Method for preparing poly organic polysulfide/sulfonated graphene conductive composite material

A conductive composite material, sulfonated graphene technology, applied in circuits, electrical components, battery electrodes and other directions, can solve the problems of unsatisfactory cycle stability, poor cycle stability of polyorganic polysulfides, etc., and achieves easy control of product composition, The effect of low environmental pollution and cheap and easy-to-obtain raw materials

Inactive Publication Date: 2010-06-09
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

US patent US 20020110737 reports a poly 2,5-dimercapto-1,3,4-thiadiazole / polyaniline intercalated layered vanadium pentoxide hybrid material, with a separate polymer and vanadium pentoxide phase Compared, the hybrid material has better charge and discharge characteristics, but its cycle stability is not ideal
So far, the problem of poor cycle stability of polyorganopolysulfides has not been fundamentally resolved

Method used

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  • Method for preparing poly organic polysulfide/sulfonated graphene conductive composite material
  • Method for preparing poly organic polysulfide/sulfonated graphene conductive composite material
  • Method for preparing poly organic polysulfide/sulfonated graphene conductive composite material

Examples

Experimental program
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Embodiment 1

[0031] Sulfonated graphene is obtained by step-by-step reduction of graphite oxide. The process is as follows: put 2g of graphite oxide into 400mL of pH=9-10 aqueous solution, after ultrasonic dispersion for 2h, add 6g of sodium borohydride and stir at 80°C React for 1 hour, centrifuge and rinse with deionized water to obtain partially reduced graphite oxide; then redisperse the partially reduced graphite oxide in 200mL deionized water, add 2.6g of diazonium p-aminobenzenesulfonic acid in an ice-water bath React for 3 hours to introduce sulfonic acid groups; finally, react the above sulfonated product with 30 g of hydrazine hydrate at 100°C for 24 hours to remove residual oxygen-containing groups, wash with deionized water until neutral, and dry. Obtain sulfonated graphene.

[0032] Dissolve 1.5g of 2,5-dimercapto-1,3,4-thiadiazole monomer in a mixed solution of 100mL deionized water / ethanol (deionized water:ethanol=1:2, volume ratio), and then add 1.5g of sulfonated graphene...

Embodiment 2

[0037]Repeat the process of Example 1 to prepare sulfonated graphene.

[0038] Dissolve 1 g of 2,5-dimercapto-1,3,4-thiadiazole monomer in a mixed solution of 100 mL deionized water / ethanol (deionized water:ethanol=1:2, volume ratio), and then add 0.1 g of sulfonated graphene, after ultrasonication for 15 minutes, slowly add 1.7g of elemental iodine in 25mL of absolute ethanol solution dropwise to the above solution, and stir and react at 40°C for 24 hours; the product is filtered and deionized water After washing with ethanol and drying, the polyorganic polysulfide / graphene conductive composite material is obtained.

[0039] The morphology of the polyorganopolysulfide / graphene conductive composite is as follows: figure 2 As shown in the SEM pictures of the graphene, it can be seen that poly-2,5-dimercapto-1,3,4-thiadiazole is gathered on the surface and edge of graphene in a submicron sheet structure.

[0040] Using the four-probe technique, the conductivity of the polyorg...

Embodiment 3

[0043] Repeat the process of Example 1 to prepare sulfonated graphene.

[0044] Dissolve 1 g of 2,5-dimercapto-1,3,4-thiadiazole monomer in a mixed solution of 100 mL deionized water / ethanol (deionized water:ethanol=1:1, volume ratio), and then add 0.05 g of sulfonated graphene, after ultrasonication for 30 minutes, slowly drop 40mL of absolute ethanol solution dissolved with 3.4g of elemental iodine into the above solution, and stir and react at 50°C for 12 hours; the product was filtered and deionized water After washing with ethanol and drying, the polyorganic polysulfide / graphene conductive composite material is obtained.

[0045] Using the four-probe technique, the electrical conductivity of the polyorganopolysulfide / graphene conductive composite was tested to be 0.11 S / cm.

[0046] The button lithium battery using the polyorganopolysulfide / graphene conductive composite material as the positive electrode material was subjected to a charge-discharge cycle test on a LAND C...

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Abstract

The invention relates to a method for preparing poly organic polysulfide / graphene conductive composite material, which is characterized by taking water-soluble sulfonated graphene as a carrier and adopting an in-situ oxidation polymerization method to deposit poly organic polysulfide on the surface of the grapheme so as to prepare the poly organic polysulfide / graphene conductive composite material. The composite material has high conductivity and excellent electrochemical properties and can be used as anode material of lithium secondary batteries.

Description

technical field [0001] The invention relates to a preparation method of a polyorganic polysulfide / sulfonated graphene conductive composite material, in particular to a poly 2,5-dimercapto-1,3,4-thiadiazole / sulfonated graphene conductive composite The invention discloses a material preparation method, belonging to the field of energy materials. Background technique [0002] As new energy storage materials, polyorganopolysulfides have attracted great attention due to their high theoretical specific capacity and environmental friendliness. In 1988, the Lawrence Berkeley laboratory of the National Energy Research Center of the United States reported the metal sodium / organic disulfide battery for the first time [J. Electrochem. Soc., Vol.135, 2905, (1999)]. In the early 1990s, Japanese researchers proposed polyorganic polysulfides as battery cathode materials, among which poly2,5-dimercapto-1,3,4-thiadiazole was the most studied. However, the slow redox rate of poly 2,5-dimerca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/60
CPCY02E60/12Y02E60/10
Inventor 王庚超金立峰李良彬李星玮
Owner EAST CHINA UNIV OF SCI & TECH
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