CN103305699B - Method for extracting platinum-palladium out of copper anode mud - Google Patents
Method for extracting platinum-palladium out of copper anode mud Download PDFInfo
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- CN103305699B CN103305699B CN201310245986.4A CN201310245986A CN103305699B CN 103305699 B CN103305699 B CN 103305699B CN 201310245986 A CN201310245986 A CN 201310245986A CN 103305699 B CN103305699 B CN 103305699B
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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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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
Technical field:
The present invention relates to hydrometallurgical processes technical field, is a kind of method of extracting platinum palladium from copper anode mud specifically.
Background technology:
Current much copper anode mud process for producing producers are in order to reclaim platinum palladium product, the main treatment process that precipitates platinum palladium from once reducing bronze in liquid that adopts, has affected the golden rate of recovery, once the about 2-10mg/L of gold content in liquid after reduction, if red-tape operati is improper, the rate of loss of gold can be higher, directly after once reducing, in liquid, reclaims platinum palladium, and platinum palladium reduction ratio is also lower, platinum reduction ratio is 50% left and right, palladium reduction ratio is 60% left and right, not only causes the Precious Metals Resources wastes such as Au, Pt, Pd, is also unfavorable for environmental protection.
Summary of the invention:
The object of the invention is to overcome the deficiency of above-mentioned prior art, and a kind of method of extracting platinum palladium from copper anode mud providing.
In order to achieve the above object, the present invention is achieved in that a kind of method of extracting platinum palladium from copper anode mud, and it comprises following processing step:
A rotary kiln baking: copper anode mud, through 93% vitriol oil pulp, enters rotary kiln baking 4-7h, output calcining adds sulfuric acid leaching copper silver in calcining, and after solid-liquid separation, filtrate enters traditional heavy silver process and reclaims silver, and copper silver leached mud enters lower step operation;
Chlorination parting of b: according to 4～6: 1 liquid-solid ratio adds clear water in copper silver leached mud, add again sodium-chlor, 93% vitriol oil, sodium chlorate, 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 copper silver leached mud, be warming up to 85-95 DEG C, stir 2-4 hour, guarantee that gold dissolves completely, then solid-liquid separation, the parting slag of sulfur-bearing lead plumbate precipitation enters traditional point silver process, and after a chlorination parting, liquid enters lower step operation;
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: pass into SO in parting liquid
2gas reduction bronze, reaction finishes rear solid-liquid separation, is once reduced bronze and afterwards liquid of reduction once;
2HAuCl
4+3SO
2+6H
2O=2Au↓+3H
2SO
4+8HCl
D zinc dust precipitation: liquid after a chlorination parting reduction is squeezed in reactor, temperature is controlled at 35-50 DEG C, adds zinc powder to stir and replaces, and stops stirring after rear liquid gold content < 0.5mg/L to be restored, carry out solid-liquid separation and obtain secondary bronze, 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↓
Bis-chlorination partings of e: secondary bronze is carried out to secondary chlorination parting with reference to step b, obtain liquid and secondary parting slag after secondary chlorination parting, secondary parting slag enters traditional point silver process, and after secondary chlorination parting, liquid enters lower step operation;
F precipitation platinum palladium: in liquid after secondary chlorination parting, add reduction inhibitor agent sodium chlorate according to 8-15kg/m3, then progressively add ammonium chloride, reaction 2-3h, to not producing precipitation, the platinum palladium obtaining precipitation, then obtain platinum palladium through ordinary method separation and Extraction;
2NH
4Cl+PtCl
6 2-=(NH
4)
2PtCl
6↓+2Cl
-
2NH
4Cl+PdCl
6 2-=(NH
4)
2PdCl
6↓+2Cl
-
Bis-bronze reduction of g: pass into sulfur dioxide liquid reduction in liquid after reducing to 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 platinum palladium from copper anode mud of the present invention has outstanding substantive distinguishing features and marked improvement, 1, processing unit configuration is simple, stable operation, is convenient to control; 2, add sodium chlorate reduction inhibitor agent, avoid platinum palladium ion to be reduced to quadrivalent ion by sexavalence, can ensure metal recovery rate.
Embodiment:
For Comprehension and Implementation better, describe the present invention in detail below in conjunction with embodiment.
Case study on implementation: copper anode mud taking contain following element as example, its constituent content is as table one
Table one copper anode mud constituent content table
Take following processing step:
A rotary kiln baking: first add 93.3% vitriol oil 1t in slurrying tank, add again copper anode mud 1t, pulping 6h under normal temperature, enter rotary kiln baking 5h through self-feeder, rotary kiln one district's temperature is controlled at 350 DEG C, two district's temperature are controlled at 480 DEG C, and three district's temperature are controlled at 550 DEG C, output calcining 1t; Calcining drops in reactor 1, adds clear water 7m
3, 93.3% sulfuric acid 700L, 85 DEG C of constant temperature, reaction 2h, puts groove filtration and obtains 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 reactor 2, and 2.8m adds water
3, 93.3% sulfuric acid 90L, sodium-chlor 70kg, sodium chlorate 70kg, sodium chlorate 70kg divides three times and adds, and adds respectively 25kg, 25kg, 20kg every 1h, and 85 DEG C of reaction 4h of constant temperature, filter parting slag and enter traditional point silver process, parting liquid 2.7m
3enter next procedure;
C sulfur dioxide gas reduction: parting liquid is squeezed in reactor 3, passes into SO
2be reduced to solution and become colorless, reaction is put groove after finishing and is filtered, and is once reduced rear liquid 2.65m
3once reduce bronze dry weight 5.99kg, after intermediate frequency ingot casting, obtain ingot 5.989kg No. 1.
D zinc dust precipitation: the rear liquid that will once reduce is squeezed in reactor 3, opens and stirs, and adds zinc powder 25kg displacement, temperature is controlled at 40 DEG C of reaction 1h, termination reaction when liquid gold content is 0.45 mg/L after chemical examination reduction after testing, filters and obtains secondary bronze weight in wet base 31.5kg, filtrate sewage disposal;
Bis-chlorination partings of e: add clear water 1.8m in reactor 4
3, secondary bronze 31.5kg; Add sodium-chlor 2kg, sulfuric acid 10kg, sodium chlorate 2kg, sodium chlorate is divided three times and is added again, and adds respectively 1 kg, 0.5 kg, 0.5kg at every turn, is warming up to 90 DEG C, and stirring reaction 2.5 hours filters and removes lead sulfate precipitation;
F precipitation platinum palladium: add ammonium chloride 25kg, sodium chlorate 5kg in reactor 4, reaction 2h, filters and obtain 3.8kg platinum palladium precipitation, then obtain platinum 13.49g, palladium 45.11g by ordinary method separation and Extraction;
G bronze reduction: platinum palladium reduction filtrate is squeezed in reactor 5, passes into excess liq sulphur dioxide reduction and obtains bronze 0.205kg.
Under this experiment condition of table two and traditional technology condition under metal recovery rate contrast table
Claims (2)
1. from copper anode mud, extract a method for platinum palladium, it is characterized in that it comprises following processing step:
A rotary kiln baking: copper anode mud, through 93% vitriol oil pulp, enters rotary kiln baking 4-7h, output calcining adds sulfuric acid leaching copper silver in calcining, and after solid-liquid separation, filtrate enters traditional heavy silver process and reclaims silver, and copper silver leached mud enters lower step operation;
Chlorination parting of b: according to 4～6: 1 liquid-solid ratio adds clear water in copper silver leached mud, add again sodium-chlor, 93% vitriol oil, sodium chlorate, 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 copper silver leached mud, be warming up to 85-95 DEG C, stir 2-4 hour, guarantee that gold dissolves completely, then solid-liquid separation, the parting slag of sulfur-bearing lead plumbate precipitation enters traditional point silver process, and after a chlorination parting, liquid enters lower step operation;
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
Bronze of c reduction: pass into SO in liquid after a chlorination parting
2gas reduction bronze, reaction finishes rear solid-liquid separation, is once reduced bronze and afterwards liquid of reduction once;
2HAuCl
4+3SO
2+6H
2O=2Au↓+3H
2SO
4+8HCl
D zinc dust precipitation: the rear liquid that will once reduce is squeezed in reactor, temperature is controlled at 35-50 DEG C, adds zinc powder to stir and replaces, and stops stirring after rear liquid gold content < 0.5mg/L to be restored, carry out solid-liquid separation and obtain secondary bronze, 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↓
Bis-chlorination partings of e: secondary bronze is carried out to secondary chlorination parting with reference to step b, obtain liquid and secondary parting slag after secondary chlorination parting, secondary parting slag enters traditional point silver process, and after secondary chlorination parting, liquid enters lower step operation;
F precipitation platinum palladium: in liquid after secondary chlorination parting according to 8-15kg/ m
3add reduction inhibitor agent, then progressively add ammonium chloride, reaction 2-3h, to not producing precipitation, liquid after the platinum palladium obtaining precipitation and the reduction of platinum palladium, then obtain platinum, palladium through ordinary method separation and Extraction;
2NH
4Cl+PtCl
6 2-=(NH
4)
2PtCl
6↓+2Cl
-
2NH
4Cl+PdCl
6 2-=(NH
4)
2PdCl
6↓+2Cl
-
Bis-bronze reduction of g: pass into sulphur dioxide reduction in liquid after reducing to platinum palladium and obtain bronze.
2HAuCl
4+3SO
2+6H
2O=2Au↓+3H
2SO
4+8HCl
2. a kind of method of extracting platinum palladium from copper anode mud according to claim 1, is characterized in that the reduction inhibitor agent described in step f is sodium chlorate.
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| CN103305699B true CN103305699B (en) | 2014-12-10 |
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| CN105543485B (en) * | 2016-03-07 | 2017-09-29 | 曹明华 | A kind of method that valuable metal is separated and recovered from copper anode mud |
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| CN1061044A (en) * | 1990-10-29 | 1992-05-13 | 中国有色金属工业总公司昆明贵金属研究所 | From copper anode mud, reclaim Au, Pt, Pd and tellurium |
| CN101555550B (en) * | 2009-05-22 | 2011-02-16 | 北京科技大学 | Method for recycling lead-tin in silver separating residue of copper anode slime of circuit board |
| CN101831553B (en) * | 2010-05-28 | 2012-06-06 | 北京科技大学 | Method for green recovery of waste circuit boards by cyanide-free full-wet whole set process |
| CN101994013B (en) * | 2010-12-10 | 2012-08-29 | 四会市鸿明贵金属有限公司 | Copper scum smelting 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 |
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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 |