CN112981132A - Lead bullion electrolytic refining method beneficial to cadmium removal - Google Patents

Lead bullion electrolytic refining method beneficial to cadmium removal Download PDF

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Publication number
CN112981132A
CN112981132A CN201911288136.6A CN201911288136A CN112981132A CN 112981132 A CN112981132 A CN 112981132A CN 201911288136 A CN201911288136 A CN 201911288136A CN 112981132 A CN112981132 A CN 112981132A
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China
Prior art keywords
lead
cadmium
stirring
liquid
precipitated
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Pending
Application number
CN201911288136.6A
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Chinese (zh)
Inventor
尹升
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Hunan Guiyang Yinxing Nonferrous Smelting Co ltd
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Hunan Guiyang Yinxing Nonferrous Smelting Co ltd
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Priority to CN201911288136.6A priority Critical patent/CN112981132A/en
Publication of CN112981132A publication Critical patent/CN112981132A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B13/00Obtaining lead
    • C22B13/06Refining
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/10General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
    • C22B9/106General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents the refining being obtained by intimately mixing the molten metal with a molten salt or slag

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The electrolytic refining method of the lead bullion beneficial to cadmium removal comprises a copper removal process, an electrolysis process and a refining process, wherein the electrolysis process obtains precipitated lead, and the refining process of the precipitated lead comprises the following steps: 1) adding the precipitated lead into an electric lead pot, and heating to melt the precipitated lead to obtain lead liquid; 2) removing dross on the surface of the lead liquid, adding NaOH into the lead liquid, and continuously stirring until snowflake-shaped lines are generated on the surface of the lead liquid, and further removing the dross on the surface; 3) adding industrial salt and covering the surface of the lead liquid; 4) and continuously heating to 500-550 ℃, adding sodium nitrate while stirring at the temperature, finishing the addition of the sodium nitrate within 0.5h, stirring for 2-2.5 h, sampling and detecting, obtaining a qualified lead product if the cadmium element reaches the standard, and continuously adding the sodium nitrate and stirring at the temperature of 500-550 ℃ if the cadmium element does not reach the standard until the cadmium element is sampled and detected to reach the standard, thus obtaining the qualified lead product. The lead product finally produced by the method meets the requirement of national standard No. 1, is convenient to operate, has low processing cost and is convenient for industrial production.

Description

Lead bullion electrolytic refining method beneficial to cadmium removal
Technical Field
The invention relates to the technical field of electric lead smelting, in particular to a lead bullion electrolytic refining method beneficial to cadmium removal.
Background
The existing crude lead refining method generally comprises fire refining and electrolytic refining, wherein the fire refining is to form a new phase different from a molten main metal by utilizing the difference of the physical property or the chemical property of an impurity metal and the main metal lead in a high-temperature melt and enrich impurities in the new phase, so that the refining aim is fulfilled. The electrolytic refining generally comprises three main processes of copper removal, electrolysis and refining, although the early investment cost is high and the production cost is slightly higher, the electrolytic refining is increasingly widely applied due to the high quality of the obtained product, stable production process and good operation condition. In the prior art, the final refining step in the electrolytic refining process is mainly to remove a scum casting mold, the step can remove partial over-standard elements such as arsenic, antimony and the like, but the separating element is not powerful, in the prior art, if the separated lead and cadmium elements obtained by electrolysis exceed the standard, the separated lead and cadmium elements can only be slowly matched and digested or returned to an electrolysis section in the production process, the production period is prolonged or the processing cost is increased, and the new requirement of the new national standard GB/T469-2913 for the lead product of the electrolytic refining is that the cadmium element in the lead product is not more than 0.0002%, so higher requirements are provided for the lead production process of the electrolytic refining.
Disclosure of Invention
The invention aims to provide a lead bullion electrolytic refining method beneficial to cadmium removal, and aims to solve the problem that cadmium element in a product obtained by electrolytic refining of the existing lead bullion exceeds the standard.
The technical problem solved by the invention is realized by adopting the following technical scheme:
the electrolytic refining method of the lead bullion beneficial to cadmium removal comprises a copper removal process, an electrolysis process and a refining process, wherein the electrolysis process obtains precipitated lead, and the refining process of the precipitated lead comprises the following steps:
1) adding the precipitated lead into an electric lead pot, and heating to melt the precipitated lead to obtain lead liquid;
2) removing dross on the surface of the lead liquid, adding NaOH into the lead liquid, and continuously stirring until snowflake-shaped lines are generated on the surface of the lead liquid, and further removing the dross on the surface;
3) adding industrial salt and covering the surface of the lead liquid;
4) and continuously heating to 500-550 ℃, adding sodium nitrate while stirring at the temperature, finishing the addition of the sodium nitrate within 0.5h, stirring for 2-2.5 h, sampling and detecting, obtaining a qualified lead product if the cadmium element reaches the standard, and continuously adding the sodium nitrate and stirring at the temperature of 500-550 ℃ if the cadmium element does not reach the standard until the cadmium element is sampled and detected to reach the standard, thus obtaining the qualified lead product.
Further, the heating temperature of the electric lead pan is 450-500 ℃.
Further, in the step 4), the content of cadmium element in the qualified lead product is less than or equal to 0.0002%.
Has the advantages that: the invention provides a lead bullion electrolytic refining method beneficial to cadmium removal, which can quickly and effectively remove cadmium in the final refining stage of electric lead under the condition that the precipitated lead and cadmium exceed standards, ensures that the finally produced lead product meets the requirements of national standard No. 1, and has the advantages of convenient operation, low processing cost and convenient industrial popularization and production.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
The method for electrolytic refining of lead bullion beneficial to cadmium removal, which is described in this embodiment, includes a copper removal process, an electrolysis process and a refining process, wherein the electrolysis process obtains precipitated lead, the precipitated lead contains 0.0006% of cadmium, and the step of continuously refining the precipitated lead includes the following steps:
1) adding the separated lead into an electric lead pot, and heating to 450 ℃ to melt the separated lead to obtain lead liquid;
2) removing the surface scum of the lead liquid in a fishing way, adding 75kg of NaOH into the lead liquid, continuously stirring until snowflake-shaped lines are generated on the surface of the lead liquid, and further removing the surface scum in the fishing way;
3) adding 100 kg of industrial salt and covering the surface of the lead liquid;
4) and continuously heating to 500 ℃, adding sodium nitrate while stirring at the temperature, finishing the addition of the sodium nitrate within 0.5h, sampling and detecting after stirring for 2h, continuously adding the sodium nitrate, keeping the stirring at the temperature of 500 ℃, and detecting that the cadmium content reaches 0.00018 percent after stirring for 6 h to obtain the lead product meeting the national standard No. 1.
Example 2
The method for electrolytic refining of lead bullion beneficial to cadmium removal, which is described in the embodiment, comprises a copper removal process, an electrolysis process and a refining process, wherein the electrolysis process is used for obtaining precipitated lead, the precipitated lead contains 0.0012% of cadmium, and the refining process of the precipitated lead comprises the following steps:
1) adding the separated lead into an electric lead pot, and heating to 500 ℃ to melt the separated lead to obtain lead liquid;
2) removing the surface scum of the lead liquid in a fishing way, adding 75kg of NaOH into the lead liquid, continuously stirring until snowflake-shaped lines are generated on the surface of the lead liquid, and further removing the surface scum in the fishing way;
3) adding 100 kg of industrial salt and covering the surface of the lead liquid;
4) and continuously heating to 550 ℃, adding sodium nitrate while stirring at the temperature, finishing the addition of the sodium nitrate within 0.5h, sampling and detecting after stirring for 2h, continuously adding the sodium nitrate, keeping the temperature of 550 ℃ for stirring, and detecting that the cadmium content reaches 0.00016% after stirring for 18 h to obtain the lead product meeting the national standard No. 1.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (3)

1. The electrolytic refining method of the lead bullion beneficial to cadmium removal comprises a copper removal process, an electrolysis process and a refining process, wherein the electrolysis process obtains precipitated lead, and the electrolytic refining process is characterized by comprising the following steps:
1) adding the precipitated lead into an electric lead pot, and heating to melt the precipitated lead to obtain lead liquid;
2) removing dross on the surface of the lead liquid, adding NaOH into the lead liquid, and continuously stirring until snowflake-shaped lines are generated on the surface of the lead liquid, and further removing the dross on the surface;
3) adding industrial salt and covering the surface of the lead liquid;
4) and continuously heating to 500-550 ℃, adding sodium nitrate while stirring at the temperature, finishing the addition of the sodium nitrate within 0.5h, stirring for 2-2.5 h, sampling and detecting, obtaining a qualified lead product if the cadmium element reaches the standard, and continuously adding the sodium nitrate and stirring at the temperature of 500-550 ℃ if the cadmium element does not reach the standard until the cadmium element is sampled and detected to reach the standard, thus obtaining the qualified lead product.
2. The lead bullion electrolytic refining method beneficial to cadmium removal as claimed in claim 1, wherein in the step 1), the heating temperature of the electric lead pan is 450-500 ℃.
3. The method for the electrolytic refining of lead bullion in favor of cadmium removal as recited in claim 1, wherein in step 4), the content of cadmium element in qualified lead products is less than or equal to 0.0002%.
CN201911288136.6A 2019-12-15 2019-12-15 Lead bullion electrolytic refining method beneficial to cadmium removal Pending CN112981132A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911288136.6A CN112981132A (en) 2019-12-15 2019-12-15 Lead bullion electrolytic refining method beneficial to cadmium removal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911288136.6A CN112981132A (en) 2019-12-15 2019-12-15 Lead bullion electrolytic refining method beneficial to cadmium removal

Publications (1)

Publication Number Publication Date
CN112981132A true CN112981132A (en) 2021-06-18

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116083733A (en) * 2022-11-29 2023-05-09 河南豫光合金有限公司 Method for removing cadmium element in crude lead

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4911755A (en) * 1989-08-28 1990-03-27 Cominco Ltd. Method for the refining of lead
CA1337579C (en) * 1989-08-25 1995-11-21 Gerald R. Larouche Method for the refining of lead
CN101555550A (en) * 2009-05-22 2009-10-14 北京科技大学 Method for recycling lead-tin in silver separating residue of copper anode slime of circuit board
CN101705372A (en) * 2009-11-25 2010-05-12 郴州市金贵银业股份有限公司 Process for extracting tin from wet lead with high tin content
CN103290429A (en) * 2013-06-17 2013-09-11 湖南省桂阳银星有色冶炼有限公司 Method for electrolyzing high-content low-grade lead bullion
CN103667737A (en) * 2013-12-31 2014-03-26 湖南省桂阳银星有色冶炼有限公司 Primary pyro-refining method for lead bullions
CN106244824A (en) * 2016-08-24 2016-12-21 安徽省陶庄湖废弃物处置有限公司 Reviver pyrogenic process basic refining bottom blowing process method

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1337579C (en) * 1989-08-25 1995-11-21 Gerald R. Larouche Method for the refining of lead
US4911755A (en) * 1989-08-28 1990-03-27 Cominco Ltd. Method for the refining of lead
CN101555550A (en) * 2009-05-22 2009-10-14 北京科技大学 Method for recycling lead-tin in silver separating residue of copper anode slime of circuit board
CN101705372A (en) * 2009-11-25 2010-05-12 郴州市金贵银业股份有限公司 Process for extracting tin from wet lead with high tin content
CN103290429A (en) * 2013-06-17 2013-09-11 湖南省桂阳银星有色冶炼有限公司 Method for electrolyzing high-content low-grade lead bullion
CN103667737A (en) * 2013-12-31 2014-03-26 湖南省桂阳银星有色冶炼有限公司 Primary pyro-refining method for lead bullions
CN106244824A (en) * 2016-08-24 2016-12-21 安徽省陶庄湖废弃物处置有限公司 Reviver pyrogenic process basic refining bottom blowing process method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116083733A (en) * 2022-11-29 2023-05-09 河南豫光合金有限公司 Method for removing cadmium element in crude lead

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