CN114686693B - Method for recycling ruthenium from ruthenium-containing material - Google Patents
Method for recycling ruthenium from ruthenium-containing material Download PDFInfo
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- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 229910052707 ruthenium Inorganic materials 0.000 title claims abstract description 107
- 239000000463 material Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000004064 recycling Methods 0.000 title description 4
- 239000007788 liquid Substances 0.000 claims abstract description 80
- 238000010521 absorption reaction Methods 0.000 claims abstract description 55
- 239000002253 acid Substances 0.000 claims abstract description 26
- 239000002893 slag Substances 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000004821 distillation Methods 0.000 claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 56
- 239000000243 solution Substances 0.000 claims description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000004090 dissolution Methods 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000007800 oxidant agent Substances 0.000 abstract description 5
- 230000001590 oxidative effect Effects 0.000 abstract description 5
- 238000001556 precipitation Methods 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000005987 sulfurization reaction Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000001035 drying Methods 0.000 description 9
- 238000005086 pumping Methods 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 238000004537 pulping Methods 0.000 description 3
- IHYNKGRWCDKNEG-UHFFFAOYSA-N n-(4-bromophenyl)-2,6-dihydroxybenzamide Chemical compound OC1=CC=CC(O)=C1C(=O)NC1=CC=C(Br)C=C1 IHYNKGRWCDKNEG-UHFFFAOYSA-N 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/12—Dry methods smelting of sulfides or formation of mattes by gases
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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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- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a method for recovering ruthenium from ruthenium-containing materials, which comprises slurrying the ruthenium-containing materials to form feed liquid, distilling under the action of strong oxidant, absorbing by acid absorption liquid to obtain primary ruthenium absorption liquid, adjusting acidity of the primary ruthenium absorption liquid, adding sodium hydrosulfide solution to precipitate to obtain ruthenium slag, adding oxidant to raise temperature to carry out secondary distillation after dissolving the ruthenium slag, absorbing by acid absorption liquid to obtain secondary ruthenium absorption liquid, concentrating and crystallizing the secondary ruthenium absorption liquid to obtain RuCl 3 ,RuCl 3 The ruthenium black is obtained through calcination and hydrogen reduction, and the ruthenium black is washed and dried to obtain the ruthenium powder product. According to the invention, the sodium hydrosulfide solution is added, so that the sulfuration and precipitation time is greatly shortened, and the production efficiency and the metal yield are improved; the ruthenium is completely vulcanized and precipitated, and the purity of the obtained ruthenium powder is more than 99.95 percent; the process is rapid to operate, the labor intensity is low, the operation efficiency is high, and the production cost is low.
Description
Technical Field
The invention belongs to the technical field of wet treatment of ruthenium-rich materials, and particularly relates to a method for recycling ruthenium from ruthenium-containing materials.
Background
At present, the wet treatment is mainly adopted in China to recycle ruthenium in ruthenium-containing materials, and the main process is that firstly, a strong oxidant is added into the slurried ruthenium-containing materials to oxidize ruthenium in feed liquid into RuO 4 Volatilizing from the feed liquid at high temperature, and absorbing by acid absorption liquid in the absorption device to obtain primary ruthenium absorption liquid. Adding Na into the primary ruthenium absorption liquid after adjusting acidity 2 S is precipitated, selective distillation process is adopted to carry out secondary oxidation distillation, and ruthenium secondary absorption liquid is concentrated and crystallized to obtain RuCl 3 ,RuCl 3 Calcining according to a set program, reducing with hydrogen to obtain ruthenium black, washing the ruthenium black to be neutral with pure water, and drying in a tube furnace to obtain the ruthenium powder product. However, na is utilized in the process 2 The S precipitation method has low precipitation efficiency, restricts the production operation efficiency, influences the yield index, and is particularly important to develop a method for efficiently recovering ruthenium from ruthenium-containing materials in order to solve the problem.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for efficiently recycling ruthenium from ruthenium-containing materials, which improves the precipitation efficiency and yield index of ruthenium, and has the advantages of rapid operation, high operation efficiency, low labor intensity and low production cost.
The invention aims at realizing the following technical scheme:
a process for recovering ruthenium from ruthenium-containing material includes slurrying the ruthenium-containing material to obtain feed liquid, distilling under the action of strong oxidant, absorbing by acid absorption liquid to obtain primary ruthenium absorption liquid, regulating acidity of primary ruthenium absorption liquid, adding sodium hydrosulfide solution, depositing to obtain ruthenium slag, dissolving ruthenium slag, adding oxidant, heating for secondary distillation, absorbing by acid absorption liquid to obtain secondary ruthenium absorption liquid, concentrating and crystallizing to obtain RuCl 3 ,RuCl 3 The ruthenium black is obtained through calcination and hydrogen reduction, and is washed and dried to obtain the ruthenium powder product, which specifically comprises the following steps:
(1) Slurrying a ruthenium-containing material with sulfuric acid to form a feed liquid, adding a sodium chlorate solution, distilling at 90-95 ℃, and absorbing with an acid absorption liquid to obtain a primary ruthenium absorption liquid; the solid-to-liquid ratio of ruthenium-containing mineral to sulfuric acid was 1g: 5-6 mL.
(2) Adjusting the pH value of the primary ruthenium absorption liquid to 5-6, adding sodium hydrosulfide solution until the pH value reaches 7-8, and precipitating after the reaction is finished to obtain ruthenium slag;
(3) Adding sulfuric acid into ruthenium slag for dissolution, controlling the solid-to-liquid ratio to be 1 g:4-5 mL, and adding sodium chlorate for dissolutionHeating the solution to 90-95 ℃ for secondary distillation, absorbing by an acid absorption solution to obtain a secondary ruthenium absorption solution, concentrating and crystallizing the secondary ruthenium absorption solution to obtain RuCl 3 ,RuCl 3 The ruthenium black is obtained through calcination and hydrogen reduction, the ruthenium black is washed to be neutral by pure water, and the ruthenium powder is obtained after drying.
In the steps (1) and (3), the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2%.
In the steps (1) and (3), the mass fraction of the sodium chlorate solution is 35%; the rate of addition of the sodium chlorate solution was 2L/h. The invention has the following advantages:
(1) The sodium hydrosulfide solution is added to greatly shorten the sulfuration and precipitation time and improve the production efficiency and the metal yield;
(2) The ruthenium is completely vulcanized and precipitated, and the purity of the obtained ruthenium powder is more than 99.95 percent;
(3) The invention has the advantages of rapid process operation, low labor intensity, high operation efficiency and low production cost.
Drawings
FIG. 1 is a schematic process flow diagram of a method for recovering ruthenium from ruthenium-containing materials.
Detailed Description
The invention is further illustrated by the following examples:
example 1
(1) Ruthenium-containing material was admixed with sulfuric acid in an amount of 1g: pulping 5-6 mL of solid-liquid ratio to form feed liquid, adding 35% sodium chlorate solution at a rate of 2L/h, distilling at a high temperature of 93 ℃, and absorbing by acid absorption liquid to obtain primary ruthenium absorption liquid; wherein the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2%.
(2) And (3) pumping the primary ruthenium absorption liquid into a 500L kettle, heating and concentrating, adding sodium bisulfide solution after the pH value of the ruthenium absorption liquid is regulated to be 5-6, precipitating to obtain ruthenium slag when the adding amount of the sodium bisulfide solution is up to 7-8, and washing and drying by pure water.
(3) Adding proper amount of sulfuric acid into ruthenium slag for dissolution, controlling the solid-to-liquid ratio to be 1 g:4-5 mL, adding sodium chlorate solution with the mass fraction of 35% at the rate of 2L/h, heating to 91 ℃ for secondary distillation, absorbing by acid absorption liquid to obtain secondary ruthenium absorption liquid, concentrating the secondary ruthenium absorption liquid, adding pure water for dilution, concentrating for acid removal, drying and crystallizing to obtain RuCl 3 ,RuCl 3 The ruthenium black is obtained through calcination and hydrogen reduction, the ruthenium black is washed by pure water until the pH value is=6.5, and the ruthenium powder is obtained after drying in a tube furnace, wherein the purity of the ruthenium powder is more than 99.96%. Wherein the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2%.
Example 2
(1) Ruthenium-containing material was admixed with sulfuric acid in an amount of 1g: pulping 5-6 mL of solid-liquid ratio to form feed liquid, adding 35% sodium chlorate solution at a rate of 2L/h, distilling at a high temperature of 94 ℃, and absorbing by acid absorption liquid to obtain primary ruthenium absorption liquid; wherein the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2%.
(2) And (3) pumping the primary ruthenium absorption liquid into a 500L kettle, heating and concentrating, adjusting the pH value of the ruthenium concentrated liquid to be 5-6, adding sodium hydrosulfide solution, precipitating to obtain ruthenium slag, and washing and pumping the ruthenium slag by pure water until the reaction pH value reaches 7-8.
(3) Adding proper amount of sulfuric acid into ruthenium slag for dissolution, controlling the solid-to-liquid ratio to be 1 g:4-5 mL, adding 35% sodium chlorate at the mass fraction of 2L/h, heating to 92 ℃ for secondary distillation, absorbing by an acid absorption liquid to obtain a secondary ruthenium absorption liquid, concentrating the secondary ruthenium absorption liquid, adding pure water for dilution, concentrating for acid removal, drying and crystallizing to obtain RuCl 3 ,RuCl 3 The ruthenium black is obtained through calcination and hydrogen reduction, the ruthenium black is washed by pure water until the pH value is=6, and the ruthenium powder is obtained after drying in a tube furnace, wherein the purity of the ruthenium powder is more than 99.95%. Wherein the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the hydrochloric acid solution isThe mass fraction of HCl is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2%.
Example 3
(1) Ruthenium-containing material was admixed with sulfuric acid in an amount of 1g: pulping 5-6 mL of solid-liquid ratio to form feed liquid, adding 35% sodium chlorate solution at a rate of 2L/h, distilling at a high temperature of 92 ℃, and absorbing by acid absorption liquid to obtain primary ruthenium absorption liquid; wherein the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2%.
(2) And (3) pumping the primary ruthenium absorption liquid into a 500L kettle, heating and concentrating, adjusting the pH value of the ruthenium concentrated liquid to be 5-6, adding sodium hydrosulfide solution, precipitating to obtain ruthenium slag, and washing and pumping the ruthenium slag by pure water until the reaction pH value reaches 7-8.
(3) Adding proper amount of sulfuric acid into ruthenium slag for dissolution, controlling the solid-to-liquid ratio to be 1 g:4-5 mL, adding sodium chlorate solution with the mass fraction of 35% at the rate of 2L/h, heating to 93 ℃ for secondary distillation, absorbing by acid absorption liquid to obtain secondary ruthenium absorption liquid, concentrating the secondary ruthenium absorption liquid, adding pure water for dilution, concentrating for acid removal, drying and crystallizing to obtain RuCl 3 ,RuCl 3 The ruthenium black is obtained through calcination and hydrogen reduction, the ruthenium black is washed by pure water until the pH value is=7, and the ruthenium powder is obtained after drying in a tube furnace, wherein the purity of the ruthenium powder is more than 99.97%. Wherein the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2%.
The embodiment is successfully applied to the recovery of ruthenium in ruthenium-containing materials, and ruthenium powder with the purity of more than 99.95% is produced, and meets the quality standard YS/T682-2008 of the ruthenium powder industry.
Claims (4)
1. A process for recovering ruthenium from a ruthenium-containing material comprising the steps of:
(1) Slurrying a ruthenium-containing material with sulfuric acid to form a feed liquid, adding a sodium chlorate solution, distilling at 90-95 ℃, and absorbing with an acid absorption liquid to obtain a primary ruthenium absorption liquid;
(2) Adjusting the pH value of the primary ruthenium absorption liquid to 5-6, adding sodium hydrosulfide solution until the pH value reaches 7-8, and precipitating after the reaction is finished to obtain ruthenium slag;
(3) Adding sulfuric acid into ruthenium slag for dissolution, controlling the solid-to-liquid ratio to be 1 g:4-5 mL, adding sodium chlorate solution, heating to 90-95 ℃ for secondary distillation, absorbing by acid absorption liquid to obtain secondary ruthenium absorption liquid, concentrating and crystallizing the secondary ruthenium absorption liquid to obtain RuCl 3 ,RuCl 3 The ruthenium black is obtained through calcination and hydrogen reduction, and the ruthenium black is washed and dried to obtain the ruthenium powder product.
2. A process for recovering ruthenium from a ruthenium-containing material according to claim 1 wherein: in the step (1), the solid-to-liquid ratio of the ruthenium-containing mineral to sulfuric acid is 1 g:5-6 mL.
3. A process for recovering ruthenium from a ruthenium-containing material according to claim 1 wherein: in the steps (1) and (3), the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2%.
4. A process for recovering ruthenium from a ruthenium-containing material according to claim 1 wherein: in the steps (1) and (3), the mass fraction of the sodium chlorate solution is 35%; the rate of addition of the sodium chlorate solution was 2L/h.
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CN101797649A (en) * | 2010-01-19 | 2010-08-11 | 兰州大学 | Method and device for preparing high-purity ruthenium |
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CN205205206U (en) * | 2015-11-18 | 2016-05-04 | 金川集团股份有限公司 | Novel device of ruthenium is drawed in distillation |
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- 2022-03-10 CN CN202210234662.XA patent/CN114686693B/en active Active
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CN101797649A (en) * | 2010-01-19 | 2010-08-11 | 兰州大学 | Method and device for preparing high-purity ruthenium |
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JP2013112857A (en) * | 2011-11-29 | 2013-06-10 | Jx Nippon Mining & Metals Corp | Method of recovering iridium |
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CN109055738A (en) * | 2018-08-27 | 2018-12-21 | 浙江特力再生资源有限公司 | Noble metal recoverying and utilizing method in a kind of osmium iridium ruthenium mine |
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Title |
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Effective date of registration: 20240508 Address after: 737199 No. 2 Jianshe Road, Jinchuan District, Jinchang City, Gansu Province (east of Beijing Road, west of Heya Road, south of Guiyang Road) Patentee after: Jinchuan Group Copper Gui Co.,Ltd. Country or region after: China Address before: No.98, Jinchuan Road, Jinchuan District, Jinchang City, Gansu Province 737100 Patentee before: JINCHUAN GROUP Co.,Ltd. Country or region before: China |