CN111304442A - Method for removing F, Cl in secondary zinc oxide soot and preparing pure electrolyte - Google Patents

Method for removing F, Cl in secondary zinc oxide soot and preparing pure electrolyte Download PDF

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Publication number
CN111304442A
CN111304442A CN201911287845.2A CN201911287845A CN111304442A CN 111304442 A CN111304442 A CN 111304442A CN 201911287845 A CN201911287845 A CN 201911287845A CN 111304442 A CN111304442 A CN 111304442A
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China
Prior art keywords
zinc oxide
secondary zinc
leaching
sulfuric acid
oxide soot
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CN201911287845.2A
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Chinese (zh)
Inventor
陈科艳
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Xuzhou Bona Environmental Protection Technology Co ltd
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Xuzhou Bona Environmental Protection Technology Co ltd
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Priority to CN201911287845.2A priority Critical patent/CN111304442A/en
Publication of CN111304442A publication Critical patent/CN111304442A/en
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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
    • 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
    • C22B7/001—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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • C22B1/248—Binding; Briquetting ; Granulating of metal scrap or alloys
    • 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
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/20—Obtaining zinc otherwise than by distilling
    • 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
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
    • 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
    • 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
    • C22B7/007—Wet processes by acid leaching
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A method for removing F, Cl in secondary zinc oxide soot and preparing pure electrolyte comprises the following steps: adding industrial sulfuric acid into the secondary zinc oxide soot, and granulating; roasting the particles obtained in the step (1) in a rotary kiln at the temperature of 600-800 ℃ for 3-5 h; adding 3-5 times of volume of electrolyte residual liquid into the roasted particles for leaching, adding industrial sulfuric acid to control the pH of a leaching end point to be 3.3-4.1, leaching for 4-5 hours, and filtering and separating to obtain a leaching solution; adding hydrogen peroxide and lime milk into the leachate, controlling the pH to be 5.0 and the temperature to be 45-65 ℃, maintaining for 1-2h, and filtering; adding C into the leaching solutionuOH and Ni (OH)2Controlling the pH value to be 2.5-4.8 and the temperature to be 35-50 ℃, maintaining for 1 hour, and filtering to obtain the pure electrolyte. The invention has smooth process, less consumption, low cost, no three wastes and environmental protection.

Description

Method for removing F, Cl in secondary zinc oxide soot and preparing pure electrolyte
Technical Field
The invention relates to the technical field of metallurgy and chemical industry, in particular to a method for removing F, Cl in secondary zinc oxide soot and preparing pure electrolyte.
Background
The zinc-containing solid wastes (such as steel dust, lead-smelting slag and the like) are treated by a high-temperature fuming method to obtain the enriched secondary zinc oxide powder, which is a secondary resource for preparing metal zinc. Some impurities in the chemical components are harmful to the wet preparation of zinc, such as Cl and F. The conventional method of heating and roasting in a multi-hearth furnace or a rotary kiln is adopted to treat the zinc oxide powder, so that the fluorine and chlorine impurities with high content cannot be effectively removed; the combined method of pretreating zinc oxide powder by alkali washing and then matching with wet dechlorination in zinc sulfate leaching solution has the defects of long process, high zinc loss, high treatment cost, complex pollution discharge treatment and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art by providing a method for removing F, Cl in the secondary zinc oxide ash and preparing a pure electrolyte, so that the method can economically, efficiently and environmentally remove impurities such as fluorine, chlorine and the like with high content in the secondary zinc oxide powder, and create necessary and sufficient conditions for subsequent electrolysis operation, thereby overcoming the defects of the prior art for treating the solid wastes.
The technical scheme of the invention is as follows:
a method for removing F, Cl in secondary zinc oxide soot and preparing pure electrolyte comprises the following steps:
(1) adding industrial sulfuric acid into the secondary zinc oxide soot, and granulating by using a granulating device;
(2) roasting the particles obtained in the step (1) in a rotary kiln at the temperature of 600-800 ℃ for 3-5 h;
(3) adding 3-5 times of volume of electrolyte residual liquid into the roasted particles for leaching, adding industrial sulfuric acid to control the pH of a leaching end point to be 3.3-4.1, leaching for 4-5 hours, and filtering and separating to obtain a leaching solution;
(4) adding hydrogen peroxide and lime milk into the leachate, controlling the pH to be 5.0, controlling the temperature to be 45-65 ℃, maintaining for 1-2h, and filtering;
(5) adding CuOH and Ni (OH) into the leaching solution2Controlling the pH value to be 2.5-4.8 and the temperature to be 35-50 ℃, maintaining for 1h, and filtering to obtain the pure electrolyte.
Preferably, in the step (1), the secondary zinc oxide soot and the industrial sulfuric acid are uniformly mixed by using a mixing device, wherein the mass percentage of the secondary zinc oxide soot to the industrial sulfuric acid is 100: (10-20), adding industrial sulfuric acid at one time.
Preferably, in the step (1), the granulating device is a disc-type granulating device, and the particle size of the granules is 8-15 mm.
Preferably, in the step (4), the adding amount of the hydrogen peroxide is 4-8 ml/L.
Preferably, in the step (5), CuOH and Ni (COH)2The control of the addition amount and the end point is realized by controlling a slurry feeding pump through a double-potential device, and the numerical value of the end point is determined that the contents of Cl ions and F ions are both less than 0.1 g/L.
The method for removing F, Cl in the secondary zinc oxide soot and preparing the pure electrolyte is simple and convenient to operate, environment-friendly and low in cost, and compared with the traditional process, the method has the advantages that the removal rate of fluorine and chlorine is over 95 percent, the improvement rate is 8-70 percent, and the method is suitable for large-scale production. The invention has smooth process, less consumption, low cost, no three wastes and environmental protection.
Detailed Description
The following examples are intended to further illustrate the present disclosure, but not to limit the scope of the claims.
Example 1
A method for removing F, Cl in secondary zinc oxide soot and preparing pure electrolyte comprises the following steps:
(1) adding industrial sulfuric acid into the secondary zinc oxide soot, uniformly mixing the secondary zinc oxide soot and the industrial sulfuric acid by using a mixing device, and granulating by using a disc type granulating device; the mass percentage of the secondary zinc oxide soot and the industrial sulfuric acid is 100: 10, adding industrial sulfuric acid at one time; the particle size of the granules is 8 mm;
(2) roasting the particles obtained in the step (1) in a rotary kiln at the temperature of 600 ℃ for 5 hours;
(3) adding 3 times of volume of electrolyte residual liquid into the roasted particles for leaching, adding industrial sulfuric acid to control the pH of a leaching end point to be 3.3, leaching for 4 hours, and filtering and separating to obtain a leaching solution;
(4) adding hydrogen peroxide and lime milk into the leachate, controlling the pH to be 5.0 and the temperature to be 45 ℃, maintaining for 2 hours, and filtering; the adding amount of hydrogen peroxide is 4 ml/L;
(5) adding CuOH and Ni (OH) into the leaching solution2Controlling the pH value to be 2.5, keeping the temperature at 50 ℃ for 1h, and filtering to obtain pure electrolyte; CuOH and Ni (OH)2The control of the addition amount and the end point is realized by controlling a slurry feeding pump through a double-potential device, and the numerical value of the end point is determined that the contents of Cl ions and F ions are both less than 0.1 g/L.
Example 2
A method for removing F, Cl in secondary zinc oxide soot and preparing pure electrolyte comprises the following steps:
(1) adding industrial sulfuric acid into the secondary zinc oxide soot, uniformly mixing the secondary zinc oxide soot and the industrial sulfuric acid by using a mixing device, and granulating by using a disc type granulating device; the mass percentage of the secondary zinc oxide soot and the industrial sulfuric acid is 100: 15, adding industrial sulfuric acid at one time; the particle size of the granules is 11 mm;
(2) roasting the particles obtained in the step (1) in a rotary kiln at the temperature of 700 ℃ for 4 hours;
(3) adding 4 times volume of electrolyte residual liquid into the roasted particles for leaching, adding industrial sulfuric acid to control the pH of the leaching end point to be 3.7, leaching for 4.5h, and filtering and separating to obtain a leaching solution;
(4) adding hydrogen peroxide and lime milk into the leachate, controlling the pH to be 5.0 and the temperature to be 55 ℃, maintaining for 1.5h, and filtering; the adding amount of hydrogen peroxide is 6 ml/L;
(5) adding CuOH and Ni (OH) into the leaching solution2Controlling the pH value to be 3.6, keeping the temperature at 45 ℃ for 1h, and filtering to obtain pure electrolyte; CuOH and Ni (OH)2The control of the addition amount and the end point is realized by controlling a slurry feeding pump through a double-potential device, and the numerical value of the end point is determined that the contents of Cl ions and F ions are both less than 0.1 g/L.
Example 3
A method for removing F, Cl in secondary zinc oxide soot and preparing pure electrolyte comprises the following steps:
(1) adding industrial sulfuric acid into the secondary zinc oxide soot, uniformly mixing the secondary zinc oxide soot and the industrial sulfuric acid by using a mixing device, and granulating by using a disc type granulating device; the mass percentage of the secondary zinc oxide soot and the industrial sulfuric acid is 100: 20, adding industrial sulfuric acid at one time; the particle size of the granules is 15 mm;
(2) roasting the particles obtained in the step (1) in a rotary kiln at the temperature of 800 ℃ for 3 hours;
(3) adding electrolyte residual liquid with 5 times volume of the roasted particles for leaching, adding industrial sulfuric acid to control the pH of the leaching end point to be 4.1, leaching for 5 hours, and filtering and separating to obtain a leaching solution;
(4) adding hydrogen peroxide and lime milk into the leachate, controlling the pH to be 5.0 and the temperature to be 65 ℃, maintaining for 1h, and filtering; the adding amount of hydrogen peroxide is 8 ml/L;
(5) adding CuOH and Ni (OH) into the leaching solution2Controlling the pH value to be 4.8 and the temperature to be 35 ℃, maintaining for 1 hour, and filtering to obtain pure electrolyte; CuOH and Ni (OH)2The control of the addition amount and the end point is realized by controlling a slurry feeding pump through a double-potential device, and the numerical value of the end point is determined that the contents of Cl ions and F ions are both less than 0.1 g/L.
The method for removing F, Cl in the secondary zinc oxide soot and preparing the pure electrolyte has the advantages of simple and convenient operation, environmental friendliness and low cost, and the removal rate of fluorine and chlorine in the method is over 95 percent, is improved by 8-70 percent compared with the traditional process, and is suitable for mass production. The invention has smooth process, less consumption, low cost, no three wastes and environmental protection.

Claims (5)

1. A method for removing F, Cl in secondary zinc oxide soot and preparing pure electrolyte is characterized by comprising the following specific steps:
(1) adding industrial sulfuric acid into the secondary zinc oxide soot, and granulating by using a granulating device;
(2) roasting the particles obtained in the step (1) in a rotary kiln at the temperature of 600-800 ℃ for 3-5 h;
(3) adding 3-5 times of volume of electrolyte residual liquid into the roasted particles for leaching, adding industrial sulfuric acid to control the pH of a leaching end point to be 3.3-4.1, leaching for 4-5 hours, and filtering and separating to obtain a leaching solution;
(4) adding hydrogen peroxide and lime milk into the leachate, controlling the pH to be 5.0, controlling the temperature to be 45-65 ℃, maintaining for 1-2h, and filtering;
(5) adding CuOH and Ni (OH) into the leaching solution2Controlling the pH value to be 2.5-4.8 and the temperature to be 35-50 ℃, maintaining for 1h, and filtering to obtain the pure electrolyte.
2. The method for removing F, Cl in the secondary zinc oxide soot and preparing a pure electrolyte as claimed in claim 1, wherein in the step (1), the secondary zinc oxide soot is uniformly mixed with the industrial sulfuric acid by using a mixing device, and the mass percentage of the secondary zinc oxide soot to the industrial sulfuric acid is 100: (10-20), adding industrial sulfuric acid at one time.
3. The method for removing F, Cl in the secondary zinc oxide soot and preparing a pure electrolyte according to claim 1, wherein in step (1), the granulating device is a disk granulating device, and the particle size of the granules is 8-15 mm.
4. The method for removing F, Cl in the zinc hypoxide soot and preparing a pure electrolyte as claimed in claim 1, wherein in step (4), the amount of hydrogen peroxide added is 4-8 ml/L.
5. The method for removing F, Cl in the secondary zinc oxide soot and preparing a pure electrolyte as claimed in claim 1, wherein in step (5), CuOH and Ni (OH)2The control of the addition amount and the end point is realized by controlling a slurry feeding pump through a double-potential device, and the numerical value of the end point is determined that the contents of Cl ions and F ions are both less than 0.1 g/L.
CN201911287845.2A 2019-12-15 2019-12-15 Method for removing F, Cl in secondary zinc oxide soot and preparing pure electrolyte Withdrawn CN111304442A (en)

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Application Number Priority Date Filing Date Title
CN201911287845.2A CN111304442A (en) 2019-12-15 2019-12-15 Method for removing F, Cl in secondary zinc oxide soot and preparing pure electrolyte

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Application Number Priority Date Filing Date Title
CN201911287845.2A CN111304442A (en) 2019-12-15 2019-12-15 Method for removing F, Cl in secondary zinc oxide soot and preparing pure electrolyte

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115232973A (en) * 2022-07-27 2022-10-25 修水县德瑞科技有限公司 Device and method for improving leaching rate of copper-zinc ash

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115232973A (en) * 2022-07-27 2022-10-25 修水县德瑞科技有限公司 Device and method for improving leaching rate of copper-zinc ash
CN115232973B (en) * 2022-07-27 2024-05-07 修水县德瑞科技有限公司 Device for improving leaching rate of copper-zinc ash and improving method thereof

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Application publication date: 20200619