CN1958814A - Method for enriching noble metals from noble antimonial alloy - Google Patents
Method for enriching noble metals from noble antimonial alloy Download PDFInfo
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- CN1958814A CN1958814A CNA2005100325983A CN200510032598A CN1958814A CN 1958814 A CN1958814 A CN 1958814A CN A2005100325983 A CNA2005100325983 A CN A2005100325983A CN 200510032598 A CN200510032598 A CN 200510032598A CN 1958814 A CN1958814 A CN 1958814A
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 229910000510 noble metal Inorganic materials 0.000 title description 10
- 229910045601 alloy Inorganic materials 0.000 title description 4
- 239000000956 alloy Substances 0.000 title description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000002386 leaching Methods 0.000 claims abstract description 28
- 229910001245 Sb alloy Inorganic materials 0.000 claims abstract description 26
- 239000002140 antimony alloy Substances 0.000 claims abstract description 26
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 24
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000011780 sodium chloride Substances 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 239000010970 precious metal Substances 0.000 claims abstract description 9
- 150000002739 metals Chemical class 0.000 claims abstract description 8
- 239000002893 slag Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 230000007062 hydrolysis Effects 0.000 claims description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract description 21
- 239000010931 gold Substances 0.000 abstract description 20
- 229910052737 gold Inorganic materials 0.000 abstract description 16
- 238000011084 recovery Methods 0.000 abstract description 7
- 239000007789 gas Substances 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 3
- 239000000779 smoke Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 229910052787 antimony Inorganic materials 0.000 description 19
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 19
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 14
- 239000011133 lead Substances 0.000 description 12
- 239000010949 copper Substances 0.000 description 9
- 238000003723 Smelting Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 238000005868 electrolysis reaction Methods 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000005272 metallurgy Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 238000000184 acid digestion Methods 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical class [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- KAPYVWKEUSXLKC-UHFFFAOYSA-N [Sb].[Au] Chemical compound [Sb].[Au] KAPYVWKEUSXLKC-UHFFFAOYSA-N 0.000 description 1
- ZVTBWAYGRKISJK-UHFFFAOYSA-N [Sb].[Hg] Chemical compound [Sb].[Hg] ZVTBWAYGRKISJK-UHFFFAOYSA-N 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229940075397 calomel Drugs 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
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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
- 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
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Abstract
一种从贵锑合金中富集贵金属的方法。将贵锑合金粉末、盐酸、氯化钠按一定的配比混合，在一定温度下，控制溶液的电位用过氧化氢进行氧化浸出，反应完毕后，在热态下滤去浸出液，滤渣用盐酸溶液和水洗涤，得到富集了贵金属的粉末产品，浸出液和洗水经还原和水解回收其它有价金属。本发明与传统的贵锑合金火法处理流程比较，有以下优点：可获得金品位在75％以上的粗金粉，可缩短金的生产周期；处理过程金富集在粗金粉中的回收率大于99.95％，不产出含金的中间渣，金的直收率高；浸出过程不产出有害气体和烟尘，提取金属后的废液经处理可排放，有利于环境保护；劳动强度低及综合成本低。A method for enriching precious metals from noble antimony alloys. Mix precious antimony alloy powder, hydrochloric acid, and sodium chloride according to a certain ratio, and at a certain temperature, control the potential of the solution and use hydrogen peroxide for oxidative leaching. After the reaction is completed, filter the leachate in a hot state, and filter the residue with hydrochloric acid The solution and water are washed to obtain a powder product enriched with precious metals, and the leaching solution and washing water are reduced and hydrolyzed to recover other valuable metals. Compared with the traditional noble-antimony alloy pyroprocessing process, the present invention has the following advantages: coarse gold powder with a gold grade of more than 75% can be obtained, and the production cycle of gold can be shortened; the recovery rate of gold enrichment in the coarse gold powder during the treatment process is greater than 99.95%, no intermediate gold-containing slag is produced, and the direct recovery rate of gold is high; no harmful gas and smoke are produced during the leaching process, and the waste liquid after metal extraction can be discharged after treatment, which is conducive to environmental protection; low labor intensity and comprehensive low cost.
Description
The invention relates to a hydrometallurgical process in the field of metallurgy, in particular to a hydrometallurgical method for effectively enriching noble metals from noble antimony alloys.
The prior treatment method of the precious antimony comprises the steps of oxidizing and converting, volatilizing a part of antimony in the form of antimonous oxide to obtain precious antimony alloy (also called the precious antimony) with further enriched precious metals, carrying out antimony electrolysis on the precious antimony alloy, enriching the precious metals, feeding the precious metals into antimony electrolysis anode mud, leaching the anode mud with nitric acid to remove copper, nickel and lead, carrying out crucible furnace smelting on nitric acid leaching slag, and finally carrying out muffle furnace converting to produce crude gold (see ① Beijing nonferrous metal design research institute, general institute, and the like, a heavy nonferrous metals design handbook (antimony mercury precious metals), p 641-646, published by metallurgy industry publishers in 1995, ② Yang Tianzu, and the like, further processing precious metal metallurgy and products, and published by Zhongnan university publishers in p 351-355, 2005).
The treatment method of the precious antimony alloy (rich in precious antimony) has the following disadvantages:
1) when the content of other metals (such as copper, nickel, lead and the like) in the noble antimony alloy is high, the electrolysis of antimony cannot be normally carried out, and noble metals gold and silver are difficult to enter antimony electrolysis anode mud;
2) the process has more returned slag, the crucible furnace smelting and the muffle furnace blowing both produce slag with higher gold content, the slag is added into the relevant smelting process as return materials, and the direct recovery rate of the noble metal is low;
3) the process of enriching the noble metal is alternated between a fire method and a wet method, the process is more, and the mechanical loss of the material containing the noble metal is larger;
4) the process of enriching the noble metals produces more pollutants. Nitric acid digestion produces nitrogen oxide containing tail gas, and smelting and converting process produces smoke containing antimony and lead.
The invention provides a method for enriching noble metals, which can effectively remove impurity metals such as antimony, copper, nickel, lead and the like at one time and basically has no pollution in the process, so as to overcome the defects of the existing noble antimony alloy treatment method.
The technical scheme adopted by the invention for achieving the aim is as follows: mixing the noble antimony alloy powder, hydrochloric acid and sodium chloride according to a certain proportion, controlling the potential of the solution at a certain temperature, carrying out oxidation leaching by using hydrogen peroxide, filtering the leaching solution in a hot state after the reaction is finished, washing filter residues by using a hydrochloric acid solution with a certain concentration and water with a certain temperature to obtain a noble metal-enriched powder product, and recovering other valuable metals by reducing and hydrolyzing the leaching solution and the washing water.
The specific technological process and technological parameters are as follows:
1. leaching out
Crushing and grinding the noble antimony alloy into powder with the particle size of 0.074-0.25 mm, and slurrying with hydrochloric acid and sodium chloride solution. And (3) measuring the potential of the system by using a platinum electrode as a working electrode and a saturated potassium chloride calomel electrode as a reference electrode, and adding hydrogen peroxide under the condition of controlling the end point potential of the system to be 200-450 mV. The leaching temperature is 35-90 ℃, the concentration of hydrochloric acid is 1.5-5.5 mol/L, the concentration of sodium chloride is 0-2 mol/L, the solid-to-liquid ratio (weight ratio) of leaching solution is 3-10: 1, the amount of hydrogen peroxide is 0.7-1.4 times of the weight of the nobleantimony alloy powder, and the reaction time is 2-6 hours.
The chemical reaction that takes place during leaching is:
2. washing machine
And washing leaching residues obtained after leaching reaction for 2-3 times at 70-85 ℃ by using hydrochloric acid with the concentration of 1.5-5.5 mol/L and the weight-liquid-solid ratio of 2-10. After acid washing, washing with 100-200 times of leached residue (weight) and hot water at 70-95 ℃ for 5-10 times. Dissolving lead chloride in leaching residues in hot water:
3. reduction of
Leaching the precious antimony alloy powder to obtain a leaching solution, adding the precious antimony alloy powder with the leaching solution amount of 1-2% (by weight) at the temperature of 40-90 ℃, and reducing for 2-5 hours. The main chemical reactions that take place during the reduction process are:
4. hydrolysis
The leachate reduced by the stibium-rich alloy powder is treated with NH at the temperature of 30-85 DEG C4HCO3、Na2CO3Or NaOH is used for adjusting the pH value to 0-3 for 2-6 hours. Hydrolysis of antimony occurs, the main chemical reaction being:
the hydrochloric acid, sodium chloride, hydrogen peroxide, ammonium bicarbonate, sodium carbonate and sodium hydroxide are all industrial reagents.
The invention is suitable for processing the precious antimony alloy (rich precious antimony) produced by smelting antimony gold concentrate, and the component range is as follows (%): 30-85 parts of Sb, 15-45 parts of Pb, 8-29 parts of Cu, 0-10 parts of Ni, 0.07-3.5 parts of Au, 0.02-0.08 part of Ag, 0.5-5 parts of As0.5 and 0.5-2 parts of Fe; it is also suitable for treating anode mud produced by electrolyzing high-antimony lead.
Compared with the traditional pyrometallurgical treatment process of the noble antimony alloy, the method has the following advantages: 1, controlling the potential of the noble antimony alloy powder in a hydrochloric acid and sodium chloride solution to dissolve metals such as antimony, copper, nickel, lead and the like, and pickling and washing leached residues with hot water to obtain crude gold powder with the gold grade of over 75 percent, so that the processes of electrolysis of the noble antimony alloy, nitric acid digestion of anode mud, crucible furnace smelting and muffle furnace converting are omitted, and the production period of gold is shortened; 2, the recovery rate of gold enriched in the crude gold powder in the treatment process is more than 99.95 percent, no gold-containing intermediate slag is produced, and the direct recovery rate of gold is high; 3, harmful gas and smoke are not produced in the process of leaching out and removing impurity metals such as copper, nickel, antimony, lead and the like, and waste liquid after metal extraction can be discharged after treatment, thereby being beneficial to environmental protection; 4, the labor intensity is low; 5 the invention has low comprehensive cost.
Drawings
FIG. 1: the invention is a process flow diagram.
Detailed Description
Example 1: the noble antimony alloy is ground until the granularity is 100 percent and is less than 0.149mm, and the main components thereof (%) are Sb 46.30, Pb 21.95, Cu 19.62, Ni 3.13, As 0.50, Fe 0.87 and Au 22226.5g/t Ag2840.5g/t; technical grade hydrochloric acid, wherein the HCl concentration (%) is 31.95% (10.14 mol/L); industrial grade sodium chloride with a NaCl content of 91.38%; technical grade hydrogen peroxide, H thereof2O2The content of (B) was 32.3%. Adding 320Lof water into a 1000L enamel reaction kettle, then adding 330L of industrial hydrochloric acid and 50kg of industrial sodium chloride of the components, installing a potential measuring device, starting stirring, heating the reaction kettle to the reaction temperature of 60 ℃, and adding the precious antimony alloy powder of the components. After stirring for 30 minutes, the technical peroxide of the above components is addedWhen the indicated value of the potential was 380mV, the addition of hydrogen peroxide was stopped. Stirring is continued, after 40 minutes, the potential indicated value is 340mV, hydrogen peroxide is added, the potential is adjusted to 380mV, and the temperature is maintained for 1 hour. The amount of hydrogen peroxide used was 91 kg. Discharging the slurry from the reaction kettle under stirring and thermal state, and vacuumizing and filtering by using a plastic filter barrel. After the filtration is finished, the filtrate is transferred into a storage tank while the filtrate is hot. 130L of industrial hydrochloric acid and 170L of water of the components are mixed and heated to 80 ℃, and the hot hydrochloric acid solution is divided into three times to wash leaching residues. And (4) transferring the washed acid to an acid washing storage tank when the acid is hot. 500L of water was heated to 85 ℃ and the leached residue after acid washing was washed 9 times. The washing water is transferred into a washing water storage tank when the washing water is hot. And transferring the leached residues out of the plastic filter barrel, and drying in an oven at the temperature of 150 ℃. The weight of the dried crude gold powder is 3100g, the gold content is 73.90%, and the silver content is 1.92%. The components of the leaching solution are as follows (g/L): sb 64.30, Pb 4.11, Cu 27.32, Ni 5.06, Au 3.10mg/L, Ag190mg/L and the volume of 730L, and the recovery rate of gold is 99.90 percent based on the content of gold in the leachate.
Cooling the leachate in a leachate storage tank to 40 ℃, filtering the precipitated lead chloride, pumping the filtrate into a 1000L enamel reaction kettle, heating to 80 ℃, adding 15kg of the antimony-rich alloy powder, stirring, reacting for 2 hours, cooling to 35 ℃, and filtering. The components of the reduced solution are as follows (g/L): sb 67.90, Pb 4.62, Cu26.08, Ni 5.38, Au 3.15mg/L, Ag 25mg/L, and the silver reduction rate is 89.47%.
Transferring the reduced leachate into 2m3And the pH value of the reaction kettle is adjusted to 2 by adding the industrial sodium carbonate under stirring at normal temperature. Filtering to obtain antimony hydrolysis residue and hydrolyzed solution. The hydrolysis residue (dry) contains 65.68% of antimony and 1.78% of lead. The hydrolyzed solution contains (g/L) Sb 0.30, Pb 2.51, Cu 25.87, Ni5.23 and Ag 11.15mg/L, and the hydrolysis recovery rate of antimony is 99.56 percent based on the antimony content of the hydrolyzed solution.
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| CNB2005100325983A CN100497672C (en) | 2005-12-22 | 2005-12-22 | Method for enriching noble metals from noble antimonial alloy |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660053A (en) * | 2009-09-22 | 2010-03-03 | 中南大学 | Method for recovering tin, antimony and lead and enriching indium from tin residue |
| CN102071324A (en) * | 2011-01-29 | 2011-05-25 | 湖南辰州矿业股份有限公司 | Process for extracting gold from high-grade gold concentrate |
| CN103028483A (en) * | 2013-01-10 | 2013-04-10 | 紫金矿业集团股份有限公司 | Method for preparing high-purity gold-loaded pyrite for experiments |
| CN107447107A (en) * | 2017-08-23 | 2017-12-08 | 中南大学 | A kind of method that rich and honour antimony control current potential is separated and recovered from base metal |
| CN111074303A (en) * | 2020-01-19 | 2020-04-28 | 北京科技大学 | A kind of method for crude antimony residue-free electrolytic separation of antimony and gold |
Families Citing this family (1)
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| CN101928838B (en) * | 2010-09-08 | 2011-12-07 | 中南大学 | Method for removing and recovering arsenic from lead anode slime |
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2005
- 2005-12-22 CN CNB2005100325983A patent/CN100497672C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660053A (en) * | 2009-09-22 | 2010-03-03 | 中南大学 | Method for recovering tin, antimony and lead and enriching indium from tin residue |
| CN102071324A (en) * | 2011-01-29 | 2011-05-25 | 湖南辰州矿业股份有限公司 | Process for extracting gold from high-grade gold concentrate |
| CN102071324B (en) * | 2011-01-29 | 2012-11-28 | 湖南辰州矿业股份有限公司 | Process for extracting gold from high-grade gold concentrate |
| CN103028483A (en) * | 2013-01-10 | 2013-04-10 | 紫金矿业集团股份有限公司 | Method for preparing high-purity gold-loaded pyrite for experiments |
| CN107447107A (en) * | 2017-08-23 | 2017-12-08 | 中南大学 | A kind of method that rich and honour antimony control current potential is separated and recovered from base metal |
| CN107447107B (en) * | 2017-08-23 | 2018-11-09 | 中南大学 | A kind of method that wealth and rank antimony control current potential is separated and recovered from base metal |
| CN111074303A (en) * | 2020-01-19 | 2020-04-28 | 北京科技大学 | A kind of method for crude antimony residue-free electrolytic separation of antimony and gold |
| CN111074303B (en) * | 2020-01-19 | 2021-03-05 | 北京科技大学 | Method for separating antimony and gold by crude antimony non-anode-residue electrolysis |
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Granted publication date: 20090610 |