leach liquor is obtained carries out the step (step 400) that galvanic deposit zinc metallurgy obtains metallic zinc, the impurity metallic elements that comprised in the zinc sulfate leach liquor form with solid metal can also be precipitated out simultaneously.Thereby, according to an example of the present invention,, obtain zinc sulfate scavenging solution and impure precipitated solid by solid-liquid separation after, also further comprise the step (step 500) that reclaims metal from impure precipitated solid with reference to figure 3.Thus, can further from the zinc sulfate leach liquor, reclaim valuable metal, reduce pollution, and reduced the industry cost environment.
Next, after the zinc sulfate leach liquor is added purifying vessel, in purifying vessel, add zinc powder (step 200) while stirring, so that the replacement(metathesis)reaction of zinc powder and impurities element takes place in purifying vessel, thereby make that the impurities element forms precipitation in the zinc sulfate leach liquor, obtain post precipitation liquid.In an embodiment of the present invention, stirring velocity is 250-350rpm.After zinc powder is added into purifying vessel, zinc powder can with the impurity element generation replacement(metathesis)reaction that comprised in the pending zinc sulfate leach liquor, make the impurity element that is comprised form precipitation.With the copper is example, and replacement(metathesis)reaction is:
Cu
2++Zn＝Zn
2++Cu↓。
During step 200, keep being in nonoxidizing atmosphere in the purifying vessel.Thus, can avoid metal newly-generated in the zinc sulfate purification of leaching liquor process oxidized, thereby avoid its redissolution.Thus, the consumption that can reduce zinc powder reduces cost, and can improve purification efficiency, can realize purifying treatment at short notice, and then the impurity element that is comprised in the zinc sulfate scavenging solution after purification is few, good purification.According to embodiments of the invention, the mode that keeps being in nonoxidizing atmosphere in the purifying vessel for example is not particularly limited and can realizes by feeding rare gas element.At embodiments of the invention, can adopt cheap nitrogen to realize nonoxidizing atmosphere.The concrete example according to the present invention is nitrogen atmosphere and the pressure that keeps 0.2-0.6MPa by feeding in purifying vessel in the nitrogen maintenance purifying vessel.Thus, can avoid leach liquor to contact, redissolve, and use nitrogen can make the purification cost lower thereby the precipitated metal that can effectively avoid the impurities element to be generated after replacement(metathesis)reaction is oxidized with air.
According to embodiments of the invention, add zinc powder amount be not particularly limited.According to concrete example of the present invention, based on the content of impurity metallic elements in the zinc sulfate leach liquor, the content of impurity nickel cobalt for example, add zinc powder amount be nickel cobalt amount 60-110 doubly.Thus, can reduce the metal zinc consumption, reduce cost.According to embodiments of the invention, add zinc powder granularity be not particularly limited.According to concrete example of the present invention, the granularity of the zinc powder that adopts accounts for 88%-95% for-0.11mm.Thus, can improve the contact area of zinc powder and sulphuric leachate, thereby further improve purification efficiency.
According to embodiments of the invention, step 200 can at high temperature be carried out, and can help the carrying out of replacement(metathesis)reaction thus.In some concrete examples, in step 200 process, can keep the temperature in the purifying vessel is 85-130 degree centigrade.Thus, can improve the speed of replacement(metathesis)reaction, further improve purification efficiency.According to embodiments of the invention, the time of purifying treatment is not particularly limited in purifying vessel.In some concrete examples, the time of carrying out replacement(metathesis)reaction in purifying vessel is 30-60 minute.Thus, can improve the better decontamination effect improving of realization.
After step 200, formed post precipitation liquid is carried out solid-liquid separation, obtain zinc sulfate scavenging solution and impure precipitated solid (step 300).The mode of solid-liquid separation is not subjected to special restriction, for example can adopt modes such as plate and frame press filtration, disk vacuum filtration.Foreign matter content is few in the zinc sulfate scavenging solution that obtains by solid-liquid separation, can be used for after the cooling preparing metallic zinc (step 400) by the galvanic deposit zinc process.In addition, can also from the purification and impurity removal matter precipitated solid that is obtained, reclaim valuable metal (step 500).According to embodiments of the invention, the method that reclaims valuable metal from the solid of contamination precipitation is not particularly limited, and can use any means as known in the art to carry out.
Present invention is described below by concrete example, and these concrete examples only are illustrative, and the scope that does not limit the present invention in any way.
Example 1
Utilize sulfuric acid that zinc ore is carried out acidleach and handle, obtain the zinc sulfate leach liquor, by detect (Cd adopts the polarogram methods analyst, and Cu, Co, Ni adopt the atom absorption method analysis) impurity component (unit: mg/l) be:
Cu19.42，Cd533.33，Co11.94，Ni6.25。
With pump the zinc sulfate leach liquor is joined pressurization and purify in the still, controlled temperature is 130 ℃, feeds nitrogen and keep to purify still internal pressure 0.6Mpa, and controlling mechanical stirring velocity simultaneously is 300r/min, according to 2.3kg/m
3Slowly add zinc powder (granularity is 88% mistake 0.11mm sieve).React after 30 minutes, resulting post precipitation liquid is pumped in the cooling tower, be cooled to 95 ℃.Afterwards, carry out solid-liquid separation, obtain the solid matter of zinc sulfate scavenging solution and cupric, cadmium, cobalt, nickel by the plate and frame filter.By detection (Cd adopts the polarogram methods analyst, and Cu, Co, Ni adopt the atom absorption method analysis), the impurity component of zinc sulfate scavenging solution (unit: mg/l) be:
Cu0.038，Cd1.32，Co1.45，Ni0.36。
Example 2
Utilize sulfuric acid that zinc ore is carried out acidleach and handle, obtain the zinc sulfate leach liquor, by detect (Cd adopts the polarogram methods analyst, and Cu, Co, Ni adopt the atom absorption method analysis) impurity component (unit: mg/l) be:
Cu6.96，Cd666.67，Co28.0，Ni10.5。
With pump the zinc sulfate leach liquor being joined pressurization purifies in the still, controlled temperature is 105 ℃, feed nitrogen and also keep purification still internal pressure 0.4Mpa, controlling mechanical stirring velocity simultaneously is 300r/min, slowly adds zinc powder (granularity is 90% mistake 0.11mm sieve) according to 3.1kg/m3.React after 45 minutes, resulting post precipitation liquid pump is gone in the cooling tower, be cooled to 90 ℃ (PLSCONFMs).Afterwards, carry out solid-liquid separation, obtain the solid matter of zinc sulfate scavenging solution and cupric, cadmium, cobalt, nickel by the plate and frame filter.
By detection (Cd adopts the polarogram methods analyst, and Cu, Co, Ni adopt the atom absorption method analysis), the impurity component of zinc sulfate scavenging solution (unit: mg/l) be:
Cu0.088，Cd0.95，Co0.87，Ni0.24。
Example 3
Utilize sulfuric acid that zinc ore is carried out acidleach and handle, obtain the zinc sulfate leach liquor, by detect (Cd adopts the polarogram methods analyst, and Cu, Co, Ni adopt the atom absorption method analysis) impurity component (unit: mg/l) be:
Cu25.0，Cd589.6，Co9.60，Ni10.43。
With pump the zinc sulfate leach liquor is joined pressurization and purify in the still, controlled temperature is 85 ℃, feeds nitrogen and keep to purify still internal pressure 0.2Mpa, and controlling mechanical stirring velocity simultaneously is 300r/min, according to 2.8kg/m
3Slowly add zinc powder (92% crosses the 0.11mm sieve).React after 60 minutes, resulting post precipitation liquid pump is gone in the cooling tower, be cooled to 85 ℃.Afterwards, carry out solid-liquid separation, obtain the solid matter of zinc sulfate scavenging solution and cupric, cadmium, cobalt, nickel by plate-and-frame filter press.
By detecting (Cd adopts the polarogram methods analyst, and Cu, Co, Ni adopt the atom absorption method analysis)), the impurity component of zinc sulfate scavenging solution (unit: mg/l) be:
Cu0.062，Cd1.17，Co1.00，Ni0.24。
Example 4
Utilize sulfuric acid that zinc ore is carried out acidleach and handle, obtain the zinc sulfate leach liquor, by detect (Cd adopts the polarogram methods analyst, and Cu, Co, Ni adopt the atom absorption method analysis) impurity component (unit: mg/l) be:
Cu?111.25，Cd?617.65，Co?20.27，Ni9.58。
With pumping into the zinc sulfate leach liquor is joined in the pressurization purification still, controlled temperature is 120 ℃, feed nitrogen and keep purification still internal pressure 0.4Mpa, controlling mechanical stirring velocity simultaneously is 300r/min, slowly adds zinc powder (95% crosses the 0.11mm sieve) according to 3.3kg/m.React after 40 minutes, resulting post precipitation liquid pump is gone in the cooling tower, be cooled to 90 ℃.Afterwards, carry out solid-liquid separation, obtain the solid matter of zinc sulfate scavenging solution and cupric, cadmium, cobalt, nickel by plate-and-frame filter press.By detection (Cd adopts the polarogram methods analyst, and Cu, Co, Ni adopt the atom absorption method analysis), the impurity component of zinc sulfate scavenging solution (unit: mg/l) be:
Cu0.029，Cd1.29，Co1.49，Ni0.27。
Example 5
Utilize sulfuric acid that zinc ore is carried out acidleach and handle, obtain the zinc sulfate leach liquor, by detect (Cd adopts the polarogram methods analyst, and Cu, Co, Ni adopt the atom absorption method analysis) impurity component (unit: mg/l) be:
Cu21.0，Cd560.3，Co8.45，Ni9.23。
With pump the zinc sulfate leach liquor is joined pressurization and purify in the still, controlled temperature is 85 ℃, feeds nitrogen and keep to purify still internal pressure 0.4Mpa, and controlling mechanical stirring velocity simultaneously is 300r/min, according to 2.65kg/m
3Slowly add zinc powder (93% crosses the 0.11mm sieve).React after 60 minutes, resulting post precipitation liquid pump is gone in the cooling tower, be cooled to 85 ℃.Afterwards, carry out solid-liquid separation, obtain the solid matter of zinc sulfate scavenging solution and cupric, cadmium, cobalt, nickel by plate-and-frame filter press.By detecting (Cd adopts the polarogram methods analyst, and Cu, Co, Ni adopt the atom absorption method analysis)), the impurity component of zinc sulfate scavenging solution (unit: mg/L) be:
Cu0.062，Cd0.88，Co1.00，Ni0.27。
Pass through the foregoing description, according to the purifying method of the zinc sulfate leach liquor of the embodiment of the invention, can realize purification at short notice as can be seen, purify the rear impurity metal content and can reach of the requirement of electrodepositing zinc technology new liquid foreign matter content to the zinc sulfate leach liquor, usually, impurity Cu in China zinc hydrometallurgy factory electrolytic solution, Cd, Co, it is respectively 0.2-0.5mg/L that Ni allows content, 1.5-2.0mg/L, 1-2mg/L, 0.5-1.5mg/L.
In the description of this specification sheets, concrete feature, structure, material or characteristics that the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means in conjunction with this embodiment or example description are contained at least one embodiment of the present invention or the example.In this manual, the schematic statement to above-mentioned term not necessarily refers to identical embodiment or example.And concrete feature, structure, material or the characteristics of description can be with the suitable manner combination in any one or more embodiment or example.
Although illustrated and described embodiments of the invention, those having ordinary skill in the art will appreciate that: can carry out multiple variation, modification, replacement and modification to these embodiment under the situation that does not break away from principle of the present invention and aim, scope of the present invention is limited by claim and equivalent thereof.
Claims (10)
1. the purifying method of a zinc sulfate leach liquor, it comprises:
A) described zinc sulfate leach liquor is joined in the purifying vessel;
B) make in the described purifying vessel and be under the nonoxidizing atmosphere, in described zinc sulfate leach liquor, add zinc powder while stirring, obtain post precipitation liquid with the precipitated impurities metal; And
C) described post precipitation liquid is carried out solid-liquid separation, obtain zinc sulfate scavenging solution and impure precipitated solid.
2. method according to claim 1, wherein said solution of zinc sulfate are the sulphuric leachates of zinc ore.
3. method according to claim 1, wherein said foreign metal are be selected from copper, cobalt, cadmium and nickel at least a.
4. method according to claim 3, it further comprises:
D) reclaim described foreign metal from described impure precipitated solid.
5. method according to claim 1 is wherein at step B) described in nonoxidizing atmosphere be nitrogen atmosphere, and pressure is 0.2-0.6MPa.
6. method according to claim 1, wherein based on the content of foreign metal in the zinc sulfate leach liquor, the addition of described zinc powder is 60-110 a times of described foreign metal content.
7. method according to claim 1, granularity accounts for 88%-95% less than the particle of 0.11mm in the wherein said zinc powder.
8. method according to claim 1 is at step B) in to make the temperature in the described purifying vessel be 85-130 degree centigrade.
9. method according to claim 1 is wherein at step B) in stirring velocity be 250-350rpm.
10. method according to claim 1, it further comprises by electro-deposition method and prepares metallic zinc.
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| CN102676816A (en) * | 2012-06-08 | 2012-09-19 | 大兴安岭云冶矿业开发有限公司 | Method for treating zinc sulfate leach liquor |
| CN102676845A (en) * | 2012-05-07 | 2012-09-19 | 成都易态科技有限公司 | Filter residue obtained after purifying zinc liquid and preparation method of filter residue |
| CN102676820A (en) * | 2012-06-08 | 2012-09-19 | 大兴安岭云冶矿业开发有限公司 | Treatment method of zinc sulfate leach solution |
| CN102899491A (en) * | 2012-10-12 | 2013-01-30 | 中南大学 | Method for floating and separating high-concentration iron ions from zinc sulfate leachate |
| CN102965507A (en) * | 2012-10-31 | 2013-03-13 | 铜陵市祥英锌业有限公司 | One-step two-stage method for removing cadmium ion in high-cadmium zinc sulfate solution |
| CN103468953A (en) * | 2013-09-26 | 2013-12-25 | 云南永昌铅锌股份有限公司 | Method for treating zinc sulfate solution |
| CN105543503A (en) * | 2015-12-28 | 2016-05-04 | 中南大学 | Method for separating and recycling cobalt in zinc sulfate electrolyte |
| CN106756025A (en) * | 2016-11-29 | 2017-05-31 | 湖南水口山有色金属集团有限公司 | A kind of method of impurity in utilization purification slag of zinc hydrometallurgy removing oxidation zinc lixiviating solution |
| CN106809870A (en) * | 2015-11-30 | 2017-06-09 | 湖南恒生制药股份有限公司 | A kind of cobalt method for cleaning impurity of medicinal zinc sulfate |
| CN110699556A (en) * | 2019-08-23 | 2020-01-17 | 白银有色集团股份有限公司 | Method for deep purification and cadmium and cobalt removal of supernatant in zinc hydrometallurgy |
| CN114107695A (en) * | 2021-10-26 | 2022-03-01 | 江西理工大学 | Method and device for synchronously and deeply removing heavy metal impurities in zinc hydrometallurgy solution |
| CN114107696A (en) * | 2021-10-26 | 2022-03-01 | 江西理工大学 | Method for directly removing copper, cadmium, cobalt and nickel from zinc hydrometallurgy solution in one step |
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| CN102676845B (en) * | 2012-05-07 | 2014-04-23 | 成都易态科技有限公司 | Filter residue obtained after purifying zinc liquid and preparation method of filter residue |
| CN102676845A (en) * | 2012-05-07 | 2012-09-19 | 成都易态科技有限公司 | Filter residue obtained after purifying zinc liquid and preparation method of filter residue |
| CN102676820A (en) * | 2012-06-08 | 2012-09-19 | 大兴安岭云冶矿业开发有限公司 | Treatment method of zinc sulfate leach solution |
| CN102676816A (en) * | 2012-06-08 | 2012-09-19 | 大兴安岭云冶矿业开发有限公司 | Method for treating zinc sulfate leach liquor |
| CN102899491A (en) * | 2012-10-12 | 2013-01-30 | 中南大学 | Method for floating and separating high-concentration iron ions from zinc sulfate leachate |
| CN102899491B (en) * | 2012-10-12 | 2013-12-04 | 中南大学 | Method for floating and separating high-concentration iron ions from zinc sulfate leachate |
| CN102965507A (en) * | 2012-10-31 | 2013-03-13 | 铜陵市祥英锌业有限公司 | One-step two-stage method for removing cadmium ion in high-cadmium zinc sulfate solution |
| CN103468953B (en) * | 2013-09-26 | 2016-04-06 | 云南永昌铅锌股份有限公司 | The method of process solution of zinc sulfate |
| CN103468953A (en) * | 2013-09-26 | 2013-12-25 | 云南永昌铅锌股份有限公司 | Method for treating zinc sulfate solution |
| CN106809870A (en) * | 2015-11-30 | 2017-06-09 | 湖南恒生制药股份有限公司 | A kind of cobalt method for cleaning impurity of medicinal zinc sulfate |
| CN105543503A (en) * | 2015-12-28 | 2016-05-04 | 中南大学 | Method for separating and recycling cobalt in zinc sulfate electrolyte |
| CN105543503B (en) * | 2015-12-28 | 2017-08-04 | 中南大学 | The method of separating and recovering cobalt in zinc sulphate electrolyte |
| CN106756025A (en) * | 2016-11-29 | 2017-05-31 | 湖南水口山有色金属集团有限公司 | A kind of method of impurity in utilization purification slag of zinc hydrometallurgy removing oxidation zinc lixiviating solution |
| CN110699556A (en) * | 2019-08-23 | 2020-01-17 | 白银有色集团股份有限公司 | Method for deep purification and cadmium and cobalt removal of supernatant in zinc hydrometallurgy |
| CN114107695A (en) * | 2021-10-26 | 2022-03-01 | 江西理工大学 | Method and device for synchronously and deeply removing heavy metal impurities in zinc hydrometallurgy solution |
| CN114107696A (en) * | 2021-10-26 | 2022-03-01 | 江西理工大学 | Method for directly removing copper, cadmium, cobalt and nickel from zinc hydrometallurgy solution in one step |
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Application publication date: 20110525 |