CN104451147A - Purification and copper removal method for hydrochloric acid-bismuth chloride solution - Google Patents
Purification and copper removal method for hydrochloric acid-bismuth chloride solution Download PDFInfo
- Publication number
- CN104451147A CN104451147A CN201410585639.0A CN201410585639A CN104451147A CN 104451147 A CN104451147 A CN 104451147A CN 201410585639 A CN201410585639 A CN 201410585639A CN 104451147 A CN104451147 A CN 104451147A
- Authority
- CN
- China
- Prior art keywords
- hydrochloric acid
- bismuth
- chloride solution
- copper
- bismuth chloride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000010949 copper Substances 0.000 title claims abstract description 71
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 68
- ZENDEJDCDBAKDT-UHFFFAOYSA-K trichlorobismuthane hydrochloride Chemical compound Cl.[Bi](Cl)(Cl)Cl ZENDEJDCDBAKDT-UHFFFAOYSA-K 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000000746 purification Methods 0.000 title claims abstract description 32
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 52
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 52
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 48
- 235000012054 meals Nutrition 0.000 claims description 22
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 14
- QAAXRTPGRLVPFH-UHFFFAOYSA-N [Bi].[Cu] Chemical compound [Bi].[Cu] QAAXRTPGRLVPFH-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 239000011701 zinc Substances 0.000 claims description 7
- 229910052725 zinc Inorganic materials 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 abstract description 2
- 239000005864 Sulphur Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 65
- 238000005303 weighing Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 150000003568 thioethers Chemical class 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005363 electrowinning Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a purification and copper removal method for hydrochloric acid-bismuth chloride solution. The method comprises the following steps: adding active bismuth powder and elemental sulphur powder in copper-containing hydrochloric acid-bismuth chloride solution simultaneously, controlling a reaction temperature to be 30-50 DEG C, and reacting for 30-90 minutes while stirring to carry out a copper removal treatment. According to the method disclosed by the invention, with the adoption of the two-step treatment, the content of copper in the purified solution is reduced to be below 3mg/L, and the mass ratio of copper to bismuth in the precipitate is greater than 0.7, thus the purpose of deep purification and copper removal for the solution is achieved.
Description
Technical field
The present invention relates to technical field of wet metallurgy, particularly relate to the method for a kind of hydrochloric acid-bismuth chloride solution purification copper removal.
Background technology
In prior art, wet processing adopts Leaching in Hydrochloric Acid-electrodeposition method to extract in the process of bismuth, copper in bismuth mineral can enter into bismuth chloride solution along with Leaching in Hydrochloric Acid process, if do not carry out purifying treatment, because the close meeting of electropotential of copper and bismuth causes copper in electrolytic deposition process to be easy to separate out at negative electrode, thus reduce the current efficiency of negative electrode and the quality of cathode product, therefore must purify copper removal to hydrochloric acid leachate.Thick bismuth electrowinning bismuth adopts hydrochloric acid-bismuth chloride system usually, and the thick bismuth of anode copper in electrolytic process still can enter electrolytic solution in the form of an ion, therefore also must carry out purification except Copper treatment to bismuth electrolytic solution.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide the method for a kind of hydrochloric acid-bismuth chloride solution purification copper removal, be intended to solve hydrochloric acid-high problem needing copper removal of bismuth chloride solution copper content in prior art.
Technical scheme of the present invention is as follows:
A method for hydrochloric acid-bismuth chloride solution purification copper removal, wherein, comprises the following steps:
Active bismuth meal and elemental sulfur powder are joined in the hydrochloric acid-bismuth chloride solution of cupric, temperature of reaction controls at 30 ~ 50 DEG C, stirring reaction 30 ~ 90min simultaneously, carries out except Copper treatment.
The method of described hydrochloric acid-bismuth chloride solution purification copper removal, wherein, in hydrochloric acid-bismuth chloride solution, the concentration of free hydrochloric acid controls at 40 ~ 120g/L.
The method of described hydrochloric acid-bismuth chloride solution purification copper removal, wherein, being 0.7 ~ 1.2 add active bismuth meal by the mol ratio of copper in bismuth with elementary and hydrochloric acid-bismuth chloride solution, is 0.5 ~ 2.5 add elemental sulfur powder by the mol ratio of copper in elemental sulfur and hydrochloric acid-bismuth chloride solution.
The method of described hydrochloric acid-bismuth chloride solution purification copper removal, wherein, the preparation method of described active bismuth meal is: control at 40 ~ 120g/L by concentration of hydrochloric acid free in hydrochloric acid-bismuth chloride solution, be 0.6 ~ 2.2 add zinc powder by the mol ratio of bismuth in simple substance zinc and hydrochloric acid-bismuth chloride solution, temperature of reaction controls at 30 ~ 60 DEG C, be stirred in solution till not having gas to produce, after filtration, cleaning, obtain active bismuth meal.
The method of described hydrochloric acid-bismuth chloride solution purification copper removal, wherein, described elemental sulfur powder is technical grade elemental sulfur powder.
The method of described hydrochloric acid-bismuth chloride solution purification copper removal, wherein, the copper content after purification in hydrochloric acid-bismuth chloride solution is down to below 3mg/L, the copper bismuth mass ratio >0.70 in the throw out obtained.
Beneficial effect: by method of the present invention, the copper content after purification in solution is down to below 3mg/L, the copper bismuth mass ratio >0.70 in throw out.Compared with prior art, the present invention has the following advantages:
That the hydrochloric acid 1, related in the present invention-bismuth chloride solution copper-stripping reaction generates is Cu
2s precipitates, instead of the CuS precipitation that sulfuration method generates.Due to Cu
2the solubility product of S is less than CuS, is more conducive to the carrying out of copper-stripping reaction, the copper content in hydrochloric acid-bismuth chloride solution can be made to be down to below 3mg/L, reach the object of deep purifying copper removal.
2, in the hydrochloric acid related in the present invention-bismuth chloride solution copper removal process, owing to adopting technical grade elemental sulfur powder instead of sulphide salt, in copper removal process, H is not had
2s gas produces, and also can not introduce other foreign ion, environmentally friendly.
3, copper bismuth mass ratio >0.70 in involved in the present invention reaction precipitation product, is easy to after fusing reclaim.
4, involved in the present invention hydrochloric acid-bismuth chloride solution macerates copper-removing method, simple to operate, technical qualification loose, and the reaction times is short.
Embodiment
The invention provides the method for a kind of hydrochloric acid-bismuth chloride solution purification copper removal, for making object of the present invention, technical scheme and effect clearly, clearly, the present invention is described in more detail below.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The method of a kind of hydrochloric acid of the present invention-bismuth chloride solution purification copper removal, it comprises the following steps:
Active bismuth meal and elemental sulfur powder are joined in the hydrochloric acid-bismuth chloride solution of cupric, temperature of reaction controls at 30 ~ 50 DEG C, stirring reaction 30 ~ 90min simultaneously, carries out except Copper treatment.
Its reaction principle is as follows:
6CuCl
2(a) + 4Bi(s) + 3S(s) = 3Cu
2S(s)↓ + 4BiCl
3(a)
Above-mentioned reaction carries out under the condition of heated and stirred, and its heating condition is 30 ~ 50 DEG C, and stirring reaction 30 ~ 90min, makes cupric ion be converted to Cu altogether
2s precipitation is with the object reaching copper removal.
Wherein, in hydrochloric acid-bismuth chloride solution, the concentration of free hydrochloric acid controls at 40 ~ 120g/L.
The addition of active bismuth meal and elemental sulfur powder is: be 0.7 ~ 1.2 add active bismuth meal by the mol ratio of copper in bismuth with elementary and hydrochloric acid-bismuth chloride solution, is 0.5 ~ 2.5 add elemental sulfur powder by the mol ratio of copper in elemental sulfur and hydrochloric acid-bismuth chloride solution.
Method of the present invention mainly comprises two steps:
The first step: prepare active bismuth meal;
Second step: hydrochloric acid-bismuth chloride solution purification copper removal.
In the first step wherein, the preparation method of active bismuth meal is specially: control at 40 ~ 120g/L by concentration of hydrochloric acid free in hydrochloric acid-bismuth chloride solution, be 0.6 ~ 2.2 add zinc powder by the mol ratio of bismuth in simple substance zinc and hydrochloric acid-bismuth chloride solution, temperature of reaction controls at 30 ~ 60 DEG C, be stirred in solution till not having gas to produce, after filtration, cleaning, obtain active bismuth meal.
Described elemental sulfur powder is technical grade elemental sulfur powder, and the present invention does not adopt sulphide salt, in copper removal process, do not have H
2s gas produces, and also can not introduce other foreign ion, environmentally friendly.
Copper content after purification in solution is down to below 3mg/L, the copper bismuth mass ratio >0.70 in the throw out be obtained by reacting, and easily reclaims after fusing.
The invention will be further described to use embodiment below.
Embodiment 1
Be that free hydrochloric acid concentration in the hydrochloric acid-bismuth chloride solution of 93g/L controls at 80g/L by bismuth-containing, then 40 DEG C are heated to, be 1.0 add zinc powder by the mol ratio of the bismuth in simple substance zinc and hydrochloric acid leachate, do not have gas to overflow in stirring reaction to solution, filter, obtain active bismuth meal after cleaning; Be that free salt concentration in the hydrochloric acid-bismuth chloride solution of 1.5g/L controls at 80g/L by cupric, heating temperatures to 40 DEG C, to be the active bismuth meal of 0.9 weighing by the mol ratio of copper in bismuth with elementary and hydrochloric acid-bismuth chloride solution, and join in hydrochloric acid-bismuth chloride solution that aforementioned cupric is 1.5g/L by the elemental sulfur powder that the mol ratio of copper in elemental sulfur and hydrochloric acid-bismuth chloride solution is 1.2 weighings simultaneously, stirring reaction 60min.After purification, cupric is that the copper in the hydrochloric acid-bismuth chloride solution of 1.5g/L is reduced to 2.5mg/L from concentration, and the copper bismuth mass ratio in throw out is 1.303.
Embodiment 2
Be that free hydrochloric acid concentration in the hydrochloric acid-bismuth chloride solution of 103g/L controls at 120g/L by bismuth-containing, then 50 DEG C are heated to, be 1.1 add zinc powder by the mol ratio of the bismuth in simple substance zinc and hydrochloric acid leachate, do not have gas to overflow in stirring reaction to solution, filter, obtain active bismuth meal after cleaning; Be that free salt concentration in the hydrochloric acid-bismuth chloride solution of 15.5g/L controls at 120g/L by cupric, heating temperatures to 50 DEG C, to be the active bismuth meal of 1.2 weighings by the mol ratio of copper in bismuth with elementary and hydrochloric acid-bismuth chloride solution, and join in hydrochloric acid-bismuth chloride solution that aforementioned cupric is 15.5g/L by the elemental sulfur powder that the mol ratio of copper in elemental sulfur and hydrochloric acid-bismuth chloride solution is 1.6 weighings simultaneously, stirring reaction 50min.After purification, cupric is that the copper in the hydrochloric acid-bismuth chloride solution of 15.5g/L is reduced to 1.6mg/L from concentration.Copper bismuth mass ratio in throw out is 0.71.
Embodiment 3
Be that free hydrochloric acid concentration in the hydrochloric acid-bismuth chloride solution of 65g/L controls at 40g/L by bismuth-containing, then 30 DEG C are heated to, be 2.2 add zinc powder by the mol ratio of the bismuth in simple substance zinc and hydrochloric acid leachate, do not have gas to overflow in stirring reaction to solution, filter, obtain active bismuth meal after cleaning; Be that free salt concentration in the hydrochloric acid-bismuth chloride solution of 12.2g/L controls at 80g/L by cupric, heating temperatures to 30 DEG C, to be the active bismuth meal of 0.7 weighing by the mol ratio of copper in bismuth with elementary and hydrochloric acid-bismuth chloride solution, and join in hydrochloric acid-bismuth chloride solution that aforementioned cupric is 12.2g/L by the elemental sulfur powder that the mol ratio of copper in elemental sulfur and hydrochloric acid-bismuth chloride solution is 2.5 weighings simultaneously, stirring reaction 90min.After purification, cupric is that the copper in the hydrochloric acid-bismuth chloride solution of 12.2g/L is reduced to 1.2mg/L from concentration.Copper bismuth mass ratio in throw out is 0.81.
Embodiment 4
Be that free hydrochloric acid concentration in the hydrochloric acid-bismuth chloride solution of 80g/L controls at 80g/L by bismuth-containing, then 60 DEG C are heated to, be 0.6 add zinc powder by the mol ratio of the bismuth in simple substance zinc and hydrochloric acid leachate, do not have gas to overflow in stirring reaction to solution, filter, obtain active bismuth meal after cleaning; Be that free salt concentration in the hydrochloric acid-bismuth chloride solution of 5.5g/L controls at 72g/L by cupric, heating temperatures to 45 DEG C, to be the active bismuth meal of 0.8 weighing by the mol ratio of copper in bismuth with elementary and hydrochloric acid-bismuth chloride solution, and join in hydrochloric acid-bismuth chloride solution that aforementioned cupric is 5.5g/L by the elemental sulfur powder that the mol ratio of copper in elemental sulfur and hydrochloric acid-bismuth chloride solution is 0.5 weighing simultaneously, stirring reaction 72min.After purification, cupric is that the copper in the hydrochloric acid-bismuth chloride solution of 5.5g/L is reduced to 1.2mg/L from concentration.Copper bismuth mass ratio in throw out is 0.75.
In sum, the present invention is by adopting two-step pretreatment, and the copper content after purification in solution is down to below 3mg/L, the copper bismuth mass ratio >0.70 in throw out, reaches the object of solution deep purification copper removal.
Should be understood that, application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (6)
1. a method for hydrochloric acid-bismuth chloride solution purification copper removal, is characterized in that, comprise the following steps:
Active bismuth meal and elemental sulfur powder are joined in the hydrochloric acid-bismuth chloride solution of cupric, temperature of reaction controls at 30 ~ 50 DEG C, stirring reaction 30 ~ 90min simultaneously, carries out except Copper treatment.
2. the method for hydrochloric acid according to claim 1-bismuth chloride solution purification copper removal, is characterized in that, in hydrochloric acid-bismuth chloride solution, the concentration of free hydrochloric acid controls at 40 ~ 120g/L.
3. the method for hydrochloric acid according to claim 1-bismuth chloride solution purification copper removal, it is characterized in that, being 0.7 ~ 1.2 add active bismuth meal by the mol ratio of copper in bismuth with elementary and hydrochloric acid-bismuth chloride solution, is 0.5 ~ 2.5 add elemental sulfur powder by the mol ratio of copper in elemental sulfur and hydrochloric acid-bismuth chloride solution.
4. the method for hydrochloric acid according to claim 1-bismuth chloride solution purification copper removal, it is characterized in that, the preparation method of described active bismuth meal is: control at 40 ~ 120g/L by concentration of hydrochloric acid free in hydrochloric acid-bismuth chloride solution, be 0.6 ~ 2.2 add zinc powder by the mol ratio of bismuth in simple substance zinc and hydrochloric acid-bismuth chloride solution, temperature of reaction controls at 30 ~ 60 DEG C, be stirred in solution till not having gas to produce, after filtration, cleaning, obtain active bismuth meal.
5. the method for hydrochloric acid according to claim 1-bismuth chloride solution purification copper removal, is characterized in that, described elemental sulfur powder is technical grade elemental sulfur powder.
6. the method for hydrochloric acid according to claim 1-bismuth chloride solution purification copper removal, is characterized in that, the copper content after purification in hydrochloric acid-bismuth chloride solution is down to below 3mg/L, the copper bismuth mass ratio >0.70 in the throw out obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410585639.0A CN104451147B (en) | 2014-10-28 | 2014-10-28 | A kind of method of chlorination of hydrochloric acid bismuth solution purification copper removal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410585639.0A CN104451147B (en) | 2014-10-28 | 2014-10-28 | A kind of method of chlorination of hydrochloric acid bismuth solution purification copper removal |
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| Publication Number | Publication Date |
|---|---|
| CN104451147A true CN104451147A (en) | 2015-03-25 |
| CN104451147B CN104451147B (en) | 2017-03-01 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2233893C1 (en) * | 2003-02-17 | 2004-08-10 | Открытое Акционерное Общество "Челябинский цинковый завод" | Method of cleaning sulfate zinc solutions from admixtures |
| EP2584055A1 (en) * | 2010-06-21 | 2013-04-24 | Sumitomo Metal Mining Co., Ltd. | Method for removal of copper ions from copper-containing nickel chloride solution, and process for production of electrolytic nickel |
-
2014
- 2014-10-28 CN CN201410585639.0A patent/CN104451147B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2233893C1 (en) * | 2003-02-17 | 2004-08-10 | Открытое Акционерное Общество "Челябинский цинковый завод" | Method of cleaning sulfate zinc solutions from admixtures |
| EP2584055A1 (en) * | 2010-06-21 | 2013-04-24 | Sumitomo Metal Mining Co., Ltd. | Method for removal of copper ions from copper-containing nickel chloride solution, and process for production of electrolytic nickel |
Non-Patent Citations (3)
| Title |
|---|
| 崔秀华等: "Mg/BiCl3存在下醛、酮的一锅法炔丙基化反应", 《复旦学报》, vol. 39, no. 4, 30 August 2000 (2000-08-30) * |
| 王继峰等: "用隔膜电积法从辉铋矿精矿中回收铋", 《湿法冶金》, vol. 31, 29 February 2012 (2012-02-29) * |
| 陈汉森: "高铋铅阳极泥电解法回收铋的工艺研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》, no. 7, 15 July 2014 (2014-07-15) * |
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