CN101519729A - Method for preparing tribasic lead sulfate by using ash of copper converter - Google Patents

Method for preparing tribasic lead sulfate by using ash of copper converter Download PDF

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Publication number
CN101519729A
CN101519729A CN200910080464A CN200910080464A CN101519729A CN 101519729 A CN101519729 A CN 101519729A CN 200910080464 A CN200910080464 A CN 200910080464A CN 200910080464 A CN200910080464 A CN 200910080464A CN 101519729 A CN101519729 A CN 101519729A
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Prior art keywords
lead sulfate
ash
slag
bismuth
copper converter
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CN200910080464A
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陈自江
李少利
安生宝
张国勇
吕登才
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Jinchuan Group Co Ltd
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Jinchuan Group Co Ltd
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    • 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 relates to a method for preparing tribasic lead sulfate by using ash of a copper converter, which comprises the step: (1) the ash of the copper converter is leached by dilute sulphuric acid to obtain leach liquor containing copper and zinc and lixiviated residues containing lead and bismuth. The method is characterized by also comprising the steps: (2) sodium chloride is added into the leached residues containing lead and bismuth, and the leached residues containing lead and bismuth are leached by concentrated sulfuric acid to obtain leach liquor containing bismuth and chloride leached residues; (3) the chloride leached residues are converted by ammonium carbonate to obtain ammonium carbonate converting residues; (4) the ammonium carbonate converting residues are dissolved by nitric acid; (5) the ammonium carbonate converting residue solution dissolved by the nitric acid is deposited by sulphuric acid; (6) the formed lead sulfate deposition and sodium hydroxide reacts to synthesize tribasic lead sulfate. The method adopts a wet process, lead in the ash is transformed into lead carbonate through sectioning leaching, and then, the lead carbonate is dissolved by nitric acid, deposited by sulphuric acid and added with sodium hydroxide to synthesize the tribasic lead sulfate. The technical process is simpler, and has good operating environment due to the adoption of the wet process.

Description

A kind of method for preparing lead sulfate tribasic with ash of copper converter
Technical field
A kind ofly prepare the method for lead sulfate tribasic, relate to a kind of preparation method of lead sulfate tribasic, particularly use wet processing prepares lead sulfate tribasic from the white cigarette ash of copper converter method with ash of copper converter.
Background technology
The cigarette ash of copper converter output contains elements such as Cu, Zn, Fe, Pb, As, Bi usually.In the technical process of handling ash of copper converter, normally cigarette ash goes out with acidleach, remove acid-soluble metal oxide or metal-salt, soak the back slag through blast furnace smelting, the lead bismuth alloy plate that is produced obtains electrolytic lead by electrolysis, and electrolytic lead is again through further transforming the synthetic lead sulfate tribasic that obtains.This process using blast furnace smelting, operating environment is poor; It is plumbous to obtain electricity earlier, and lead sulfate tribasic is produced in regeneration, and technical process is long.
Summary of the invention
The objective of the invention is the deficiency that exists at above-mentioned prior art, provide that a kind of technological process is simple, good operational environment prepare the method for lead sulfate tribasic by ash of copper converter with wet processing.
The objective of the invention is to be achieved through the following technical solutions.
A kind ofly prepare the method for lead sulfate tribasic with ash of copper converter, its step comprises:
(1) ash of copper converter is leached with dilute sulphuric acid, obtain the leach liquor and leaded, the bismuth leached mud of cupric, zinc;
It is characterized in that its step also comprises:
(2) leaded, bismuth leached mud are added sodium-chlor and leach, obtain bismuth-containing leach liquor and villaumite leached mud with the vitriol oil;
(3) the villaumite leached mud is transformed with volatile salt obtain volatile salt and transform slag;
(4) volatile salt is transformed the slag nitric acid dissolve;
(5) volatile salt behind the nitric acid dissolve is transformed slag lysate sulfuric acid precipitation;
(6) lead sulfate that precipitation obtained precipitation with the synthetic lead sulfate tribasic of sodium hydroxide,
A kind of method for preparing lead sulfate tribasic with ash of copper converter of the present invention, it is characterized in that described adding sodium-chlor sulfuric acid leaching process, the sodium-chlor add-on is to soak 25%~30% of bismuth slag dry weight, sulfuric acid concentration is: 200~300g/l, extraction temperature is 75~100 ℃, extraction time is 1.5~2.5 hours, and the solid-liquid weight ratio is 3~4:1, control terminal point acidity 90~100g/l.
Of the present inventionly a kind ofly prepare the method for lead sulfate tribasic, it is characterized in that the described villaumite leached mud is transformed with volatile salt obtains volatile salt and transform the slag process with ash of copper converter; Solvent and solute weight ratio 2.5~3.5:1,2~3 hours reaction times.
A kind of method for preparing lead sulfate tribasic with ash of copper converter of the present invention, it is characterized in that described volatile salt being transformed slag nitric acid dissolve process, the mass concentration of salpeter solution is 12%~16%, and the reaction times is 1.5~2.0 hours, and the solid-liquid weight ratio is: 4~5:1.
A kind of method for preparing lead sulfate tribasic with ash of copper converter of the present invention, it is characterized in that described volatile salt being transformed slag with nitric acid dissolve process sulfuric acid precipitation process, the mass concentration 35%~43% of sulphuric acid soln, temperature are 35~45 ℃, and the reaction times is 2~2.5 hours.
A kind of method for preparing lead sulfate tribasic with ash of copper converter of the present invention, it is characterized in that described with lead sulfate with the synthetic lead sulfate tribasic process of sodium hydroxide, the mass concentration that adds the solution of sodium hydroxide is 18%~25%, liquid-solid ratio 2.5~3.5:1, control terminal point PH=8.5-9.0.
Method of the present invention all adopts wet process, leaches by segmentation the lead in the cigarette ash is changed into lead carbonate, then with pin acid dissolving, sulfuric acid precipitation adds the synthetic lead sulfate tribasic of sodium hydroxide again, and this technological process is simpler, adopt wet process, good operational environment.
Embodiment
A kind ofly prepare the method for lead sulfate tribasic with ash of copper converter, its step comprises:
(1) ash of copper converter is leached with dilute sulphuric acid, obtain the leach liquor and leaded, the bismuth leached mud of cupric, zinc; (2) leaded, bismuth leached mud are added sodium-chlor and leach, obtain bismuth-containing leach liquor and villaumite leached mud with the vitriol oil; (3) the villaumite leached mud is transformed with volatile salt obtain volatile salt and transform slag; (3) volatile salt is transformed the slag nitric acid dissolve; (4) volatile salt behind the nitric acid dissolve is transformed slag lysate sulfuric acid precipitation; (5) the lead sulfate precipitation that precipitation is obtained is synthesized lead sulfate tribasic with sodium hydroxide.
Described adding sodium-chlor vitriol oil leaching process, sodium-chlor add-on are to soak 25%~30% of bismuth slag dry weight, and sulfuric acid concentration is: 260-300g/l, extraction temperature is 75~100 ℃, extraction time is 1.5~2.5 hours, and solid-to-liquid ratio is 4~4.5, control terminal point acidity 90~100g/l.
The described villaumite leached mud is transformed with volatile salt obtains volatile salt and transforms the slag process; Solvent and solute weight ratio 2.5~3.5:1,2~3 hours reaction times.
Described volatile salt is transformed slag nitric acid dissolve process, the mass concentration of salpeter solution is 12%~16%, and the reaction times is 1.5~2.0 hours, and the solid-liquid weight ratio is: 4~4.5:1.
Described volatile salt is transformed slag with nitric acid dissolve process sulfuric acid precipitation process, the mass concentration 35%~43% of sulphuric acid soln, temperature are 35~45 ℃, and the reaction times is 2~2.5 hours.
Described with lead sulfate with the synthetic lead sulfate tribasic process of sodium hydroxide, the mass concentration that adds the solution of sodium hydroxide is 18%~25%, solvent and solute weight ratio 2.5~3.5:1, control terminal point PH=8.5-9.0.
Embodiment
(1) villaumite leaches
Figure A200910080464D00051
(2) chlorine soaks the slag conversion
(3) transform the slag dissolving
Figure A200910080464D00061
(4) transform slag dissolving back heavyization of liquid
Figure A200910080464D00062
(5) lead sulfate tribasic is synthetic
Figure A200910080464D00071

Claims (6)

1. one kind prepares the method for lead sulfate tribasic with ash of copper converter, and its step comprises:
(1) ash of copper converter is leached with dilute sulphuric acid, obtain the leach liquor and leaded, the bismuth leached mud of cupric, zinc;
It is characterized in that its step also comprises:
(2) leaded, bismuth leached mud are added sodium-chlor and leach, obtain bismuth-containing leach liquor and villaumite leached mud with the vitriol oil;
(3) the villaumite leached mud is transformed with volatile salt obtain volatile salt and transform slag;
(4) volatile salt is transformed the slag nitric acid dissolve;
(5) volatile salt behind the nitric acid dissolve is transformed slag lysate sulfuric acid precipitation;
(6) the lead sulfate precipitation that precipitation is obtained is synthesized lead sulfate tribasic with sodium hydroxide.
2. a kind of method for preparing lead sulfate tribasic with ash of copper converter according to claim 1, it is characterized in that described adding sodium-chlor sulfuric acid leaching process, the sodium-chlor add-on is to soak 25%~30% of bismuth slag dry weight, sulfuric acid concentration is: 200~300g/l, extraction temperature is 75~100 ℃, extraction time is 1.5~2.5 hours, and solid-to-liquid ratio is 3~4: 1, control terminal point acidity 90~100g/l.
3. according to claim 1ly a kind ofly prepare the method for lead sulfate tribasic, it is characterized in that the described villaumite leached mud is transformed with volatile salt obtains volatile salt and transform the slag process with ash of copper converter; Liquid-solid ratio 2.5~3.5: 1,2~3 hours reaction times.
4. a kind of method for preparing lead sulfate tribasic with ash of copper converter according to claim 1, it is characterized in that described volatile salt being transformed slag nitric acid dissolve process, the mass concentration of salpeter solution is 12%~16%, and the reaction times is 1.5~2.0 hours, and solid-to-liquid ratio is: 4~5: 1.
5. a kind of method for preparing lead sulfate tribasic with ash of copper converter according to claim 1, it is characterized in that described volatile salt being transformed slag with nitric acid dissolve process sulfuric acid precipitation process, the mass concentration 35%~43% of sulphuric acid soln, temperature is 35~45 ℃, and the reaction times is 2~2.5 hours.
6. a kind of method for preparing lead sulfate tribasic with ash of copper converter according to claim 1, it is characterized in that described with lead sulfate with the synthetic lead sulfate tribasic process of sodium hydroxide, the mass concentration that adds the solution of sodium hydroxide is 18%~25%, liquid-solid ratio 2.5~3.5: 1, control terminal point PH=8.5-9.0.
CN200910080464A 2009-03-19 2009-03-19 Method for preparing tribasic lead sulfate by using ash of copper converter Pending CN101519729A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103397180A (en) * 2013-08-07 2013-11-20 江西铜业股份有限公司 Method for recovering tellurium, bismuth, antimony, and copper from complex material
CN104445380A (en) * 2014-12-12 2015-03-25 郴州市金贵银业股份有限公司 Preparation method of lead sulfate tribasic
CN105420508A (en) * 2015-12-09 2016-03-23 永兴县灿阳贵金属有限责任公司 Method for extracting lead and bismuth from precious metal smelting waste residues
CN106435179A (en) * 2016-10-28 2017-02-22 广东工业大学 Leaching method of metals in lead-zinc sulfide mineral tailings and application of leaching method
CN107641225A (en) * 2017-08-18 2018-01-30 西北矿冶研究院 Sole material made of acid-leaching modified white ash
CN108084490A (en) * 2017-11-27 2018-05-29 西北矿冶研究院 Pasty acid-leaching modified white smoke ash composite lead salt stabilizer and preparation method thereof
CN113975702A (en) * 2021-10-14 2022-01-28 昆明理工大学 Method for removing dioxin POPs in copper smelting soot through synergistic retardation of microwave and sulfuric acid

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103397180A (en) * 2013-08-07 2013-11-20 江西铜业股份有限公司 Method for recovering tellurium, bismuth, antimony, and copper from complex material
CN103397180B (en) * 2013-08-07 2016-01-20 江西铜业股份有限公司 A kind of method reclaiming tellurium, bismuth, antimony, copper from complex feedstock
CN104445380A (en) * 2014-12-12 2015-03-25 郴州市金贵银业股份有限公司 Preparation method of lead sulfate tribasic
CN105420508A (en) * 2015-12-09 2016-03-23 永兴县灿阳贵金属有限责任公司 Method for extracting lead and bismuth from precious metal smelting waste residues
CN106435179A (en) * 2016-10-28 2017-02-22 广东工业大学 Leaching method of metals in lead-zinc sulfide mineral tailings and application of leaching method
CN107641225A (en) * 2017-08-18 2018-01-30 西北矿冶研究院 Sole material made of acid-leaching modified white ash
CN108084490A (en) * 2017-11-27 2018-05-29 西北矿冶研究院 Pasty acid-leaching modified white smoke ash composite lead salt stabilizer and preparation method thereof
CN113975702A (en) * 2021-10-14 2022-01-28 昆明理工大学 Method for removing dioxin POPs in copper smelting soot through synergistic retardation of microwave and sulfuric acid

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