CN114751839A - Method for circularly regenerating EDTA (ethylene diamine tetraacetic acid) from copper anode slime pressurizing decoppering material EDTA deleading liquid - Google Patents
Method for circularly regenerating EDTA (ethylene diamine tetraacetic acid) from copper anode slime pressurizing decoppering material EDTA deleading liquid Download PDFInfo
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- CN114751839A CN114751839A CN202210232696.5A CN202210232696A CN114751839A CN 114751839 A CN114751839 A CN 114751839A CN 202210232696 A CN202210232696 A CN 202210232696A CN 114751839 A CN114751839 A CN 114751839A
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- edta
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- deleading
- decoppering
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- 229960001484 edetic acid Drugs 0.000 title claims abstract description 56
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 28
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 24
- 239000010949 copper Substances 0.000 title claims abstract description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 23
- 239000007788 liquid Substances 0.000 title claims abstract description 21
- 230000001172 regenerating effect Effects 0.000 title claims abstract description 5
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 12
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 11
- 230000008929 regeneration Effects 0.000 claims abstract description 10
- 238000011069 regeneration method Methods 0.000 claims abstract description 10
- 238000004064 recycling Methods 0.000 claims abstract description 8
- 125000004122 cyclic group Chemical group 0.000 claims abstract description 4
- 238000001556 precipitation Methods 0.000 claims description 22
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 16
- 239000006228 supernatant Substances 0.000 claims description 16
- 239000012141 concentrate Substances 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 6
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 230000001502 supplementing effect Effects 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 8
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 7
- 239000002253 acid Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000000956 alloy Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
-
- 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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for circularly regenerating EDTA (ethylene diamine tetraacetic acid) from EDTA deleading liquid of a copper anode slime pressurizing decoppering material, which is realized by regeneration of the EDTA and deacidification of the EDTA circulating liquid. The regeneration of EDTA uses gaseous hydrogen sulfide, and the EDTA quality of regeneration is better, adopts barium carbonate to the circulation EDTA solution many times remove the acid, and other impurity elements can not be introduced to this process. The method has simple process and convenient operation, and can effectively realize the recycling of EDTA. The method has the advantages of short flow, simple operation, no other impurity elements, low energy consumption, realization of cyclic utilization of reagents and the like; the recycling of EDTA in the whole process reduces the deleading cost by at least 1/5.
Description
Technical Field
The invention relates to a method for recycling a copper anode slime pressurizing decoppering material deleading reagent, which is mainly applied to the fields of smelting of other rare and noble metals such as nickel, copper, silver, selenium, tellurium and the like and the chemical industry.
Background
The copper anode mud is mud-shaped matter attached to the surface of an anode matrix or precipitated at the bottom of an electrolytic bath or suspended in an electrolyte in copper electrolytic refining. The copper anode slime is rich in most of precious metals and some rare elements in ores, concentrates or fluxes, so that the copper anode slime has high comprehensive recovery value. Usually, the copper anode slime mainly contains impurity elements such as Cu, Pb, Bi, and Te. At present, the domestic copper anode slime treatment process is pressure leaching, a leaching reagent is sulfuric acid, and only most of impurity elements such as Cu, Te and the like can be leached. The slag rate in the pressurizing process is about 65% on average, and Pb is basically left in the pressurized slag. The lead content is too high, so that the alloy production period is longer, and the precious metal content in smelting slag and blowing slag is high. Therefore, further impurity removal is required for the pressurized decoppering material. The common impurity removal process comprises Pb removal and Bi removal, wherein the lead removal process comprises two process routes, namely, the lead removal is carried out by using acetic acid after sodium carbonate is modified, and the lead removal is carried out by using EDTA. When EDTA is adopted to delead the pressurized copper-removing material, the deleading efficiency is high, but the reagent is very expensive, which directly causes higher production cost.
Disclosure of Invention
In view of the above situation, the present invention aims to provide a method for recycling EDTA in EDTA deleading solution for copper anode slime pressure decoppering, aiming at the problem of high EDTA deleading cost.
The technical scheme adopted by the invention is as follows:
a method for circularly regenerating EDTA from a copper anode slime pressurizing decoppering material EDTA deleading liquid comprises the following steps:
(1) introducing hydrogen sulfide gas into anode slime pressurized decoppering material EDTA (ethylene diamine tetraacetic acid) deleading liquid for lead precipitation, wherein the flow rate of the hydrogen sulfide gas is 1-1.2L/min, the temperature is controlled at 20-50 ℃, the reaction time is 1.5-3 h, taking supernatant after the reaction is finished, adding sodium sulfide into the supernatant until no black precipitate is generated, and filtering to obtain lead concentrate and lead precipitation liquid;
(2) supplementing 150g/L of EDTA solution into the solution obtained in the step (1) after lead precipitation according to the solid-to-liquid ratio of 0.2-0.3 t:1m3Adding anode slime to pressurize the decoppering material to continuously perform deleading to obtain a deleading material and a deleading solution;
(3) continuously introducing hydrogen sulfide gas into the deleading solution obtained in the step (2) to precipitate lead, wherein the flow rate of the hydrogen sulfide gas is 1-1.2L/min, the temperature is controlled at 20-50 ℃, the reaction time is 1.5-3 h, taking supernatant after the reaction is finished, adding sodium sulfide into the supernatant until no black precipitate is generated, and filtering to obtain lead concentrate and lead precipitation solution;
(4) repeating the steps (1) to (3) until H in the obtained lead precipitation liquid+After the concentration reaches 80-120 g/L, the solution after lead precipitation is 80-85 kg of solution to 1m according to the solid-to-liquid ratio3Adding barium carbonate, controlling the temperature at 30-40 ℃, reacting for 2-3 h, taking supernatant, adding barium carbonate solid until no bubbles are generated, and filtering to obtain barium sulfate and deacidified lead precipitation liquid;
(5) and (4) continuously carrying out pressure decoppering on the solution after the lead precipitation after deacidification according to the step (1) to precipitate the lead, thereby realizing EDTA (ethylene diamine tetraacetic acid) cyclic regeneration.
The invention has the beneficial effects that:
the method is realized by regeneration of EDTA and deacidification of EDTA circulating liquid. The regeneration of EDTA uses gaseous hydrogen sulfide, and the EDTA quality of regeneration is better, adopts barium carbonate to remove acid to the EDTA solution of circulation many times, and other impurity elements can not be introduced to this process. The method has simple process and convenient operation, and can effectively realize the recycling of EDTA. The method has the advantages of short flow, simple operation, no other impurity elements, low energy consumption, realization of cyclic utilization of reagents and the like; the recycling of EDTA in the whole process reduces the deleading cost by at least 1/5.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
(1) To 20m3Pumping 10m into the steel-titanium composite kettle3Heating the EDTA deleading solution (lead concentration is 40 g/L), introducing hydrogen sulfide gas at the flow rate of 1-1.2L/min, reacting for 1.5h, taking the supernatant after the reaction, adding sodium sulfide into the supernatant until no black precipitate is generated, filtering to obtain 396kg of lead concentrate, and precipitating with lead solution 9.89m3;
(2) 150g/L of EDTA solution is added into the lead precipitation solution, and the volume is added to 10m3Then 2.5t (dry weight) of copper anode mud is added to pressurize the copper removing material for lead removal, and 2.02t of lead removing material is produced and delivered to an alloy converting furnace for producing the duoer alloy.
(3) 9.9m of deleading liquid (39.5 g/L) produced in the step (2)3The treatment is carried out according to the step (1), 372kg of lead concentrate is produced, and 9.62m of lead deposition liquid is produced3After 6 times of deleading, 2.59t of lead concentrate and 11.78t of deleading material are produced, and the volume of the solution after lead precipitation is 9.68m3,H+The concentration reaches 86 g/L;
(4) heating the solution after lead precipitation produced in the step (3) to 30 ℃, adding 800kg of barium carbonate, reacting for 2 hours, taking the supernatant, adding barium carbonate solid until no bubbles are produced, and filtering;
(5) drying the barium sulfate obtained in the step (4), producing 826kg of barium sulfate, externally feeding the barium sulfate to a copper smelting workshop, wherein the volume of the EDTA solution after deacidification is 9.22m3And (3) after a small amount of EDTA solution is supplemented, the step (1) is repeated to continuously perform pressurization decoppering and deleading of the copper material, so that EDTA cyclic regeneration is realized.
The cost of the reagent for removing lead by adopting the method is reduced to 83 yuan/t from 565 yuan/t according to the weight of the produced product.
Example 2
(1) To 20m3Pumping 10m into the steel-titanium composite kettle3Heating the EDTA deleading solution (lead concentration is 43 g/L) to 45 ℃, introducing hydrogen sulfide gas at the flow rate of 1-1.2L/min, reacting for 2h, taking the supernatant after the reaction is finished, adding sodium sulfide into the supernatant until no black precipitate is generated, filtering,399.5kg of lead concentrate is co-produced, and 9.72m of lead precipitation liquid3;
(2) 150g/L of EDTA solution is added into the lead precipitation solution, and the volume is added to 10m3Adding 2.5t (dry weight) of copper anode mud into the lead precipitation solution, pressurizing and deleading to produce 1.98t of deleading material, and delivering to an alloy converting furnace to produce the duoer alloy.
(3) 9.6m of deleading liquid (40.12 g/L) produced in the step (2)3The treatment is carried out according to the step (1), 395kg of lead concentrate is produced, and 9.76m of lead precipitation liquid is produced3After 5 times of deleading, 2.68t of lead concentrate is produced, 10.92t of deleading material is produced, and the volume of the solution after lead precipitation is 9.71m3,H+The concentration reaches 91 g/L;
(4) heating the solution after lead precipitation, which is produced in the step (3), to 30 ℃, adding 820kg of barium carbonate, reacting for 3 hours, taking the supernatant, adding barium carbonate solid until no bubbles are produced, and filtering;
(5) drying the barium sulfate obtained in the step (4), producing 855kg of barium sulfate, externally feeding the barium sulfate to a copper smelting workshop, and enabling the volume of the EDTA solution after deacidification to be 9.36m3And (3) after a small amount of EDTA solution is supplemented, the step (1) is repeated to continuously perform pressurization decoppering and deleading of the copper material, so that EDTA cyclic regeneration is realized.
The cost of the reagent for removing lead by adopting the method is reduced to 102 yuan/t from 565 yuan/t according to the weight of the produced product.
Claims (3)
1. A method for circularly regenerating EDTA from a copper anode slime pressurizing decoppering material EDTA deleading liquid comprises the following steps:
(1) introducing hydrogen sulfide gas into the anode slime pressurizing decoppering material EDTA deleading solution to precipitate lead, controlling the temperature at 20-50 ℃, reacting for 1.5-3 h, taking supernatant after the reaction is finished, adding sodium sulfide into the supernatant until no black precipitate is generated, and filtering to obtain lead concentrate and lead-precipitated solution;
(2) supplementing an EDTA solution into the solution obtained in the step (1) after lead precipitation, adding anode slime to pressurize a decoppering material, and continuously performing deleading to obtain a deleading material and a deleading solution;
(3) continuously introducing hydrogen sulfide gas into the deleading solution obtained in the step (2) to precipitate lead, controlling the temperature at 20-50 ℃, reacting for 1.5-3 h, taking supernatant after the reaction is finished, adding sodium sulfide into the supernatant until no black precipitate is generated, and filtering to obtain lead concentrate and lead-precipitated solution;
(4) repeating the steps (1) to (3) until H in the obtained lead precipitation liquid+After the concentration reaches 80-120 g/L, the solution after lead precipitation is 80-85 kg of solution to 1m according to the solid-to-liquid ratio3Adding barium carbonate, controlling the temperature at 30-40 ℃, reacting for 2-3 hours, taking supernatant, adding barium carbonate solid until no bubbles are generated, and filtering to obtain barium sulfate and deacidified lead precipitation liquid;
(5) and (4) continuously carrying out pressure decoppering on the solution after the lead precipitation after deacidification according to the step (1) to precipitate the lead, thereby realizing EDTA (ethylene diamine tetraacetic acid) cyclic regeneration.
2. The method for recycling EDTA from the copper anode slime pressure decoppering material EDTA deleading solution according to claim 1, characterized in that: in the steps (1) and (3), the flow rate of the hydrogen sulfide gas is 1-1.2L/min.
3. The method for recycling EDTA from the copper anode slime pressure decoppering material EDTA deleading solution according to claim 1, characterized in that: in the step (2), the concentration of the EDTA solution is 150 g/L.
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CN202210232696.5A CN114751839A (en) | 2022-03-10 | 2022-03-10 | Method for circularly regenerating EDTA (ethylene diamine tetraacetic acid) from copper anode slime pressurizing decoppering material EDTA deleading liquid |
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CN202210232696.5A CN114751839A (en) | 2022-03-10 | 2022-03-10 | Method for circularly regenerating EDTA (ethylene diamine tetraacetic acid) from copper anode slime pressurizing decoppering material EDTA deleading liquid |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB824275A (en) * | 1955-01-20 | 1959-11-25 | Dow Chemical Co | Improvements in and relating to the recovery of complexing agents from spent solutions |
CN102586584A (en) * | 2012-04-01 | 2012-07-18 | 大冶有色金属有限责任公司 | Method for selectively separating valuable metals from complex lead-containing precious metal material |
CN105907986A (en) * | 2016-06-29 | 2016-08-31 | 江西铜业集团公司 | Extracting method for lead in silver separating residues |
CN113401995A (en) * | 2021-05-27 | 2021-09-17 | 南方环境有限公司 | Method for treating and recycling heavy metal contaminated soil leaching waste liquid |
-
2022
- 2022-03-10 CN CN202210232696.5A patent/CN114751839A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB824275A (en) * | 1955-01-20 | 1959-11-25 | Dow Chemical Co | Improvements in and relating to the recovery of complexing agents from spent solutions |
CN102586584A (en) * | 2012-04-01 | 2012-07-18 | 大冶有色金属有限责任公司 | Method for selectively separating valuable metals from complex lead-containing precious metal material |
CN105907986A (en) * | 2016-06-29 | 2016-08-31 | 江西铜业集团公司 | Extracting method for lead in silver separating residues |
CN113401995A (en) * | 2021-05-27 | 2021-09-17 | 南方环境有限公司 | Method for treating and recycling heavy metal contaminated soil leaching waste liquid |
Non-Patent Citations (1)
Title |
---|
雷鸣 等: ""EDTA及其回收溶液治理重金属污染土壤的研究"", 环境工程学报, vol. 1, no. 5, 31 May 2007 (2007-05-31), pages 88 - 93 * |
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