CN1045795C - Method for recovering platinum and lead from anode slime of hydrogen peroxide production by electrolysis - Google Patents
Method for recovering platinum and lead from anode slime of hydrogen peroxide production by electrolysis Download PDFInfo
- Publication number
- CN1045795C CN1045795C CN96112946A CN96112946A CN1045795C CN 1045795 C CN1045795 C CN 1045795C CN 96112946 A CN96112946 A CN 96112946A CN 96112946 A CN96112946 A CN 96112946A CN 1045795 C CN1045795 C CN 1045795C
- Authority
- CN
- China
- Prior art keywords
- naoh
- lead
- platinum
- anode
- hydrogen peroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 238000005868 electrolysis reaction Methods 0.000 title description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 84
- 238000004070 electrodeposition Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 7
- 239000010440 gypsum Substances 0.000 claims abstract description 7
- 239000002893 slag Substances 0.000 claims abstract description 7
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 6
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 6
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004571 lime Substances 0.000 claims abstract description 6
- 239000012452 mother liquor Substances 0.000 claims abstract description 6
- 239000010802 sludge Substances 0.000 claims description 15
- 230000029087 digestion Effects 0.000 claims description 9
- 238000013019 agitation Methods 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 5
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- 230000008929 regeneration Effects 0.000 claims description 4
- 238000011069 regeneration method Methods 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 9
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 239000000706 filtrate Substances 0.000 abstract description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract 2
- 238000009835 boiling Methods 0.000 abstract 2
- 238000002791 soaking Methods 0.000 abstract 2
- 238000007796 conventional method Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 238000007654 immersion Methods 0.000 abstract 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 229910052785 arsenic Inorganic materials 0.000 description 3
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000006256 anode slurry Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- 229910001020 Au alloy Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- CJHOCIMVIOUHQV-UHFFFAOYSA-N [Cu].[Bi].[Pb].[Sb] Chemical compound [Cu].[Bi].[Pb].[Sb] CJHOCIMVIOUHQV-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- ONVGIJBNBDUBCM-UHFFFAOYSA-N silver;silver Chemical compound [Ag].[Ag+] ONVGIJBNBDUBCM-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- Treatment Of Sludge (AREA)
- Electrolytic Production Of Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
A method for recovering platinum and lead from anode slime produced by electrolyzing hydrogen peroxide is characterized by comprising the following steps: the anode mud is soaked and boiled by NaOH, the immersion liquid is used for recovering crude lead by electrodeposition, the mother liquor is regenerated by lime, gypsum is recovered, the filtrate is returned to the NaOH for soaking and boiling after the concentration is verified and the loss is supplemented, the soaking and boiling slag is dissolved by aqua regia, the residual lead is removed by sulfuric acid, and the pure platinum product is obtained by purifying by a conventional method. The method has the advantages of simple equipment, simple method, no environmental pollution and good lead removal effect, can quickly obtain a pure platinum product with the purity of 99.9 percent, and is particularly suitable for recovering platinum and lead from anode mud generated in hydrogen peroxide electrolytic production.
Description
The wet method that the present invention relates to precious metal is refined, and particularly the anode sludge from electrolytic hydrogen peroxide solution production reclaims platinum and lead.
Reclaim platinum and lead from the anode sludge of electrolytic hydrogen peroxide solution production, traditional extracting method is with anode sludge melting lead 2-base alloy, with enrichment platinum, will extract platinum behind the alloy ash stripping lead again, consumes greatly, and environmental pollution is serious.
" precious metal ", 1992,13 (2), P.30-34 reported a kind of " the high pressure dearsenification of the lead anode slurry of the low gold and silver of high arsenic " technology.This article is a raw material with the low gold and silver lead anode slurry of high arsenic, adopts pressurization to leach dearsenification; Dearsenification slag nitration mixture leaches antimony, bismuth, copper, lead; Leached mud melting, electrolysis get finished product silver; Silver anode slime is carried gold.Leach in the operation in pressurization, this article NaOH digestion (concentration 30-80g/L is good with 50g/L), digestion temperature 110-150 ℃ (150 ℃ is good), and time 2-4 hour (2 hours is good), oxygen is pressed 6kg/cm
2, stagnation pressure 6.8kg/cm
2The arsenic extrusion rate of this article is at 73.4-94.14%, takes off the gold and silver alloy of output purity-99% behind the antimony bismuth copper-lead.This technology purpose is to leach dearsenification, and lead is stayed and soaked in the slag, and this technology needs high-tension apparatus, operates not too safe.
The objective of the invention is to overcome the weak point that prior art exists, provide a kind of from the anode sludge of electrolytic hydrogen peroxide solution production the wet high-effective deleading, reclaim platinum and plumbous method with prior art then.Use the inventive method, environment do not polluted, and consume low, direct output lead bullion, and obtain pure platinum product very soon.
Technical scheme of the present invention is with the NaOH digestion anode sludge, with efficient deleading, uses prior art then and reclaims platinum and lead.
The inventive method comprises with the NaOH digestion anode sludge, it is characterized in that having following concrete operation:
A, at solid-liquid than (be the solid/liquid ratio, unit is g/mL or kg/L)=1: 8-25, in the 100-300g/LNaOH solution, under the temperature 20-95 ℃ of condition, the said anode sludge 1-4 of agitation leach hour;
B, leach liquor be at 1-3V, 100-300A/cm
2The direct current electrodeposition is 6-20 hour under the current density, and output also reclaims lead bullion;
C, electrodeposition mother liquor add 0.1-0.5 times of heavy lime of anode pug or milk of lime, under the 60-95 ℃ of condition, stir the output gypsum deposition and the NaOH that regenerates 1-4 hour:
D, the regeneration NaOH solution that removes gypsum return NaOH digestion operation A through calibrating concentration, after replenishing loss:
E, NaOH digestion slag add H through aqua regia dissolution, after catching up with nitre
2SO
4, be PbSO to precipitate residual lead
4
Solution behind F, the deleading is purified and the pure platinum of output with ordinary method.
In operation A preferential recommend the solid-liquid ratio be 1: 15-20, the concentration of NaOH is 180-200g/L.
Compare with prior art, the present invention has following advantage:
1, the inventive method is free from environmental pollution, obvious social benefit:
2, NaOH can regenerate, so consume low:
3, can attached product lead bullion;
4, device simple, simple to operate:
5, the pure platinum product of very fast acquisition is good in economic efficiency,
Embodiment 1
A kind of anode sludge of electrolytic hydrogen peroxide solution production gained, its main component is: Pb56.87 (weight %), Pt.423.5g/t. get the said anode sludge of 200 grams, at solid-liquid than 1: 15,90 ℃ of following agitation leachs are 2 hours in the 200g/L NaOH solution, filtrate and wash water are under normal temperature (20 ℃), at 3V, 150A/cm
2The direct current electrodeposition is 8 hours under the condition, and output contains the lead bullion of 70%Pb, leached mud slag rate only 4%.
The electrodeposition mother liquor adds 100 gram lime, and 80 ℃ were stirred 2 hours down, and output gypsum, mother liquor return next time through calibrating concentration and after replenishing 7%NaOH and leach, and NaOH digestion slag adds H through aqua regia dissolution, after catching up with nitre
2SO
4, be PbSO to precipitate residual lead
4Solution behind the deleading is purified and the pure platinum of output product purity 99.9%, the rate of recovery 97% of platinum with precipitation ammonium chloroplatinate method.
Embodiment 2
Get the said anode sludge 100 grams of embodiment 1,, obtain 6 gram leached muds in agitation leach 4 hours in 120g/L NaOH 2.5L solution under 23 ℃.The latter adds H through aqua regia dissolution, after catching up with nitre
2SO
4, be PbSO to precipitate residual lead
4, obtain platiniferous solution.The NaOH leached mud is through 23 ℃, and 3V, 100A/cm2 electrodeposition reclaimed plumbous in 15 hours, and the electrodeposition mother liquor adds 20 gram lime, and 80 ℃ were stirred 2 hours down, output gypsum, and regeneration NaOH.Platiniferous solution is purified and the pure platinum of output with precipitation ammonium chloroplatinate method.Product purity 99.9%, the rate of recovery 97% of platinum.
Embodiment 3
The described anode sludge 100 grams of embodiment 1, than 1: 10, agitation leach 4 hours in regenerated NaOH (concentration adds to 2809/L) 1L solution obtains 20 and restrains leached muds under 80 ℃ at solid-liquid.Latter's agitation leach 2 hours in regenerated NaOH (concentration adds to 280g/L) 0.4L solution obtains 10 gram leached muds.The agitation leach 2 hours in regenerated NaOH (concentration adds to 280g/L) 0.4L solution again of this leached mud obtains 4 gram leached muds.Latter's enrichment whole platinum.
Three leach liquors are pressed method electrodeposition recovery lead bullion and the lime regeneration NaOH of embodiment 1.The method of enriched substance embodiment 1 obtains pure platinum product through the aqua regia dissolution platinum of purifying.
Claims (2)
1, a kind of anode sludge from electrolytic hydrogen peroxide solution production reclaims platinum and plumbous method, comprises with the NaOH digestion anode sludge, it is characterized in that having following concrete operation:
A, at the solid-liquid ratio, i.e. solid/liquid ratio, unit is g/mL or kg/L=1: in the 8-25.100-300g/L NaOH solution, under the temperature 20-95 ℃ of condition, the said anode sludge 1-4 of agitation leach hour:
B, leach liquor be at 1-3V, 100-300A/cm
2The direct current electrodeposition is 6-20 hour under the current density, and output also reclaims lead bullion;
C, electrodeposition mother liquor add 0.1-0.5 times of heavy lime of anode pug or milk of lime, under 60～95 ℃ of conditions, stir the output gypsum deposition and the NaOH that regenerates 1-4 hour:
D, the regeneration NaOH solution that removes gypsum return NaOH and leach and boil preface A through calibrating concentration, after replenishing loss;
E, NaOH digestion slag add H through aqua regia dissolution, after catching up with nitre
2SO
4, be PbSO to precipitate residual lead
4
Solution behind F, the deleading is purified and the pure platinum of output with ordinary method.
2, according to the method for claim 1, it is characterized in that the solid-liquid ratio in operation A is 1: the concentration of 15-20.NaOH is 180-200g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96112946A CN1045795C (en) | 1996-09-16 | 1996-09-16 | Method for recovering platinum and lead from anode slime of hydrogen peroxide production by electrolysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96112946A CN1045795C (en) | 1996-09-16 | 1996-09-16 | Method for recovering platinum and lead from anode slime of hydrogen peroxide production by electrolysis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1158904A CN1158904A (en) | 1997-09-10 |
| CN1045795C true CN1045795C (en) | 1999-10-20 |
Family
ID=5121673
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96112946A Expired - Fee Related CN1045795C (en) | 1996-09-16 | 1996-09-16 | Method for recovering platinum and lead from anode slime of hydrogen peroxide production by electrolysis |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1045795C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328398C (en) * | 2004-06-26 | 2007-07-25 | 昆明贵金属研究所 | Method for extracting platinum-palladium and base metal from platinum metal sulphide ore |
| CN102517453A (en) * | 2011-12-09 | 2012-06-27 | 中国航空工业集团公司北京航空材料研究院 | Method for recycling platinum from waste platinum crucibles |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1047888A (en) * | 1989-06-03 | 1990-12-19 | 中国有色金属工业总公司昆明贵金属研究所 | A kind of method of lead anode slurry wet processing |
| CN1057865A (en) * | 1990-06-23 | 1992-01-15 | 中国有色金属工业总公司昆明贵金属研究所 | A kind of solder anode slime nitric acid slag extracts the method for silver and gold |
| CN1058993A (en) * | 1990-08-04 | 1992-02-26 | 中国有色金属工业总公司昆明贵金属研究所 | Method for extracting silver from low-silver-content tin anode mud |
| CN1059938A (en) * | 1990-09-12 | 1992-04-01 | 云南师范大学 | Wet process for preparing silver nitrate from anode mud of electrolytic lead |
| CN1079510A (en) * | 1992-06-02 | 1993-12-15 | 中国有色金属工业总公司昆明贵金属研究所 | Wet processing method for high-arsenic lead anode mud |
-
1996
- 1996-09-16 CN CN96112946A patent/CN1045795C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1047888A (en) * | 1989-06-03 | 1990-12-19 | 中国有色金属工业总公司昆明贵金属研究所 | A kind of method of lead anode slurry wet processing |
| CN1057865A (en) * | 1990-06-23 | 1992-01-15 | 中国有色金属工业总公司昆明贵金属研究所 | A kind of solder anode slime nitric acid slag extracts the method for silver and gold |
| CN1058993A (en) * | 1990-08-04 | 1992-02-26 | 中国有色金属工业总公司昆明贵金属研究所 | Method for extracting silver from low-silver-content tin anode mud |
| CN1059938A (en) * | 1990-09-12 | 1992-04-01 | 云南师范大学 | Wet process for preparing silver nitrate from anode mud of electrolytic lead |
| CN1079510A (en) * | 1992-06-02 | 1993-12-15 | 中国有色金属工业总公司昆明贵金属研究所 | Wet processing method for high-arsenic lead anode mud |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1158904A (en) | 1997-09-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100467631C (en) | Method for recovering gold and copper from gold-plated printed circuit board waste material | |
| WO2019128862A1 (en) | Method for pretreating incineration ash of circuit board and recovering bromine | |
| CN105779770B (en) | Method for recycling valuable metal in waste circuit board | |
| CN106119554A (en) | High Purity Gold the method being enriched with silver, platinum and palladium is prepared from silver anode slime | |
| CN108624759B (en) | Method for comprehensively recovering valuable metals from white smoke | |
| CN107354484A (en) | Method for removing chlorine in zinc electrolysis waste liquid | |
| CN109678196B (en) | Method for fully recycling anions and cations in microetching waste liquid | |
| KR101199513B1 (en) | Valuable metal recovery method from waste solder | |
| CN109468465B (en) | Process for recovering metal copper and nickel salt from waste ABS electroplated part | |
| CN108070722B (en) | Method for recovering valuable metals from copper precipitation slag of silver electrolysis mother liquor | |
| CN103334013A (en) | Novel leaching process of extracting precious metals such as gold, silver and the like from silver separating residues | |
| CN1045795C (en) | Method for recovering platinum and lead from anode slime of hydrogen peroxide production by electrolysis | |
| CN101760624A (en) | Method for extracting gold by using circuit board anode mud | |
| CN113373314B (en) | Method for efficiently recycling scattered metal tellurium from cuprous telluride residues | |
| CN113564622B (en) | Method for efficiently separating copper and tellurium from copper telluride material | |
| JP2005054249A (en) | Method for removing copper from anode slime after copper electrolysis | |
| CN101033505A (en) | Method of leaching valuable metal from anode sludge with high content of antimony, bismuth and copper | |
| CN107326396A (en) | A kind of preparation method of silver electrolyte | |
| CN1045794C (en) | Method for extracting gold, silver and valuable metals from high-arsenic lead anode mud | |
| JP4071041B2 (en) | Regeneration method of copper alloy pickling waste liquid | |
| CN110484747B (en) | Process for selectively extracting palladium from crude silver | |
| CN113604678A (en) | Method for recovering zinc in tin smelting smoke dust through ammonia leaching-extraction process | |
| CN112126791A (en) | Method for recycling high-purity copper from metal waste | |
| CN219342235U (en) | System for recycling lead from scrap copper electrolysis anode slime | |
| CN115044772B (en) | Method for step separation and extraction of zinc, tin, lead and noble metal from electroplating sludge smelting ash |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |