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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- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 28
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 17
- 239000010949 copper Substances 0.000 title claims abstract description 17
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000007788 liquid Substances 0.000 claims abstract description 43
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 29
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 21
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052737 gold Inorganic materials 0.000 claims abstract description 16
- 239000010931 gold Substances 0.000 claims abstract description 16
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims abstract description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 12
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052709 silver Inorganic materials 0.000 claims abstract description 12
- 239000004332 silver Substances 0.000 claims abstract description 12
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003112 inhibitor Substances 0.000 claims abstract description 5
- 238000002386 leaching Methods 0.000 claims abstract description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 4
- 229910000906 Bronze Inorganic materials 0.000 claims description 19
- 239000010974 bronze Substances 0.000 claims description 19
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 238000001556 precipitation Methods 0.000 claims description 14
- YCKOAAUKSGOOJH-UHFFFAOYSA-N copper silver Chemical compound [Cu].[Ag].[Ag] YCKOAAUKSGOOJH-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 8
- 239000011701 zinc Substances 0.000 claims description 8
- 239000002893 slag Substances 0.000 claims description 7
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 101150003085 Pdcl gene Proteins 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 235000010269 sulphur dioxide Nutrition 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 3
- 239000010865 sewage Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000004291 sulphur dioxide Substances 0.000 claims description 2
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims 1
- 238000001914 filtration Methods 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract description 2
- 241000430525 Aurinia saxatilis Species 0.000 abstract 1
- 239000012141 concentrate Substances 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 230000019635 sulfation Effects 0.000 abstract 1
- 238000005670 sulfation reaction Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 3
- 239000000470 constituent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 description 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 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
Landscapes
- Manufacture And Refinement Of Metals (AREA)
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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| CN201310245986.4A CN103305699B (en) | 2013-06-20 | 2013-06-20 | Method for extracting platinum-palladium out of copper anode mud |
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|---|---|---|---|
| CN201310245986.4A CN103305699B (en) | 2013-06-20 | 2013-06-20 | Method for extracting platinum-palladium out of copper anode mud |
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|---|---|
| CN103305699A CN103305699A (en) | 2013-09-18 |
| CN103305699B true CN103305699B (en) | 2014-12-10 |
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| 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 |
| 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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