CN105112670A - Comprehensive recovery method for platinum and palladium in silver electrolyte - Google Patents
Comprehensive recovery method for platinum and palladium in silver electrolyte Download PDFInfo
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- CN105112670A CN105112670A CN201510564702.7A CN201510564702A CN105112670A CN 105112670 A CN105112670 A CN 105112670A CN 201510564702 A CN201510564702 A CN 201510564702A CN 105112670 A CN105112670 A CN 105112670A
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Abstract
The invention discloses a comprehensive recovery method for platinum and palladium in a silver electrolyte. The comprehensive recovery method comprises the following steps: adding a precipitant into the silver electrolyte containing greater than or equal to 0.1g/L of palladium and 1-10g/L of nitric acid in a reaction kettle to precipitate platinum and palladium, and filtering to obtain platinum and palladium concentrates, and platinum and palladium precipitation solution; washing the platinum and palladium concentrates with dilute nitric acid, then drying and calcining, and removing organic matters to obtain a crude platinum-palladium alloy; dissolving the crude platinum-palladium alloy with aqua regia and filtering; adding alkali in the filtrate to neutralize, completely dissolving a red precipitate and then filtering to obtain a filter residue which is a platinum concentrate, adding hydrochloric acid in the filtrate, and filtering after the reaction is concluded to obtain a filter residue which is a trans-diamminedichloropalladium precipitate; adding ammonia water to dissolve the trans-diamminedichloropalladium precipitate, cooling and then filtering; heating the obtained filtrate to 40-60 DEG C, adding hydrazine hydrate to reduce palladium according to a ratio of hydrazine hydrate to palladium being 0.5-1:1, and filtering to obtain a sponge palladium product. The precipitant used in the comprehensive recovery method disclosed by the invention is high in selectivity, and used for precipitating palladium and platinum in the silver electrolyte only, but not precipitating base metals of silver, copper, lead, bismuth and the like. The platinum and palladium concentrates do not contain the base metals and are easy to separate and purify, and the silver electrolyte is purified while platinum and palladium in the silver electrolyte are efficiently recovered; and due to return use, the production cost is reduced, the benefits are increased, and remarkable technical effects are obtained.
Description
Technical field
The present invention is a kind of method reclaiming precious metal, specifically the comprehensive recovering process of platinum palladium in a kind of silver electrolyte.
Background technology
In silver-colored electrolytic process, the palladium in Ag positive plate has 30 ~ 60%, and platinum has 5 ~ 10% to be entered electrolytic solution by dissolving.The several all after dates of electrolysis, the Pd in electrolytic solution
2+, Pt
2+continuous enrichment raises, and is easily reduced to metal, Precipitation on negative electrode, thus the quality affecting silver products, and cause the loss of precious metal.Therefore need to carry out purifying treatment to electrolytic solution, and reclaim platinum metallic palladium.
At present, from silver electrolyte, the production method of Recovery Purifying platinum palladium mainly contains concentrated calcination method, hydrochloric acid sinks silver-copper/iron substitution method, active carbon adsorption, the butyl xanthate precipitator method etc.Concentrated calcination method and hydrochloric acid sink silver-copper/iron substitution method exist complex operation, silver loss large, produce the shortcomings such as toxic gas, the impure kind of Pt Pd concentrate that obtains is many, content is higher; Active carbon adsorption needs pre-treatment, parsing and regeneration, and platinum palladium adsorption efficiency is low, and a large amount of silver is also adsorbed, and desorbed solution also needs removal of impurities and enrichment just can obtain Pt Pd concentrate; Butyl xanthate precipitator method selectivity is extensive, and a large amount of silver is also by co-precipitation, and the Pt Pd concentrate obtained is impure, is unfavorable for follow-up Refining, and after precipitation, liquid returns silver-colored electrolysis, can have a negative impact, the defective silver powder of output.
In traditional Refining process of palladium, flow process is that strong acid dissolution-ammonium chloride sinks palladium-hot water dissolving-ammonia neutralization removal of impurities-hcl acidifying removal of impurities-ammonia solvent-hydrazine hydrate reduction, obtains palladium sponge product.Due to most of smeltery palladium concentrate containing base metal impurity and organism more, the solution base metal obtained after strong acid dissolution and organic content high, subsequent purification and palladium direct yield are had a negative impact; From strong acid solution, precipitate palladium not thorough, residual palladium 1 ~ 2g/L in filtrate, affects product direct yield.
Summary of the invention
The object of the invention is for above-mentioned prior art Problems existing, the comprehensive recovering process of platinum palladium in a kind of silver electrolyte is proposed, platinum palladium in the method energy high efficiente callback silver electrolyte, obtain the Pt Pd concentrate that foreign matter content is low, after calcining, obtain the higher platinum-nickel alloys of purity, then palladium sponge and platinum concentrate can be obtained after Refining, purify silver electrolyte simultaneously and return use, reduce production cost, increase economic benefit.
Object of the present invention is realized by following means:
A comprehensive recovering process for platinum palladium in silver electrolyte, is characterized in that:
(1) silver electrolyte is from silver-colored electrolysis operating system, is wherein more than or equal to 0.1g/L, containing nitric acid 1 ~ 10g/L containing palladium;
(2) described silver electrolyte is transferred to reactor, be heated to 30 ~ 80 DEG C, then add precipitation agent, by the platinum palladium precipitation in silver electrolyte, cold filtration precipitates, and obtains Pt Pd concentrate and heavy platinum palladium liquid;
(3) dust technology washing 2 ~ 3 post-dryings of Pt Pd concentrate pH=0.5 ~ 1, calcining, will wherein organism be burned except abandoning, and residue is platina palldium alloy;
(4) platina palldium alloy aqua regia dissolution, liquid-solid ratio is 5 ~ 15:1, and temperature is 60 ~ 90 DEG C, extraction time 2 ~ 5h, and reaction terminates rear filtration;
(5) filtrate of step (4) directly adds alkali and is neutralized to pH=1 ~ 2, and then add ammoniacal liquor and be neutralized to pH=9 ~ 10, temperature 50 ~ 90 DEG C, red precipitate all dissolves rear filtration, and filter residue is platinum concentrate;
(6) step (5) gained filtrate adds hydrochloric acid, control pH=1, temperature 30 ~ 50 DEG C, and reaction 30min, filters after reaction terminates, and filter residue is the sub-palladium precipitation of dichloro two ammino;
(7) sub-for dichloro two ammino palladium precipitation is added ammonia solvent, liquid-solid ratio 1 ~ 3:1, be heated to 60 ~ 90 DEG C, yellow mercury oxide filters after cooling till disappearing;
(8) step (7) gained filtrate is heated to 40 ~ 60 DEG C, by hydrazine hydrate: palladium=0.5 ~ 1:1 adds hydrazine hydrate reduction palladium, filters and obtains palladium sponge product, seals preservation after washing, drying.
The precipitation agent added in step (2) is dimethylglyoxime, feed postition: add in reactor after adding deionized water and stirring dispersion by liquid-solid ratio 2:1, add-on is 2.6 ~ 3 times of platinum palladium content in silver electrolyte.
The heavy platinum palladium liquid that step (2) obtains returns silver-colored electrolyzer and continues electrolysis.
Drying in step (3) is carried out in loft drier, calcines and carries out in retort furnace, controls platinum palladium content >=98% in platina palldium alloy, calcining temperature 300 ~ 600 DEG C, calcination time 1 ~ 4h.
Calcining flow process is returned to reclaim platinum palladium further after the filter residue deionized water wash 2 ~ 3 times of step (4).
Alkali described in step (5) is the one in sodium hydroxide, potassium hydroxide, ammoniacal liquor.
Step (5) gained platinum concentrate ammonia scrubbing 2 ~ 3 times, allows residual palladium transfer in filtrate.
The 5% dilute hydrochloric acid solution washing 2 ~ 3 times of the sub-palladium precipitation of step (6) gained dichloro two ammino, filtrate is acidizing fluid, containing a small amount of palladium, adds zinc powder and carries out displacement Recover palladium.
Calcining flow process is returned after step (7) gained filter residue ammonia scrubbing 2 ~ 3 times.
Feature of the present invention: precipitation agent selectivity used in invention is strong, the palladium in a precipitated silver electrolytic solution and platinum, and the not base metal such as precipitated silver, copper, lead, bismuth, the Pt Pd concentrate therefore obtained after washing hardly containing base metal impurity; Solution after heavy platinum palladium returns electrolysis, can not have a negative impact to electrolysis, output 1
#qualified silver powder, silver powder is containing palladium≤0.001%; Obtain Pt Pd concentrate after calcining, the burned volatilization of organic components is except abandoning, and divalence platinum palladium is reduced to platinum-nickel alloys, purity > 98%; The higher platinum-nickel alloys of purity through aqua regia dissolution-alkali and ammoniacal liquor directly in and after removal of impurities-hcl acidifying removal of impurities-ammonia solvent-hydrazine hydrate reduction, obtain palladium sponge product, and enrichment output platinum concentrate; Eliminate traditional ammonium chloride in Refining process and sink palladium flow process, reduce palladium dispersion on stream.
Platinum palladium in energy high efficiente callback silver electrolyte of the present invention, obtain the Pt Pd concentrate that foreign matter content is low, the higher platinum-nickel alloys of purity is obtained after calcining, palladium sponge and platinum concentrate can be obtained again after Refining, purify silver electrolyte simultaneously and return use, reduce production cost, increase economic benefit, achieve significant technique effect.
Accompanying drawing explanation
Fig. 1 is principle process flow sheet of the present invention.
Embodiment
Below in conjunction with the production instance of applicant unit, the invention will be further described, but protection scope of the present invention is not limited to these embodiments.
Embodiment one:
(1) get silver-colored electrolysis production system electrolytic solution 2m3, wherein containing palladium is 0.12g/L, and platiniferous is 0.01g/L, containing nitric acid 2g/L.
(2) silver electrolyte is transferred to reactor, be heated to 46 DEG C, then add precipitation agent dimethylglyoxime (adding after adding deionized water and stirring dispersion by liquid-solid ratio 2:1) by 2.6 times of platinum palladium content, the reaction times is 15min, cooled and filtered, obtains Pt Pd concentrate and heavy platinum palladium liquid.Heavy platinum palladium liquid is containing palladium 0.0006g/L, platiniferous 0.0007g/L, and palladium deposition rate is 99.5%, and platinum deposition rate is 93%, and after returning electrolyzer continuation electrolysis, output silver powder is containing palladium 0.0003%.
(3) dust technology of Pt Pd concentrate pH=0.5 is put into loft drier after washing 2 times and is dried, and composition is: containing palladium 28.3%, platinum 2.1%, silver 0.07%, copper 0.04%, bismuth 0.005%, and plumbous 0.003%, residue content is mainly organism.
(4) Pt Pd concentrate that step (3) obtains is put into retort furnace to calcine, calcining temperature 350 DEG C, calcining 3h.Organism is burned except abandoning, and residue is platina palldium alloy, containing palladium 93.5%, and platiniferous 5.1%.
(5) by platina palldium alloy aqua regia dissolution, liquid-solid ratio is 8:1, and temperature is 70 DEG C, extraction time 4.5h; Reaction terminates rear filtration, returns calcining flow process after filter residue deionized water wash 2 times.
(6) the filtrate direct hydrogenation sodium oxide that step (5) obtains is neutralized to pH=1.5, then adds ammoniacal liquor and be neutralized to pH=9, be heated to 80 DEG C, filter after red precipitate all dissolves, filter residue is platinum concentrate, with ammonia scrubbing 2 times.Platinum concentrate platiniferous 45.2%.
(7) filtrate that step (6) obtains is added hydrochloric acid, control pH=1, temperature 35 DEG C, reaction 30min, filters after reaction terminates.Filter residue is the sub-palladium precipitation of dichloro two ammino, washs 2 times with 5% dilute hydrochloric acid solution; Filtrate is acidizing fluid, containing palladium 0.07g/L, adds zinc powder and carries out displacement Recover palladium.
(8) sub-for dichloro two ammino palladium precipitation is added ammonia solvent, liquid-solid ratio 1.5:1; Be heated to 70 DEG C, till yellow mercury oxide disappears; Filter after cooling, after filter residue ammonia scrubbing 2 times, return calcining flow process.
(9) filtrate that step (8) obtains is heated to 45 DEG C, by hydrazine hydrate: palladium=0.6:1 adds hydrazine hydrate reduction palladium, filters and obtain palladium sponge product, after washing, drying, seal preservation.Product is containing palladium 99.993%.
Embodiment two:
(1) get silver-colored electrolysis production system electrolytic solution 2m3, wherein containing palladium is 0.25g/L, and platiniferous is 0.018g/L, containing nitric acid 6g/L.
(2) silver electrolyte is transferred to reactor, be heated to 70 DEG C, then add precipitation agent dimethylglyoxime (adding after adding deionized water and stirring dispersion by liquid-solid ratio 2:1) by 2.8 times of platinum palladium content, the reaction times is 30min, cooled and filtered, obtains Pt Pd concentrate and heavy platinum palladium liquid.Heavy platinum palladium liquid is containing palladium 0.0004g/L, platiniferous 0.0002g/L, and palladium deposition rate is 99.8%, and platinum deposition rate is 98.9%, and after returning electrolyzer continuation electrolysis, output silver powder is containing palladium 0.0002%.
(3) dust technology of Pt Pd concentrate pH=1 is put into loft drier after washing 3 times and is dried, and composition is: containing palladium 28.9%, platinum 1.8%, silver 0.05%, copper 0.02%, bismuth 0.003%, and plumbous 0.004%, residue content is mainly organism.
(4) Pt Pd concentrate that step (3) obtains is put into retort furnace to calcine, calcining temperature 600 DEG C, calcining 2h.Organism is burned except abandoning, and residue is platina palldium alloy, containing palladium 94.6%, and platiniferous 4.3%.
(5) by platina palldium alloy aqua regia dissolution, liquid-solid ratio is 12:1, and temperature is 85 DEG C, extraction time 3h; Reaction terminates rear filtration, returns calcining flow process after filter residue deionized water wash 3 times.
(6) filtrate that step (5) obtains directly is added ammoniacal liquor and be neutralized to pH=9.5, be heated to 80 DEG C, filter after red precipitate all dissolves, filter residue is platinum concentrate, with ammonia scrubbing 3 times.Platinum concentrate platiniferous 47.8%.
(7) filtrate that step (6) obtains is added hydrochloric acid, control pH=1, temperature 40 DEG C, reaction 30min, filters after reaction terminates.Filter residue is the sub-palladium precipitation of dichloro two ammino, washs 3 times with 5% dilute hydrochloric acid solution; Filtrate is acidizing fluid, containing palladium 0.05g/L, adds zinc powder and carries out displacement Recover palladium.
(8) sub-for dichloro two ammino palladium precipitation is added ammonia solvent, liquid-solid ratio 2:1; Be heated to 85 DEG C, till yellow mercury oxide disappears; Filter after cooling, after filter residue ammonia scrubbing 3 times, return calcining flow process.
(9) filtrate that step (8) obtains is heated to 55 DEG C, by hydrazine hydrate: palladium=1:1 adds hydrazine hydrate reduction palladium, filters and obtain palladium sponge product, after washing, drying, seal preservation.Product is containing palladium 99.994%.
Claims (9)
1. the comprehensive recovering process of platinum palladium in silver electrolyte, is characterized in that:
(1) silver electrolyte is from silver-colored electrolysis production system, is wherein more than or equal to 0.1g/L, containing nitric acid 1 ~ 10g/L containing palladium;
(2) described silver electrolyte is transferred to reactor, be heated to 30 ~ 80 DEG C, then add precipitation agent, by the platinum palladium precipitation in silver electrolyte, cold filtration precipitates, and obtains Pt Pd concentrate and heavy platinum palladium liquid;
(3) dust technology washing 2 ~ 3 post-dryings of Pt Pd concentrate pH=0.5 ~ 1, calcining, will wherein organism be burned except abandoning, and residue is platina palldium alloy;
(4) platina palldium alloy aqua regia dissolution, liquid-solid ratio is 5 ~ 15:1, and temperature is 60 ~ 90 DEG C, extraction time 2 ~ 5h, and reaction terminates rear filtration;
(5) filtrate of step (4) directly adds alkali and is neutralized to pH=1 ~ 2, and then add ammoniacal liquor and be neutralized to pH=9 ~ 10, temperature 50 ~ 90 DEG C, red precipitate all dissolves rear filtration, and filter residue is platinum concentrate;
(6) step (5) gained filtrate adds hydrochloric acid, control pH=1, temperature 30 ~ 50 DEG C, and reaction 30min, filters after reaction terminates, and filter residue is the sub-palladium precipitation of dichloro two ammino;
(7) sub-for dichloro two ammino palladium precipitation is added ammonia solvent, liquid-solid ratio 1 ~ 3:1, be heated to 60 ~ 90 DEG C, yellow mercury oxide filters after cooling till disappearing;
(8) step (7) gained filtrate is heated to 40 ~ 60 DEG C, by hydrazine hydrate: palladium=0.5 ~ 1:1 adds hydrazine hydrate reduction palladium, filters and obtains palladium sponge product, seals preservation after washing, drying.
2. the comprehensive recovering process of platinum palladium in silver electrolyte according to claim 1, it is characterized in that the precipitation agent added in step (2) is dimethylglyoxime, feed postition: add in reactor after adding deionized water and stirring dispersion by liquid-solid ratio 2:1, add-on is 2.6 ~ 3 times of platinum palladium content in silver electrolyte.
3. the comprehensive recovering process of platinum palladium in silver electrolyte according to claim 1, is characterized in that heavy platinum palladium liquid that step (2) obtains returns silver-colored electrolyzer and continues electrolysis.
4. the comprehensive recovering process of platinum palladium in silver electrolyte according to claim 1, it is characterized in that the drying in step (3) is carried out in loft drier, calcine and carry out in retort furnace, control platinum palladium content >=98% in platina palldium alloy, calcining temperature 300 ~ 600 DEG C, calcination time 1 ~ 4h.
5. the comprehensive recovering process of platinum palladium in silver electrolyte according to claim 1, returns calcining flow process to reclaim platinum palladium further after it is characterized in that the filter residue deionized water wash 2 ~ 3 times of step (4).
6. the comprehensive recovering process of platinum palladium in silver electrolyte according to claim 1, is characterized in that the alkali described in step (5) is the one in sodium hydroxide, potassium hydroxide, ammoniacal liquor.
7. the comprehensive recovering process of platinum palladium in silver electrolyte according to claim 1 or 6, is characterized in that step (5) gained platinum concentrate ammonia scrubbing 2 ~ 3 times, allows residual palladium transfer in filtrate.
8. the comprehensive recovering process of platinum palladium in silver electrolyte according to claim 1, it is characterized in that the sub-palladium precipitation of step (6) gained dichloro two ammino 5% dilute hydrochloric acid solution washs 2 ~ 3 times, filtrate is acidizing fluid, containing a small amount of palladium, adds zinc powder and carries out displacement Recover palladium.
9. the comprehensive recovering process of platinum palladium in silver electrolyte according to claim 1, returns calcining flow process after it is characterized in that step (7) gained filter residue ammonia scrubbing 2 ~ 3 times.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105695750A (en) * | 2016-03-07 | 2016-06-22 | 紫金矿业集团股份有限公司 | Method for removing platinum and palladium out of silver electrolyte and concentrating platinum and palladium |
| CN106222437A (en) * | 2016-08-29 | 2016-12-14 | 金川集团股份有限公司 | A kind of method of refine palladium from alkalescence strip liquor |
| CN107099675A (en) * | 2017-05-27 | 2017-08-29 | 许良秋 | A kind of cleaning refinery practice of palladium |
| CN109023421A (en) * | 2018-08-15 | 2018-12-18 | 云南铜业股份有限公司西南铜业分公司 | A kind of purifying treatment method of silver electrolyte |
| RU2689268C1 (en) * | 2018-12-03 | 2019-05-24 | Открытое акционерное общество "Красноярский завод цветных металлов имени В.Н. Гулидова" | Method of producing palladium metal |
| CN110484747A (en) * | 2019-09-02 | 2019-11-22 | 湖南省佳川冶金科技有限公司 | A kind of technique of the selective extraction palladium from thick silver |
| CN113215405A (en) * | 2021-04-23 | 2021-08-06 | 郴州百一环保高新材料有限公司 | Method for recovering rare and noble metals from waste three-way catalyst |
| CN114410980A (en) * | 2022-01-24 | 2022-04-29 | 上海第二工业大学 | Process and production line for efficiently extracting noble metal gold, silver and palladium |
| CN114686692A (en) * | 2022-03-04 | 2022-07-01 | 金川集团股份有限公司 | Method for extracting metal platinum and palladium from high copper-containing silver electrolysis waste liquid |
| CN114774700A (en) * | 2022-04-27 | 2022-07-22 | 长沙华时捷环保科技发展股份有限公司 | Method for efficiently extracting platinum and palladium resources in silver electrolysis system |
| CN115109941A (en) * | 2022-07-29 | 2022-09-27 | 金浦新材料股份有限公司 | Method for recovering palladium from palladium-carbon catalyst impregnation liquid |
| CN116716484A (en) * | 2023-08-11 | 2023-09-08 | 云南贵金属实验室有限公司 | Method for recovering palladium and dimethylglyoxime from palladium-refining palladium-removing slag |
| CN117049971A (en) * | 2023-08-22 | 2023-11-14 | 株洲环冠新材料科技有限公司 | Amino modified material and preparation method and application thereof |
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| CN105695750A (en) * | 2016-03-07 | 2016-06-22 | 紫金矿业集团股份有限公司 | Method for removing platinum and palladium out of silver electrolyte and concentrating platinum and palladium |
| CN106222437A (en) * | 2016-08-29 | 2016-12-14 | 金川集团股份有限公司 | A kind of method of refine palladium from alkalescence strip liquor |
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| CN110484747B (en) * | 2019-09-02 | 2020-06-02 | 湖南省佳川冶金科技有限公司 | Process for selectively extracting palladium from crude silver |
| CN113215405A (en) * | 2021-04-23 | 2021-08-06 | 郴州百一环保高新材料有限公司 | Method for recovering rare and noble metals from waste three-way catalyst |
| CN114410980A (en) * | 2022-01-24 | 2022-04-29 | 上海第二工业大学 | Process and production line for efficiently extracting noble metal gold, silver and palladium |
| CN114686692A (en) * | 2022-03-04 | 2022-07-01 | 金川集团股份有限公司 | Method for extracting metal platinum and palladium from high copper-containing silver electrolysis waste liquid |
| CN114774700A (en) * | 2022-04-27 | 2022-07-22 | 长沙华时捷环保科技发展股份有限公司 | Method for efficiently extracting platinum and palladium resources in silver electrolysis system |
| CN114774700B (en) * | 2022-04-27 | 2024-05-24 | 长沙华时捷环保科技发展股份有限公司 | Method for efficiently extracting platinum-palladium resources in silver electrolysis system |
| CN115109941A (en) * | 2022-07-29 | 2022-09-27 | 金浦新材料股份有限公司 | Method for recovering palladium from palladium-carbon catalyst impregnation liquid |
| CN115109941B (en) * | 2022-07-29 | 2024-05-28 | 金浦新材料股份有限公司 | Method for recovering palladium from palladium-carbon catalyst impregnating solution |
| CN116716484A (en) * | 2023-08-11 | 2023-09-08 | 云南贵金属实验室有限公司 | Method for recovering palladium and dimethylglyoxime from palladium-refining palladium-removing slag |
| CN116716484B (en) * | 2023-08-11 | 2023-10-03 | 云南贵金属实验室有限公司 | Method for recovering palladium and dimethylglyoxime from palladium-refining palladium-removing slag |
| CN117049971A (en) * | 2023-08-22 | 2023-11-14 | 株洲环冠新材料科技有限公司 | Amino modified material and preparation method and application thereof |
| CN117049971B (en) * | 2023-08-22 | 2024-04-09 | 株洲环冠新材料科技有限公司 | Amino modified material and preparation method and application thereof |
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