CN102994766A - Method for comprehensively recovering valuable metal from copper tellurium slag - Google Patents
Method for comprehensively recovering valuable metal from copper tellurium slag Download PDFInfo
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- CN102994766A CN102994766A CN2012105371422A CN201210537142A CN102994766A CN 102994766 A CN102994766 A CN 102994766A CN 2012105371422 A CN2012105371422 A CN 2012105371422A CN 201210537142 A CN201210537142 A CN 201210537142A CN 102994766 A CN102994766 A CN 102994766A
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- tellurium
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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for comprehensively recovering valuable metal from copper tellurium slag. The copper tellurium slag is dissolved by using nitric acid, so that silver, copper and bismuth in the copper tellurium slag are basically dissolved in a solution; tellurium is oxidized into tellurium oxide, thereby entering undissolved slag. Silver, copper and bismuth are separated and recovered via fractional precipitation of the solution; and tellurium is separated and recovered via alkaline leaching of the undissolved slag. The method solves the problems that cost of a conventional process is high, copper recovery rate and tellurium recovery rate are not high, and that silver and bismuth cannot be recovered in the conventional process; influences on the environment of the production process are reduced; a whole process is simple; and pollutions toward the environment is small. The method is simple in the whole production process, low in cost and small pollutions toward the environment, has high comprehensive recovery rate, and realizes complete separation of silver, copper, bismuth and tellurium. The obtained products have high purity; and the recovery rate of silver, copper, bismuth and tellurium is higher than 99%.
Description
Technical field:
The present invention relates to a kind of copper tellurium slag recovery method, be specifically related to a kind of from copper tellurium slag the method for comprehensively recovering valuable metal.
Background technology:
Soak the copper process at the wet processing anode sludge at present, the tellurium in the anode sludge has 25-50% to enter copper leached solution, and this part tellurium mainly reclaims with copper powder displacement output copper tellurium slag.Copper tellurium slag major ingredient is tellurium copper, contains in addition the metals such as copper, bismuth, silver.The comprehensive recovery of traditional copper tellurium slag mainly contains following two kinds of methods:
Method one: copper tellurium slag adopts sulfuric acid adding oxygenant to soak copper, and then alkali soaks a minute tellurium.Its shortcoming is: copper, tellurium leaching yield are low; Need a large amount of expensive oxygenants; Silver, bismuth in the raw material can not get Separation and Recovery; Production Flow Chart is complicated.
Method two: copper tellurium slag is first through the sulfuric acid acidation roasting, and then alkali soaks a minute tellurium.Its shortcoming is: raw material will be admixed a large amount of vitriol oils and carry out roasting, and the agglomerate after the roasting needs ball milling, thereby causes the production unit seriously corroded, and production environment is poor; Production Flow Chart is complicated, and environmental protection pressure is large; Silver, bismuth in the raw material can not get Separation and Recovery.
Summary of the invention:
The rate of recovery that the purpose of this invention is to provide a kind of silver, copper, bismuth, tellurium is high, the method for technique is simple, environmental pollution is little from copper tellurium slag comprehensively recovering valuable metal.
Of the present invention from copper tellurium slag the method for comprehensively recovering valuable metal, it is characterized in that, may further comprise the steps:
(1) nitric acid dissolve: in copper tellurium slag: quality is than being the ratio of 1:1.0-1.5, first add entry to stirred autoclave, then drop into copper tellurium slag to reactor while stirring, and start the acid gas absorption tower, after adding again in copper tellurium slag: mass percent is that 75% concentrated nitric acid mass ratio is the ratio of 1:2-2.5, adding mass percent in the reactor is 75% concentrated nitric acid, temperature of reaction is controlled to be 85-90 ℃ in the acid adding process, 85-90 ℃ of the complete rear insulation of acid adding 2-3 hour, the acid gas that reaction process produces absorbs into diluted acid water by the water in the acid gas absorption tower and returns recycling; Treat that the dissolving of copper tellurium slag is complete, blast air reaction solution is cooled to below 40 ℃ that solid-liquid separation obtains insoluble slag and solution, with the nitric acid acidified water washing insoluble slag of PH=1, it is colourless to be washed till washing water, the insoluble slag after obtaining washings and washing;
(2) the heavy silver of chlorination: solution and the washings of step (1) acquisition are merged, the heavy silver of dropping chloride solution chlorination, liquid after filtration obtains silver chloride and divides silver after the washing of silver chloride process, adds hydrazine hydrate reduction, gets final product output fine silver powder; Divide the rear liquid of silver to transfer the heavy bismuth in PH to 2.5 ~ 3 with soda ash, liquid after filtration obtains Bismuth Subcarbonate and divides bismuth, Bismuth Subcarbonate is through the thick bismuth of retailoring output; Liquid transfers the heavy copper in PH to 6.0 ~ 6.5 to obtain copper hydroxide with calcium hydroxide after dividing bismuth;
(3) alkali soaks: it is molten that the insoluble slag after the washing that step (1) is obtained carries out alkali, alkali number is by tellurium: the sodium hydroxide molar ratio is that 1:0.7-0.8 adds, the control free alkali is 60-80g/l, temperature 80-90 ° of C, stirring reaction 2-3 hour, filtration obtains leached mud and tellurium alkali lye, and leached mud returns the smelting system in early stage, and tellurium alkali lye is through adding the sodium sulphite removal of impurities, adding in the sulfuric acid and the pure tellurium dioxide of output.
Described solid-liquid separation preferably adopts press filtration to carry out solid-liquid separation.
Described villaumite is preferably sodium-chlor.
The present invention adopts nitric acid dissolve copper tellurium slag, make silver, copper, this dissolving of bismuthino in the copper tellurium slag enter solution, tellurium is oxidized to tellurium dioxide and enters insoluble slag, and solution is by fractional precipitation Separation and Recovery silver, bismuth, copper, and insoluble slag soaks the Separation and Recovery tellurium by alkali, efficiently solve cost height in the traditional technology, but copper, the problem that the tellurium rate of recovery is not high, silver-colored, bismuth can not get Separation and Recovery have reduced the impact of production process on environment, whole flow process is simple, and environmental pollution is little.
Compared with prior art, the invention has following positively effect:
(1) Production Flow Chart is simple, and one time nitric acid dissolve can be realized the dissolving of silver, copper, bismuth and the oxidation of tellurium;
(2) low, the comprehensive organic efficiency of cost is high, has realized the fully separation of silver, copper, bismuth, tellurium, the product purity height of acquisition, and the rate of recovery of silver, copper, bismuth, tellurium is all more than 99%;
(3) environmental pollution is little.
Embodiment:
Following examples are to further specify of the present invention, rather than limitation of the present invention.
Embodiment 1:
Get 2 tons of copper tellurium slags, by massfraction, its component is: copper: 35.6%, and tellurium 13.92%, bismuth 6.34%, silver 3.16%.
(1) adds pure water 2000L to stirred autoclave, drop into above-mentioned 2 tons of copper tellurium slags to reactor while stirring, and unlatching acid gas absorption tower, be that 75% concentrated nitric acid mass ratio is that to get mass percent be 75% concentrated nitric acid for the ratio of 1 ﹕ 2 in copper Di Zha ﹕ mass percent, add mass percent in the reactor as 75% concentrated nitric acid take the flow velocity that is about 5L/ minute, 85-90 ° of C of acid adding process control temperature of reaction, 85-90 ° of the complete insulation of acid adding C2 hour.The acid gas that reaction process produces absorbs into diluted acid water by the water in the acid gas absorption tower, can return for dissolved copper tellurium slag after concentrated.Treat that the dissolving of copper tellurium slag is complete, blast air reaction solution is cooled to below 40 ℃, adopt press filtration to carry out solid-liquid separation, obtain insoluble slag and solution, with the nitric acid acidified water washing insoluble slag of PH ≈ 1, it is colourless to be washed till washing water, insoluble slag and washings after obtaining washing.
Insoluble slag cupric 0.25% after the washing, silver 0.06%, bismuth 0.11%, tellurium 37.66%.
(2) solution that step (1) is obtained and washings merging, it is heavy silver-colored to drip the chlorination of 250g/l sodium chloride solution, filters to obtain silver chloride and the rear liquid of minute silver, and silver chloride adds hydrazine hydrate reduction through after washing, can output fine silver powder.Divide the rear liquid of silver to transfer the heavy bismuth in PH to 2.5 ~ 3 with soda ash, liquid after filtration obtains Bismuth Subcarbonate and divides bismuth, Bismuth Subcarbonate is through the thick bismuth of retailoring output.Liquid transfers the heavy copper of PH to 6.0-6.5 to obtain copper hydroxide with calcium hydroxide after dividing bismuth.
(3) it is molten that the insoluble slag after the washing that step (1) is obtained carries out alkali, alkali number is by tellurium: the sodium hydroxide molar ratio is that 1:0.7 adds, the control free alkali is between the 60-80g/l, between the temperature 80-90 ° of C, stirring reaction 2 hours, filtration obtains leached mud and tellurium alkali lye, and leached mud returns the smelting system in early stage, and tellurium alkali lye is through adding the sodium sulphite removal of impurities, adding in the sulfuric acid and the pure tellurium dioxide of output.
Through after the processing of present embodiment, the silver in the copper tellurium slag, copper, bismuth, the tellurium rate of recovery are respectively 99.05%, 99.32%, 99.12%, 99.12%.
Embodiment 2:
Get 1.8 tons of copper tellurium slags, by massfraction, its component is: copper: 30.3%, and tellurium 15.62%, bismuth 5.52%, silver 2.28%.
(1) in reactor, adds pure water 2700L, drop into above-mentioned 1.8 tons of copper tellurium slags to reactor while stirring, and unlatching acid gas absorption tower, be that 75% concentrated nitric acid mass ratio is that to measure mass percent be 75% concentrated nitric acid for the ratio of 1 ﹕ 2.5 in copper tellurium slag ﹕ mass percent, add nitric acid with about 5L/ minute flow velocity toward reactor, temperature of reaction is controlled to be 85-90 ℃ in the acid adding process, 85-90 ° of the complete rear insulation of acid adding C3 hour, the acid gas that reaction process produces absorbs into diluted acid water by the water in the acid gas absorption tower, can return for dissolved copper tellurium slag after concentrated.It is complete to treat that copper tellurium slag dissolves, and blasts air reaction solution is cooled to below 40 ℃, adopts press filtration to carry out solid-liquid separation, obtains insoluble slag and solution, and with the nitric acid acidified water washing insoluble slag of PH ≈ 1, it is colourless to be washed till washing water, the insoluble slag after obtaining washings and washing.
Insoluble slag cupric 0.18% after the washing, silver 0.035%, bismuth 0.10%, tellurium 38.78%.
(2) solution that step (1) is obtained and washings merging, it is heavy silver-colored to drip the chlorination of 100g/l sodium chloride solution, filters to obtain silver chloride and the rear liquid of minute silver, and silver chloride adds hydrazine hydrate reduction through after washing, can output fine silver powder.Divide the rear liquid of silver to transfer the heavy bismuth in PH to 2.5 ~ 3 with soda ash, liquid after filtration obtains Bismuth Subcarbonate and divides bismuth, Bismuth Subcarbonate is through the thick bismuth of retailoring output.Liquid transfers the heavy copper of PH to 6.0-6.5 to obtain copper hydroxide with calcium hydroxide after dividing bismuth.
(3) it is molten that the insoluble slag after the washing that step (1) is obtained carries out alkali, alkali number is by tellurium: the sodium hydroxide molar ratio is that 1:0.8 adds, the control free alkali is between the 60-80g/l, between the temperature 80-90 ° of C, stirring reaction 3 hours, filtration obtains leached mud and tellurium alkali lye, and leached mud returns the smelting system in early stage, and tellurium alkali lye is through adding the sodium sulphite removal of impurities, adding in the sulfuric acid and the pure tellurium dioxide of output.
Through after the processing of present embodiment, the silver in the copper tellurium slag, copper, bismuth, the tellurium rate of recovery are respectively 99.21%, 99.42%, 99.10%, 99.35%.
Claims (3)
1. the method for a comprehensively recovering valuable metal from copper tellurium slag is characterized in that, may further comprise the steps:
(1) nitric acid dissolve: in copper tellurium slag: quality is than being the ratio of 1:1.0-1.5, first add entry to stirred autoclave, then drop into copper tellurium slag to reactor while stirring, and start the acid gas absorption tower, after adding again in copper tellurium slag: mass percent is that 75% concentrated nitric acid mass ratio is the ratio of 1:2-2.5, adding mass percent in the reactor is 75% concentrated nitric acid, temperature of reaction is controlled to be 85-90 ℃ in the acid adding process, 85-90 ° of the complete rear insulation of acid adding C2-3 hour, the acid gas that reaction process produces absorbs into diluted acid water by the water in the acid gas absorption tower and returns recycling; Treat that the dissolving of copper tellurium slag is complete, blast air reaction solution is cooled to below 40 ℃ that solid-liquid separation obtains insoluble slag and solution, with the nitric acid acidified water washing insoluble slag of PH=1, it is colourless to be washed till washing water, the insoluble slag after obtaining washings and washing;
(2) the heavy silver of chlorination: solution and the washings of step (1) acquisition are merged, the heavy silver of dropping chloride solution chlorination, liquid after filtration obtains silver chloride and divides silver after the washing of silver chloride process, adds hydrazine hydrate reduction, gets final product output fine silver powder; Divide the rear liquid of silver to transfer the heavy bismuth in PH to 2.5 ~ 3 with soda ash, liquid after filtration obtains Bismuth Subcarbonate and divides bismuth, Bismuth Subcarbonate is through the thick bismuth of retailoring output; Liquid transfers the heavy copper in PH to 6.0 ~ 6.5 to obtain copper hydroxide with calcium hydroxide after dividing bismuth;
(3) alkali soaks: it is molten that the insoluble slag after the washing that step (1) is obtained carries out alkali, alkali number is by tellurium: the sodium hydroxide molar ratio is that 1:0.7-0.8 adds, the control free alkali is 60-80g/l, temperature 80-90 ° of C, stirring reaction 2-3 hour, filtration obtains leached mud and tellurium alkali lye, and leached mud returns the smelting system in early stage, and tellurium alkali lye is through adding the sodium sulphite removal of impurities, adding in the sulfuric acid and the pure tellurium dioxide of output.
According to claim 1 from copper tellurium slag the method for comprehensively recovering valuable metal, it is characterized in that described solid-liquid separation adopts press filtration to carry out solid-liquid separation.
According to claim 1 from copper tellurium slag the method for comprehensively recovering valuable metal, it is characterized in that described villaumite is sodium-chlor.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103882235A (en) * | 2014-04-15 | 2014-06-25 | 中国地质科学院矿产综合利用研究所 | Method for step recovery of iron, copper and noble metal from copper smelting waste slag |
| CN104445105A (en) * | 2014-11-24 | 2015-03-25 | 西北矿冶研究院 | Method for enriching and recovering tellurium dioxide from tellurium-containing soda residue |
| CN104928483A (en) * | 2015-05-15 | 2015-09-23 | 西北矿冶研究院 | Method for comprehensively recovering silver, selenium, tellurium and copper from copper telluride residues |
| CN104962749A (en) * | 2015-06-19 | 2015-10-07 | 郴州市金贵银业股份有限公司 | Treatment method of alkaline copper sediment in silver electrolysis mother liquor |
| CN107142377A (en) * | 2017-04-27 | 2017-09-08 | 永兴鑫裕环保镍业有限公司 | The technique of extracting and developing copper and tellurium from copper tellurium slag |
| CN108913912A (en) * | 2018-08-01 | 2018-11-30 | 济源职业技术学院 | A kind of device of the waste recycling copper generated from Copper making |
| CN112063854A (en) * | 2020-09-02 | 2020-12-11 | 河南豫光金铅股份有限公司 | Method for comprehensively recovering bismuth, silver and copper metals by taking precious lead as raw material |
| CN113697778A (en) * | 2021-08-20 | 2021-11-26 | 金隆铜业有限公司 | Treatment method of copper-tellurium slag |
| CN115716639A (en) * | 2022-11-30 | 2023-02-28 | 郴州雄风环保科技有限公司 | Process for leaching tellurium from gold, silver and copper-containing tellurium slag |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103882235B (en) * | 2014-04-15 | 2015-08-19 | 中国地质科学院矿产综合利用研究所 | Method for step recovery of iron, copper and noble metal from copper smelting waste slag |
| CN103882235A (en) * | 2014-04-15 | 2014-06-25 | 中国地质科学院矿产综合利用研究所 | Method for step recovery of iron, copper and noble metal from copper smelting waste slag |
| CN104445105A (en) * | 2014-11-24 | 2015-03-25 | 西北矿冶研究院 | Method for enriching and recovering tellurium dioxide from tellurium-containing soda residue |
| CN104928483A (en) * | 2015-05-15 | 2015-09-23 | 西北矿冶研究院 | Method for comprehensively recovering silver, selenium, tellurium and copper from copper telluride residues |
| CN104962749A (en) * | 2015-06-19 | 2015-10-07 | 郴州市金贵银业股份有限公司 | Treatment method of alkaline copper sediment in silver electrolysis mother liquor |
| CN107142377B (en) * | 2017-04-27 | 2018-12-21 | 永兴鑫裕环保镍业有限公司 | The technique of extracting and developing copper and tellurium from copper tellurium slag |
| CN107142377A (en) * | 2017-04-27 | 2017-09-08 | 永兴鑫裕环保镍业有限公司 | The technique of extracting and developing copper and tellurium from copper tellurium slag |
| CN108913912A (en) * | 2018-08-01 | 2018-11-30 | 济源职业技术学院 | A kind of device of the waste recycling copper generated from Copper making |
| CN108913912B (en) * | 2018-08-01 | 2020-11-13 | 济源职业技术学院 | Device for recovering copper from waste slag generated in copper smelting |
| CN112063854A (en) * | 2020-09-02 | 2020-12-11 | 河南豫光金铅股份有限公司 | Method for comprehensively recovering bismuth, silver and copper metals by taking precious lead as raw material |
| CN112063854B (en) * | 2020-09-02 | 2022-08-26 | 河南豫光金铅股份有限公司 | Method for comprehensively recovering bismuth, silver and copper metals by taking precious lead as raw material |
| CN113697778A (en) * | 2021-08-20 | 2021-11-26 | 金隆铜业有限公司 | Treatment method of copper-tellurium slag |
| CN113697778B (en) * | 2021-08-20 | 2023-12-26 | 金隆铜业有限公司 | Copper tellurium slag treatment method |
| CN115716639A (en) * | 2022-11-30 | 2023-02-28 | 郴州雄风环保科技有限公司 | Process for leaching tellurium from gold, silver and copper-containing tellurium slag |
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