CN115369416A - Method for separating and recovering tellurium and copper from copper telluride slag - Google Patents

Method for separating and recovering tellurium and copper from copper telluride slag Download PDF

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Publication number
CN115369416A
CN115369416A CN202210900727.XA CN202210900727A CN115369416A CN 115369416 A CN115369416 A CN 115369416A CN 202210900727 A CN202210900727 A CN 202210900727A CN 115369416 A CN115369416 A CN 115369416A
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China
Prior art keywords
copper
slag
leaching
tellurium
roasting
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CN202210900727.XA
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Chinese (zh)
Inventor
解滢涛
吴艳新
夏胜文
刘腾腾
王拥军
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Jiyuan Yuguang Nonferrous Metallurgy Design And Research Institute Co ltd
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Jiyuan Yuguang Nonferrous Metallurgy Design And Research Institute Co ltd
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Priority to CN202210900727.XA priority Critical patent/CN115369416A/en
Publication of CN115369416A publication Critical patent/CN115369416A/en
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • C25B1/01Products
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/02Roasting processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00Obtaining copper
    • C22B15/0002Preliminary treatment
    • C22B15/001Preliminary treatment with modification of the copper constituent
    • C22B15/0013Preliminary treatment with modification of the copper constituent by roasting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00Obtaining copper
    • C22B15/0063Hydrometallurgy
    • C22B15/0065Leaching or slurrying
    • C22B15/0082Leaching or slurrying with water
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • C25B1/50Processes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses a method for separating and recovering tellurium and copper from copper telluride slag. Firstly, crushing copper telluride slag, adding sodium hydroxide into a copper telluride slag material obtained after crushing, then heating and roasting to obtain primary roasting slag; cooling the obtained primary roasting slag to room temperature, adding the primary roasting slag into a ball mill for ball milling, and leaching the materials obtained after ball milling to obtain leaching solution and leaching slag; the leaching solution, namely the sodium tellurate solution, is treated by an electrodeposition process to obtain metal tellurium, and leaching residues enter a copper residue recycling process for utilization. According to the technical scheme, the copper telluride slag is cooperatively treated by a pyrogenic method and a wet method, and is treated by the roasting furnace, so that the treatment capacity is greatly improved.

Description

Method for separating and recovering tellurium and copper from copper telluride slag
1. The technical field is as follows:
the invention relates to the field of chemistry and metallurgy, in particular to a method for separating and recovering tellurium and copper from copper telluride residues.
2. Background art:
the copper telluride slag (or the copper tellurium slag) is a byproduct generated in the process of extracting noble metals from copper smelting anode mud, has excellent tellurium performance, can be used as a main material of an alloy additive, a semiconductor, a refrigeration element and an optical element, and is widely applied to the fields of metallurgy, petroleum, chemical engineering, aerospace, electronics and the like; copper is widely used in the fields of electrical industry, light industry, mechanical manufacturing, building industry, national defense industry and the like. At present, because the smelting industry generates a large amount of copper telluride slag every year, the development of a more effective method for treating the copper telluride slag is the focus of research at present.
In the prior art, methods for separating tellurium and copper from copper telluride slag include sulfation roasting process, alkaline oxidation pressure leaching process, reduction process after acidic oxidation leaching, extraction and other processes.
Nonferrous metals (metallurgy part) 2017, 8 th publication of a research on recovery method by sulfating roasting-water leaching decoppering-alkali leaching tellurium-electrodeposition process, and researches on hardness of tellurium leaching by NaOH concentration and temperature and hydrolysis impurity removal and tellurium electrodeposition process.
In addition, some patent documents report about the copper telluride slag treatment technology. For example: 1. the invention patent application CN201410698581.0 discloses a method for extracting tellurium and copper from copper telluride residues, which comprises the steps of mixing the copper telluride residues with hydrogen peroxide and sulfuric acid for oxidation leaching to obtain a leaching solution, mixing the leaching solution with an oxalic acid copper removing agent for reaction to obtain copper oxalate and oxalic acid copper removing liquid, and reducing the oxalic acid copper removing liquid by using sodium sulfite or sulfur dioxide gas to obtain tellurium. 2. The invention patent application CN 201811014619.2 discloses a method for extracting tellurium from copper telluride or copper tellurium slag, which comprises the steps of mixing copper telluride slag and a vulcanizing agent according to a certain proportion, carrying out a vulcanization reaction to obtain a vulcanization product mixed by elemental tellurium and a copper sulfide substance, placing the vulcanization product in a vacuum furnace for vacuum distillation, and separating tellurium from the mixture to obtain elemental tellurium and copper sulfide slag. 3. The invention patent application CN104928483A discloses a method for comprehensively recovering silver, arsenic, tellurium and copper from copper telluride residues.
3. The invention content is as follows:
the technical problem to be solved by the invention is as follows: according to the development state of the existing treatment technology of the copper telluride slag, in order to better separate and recover tellurium and copper in the copper telluride slag and find a process more suitable for the operation of industrial large-scale equipment, the invention provides a method for treating the copper telluride slag to recover tellurium and copper by adopting a fire method and a wet method, namely the invention provides a novel method for separating and recovering tellurium and copper from the copper telluride slag.
In order to solve the problems, the invention adopts the technical scheme that:
the invention provides a method for separating and recovering tellurium and copper from copper telluride residues, which comprises the following steps:
a. firstly, putting copper telluride slag into a jaw crusher for crushing until the granularity of the material is 3-5 mm;
b. b, adding sodium hydroxide into the copper telluride slag material obtained after crushing in the step a, and then putting the copper telluride slag material into a roasting furnace for primary roasting at the roasting temperature of 600-650 ℃ for 1-2 hours to obtain primary roasting slag;
c. cooling the primary roasting slag obtained in the step b to room temperature, adding the primary roasting slag into a ball mill for ball milling, and adding water into the materials obtained after ball milling for water leaching to obtain leaching solution and leaching slag;
d. and treating the sodium tellurate solution through an electrodeposition process to obtain metal tellurium, and recycling leaching residues in a copper residue recycling process.
According to the method for separating and recovering tellurium and copper from copper telluride slag, the adding amount of the sodium hydroxide in the step b is 1-1.2 times of the molar weight of the reaction theoretical value of the crushed copper telluride slag material.
According to the method for separating and recovering tellurium and copper from copper telluride residues, the granularity of the ball-milled materials in the step c is 1-1.5 mm.
According to the method for separating and recovering tellurium and copper from copper telluride slag, in the water leaching process in the step c, the adding amount mass ratio of water to the ball-milled materials is 5-7: 1.
according to the method for separating and recovering tellurium and copper from copper telluride slag, in the step c, the leaching time is 2-3 h in the water leaching process, and the leaching temperature is 50-70 ℃.
The invention has the following positive beneficial effects:
1. according to the technical scheme, the copper telluride slag is cooperatively treated by a pyrogenic method and a wet method, and the roasting furnace is used for treatment, so that the treatment capacity of the copper telluride slag is greatly improved.
2. According to the technical scheme, alkali roasting is adopted, water leaching is carried out, the purity of the obtained leaching residue copper can reach 98%, and the leaching solution is subjected to the existing electrodeposition process, so that tellurium metal is obtained, and the purpose of separating copper and tellurium is achieved.
4. Description of the drawings:
FIG. 1 is a schematic flow diagram of a method for separating and recovering tellurium and copper from copper telluride residues.
5. The specific implementation mode is as follows:
the invention is further illustrated by the following examples, which do not limit the scope of the invention.
Example 1:
the invention relates to a method for separating and recovering tellurium and copper from copper telluride residues, which comprises the following detailed steps:
a. firstly, 50g of copper telluride slag is put into a jaw crusher to be crushed until the granularity of the material is 5mm; the main components and the mass percentage content of the tellurium copper slag are 21.63 percent of Te and 40.01 percent of Cu;
b. b, putting the copper telluride slag material obtained after crushing in the step a into a roasting furnace for heating, adding 75g of sodium hydroxide (the purity of the sodium hydroxide is 99%) when the temperature is raised to 300 ℃, continuing heating after the sodium hydroxide is put into the roasting furnace, raising the temperature to 600 ℃ for roasting reaction, wherein the roasting time is 1h, and obtaining 130g of primary roasting slag after roasting;
c. cooling the primary roasting slag obtained in the step b to room temperature, and then adding the primary roasting slag into a ball mill for ball milling, wherein the granularity of ball milling materials is controlled to be 1mm; adding 500ml of water into 100g of the obtained material after ball milling, putting the mixture into a water leaching kettle for water leaching, wherein the water leaching temperature is 60 ℃, the water leaching time is 2 hours, and leaching solution and leaching residues are obtained after water leaching, wherein 27.1g of the leaching solution and the leaching residues contain Cu97.3 percent through detection;
d. the obtained leaching solution is a sodium tellurate solution, the sodium tellurate solution is treated through an electrodeposition process to obtain metal tellurium, and leaching residues enter a copper residue recycling process for utilization.
Example 2:
the invention relates to a method for separating and recovering tellurium and copper from copper telluride residues, which comprises the following detailed steps:
a. firstly, 50g of copper telluride slag is put into a jaw crusher to be crushed until the granularity of the material is 5mm; the main components and the mass percentage content of the tellurium copper slag are 21.63 percent of Te and 40.01 percent of Cu;
b. b, putting the copper telluride slag material obtained after crushing in the step a into a roasting furnace for heating, adding 75g of sodium hydroxide (the purity of the sodium hydroxide is 99%) when the temperature is raised to 300 ℃, continuing heating after the sodium hydroxide is put into the roasting furnace, raising the temperature to 650 ℃ for roasting reaction, wherein the roasting time is 1h, and obtaining 130g of primary roasting slag after roasting;
c. cooling the primary roasting slag obtained in the step b to room temperature, and then adding the primary roasting slag into a ball mill for ball milling, wherein the granularity of ball milling materials is controlled to be 1.5mm; adding 600ml of water into 100g of the obtained material after ball milling, putting the mixture into a water leaching kettle for water leaching, wherein the water leaching temperature is 60 ℃, the water leaching time is 2.5 hours, and leaching liquid and leaching residues are obtained after water leaching, wherein the leaching liquid and the leaching residues contain Cu by 97.6 percent through detection;
d. and treating the sodium tellurate solution through an electrodeposition process to obtain metal tellurium, and recycling leaching residues in a copper residue recycling process.
Example 3:
the invention relates to a method for separating and recovering tellurium and copper from copper telluride residues, which comprises the following detailed steps:
a. firstly, 50g of copper telluride slag is put into a jaw crusher to be crushed until the granularity of the material is 5mm; the main components and the mass percentage content of the tellurium copper slag are 21.63 percent of Te and 40.01 percent of Cu;
b. b, putting the copper telluride slag material obtained after crushing in the step a into a roasting furnace for heating, adding 50g of sodium hydroxide (the purity of the sodium hydroxide is 99%) when the temperature is raised to 300 ℃, continuing heating after the sodium hydroxide is put into the roasting furnace, raising the temperature to 620 ℃ for roasting reaction, wherein the roasting time is 1.5h, and obtaining 90g of primary roasting slag after roasting;
c. cooling the primary roasting slag obtained in the step b to room temperature, and then adding the primary roasting slag into a ball mill for ball milling, wherein the granularity of ball milling materials is controlled to be 1mm; adding 500ml of water into 80g of the obtained material after ball milling, putting the mixture into a water leaching kettle for water leaching, wherein the water leaching temperature is 50 ℃, the water leaching time is 2.5 hours, and leaching solution and leaching residues are obtained after water leaching, wherein the leaching solution and the leaching residues contain 98.02 percent of Cu through detection;
d. and treating the sodium tellurate solution through an electrodeposition process to obtain metal tellurium, and recycling leaching residues in a copper residue recycling process.

Claims (5)

1. A method for separating and recovering tellurium and copper from copper telluride slag, which is characterized by comprising the following steps:
a. firstly, putting copper telluride slag into a jaw crusher for crushing until the granularity of the material is 3-5 mm;
b. b, adding sodium hydroxide into the copper telluride slag material obtained after crushing in the step a, and then putting the copper telluride slag material into a roasting furnace for primary roasting at the roasting temperature of 600-650 ℃ for 1-2 hours to obtain primary roasting slag;
c. cooling the primary roasting slag obtained in the step b to room temperature, adding the primary roasting slag into a ball mill for ball milling, and adding water into the materials obtained after ball milling for water leaching to obtain leaching solution and leaching slag;
d. and treating the sodium tellurate solution through an electrodeposition process to obtain metal tellurium, and recycling leaching residues in a copper residue recycling process.
2. The method for separating and recovering tellurium and copper from copper telluride slag as in claim 1, wherein the method comprises the following steps: and the addition amount of the sodium hydroxide in the step b is 1-1.2 times of the molar amount of the reaction theoretical value of the crushed copper telluride slag material.
3. The method for separating and recovering tellurium and copper from copper telluride slag as in claim 1, wherein the method comprises the following steps: and c, the granularity of the ball-milled material is 1-1.5 mm.
4. The method for separating and recovering tellurium and copper from copper telluride slag as in claim 1, wherein the method comprises the following steps: in the water immersion process in the step c, the adding amount mass ratio of water to the ball-milled materials is 5-7: 1.
5. the method for separating and recovering tellurium and copper from copper telluride slag as in claim 1, wherein the method comprises the following steps: in the water leaching process in the step c, the leaching time is 2-3 h, and the leaching temperature is 50-70 ℃.
CN202210900727.XA 2022-07-28 2022-07-28 Method for separating and recovering tellurium and copper from copper telluride slag Pending CN115369416A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115716639A (en) * 2022-11-30 2023-02-28 郴州雄风环保科技有限公司 Process for leaching tellurium from gold, silver and copper-containing tellurium slag

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115716639A (en) * 2022-11-30 2023-02-28 郴州雄风环保科技有限公司 Process for leaching tellurium from gold, silver and copper-containing tellurium slag

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