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Ammonia aromatic graphene and preparation method thereof

A graphene and aromatization technology, applied in the field of ammoniated aromatic graphene and its preparation, can solve problems such as low graphene yield and difficulty in commercialization, and achieve the effects of solving difficulty in commercial production, increasing yield, and solving low yield

Active Publication Date: 2018-10-09
重庆中安材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of this, the purpose of the present invention is to provide a kind of ammoniated aromatic graphene and preparation method thereof, solve the technical problem that current graphene output is low and difficult to commercialize

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0026] A preparation method for ammoniated aromatic graphene, comprising the following steps:

[0027] a) dissolving the higher alkyne polymer of acetylene tail gas in an alcohol solvent to obtain the first mixed solution;

[0028] b) dissolving nickel acetate in aqueous ammonia into the first mixed solution obtained in step a) through a metering jet pump, and reacting by heating to obtain a second mixed solution;

[0029] c) cooling the second mixed solution obtained in step b) to room temperature, then adding hydrazine hydrate to react to obtain a mixture of methylpyrazole and aromatic graphene microcrystalline nickel; The mixture of graphene microcrystalline nickel is cooled to room temperature, diluted with deionized water, then filtered to obtain metallic nickel and carbon solids, sent to an alcohol eluting tower, and the metallic nickel is eluted and extracted, and the eluent is returned to the reaction In the material, a mixture of methylpyrazole and aromatic graphene ...

Embodiment 1

[0053] a) Dissolve 10 g of acetylene tail gas higher alkyne polymer in 160 g of ethanol solvent to obtain the first mixed solution.

[0054] b) Dissolve 0.5g of nickel acetate in an appropriate amount of ammonia water and add it to the first mixed solution obtained in step a) through a metering jet pump. Under the conditions of temperature at 85°C and pressure at 200KPa, conduct a closed reaction for 12 hours to obtain the second mixed solution .

[0055] c) Cool the second mixed solution obtained in step b) to room temperature, then add 5 g of hydrazine hydrate, react at a temperature of 80 °C and a pressure of 600 KPa for 12 hours, and then stand still for 12 hours to obtain methylpyrazole and aromatic Graphene microcrystalline nickel mixture; then add 230g deionized water, heat and stir at 98°C for 5h, filter to obtain metallic nickel and carbon solids; then elute with methanol to recover metallic nickel, return the eluent to obtain methylpyrazoles and aromatic graphene mi...

Embodiment 2

[0059] a) Dissolve 10 g of acetylene tail gas higher alkyne polymer in 180 g of ethanol solvent to obtain the first mixed solution.

[0060] b) Dissolve 0.4g of nickel acetate in an appropriate amount of ammonia water and add it into the first mixed solution obtained in step a) through a metering jet pump. Under the conditions of temperature at 75°C and pressure at 220KPa, conduct a closed reaction for 14 hours to obtain the second mixed solution .

[0061] c) Cool the second mixed solution obtained in step b) to room temperature, then add 7g of hydrazine hydrate, react at a temperature of 70°C and a pressure of 500KPa for 14h, and then stand for 13h to obtain methylpyrazole and aromatic Graphene microcrystalline nickel mixture; then add 200g deionized water, heat and stir at 100°C for 4h, filter to obtain metallic nickel and carbon solids; then elute with methanol to recover metallic nickel, return the eluent to obtain methylpyrazoles and aromatic graphene mixture.

[0062]...

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Abstract

The invention discloses a preparation method of ammoniated and aromatized graphene. The preparation method of the ammoniated and aromatized graphene comprises the following steps of adding an ammonia water solution containing nickel acetate into a mixed solution of an acetylene tail gas higher alkyne polymer and an alcohol solvent through a metering injection pump, and enabling a first obtained mixture to react to obtain a second mixed solution; afterward, adding hydrazine hydrate into the second mixed solution, enabling a second obtained mixture to react to obtain a mixture of methylpyrazole and aromatized graphene microcrystalline nickel; subsequently, cooling the mixture to a room temperature, adding deionized water into the mixture for thinning, filtering a third obtained mixture to obtain metallic nickel and a carbon solid, sending the metallic nickel and the carbon solids into an alcohol elution tower, eluting and extracting out the metallic nickel, and returning eluent to reactants, so as to obtain a mixture of the methylpyrazole and aromatized graphene; adding ammonium salt into the mixture, so as to obtain a mixture of the methylpyrazole and ammoniated graphene; distilling off the methylpyrazole from the mixture, so as to obtain the ammoniated and aromatized graphene. According to the ammoniated and aromatized graphene and the preparation method thereof, the ammoniated and aromatized graphene prepared by adopting the above technical scheme is used as a raw material for preparing graphene; the yield, the efficiency and the quality of the graphene are improved; therefore, the problems that the graphene is low in yield and is difficult in commercial production are solved.

Description

technical field [0001] The invention relates to the field of graphene, in particular to an ammoniated aromatic graphene and a preparation method thereof. Background technique [0002] Graphene is a two-dimensional crystal that is stripped from graphite and composed of carbon atoms with only one atomic thickness. It is currently the thinnest and highest-strength material in nature, and it exhibits excellent physical and chemical properties, such as a large specific surface area. , high electron migration rate, good chemical properties, excellent thermal conductivity, high elastic modulus and mechanical strength, etc., making it a hot spot in current scientific and industrial research. [0003] The current preparation methods of graphene mainly include mechanical ball milling exfoliation method, silicon carbide epitaxial growth method, chemical vapor deposition method, graphite oxide reduction method, graphite intercalation method and organic synthesis method. However, most o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D231/12C01B32/182C22B23/00C22B7/00
CPCC07D231/12C22B7/006C22B23/0461Y02P10/20
Inventor 李新勇
Owner 重庆中安材料科技有限公司