CN103305699A - Method for extracting platinum-palladium out of copper anode mud - Google Patents

Method for extracting platinum-palladium out of copper anode mud Download PDF

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CN103305699A
CN103305699A CN2013102459864A CN201310245986A CN103305699A CN 103305699 A CN103305699 A CN 103305699A CN 2013102459864 A CN2013102459864 A CN 2013102459864A CN 201310245986 A CN201310245986 A CN 201310245986A CN 103305699 A CN103305699 A CN 103305699A
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liquid
palladium
platinum
parting
gold
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CN103305699B (en
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王兴
崔家友
于卫军
侯绍军
杨晓宇
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SHANDONG HUMON MELT STOCK Ltd
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Abstract

The invention discloses a method for extracting platinum-palladium out of copper anode mud. The method is characterized in that the platinum-palladium is extracted by employing a secondary gold dust chlorination gold leaching liquid, and the method comprises the following process steps of: firstly, carrying out sulfation roasting on the copper anode mud, carrying out primary chlorination gold leaching, carrying out sulfur dioxide gas reduction so as to obtain a primary reduction liquid, and subsequently carrying out zinc powder replacement so as to enrich gold, silver, platinum and palladium into secondary gold powder; secondly, dissolving the secondary gold powder, removing the impurities, filtering the obtained filtered residue, carrying out secondary chlorination gold leaching, adding ammonium chloride and a reduction inhibitor sodium chlorate into the filtered liquid, and reacting so as to obtain platinum and palladium precipitate; and finally reducing the filtered liquid by using a liquid sulfur dioxide to leach the gold. The method is simple in process equipment arrangement and convenient to operate; the recycling rate of the gold in the copper anode mud is increased; and meanwhile the platinum-palladium is effectively enriched in platinum-palladium concentrate.

Description

A kind of method of from copper anode mud, extracting the platinum palladium
Technical field:
The present invention relates to the hydrometallurgical processes technical field, is a kind of method of extracting the platinum palladium from copper anode mud specifically.
Background technology:
At present a lot of copper anode mud process for producing producers are in order to reclaim platinum palladium product, the main employing from once reducing behind the bronze treatment process of precipitation platinum palladium the liquid influenced the golden rate of recovery, once the about 2-10mg/L of gold content in the liquid of reduction back, if red-tape operati is improper, the rate of loss of gold can be higher, directly once reclaiming the platinum palladium in the liquid of reduction back, and platinum palladium reduction ratio is also lower, the platinum reduction ratio is about 50%, the palladium reduction ratio is about 60%, not only causes the precious metal wastings of resources such as Au, Pt, Pd, also is unfavorable for environmental protection.
Summary of the invention:
The objective of the invention is to overcome the deficiency of above-mentioned prior art, and a kind of method of from copper anode mud, extracting the platinum palladium that provides.
In order to achieve the above object, the present invention is achieved in that a kind of method of extracting the platinum palladium from copper anode mud, and it comprises following processing step:
The a rotary kiln baking: copper anode mud enters rotary kiln baking 4-7h through 93% vitriol oil pulp, and the output calcining adds sulfuric acid leaching copper silver in calcining, and after the solid-liquid separation, filtrate enters traditional heavy silver process and reclaims silver, and copper silver leached mud enters down the step operation;
Chlorination parting of b: according to 4～6: 1 liquid-solid ratio adds clear water in copper silver leached mud, add sodium-chlor, 93% vitriol oil, sodium chlorate again, sodium chlorate add-on and copper silver leached mud gold content ratio are 10:1, sodium-chlor and sodium chlorate weight ratio 1:1, the weight ratio 1:1 of lead in sulfuric acid and the copper silver leached mud, be warming up to 85-95 ℃, stirred 2-4 hour, guarantee that gold dissolves fully, solid-liquid separation then, the parting slag of sulfur-bearing lead plumbate precipitation enters traditional branch silver process, and liquid enters down the step operation behind the chlorination parting;
Pb+H 2SO 4==PbSO 4↓+H 2↑
2Au+ClO 3 -+6H ++7Cl -=2AuCl 4 -+3H 2O
3Pt+ClO 3 -+6H ++11Cl -=3PtCl 4 2-+3H 2O
3Pd+ClO 3 -+6H ++11Cl -=3PdCl 4 2-+3H 2O
3PtCl 4 2-+ClO 3 -+6H ++5Cl -=3PtCl 6 2-+3H 2O
3PdCl 4 2-+ClO 3 -+6H ++5Cl -=3PdCl 6 2-+3H 2O
A bronze reduction of c: in parting liquid, feed SO 2Gas reduction bronze, reaction finish the back solid-liquid separation, are once reduced bronze and liquid after the reduction once;
2HAuCl 4+3SO 2+6H 2O=2Au↓+3H 2SO 4+8HCl
D zinc dust precipitation: a chlorination parting reduction back liquid is squeezed in the reactor, temperature control adds the zinc powder stirring and replaces at 35-50 ℃, stops to stir behind back liquid gold content＜0.5mg/L to be restored, carry out solid-liquid separation and obtain the secondary bronze, the displaced liquid sewage disposal;
Zn+PtCl 4 2-=Zn 2++4Cl -+Pt↓
Zn+PdCl 4 2-=Zn 2++4Cl -+Pd↓
3Zn+2AuCl 4 -=3Zn 2++8Cl -+2Au↓
E secondary chlorination parting: the secondary bronze is carried out secondary chlorination parting with reference to step b, obtain liquid and secondary parting slag behind the secondary chlorination parting, secondary parting slag enters traditional branch silver process, and liquid enters down the step operation behind the secondary chlorination parting;
F precipitation platinum palladium: add the reduction inhibitor agent sodium chlorate according to 8-15kg/m3 in the liquid behind the secondary chlorination parting, progressively add ammonium chloride then, reaction 2-3h, to not producing precipitation, the platinum palladium that obtains precipitation obtains the platinum palladium through conventional method separation and Extraction again;
2NH 4Cl+PtCl 6 2-=(NH 4) 2PtCl 6↓+2Cl -
2NH 4Cl+PdCl 6 2-=(NH 4) 2PdCl 6↓+2Cl -
G secondary bronze reduces: feed the sulfur dioxide liquid reduction in the liquid after reducing to the platinum palladium and obtain bronze.
2HAuCl 4+3SO 2+6H 2O=2Au↓+3H 2SO 4+8HCl
The invention has the beneficial effects as follows: compared with the prior art a kind of method of extracting the platinum palladium from copper anode mud of the present invention has outstanding substantive distinguishing features and marked improvement, and 1, the processing unit configuration is simple, stable operation is convenient to control; 2, add the sodium chlorate reduction inhibitor agent, avoid the platinum palladium ion to be reduced to quadrivalent ion by sexavalence, can guarantee metal recovery rate.
Embodiment:
In order to understand better and to implement, describe the present invention in detail below in conjunction with embodiment.
Case study on implementation: copper anode mud is example with what contain following element, its constituent content such as table one
Table one copper anode mud constituent content table
Figure 2013102459864100002DEST_PATH_IMAGE001
Take following processing step:
A rotary kiln baking: in the pulp groove, add 93.3% vitriol oil 1t earlier, add copper anode mud 1t again, pulping 6h under the normal temperature, enter rotary kiln baking 5h through self-feeder, rotary kiln one district's temperature control is at 350 ℃, two district's temperature controls are at 480 ℃, and three district's temperature are controlled at 550 ℃ output calcining 1t; Calcining drops in the reactor 1, adds clear water 7m 3, 93.3% sulfuric acid 700L, 85 ℃ of constant temperature, reaction 2h is put the groove filtration and is obtained copper silver leached mud 700kg, and filtrate enters traditional heavy silver process and reclaims silver;
Chlorination parting of b: copper silver leached mud drops in the reactor 2, adds water 2.8m 3, 93.3% sulfuric acid 90L, sodium-chlor 70kg, sodium chlorate 70kg, sodium chlorate 70kg divide three addings, add 25kg, 25kg, 20kg respectively every 1h, and 85 ℃ of reactions of constant temperature 4h filters the parting slag and enters traditional branch silver process, parting liquid 2.7m 3Enter next procedure;
The reduction of c sulfur dioxide gas: parting liquid is squeezed in the reactor 3, feeds SO 2Be reduced to solution and become colorless, put groove after reaction finishes and filter, liquid 2.65m after once being reduced 3Once reduce bronze dry weight 5.99kg, obtain ingot 5.989kg behind the intermediate frequency ingot casting No. 1.
The d zinc dust precipitation: the back liquid that will once reduce is squeezed in the reactor 3, opens and stirs, and adds zinc powder 25kg displacement, temperature control is at 40 ℃ of reaction 1h, termination reaction when chemical examination reduction back liquid gold content is 0.45 mg/L is after testing filtered and is obtained secondary bronze weight in wet base 31.5kg, filtrate sewage disposal;
E secondary chlorination parting: in reactor 4, add clear water 1.8m 3, secondary bronze 31.5kg; Add sodium-chlor 2kg, sulfuric acid 10kg, sodium chlorate 2kg again, sodium chlorate is divided three addings, adds 1 kg, 0.5 kg, 0.5kg respectively at every turn, is warming up to 90 ℃, and stirring reaction 2.5 hours filters and removes the lead sulfate precipitation;
F precipitation platinum palladium: add ammonium chloride 25kg, sodium chlorate 5kg in reactor 4, reaction 2h filters and obtains 3.8kg platinum palladium precipitation, obtains platinum 13.49g, palladium 45.11g with the ordinary method separation and Extraction again;
The reduction of g bronze: platinum palladium reduction filtrate is squeezed in the reactor 5, feeds the excess liq sulphur dioxide reduction and obtains bronze 0.205kg.
Under this experiment condition of table two and the traditional technology condition under the metal recovery rate contrast table
Figure 2013102459864100002DEST_PATH_IMAGE002

Claims (2)

1. method of extracting the platinum palladium from copper anode mud is characterized in that it comprises following processing step:
The a rotary kiln baking: copper anode mud enters rotary kiln baking 4-7h through 93% vitriol oil pulp, and the output calcining adds sulfuric acid leaching copper silver in calcining, and after the solid-liquid separation, filtrate enters traditional heavy silver process and reclaims silver, and copper silver leached mud enters down the step operation;
Chlorination parting of b: according to 4～6: 1 liquid-solid ratio adds clear water in copper silver leached mud, add sodium-chlor, 93% vitriol oil, sodium chlorate again, sodium chlorate add-on and copper silver leached mud gold content ratio are 10:1, sodium-chlor and sodium chlorate weight ratio 1:1, the weight ratio 1:1 of lead in sulfuric acid and the copper silver leached mud, be warming up to 85-95 ℃, stirred 2-4 hour, guarantee that gold dissolves fully, solid-liquid separation then, the parting slag of sulfur-bearing lead plumbate precipitation enters traditional branch silver process, and liquid enters down the step operation behind the chlorination parting;
Pb+H 2SO 4==PbSO 4↓+H 2↑
2Au+ClO 3 -+6H ++7Cl -=2AuCl 4 -+3H 2O
3Pt+ClO 3 -+6H ++11Cl -=3PtCl 4 2-+3H 2O
3Pd+ClO 3 -+6H ++11Cl -=3PdCl 4 2-+3H 2O
3PtCl 4 2-+ClO 3 -+6H ++5Cl -=3PtCl 6 2-+3H 2O
3PdCl 4 2-+ClO 3 -+6H ++5Cl -=3PdCl 6 2-+3H 2O
A bronze reduction of c: in parting liquid, feed SO 2Gas reduction bronze, reaction finish the back solid-liquid separation, are once reduced bronze and liquid after the reduction once;
2HAuCl 4+3SO 2+6H 2O=2Au↓+3H 2SO 4+8HCl
D zinc dust precipitation: a chlorination parting reduction back liquid is squeezed in the reactor, temperature control adds the zinc powder stirring and replaces at 35-50 ℃, stops to stir behind back liquid gold content＜0.5mg/L to be restored, carry out solid-liquid separation and obtain the secondary bronze, the displaced liquid sewage disposal;
Zn+PtCl 4 2-=Zn 2++4Cl -+Pt↓
Zn+PdCl 4 2-=Zn 2++4Cl -+Pd↓
3Zn+2AuCl 4 -=3Zn 2++8Cl -+2Au↓
E secondary chlorination parting: the secondary bronze is carried out secondary chlorination parting with reference to step b, obtain liquid and secondary parting slag behind the secondary chlorination parting, secondary parting slag enters traditional branch silver process, and liquid enters down the step operation behind the secondary chlorination parting;
F precipitation platinum palladium: add reduction inhibitor agent according to 8-15kg/m3 in the liquid behind the secondary chlorination parting, progressively add ammonium chloride then, reaction 2-3h, to not producing precipitation, the platinum palladium that obtains precipitation obtains platinum, palladium through conventional method separation and Extraction again;
2NH 4Cl+PtCl 6 2-=(NH 4) 2PtCl 6↓+2Cl -
2NH 4Cl+PdCl 6 2-=(NH 4) 2PdCl 6↓+2Cl -
G secondary bronze reduces: feed the sulfur dioxide liquid reduction in the liquid after reducing to the platinum palladium and obtain bronze.
2. 2HAuCl 4+3SO 2+6H 2O=2Au↓+3H 2SO 4+8HCl
A kind of method of extracting the platinum palladium from copper anode mud according to claim 1 is characterized in that the reduction inhibitor agent described in the step f is sodium chlorate.
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Cited By (19)

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CN104372176A (en) * 2014-11-22 2015-02-25 王景龙 Method for extracting gold, silver and palladium from waste mobile phone
CN104762479A (en) * 2015-04-01 2015-07-08 郴州雄风环保科技有限公司 Process for comprehensively recovering rare and precious metals including gold, silver, platinum and palladium from gold-bearing wastes
CN105256138A (en) * 2015-11-18 2016-01-20 金川集团股份有限公司 Method for separating platinum group metal from platinum group metal-contained solution
CN105543485A (en) * 2016-03-07 2016-05-04 曹明华 Method for separating and recovering valuable metals from copper anode slime
CN105603205A (en) * 2016-01-12 2016-05-25 江西新金叶实业有限公司 Direct gold, platinum and palladium separating and extracting method
CN105821215A (en) * 2016-04-19 2016-08-03 浙江亚栋实业有限公司 Method for recycling metal bismuth from anode slime
CN105905874A (en) * 2016-04-19 2016-08-31 浙江亚栋实业有限公司 Method of recycling tellurium from anode mud
CN106119567A (en) * 2016-09-07 2016-11-16 深圳市真牛精工科技有限公司 A kind of method of gold of purifying metals
CN107312932A (en) * 2017-06-22 2017-11-03 中南大学 A kind of method of valuable metal in separate precious metal enrichment material
CN108239699A (en) * 2016-12-26 2018-07-03 北京有色金属研究总院 A kind of method of valuable metal in leaded zinc-silver material of synthetical recovery
CN109593969A (en) * 2018-12-14 2019-04-09 许金刚 A kind of molten gold process of no cyanogen
CN110964920A (en) * 2018-09-28 2020-04-07 荆门市格林美新材料有限公司 Method for recovering refined platinum from crude ammonium chloroplatinate
CN110964918A (en) * 2018-09-28 2020-04-07 荆门市格林美新材料有限公司 Recovery method for recovering gold and tellurium from platinum-palladium concentrate and enriching platinum and palladium
CN110964905A (en) * 2018-09-28 2020-04-07 荆门市格林美新材料有限公司 Method for purifying crude ammonium chloroplatinate
CN110964919A (en) * 2018-09-28 2020-04-07 荆门市格林美新材料有限公司 Preparation method of spongy platinum
CN110964903A (en) * 2018-09-28 2020-04-07 荆门市格林美新材料有限公司 Recovery method for recovering gold from platinum-palladium concentrate
CN110964922A (en) * 2018-09-28 2020-04-07 荆门市格林美新材料有限公司 Method for recovering refined platinum from crude ammonium chloroplatinate
CN111606308A (en) * 2020-06-04 2020-09-01 江西铜业技术研究院有限公司 Method for efficiently separating and recycling tellurium from copper anode slime copper separation slag
CN112725633A (en) * 2021-02-07 2021-04-30 厦门海峡黄金珠宝产业园有限公司 Negative pressure type gold chlorination and separation process

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CN104372176A (en) * 2014-11-22 2015-02-25 王景龙 Method for extracting gold, silver and palladium from waste mobile phone
CN104762479A (en) * 2015-04-01 2015-07-08 郴州雄风环保科技有限公司 Process for comprehensively recovering rare and precious metals including gold, silver, platinum and palladium from gold-bearing wastes
CN105256138A (en) * 2015-11-18 2016-01-20 金川集团股份有限公司 Method for separating platinum group metal from platinum group metal-contained solution
CN105603205A (en) * 2016-01-12 2016-05-25 江西新金叶实业有限公司 Direct gold, platinum and palladium separating and extracting method
CN105543485A (en) * 2016-03-07 2016-05-04 曹明华 Method for separating and recovering valuable metals from copper anode slime
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CN105905874A (en) * 2016-04-19 2016-08-31 浙江亚栋实业有限公司 Method of recycling tellurium from anode mud
CN105905874B (en) * 2016-04-19 2018-01-23 浙江亚栋实业有限公司 A kind of method that tellurium is reclaimed from the earth of positive pole
CN106119567B (en) * 2016-09-07 2019-02-15 深圳市真牛精工科技有限公司 A method of gold of purifying metals
CN106119567A (en) * 2016-09-07 2016-11-16 深圳市真牛精工科技有限公司 A kind of method of gold of purifying metals
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CN108239699A (en) * 2016-12-26 2018-07-03 北京有色金属研究总院 A kind of method of valuable metal in leaded zinc-silver material of synthetical recovery
CN107312932A (en) * 2017-06-22 2017-11-03 中南大学 A kind of method of valuable metal in separate precious metal enrichment material
CN110964903A (en) * 2018-09-28 2020-04-07 荆门市格林美新材料有限公司 Recovery method for recovering gold from platinum-palladium concentrate
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CN110964918A (en) * 2018-09-28 2020-04-07 荆门市格林美新材料有限公司 Recovery method for recovering gold and tellurium from platinum-palladium concentrate and enriching platinum and palladium
CN110964905A (en) * 2018-09-28 2020-04-07 荆门市格林美新材料有限公司 Method for purifying crude ammonium chloroplatinate
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CN111606308A (en) * 2020-06-04 2020-09-01 江西铜业技术研究院有限公司 Method for efficiently separating and recycling tellurium from copper anode slime copper separation slag
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CN112725633A (en) * 2021-02-07 2021-04-30 厦门海峡黄金珠宝产业园有限公司 Negative pressure type gold chlorination and separation process
CN112725633B (en) * 2021-02-07 2022-04-26 厦门海峡黄金珠宝产业园有限公司 Negative pressure type gold chlorination and separation process

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Inventor after: Wang Xing

Inventor after: Cui Jiayou

Inventor after: Yu Weijun

Inventor after: Hou Shaobin

Inventor after: Yang Xiaoyu

Inventor before: Wang Xing

Inventor before: Cui Jiayou

Inventor before: Yu Weijun

Inventor before: Hou Shaojun

Inventor before: Yang Xiaoyu

COR Change of bibliographic data

Free format text: CORRECT: INVENTOR; FROM: WANG XING CUI JIAYOU YU WEIJUN HOU SHAOJUN YANG XIAOYU TO: WANG XING CUI JIAYOU YU WEIJUN HOU SHAOBIN YANG XIAOYU