CN101748276A - Process for extracting, separating and purifying Ag, Au, Pd and Pt - Google Patents
Process for extracting, separating and purifying Ag, Au, Pd and Pt Download PDFInfo
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- CN101748276A CN101748276A CN200910266628A CN200910266628A CN101748276A CN 101748276 A CN101748276 A CN 101748276A CN 200910266628 A CN200910266628 A CN 200910266628A CN 200910266628 A CN200910266628 A CN 200910266628A CN 101748276 A CN101748276 A CN 101748276A
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to a process for extracting, separating and purifying Ag, Au, Pd and Pt. The process comprises the following steps of: precipitating and separating Ag in the form of AgC1, then adding ammonia water for dissolving, reducing hydrazine hydrate to obtain Ag; extracting by using dibutyl carbitol, and back-extracting Au with 5 percent of oxalic acid with a direct acceptance rate of more than or equal to 99.9 percent; extracting Pd with n-octyl sulfur ether, wherein the extraction rate of palladium is more than or equal to 99.99 percent, and then back-extracting the palladium with 3mol/L ammonia water; and finally, extracting Pt with tri-n-octylamine, back-extracting platinum with alkaline water and reducing to obtain platinum.
Description
Technical field
The present invention relates to a kind of extracting and separating precious metals ag, Au, Pd, Pt continuous production processes working method.
Background technology
Traditional precious metal separates and adopts the aqua regia dissolution precious metal, then selective reduction precious metal progressively; Various precious metals need repeatedly to purify just can obtain pure metal, and yield is low; And produce a large amount of waste acid waters in process of production, the discharging large quantity of exhaust gas, along with requirement on environmental protection is more and more stricter, these technologies will progressively be eliminated.
The aqua regia dissolution method:
Au+HNO
3+4HCl→HAuCl
4+2H
2O+NO
Ag+2HNO
3→AgNO
3+H
2O+NO
2
3Pt+4HNO
3+18HCl→3H
2PtCl
6+8H
2O+4NO
3Pd+2HNO
3+12HCl→3H
2PdCl
4+4H
2O+2NO
Produce in the aqua regia dissolution method technology and contain obnoxious flavoures such as NO, NO2 in a large number, environmental pollution severity, need simultaneously with hydrochloric acid repeatedly evaporate to dryness destroy the troublesome operation of nitro-compound, this technology is eliminated substantially.
The external now general aqueous solution chlorination method that adopts, the chlorination rate of general gold, palladium, platinum is all than higher, and tail gas absorbs with ammoniacal liquor, and environmental pollution is little; With organic solvent extraction separate precious metal selectivity height, precious metal recovery per pass, purity height.
2Ag+Cl
2→2AgCl
Pt+2HCl+Cl
2→H
2PtCl
6
Pd+2HCl+Cl
2→H
2PdCl
6
2Au+2HCl+2Cl
2→2HAuCl
4
Hydrochloric acid in can concentrated solution in the chlorinated solution makes silver separate with silver nitride precipitation, and the palladium that obtains, platinum, gold solution can be adjusted acidity, with extraction agent extraction of palladium, platinum, gold respectively.
The aurin of Sweden Boliden company invention is practiced technology, and HCl and chlorine with heat in Glass Containers leach gold and platinum metals, and remaining silver generates silver nitride precipitation, reclaims or circulation with method of cementation then.Most of gold is precipitated in the first step with the proof gold form; Sedimentary gold of second step contains impurity and returns the leaching stage.
The refining process of China's palladium is still continued to use the process integration that the inferior palladium of ammonium palladic chloride repeated precipitation process and dichloro two ammoniums combines, and integrated process can be concise to 99.99% pure palladium with 80%～90% thick palladium.Treatment process is loaded down with trivial details.
International nickel Co. Ltd. Inco. Ltd. (Inco) Niflumic Acid (Acton) is with dibutyl carbitol collection gold (DBC), and with tributyl phosphate (TBP) extraction platinum, because that TBP has is necessarily water-soluble, solution loss is bigger behind the thioether collection palladium; The strip liquor acidifying has a large amount of sodium-chlor crystallizations to separate out when concentrating, and is difficult for being connected with the concise of platinum.
Therefore, the objective of the invention is to: improve dissolution process, extraction agent, extraction conditions, stripping process condition and the precious metal reductive agent of precious metal, reach high-recovery, highly purified precious metal, the novel process of non-environmental-pollution.
Summary of the invention
The extraction agent that the present invention comprised comprises: collection gold dibutyl carbitol (DBC), and di-n-octyl thioether (DOS) xylene solution extraction of palladium is used tri-n-octyl amine (TOA) xylene solution extraction platinum at last;
Technology of the present invention is fit to separate precious metal and forms Ag, Au, Pd, Pt and contain a small amount of base metal Cu, Sn, Pb, Ni etc.; Wherein precious metal dissolving solution composition is Au 0～250g/L, optimum concentration range 10～45g/L, and aqueous phase acidity 1～7molHCl is between best HCl 1.5～2.5mol; Pd 0～90g/L, optimum concentration range 10～30g/L, aqueous phase acidity 0～4molHCl is between best HCl 0.05～1.0mol; Pt 0～90g/L, optimum concentration range 20～50g/L, aqueous phase acidity 1～7molHCl is between best HCl 3～5mol.
Extraction agent dibutyl carbitol of the present invention can be 100% dibutyl carbitol, also can be the solution of alkane, aromatic hydrocarbons; The concentration range 1～30% of di-n-octyl thioether (DOS) xylene solution, best 10～20%; Tri-n-octyl amine (TOA) xylene solution 1～30%, best 10～20%.
According to this technology Separation and Recovery precious metals ag, Au, Pd, Pt, wherein the Au rate of recovery reaches more than 99.9%, and purity is more than 99.9%; Wherein the Pd rate of recovery reaches more than 99.9%, and purity is more than 99.9%; The percentage extraction of Pt can reach 99.99%, and the rate of recovery is greater than 99%, and purity is greater than 99.9%.
Description of drawings
Fig. 1 is extracting and separating purification Ag, Au, Pd, the process frame chart of Pt
Specific embodiment
Embodiment 1: precious metal liquid composition table composed as follows
| Component | ??Au | ??Pd | ??Pt | ??Cu | ??Fe | ??Sn | ??Pb |
| Content (g/L) | ??8.18 | ??20 | ??19.5 | ??7 | ??2.1 | ??1.2 | ??0.2 |
Get the above-mentioned precious metal solution of 1L, adjusting acidity is 2.5mol/L hydrochloric acid, and with the 1LDBC extraction, extraction time 5min divides the phase of anhydrating, with 0.5mol/L salt pickling organic phase; Divide the phase of anhydrating, organic phase at 80 ℃ of reductase 12 h, promptly gets golden yellow cake of gold with 5% oxalic acid solution, golden percentage extraction 99.99%, the rate of recovery 99.9%; Water merges, and boils off water and acid, and adjusting acidity is 0.1mol/L hydrochloric acid, with 1L15%DOS xylene solution extraction of palladium, and mixed phase 5min, the palladium percentage extraction is greater than 99.99%.Divide the phase of anhydrating, with the back extraction of 3mol/L ammoniacal liquor, back extraction ratio is 96%, and water promptly gets pure palladium with hydrazine hydrate reduction, and organic phase is applied mechanically by regeneration, and palladium purity is greater than 99.9%; Water concentrates removes portion water, adjusting acidity is 3mol/L hydrochloric acid, with 1L10% tri-n-octyl amine (TOA) xylene solution extraction platinum, divides the phase of anhydrating, organic phase is colourless to water with 0.1mol/L salt acid elution, divide the phase of anhydrating, organic phase alkali aqueous solution back extraction is with hydrazine hydrate reductive water solution, promptly get spongy platinum, platinum percentage extraction 99.99%, back extraction ratio 99%, reduction platinum purity is greater than 99.9.
Embodiment 2: precious metal liquid composition table composed as follows
| Component | ??Au | ??Pd | ??Pt | ??Cu | ??Fe | ??Sn | ??Pb |
| Content (g/L) | ??11.28 | ??18 | ??17.5 | ??8.2 | ??2.6 | ??1.4 | ??0.21 |
Get the above-mentioned precious metal solution of 500ml, adjusting acidity is 2.0mol/L hydrochloric acid, and with the 500mlDBC extraction, extraction time 5min divides the phase of anhydrating, with 0.5mol/L salt pickling organic phase; Divide the phase of anhydrating, organic phase at 80 ℃ of reductase 12 h, promptly gets golden yellow cake of gold with 5% oxalic acid solution, golden percentage extraction 99.99%, the rate of recovery 99.9%; Water merges, and boils off water and acid, and adjusting acidity is 0.1mol/L hydrochloric acid, with 500ml 15%DOS xylene solution extraction of palladium, and mixed phase 5min, the palladium percentage extraction is greater than 99.99%.Divide the phase of anhydrating, with the back extraction of 3mol/L ammoniacal liquor, back extraction ratio is 96%, and water promptly gets pure palladium with hydrazine hydrate reduction, and organic phase is applied mechanically by regeneration, and palladium purity is greater than 99.9%; Water concentrates removes portion water, adjusting acidity is 3mol/L hydrochloric acid, with 500ml15% tri-n-octyl amine (TOA) xylene solution extraction platinum, divides the phase of anhydrating, organic phase is colourless to water with 0.1mol/L salt acid elution, divide the phase of anhydrating, organic phase alkali aqueous solution back extraction is with hydrazine hydrate reductive water solution, promptly get spongy platinum, platinum percentage extraction 99.99%, back extraction ratio 99%, reduction platinum purity is greater than 99.9.
Claims (2)
1. the method for a separate precious metal, be fit to separate precious metal and form Ag, Au, Pd, Pt and contain a small amount of base metal Cu, Sn, Pb, Ni, it is characterized in that precious metal dissolving solution composition is Au 0～250g/L, optimum concentration range 30～90g/L, aqueous phase acidity 1～7molHCl is between best HCl1.5～2.5mol; Pd0～90g/L, optimum concentration range 10～30g/L, aqueous phase acidity 0～4molHCl is between best HCl0.05～1.0mol; Pt0～90g/L, optimum concentration range 20～50g/L, aqueous phase acidity 1～7molHCl is between best HCl3～5mol.
2. method according to claim 1 is characterized in that the extraction agent dibutyl carbitol is the solution of 100% dibutyl carbitol, alkane or aromatic hydrocarbons; The concentration range 1～30% of di-n-octyl thioether (DOS) xylene solution, best 10～20%; Tri-n-octyl amine (TOA) xylene solution 1～30%, best 10～20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910266628A CN101748276A (en) | 2009-12-31 | 2009-12-31 | Process for extracting, separating and purifying Ag, Au, Pd and Pt |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910266628A CN101748276A (en) | 2009-12-31 | 2009-12-31 | Process for extracting, separating and purifying Ag, Au, Pd and Pt |
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| Publication Number | Publication Date |
|---|---|
| CN101748276A true CN101748276A (en) | 2010-06-23 |
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|---|---|---|---|
| CN200910266628A Pending CN101748276A (en) | 2009-12-31 | 2009-12-31 | Process for extracting, separating and purifying Ag, Au, Pd and Pt |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985691A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for preparing high-purity gold |
| CN102994771A (en) * | 2011-09-13 | 2013-03-27 | 郴州市金贵银业股份有限公司 | Method for extracting palladium sponge from silver electrolysis anode slime parting liquid |
| CN105907976A (en) * | 2016-06-30 | 2016-08-31 | 华南理工大学 | Method for recovering palladium (Pd) from electron components of waste mobile phone |
| CN106282571A (en) * | 2016-08-15 | 2017-01-04 | 赣州市赤鼎再生资源有限公司 | A kind of comprehensive recycling process of stannum copper gold silver waste material |
| CN111363920A (en) * | 2020-04-07 | 2020-07-03 | 金川集团股份有限公司 | Method for extracting gold from silver-containing liquid |
| CN113337723A (en) * | 2021-06-10 | 2021-09-03 | 广东先导稀材股份有限公司 | Method for separating and extracting silver, palladium, copper and germanium from silver separating slag |
| CN114934178A (en) * | 2022-06-21 | 2022-08-23 | 中国地质科学院郑州矿产综合利用研究所 | Method for recovering gold from gold smelting slag chloridizing roasting leacheate |
-
2009
- 2009-12-31 CN CN200910266628A patent/CN101748276A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985691A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for preparing high-purity gold |
| CN102994771A (en) * | 2011-09-13 | 2013-03-27 | 郴州市金贵银业股份有限公司 | Method for extracting palladium sponge from silver electrolysis anode slime parting liquid |
| CN102994771B (en) * | 2011-09-13 | 2014-03-26 | 郴州市金贵银业股份有限公司 | Method for extracting palladium sponge from silver electrolysis anode slime parting liquid |
| CN105907976A (en) * | 2016-06-30 | 2016-08-31 | 华南理工大学 | Method for recovering palladium (Pd) from electron components of waste mobile phone |
| CN106282571A (en) * | 2016-08-15 | 2017-01-04 | 赣州市赤鼎再生资源有限公司 | A kind of comprehensive recycling process of stannum copper gold silver waste material |
| CN106282571B (en) * | 2016-08-15 | 2018-02-02 | 赣州市赤鼎再生资源有限公司 | A kind of comprehensive recycling process of tin copper gold and silver waste material |
| CN111363920A (en) * | 2020-04-07 | 2020-07-03 | 金川集团股份有限公司 | Method for extracting gold from silver-containing liquid |
| CN113337723A (en) * | 2021-06-10 | 2021-09-03 | 广东先导稀材股份有限公司 | Method for separating and extracting silver, palladium, copper and germanium from silver separating slag |
| CN114934178A (en) * | 2022-06-21 | 2022-08-23 | 中国地质科学院郑州矿产综合利用研究所 | Method for recovering gold from gold smelting slag chloridizing roasting leacheate |
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Open date: 20100623 |