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Heteropoly acid modified carbon nano tube and/or graphene reinforced lead-based composite anode preparation method

A graphene composite and carbon nanotube technology, applied in chemical instruments and methods, carbon compounds, electrodes, etc., can solve problems such as limited service life, high cost, and insufficient mechanical properties, and achieve low environmental impact, low cost, and prevent easy reunion effect

Active Publication Date: 2018-11-06
KUNMING HENDERA SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Compared with the traditional lead and its alloy anodes, the performance of the above-mentioned anodes has been improved, but there are still problems of high cost, limited service life, and insufficient mechanical properties, which limit its widespread use

Method used

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  • Heteropoly acid modified carbon nano tube and/or graphene reinforced lead-based composite anode preparation method
  • Heteropoly acid modified carbon nano tube and/or graphene reinforced lead-based composite anode preparation method
  • Heteropoly acid modified carbon nano tube and/or graphene reinforced lead-based composite anode preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Such as figure 1 As shown, the carbon nanotubes modified by the heteropolyacid enhances the preparation method of the lead-based composite anode, and its specific steps are as follows:

[0028] Step 1, amination modification treatment: subjecting carbon nanotubes to amination modification treatment;

[0029] Step 1.1, Carboxylation: oxidize the multi-walled carbon nanotubes in a mixed solution of sulfuric acid (98wt%) and nitric acid (68wt%) at a volume ratio of 3:1 at a temperature of 60°C for 4 hours, then filter and deionize Washing with water until neutral, drying in vacuum at 50°C to obtain carboxylated multi-walled carbon nanotubes;

[0030] Step 1.2, acid chlorination: Add 1 g of the carboxylated multi-walled carbon nanotubes obtained in step 1.1 to 20 mL of thionyl chloride, stir and reflux at 70°C for 24 hours, filter and wash with tetrahydrofuran, and dry under vacuum at 50°C to obtain polyacyl chloride walled carbon nanotubes;

[0031] Step 1.3, Amidation...

Embodiment 2

[0039] Such as figure 1 Shown, the graphene reinforced lead-based composite anode preparation method of this heteropolyacid modification, its specific steps are as follows:

[0040] Step 1, amination modification treatment: subjecting graphene to amination modification treatment;

[0041] Step 1.1, carboxylation: oxidize graphene in a mixed solution of sulfuric acid (98wt%) and nitric acid (68wt%) with a volume ratio of 3:1 at a temperature of 60°C for 4 hours, then filter and wash with deionized water until Neutral, vacuum dried at 50°C to obtain carboxylated graphene;

[0042] Step 1.2, acyl chloride: 1 g of the carboxylated graphene obtained in step 1.1 was added to 20 mL of thionyl chloride, stirred and refluxed at 70° C. for 24 hours, filtered, washed with tetrahydrofuran, and vacuum-dried at 50° C. to obtain graphene acyl chloride;

[0043] Step 1.3, amidation: Add 1 g of the acyl chloride graphene obtained in step 1.2, add 5 g of ammonium carbonate, dropwise add 50 m...

Embodiment 3

[0049] Such as figure 1 Shown, this heteropolyacid modified carbon nanotube and graphene reinforced lead-based composite anode preparation method, its specific steps are as follows:

[0050] Step 1, amination modification treatment: subjecting carbon nanotubes and graphene to amination modification treatment;

[0051] Step 1.1, carboxylation: put carbon nanotubes and graphene mixed particles with a mass ratio of 1:1 in a mixed solution of sulfuric acid (98wt%) and nitric acid (68wt%) with a volume ratio of 3:1, at a temperature of 60 ℃ oxidation for 4 hours, then filter, wash with deionized water until neutral, and vacuum dry at 50 ℃ to obtain carboxylated carbon nanotubes and graphene;

[0052] Step 1.2, acyl chloride: Add 1 g of the carboxylated carbon nanotubes and graphene obtained in step 1.1 to 20 mL of thionyl chloride, stir and reflux at 70°C for 24 hours, filter and wash with tetrahydrofuran, and dry under vacuum at 50°C to obtain acid chloride carbon nanotubes and...

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Abstract

The invention relates to a heteropoly acid modified carbon nano tube and / or graphene reinforced lead-based composite anode preparation method, and belongs to the technical field of novel material preparation. Carbon nano tube and / or graphene are / is subjected to amination modified processing, heteropoly acid is dissolved in hot water to obtain a heteropoly acid solution with the concentration of 0.0001-0.01mol / L, the carbon nano tube and / or the graphene and a dispersing agent are added, 0.0005-0.2mol barium chloride is added, even stirring is carried out, then standing is carried out for 24 hours, and heteropoly acid modified carbon nano tube and / or grapheme composite powder bodies are obtained by filtering; a high-energy ball is subjected to grinding and alloying; and a heteropoly acid modified carbon nano tube and / or graphene reinforced lead-based composite anode is obtained by powder metallurgical molding. Technological operation is simple, the obtained composite anode is low in cost, the catalytic performance is excellent, and the service life is similar to that of a traditional lead anode.

Description

technical field [0001] The invention relates to a method for preparing a heteropolyacid-modified carbon nanotube and / or graphene-reinforced lead-based composite anode, and belongs to the technical field of new material preparation. Background technique [0002] Industrial electrowinning generally uses lead alloys as anodes, because of its low price, easy processing and molding, and relatively stable electrochemical performance in sulfuric acid solution, such as zinc electrowinning generally uses Pb–Ag (0.5wt.%~1.0wt.%) Anode, copper electrowinning uses Pb-Sb, Pb-Ca-Sn anode. However, there are many defects in the production of lead alloy anodes, mainly including: high oxygen evolution potential, high density, low strength, easy deformation and short circuit. For many years, the metallurgical industry has been committed to the research and development of new energy-saving anode materials with high strength, corrosion resistance, good conductivity, low oxygen evolution potent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25C7/02B22F9/04C01B32/168C01B32/194C22C1/05C22C11/00
CPCC22C1/05C22C11/00C22C26/00C25C7/02C01B32/168C01B32/194B22F9/04B22F2999/00B22F2998/10B22F2009/043B22F2009/041C22C2026/002B22F3/02B22F3/1007B22F2201/01
Inventor 杨长江翟大成沈庆峰
Owner KUNMING HENDERA SCI & TECH
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