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Aromatic nitrile graphene and preparation method thereof

A technology for aromatic nitrile and graphene, which is applied in the field of aromatic nitrile graphene and its preparation, and can solve the problems of low yield and difficulty in commercialization of graphene.

Active Publication Date: 2018-01-09
重庆中安材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of this, the purpose of the present invention is to provide a kind of aromatic nitrile 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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  • Aromatic nitrile graphene and preparation method thereof
  • Aromatic nitrile graphene and preparation method thereof
  • Aromatic nitrile graphene and preparation method thereof

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preparation example Construction

[0022] A preparation method for aromatic nitrile graphene, comprising the following steps:

[0023] a) passing acetic acid and ammonia water through a molecular sieve synthesis tower, gas-phase synthesis reaction to obtain adiponitrile, hydrogen, carbon dioxide and water, cooling to obtain adiponitrile oily liquid and collecting hydrogen;

[0024] b) adding nickel acetate to the adiponitrile obtained in step a), and reacting to synthesize caprolactam;

[0025] c) adding palladium acetate to the caprolactam obtained in step b), and introducing the hydrogen collected in step a), reacting to obtain aromatic nitrile graphene microcrystals;

[0026] d) adding deionized water to the aromatic nitrile graphene microcrystals obtained in step c), hydrolyzing to remove metal palladium, then heating to remove water, cooling to below 40°C, adding hydrazine hydrate to replace metal nickel, and filtering the product After metal nickel and carbon solids are obtained, elute the solids with an...

Embodiment 1

[0047] 4L acetic acid and 1L ammonia water are heated to 250°C and passed through the DPZSM-5 molecular sieve (the loading capacity of dibutyl phosphate is 3%) synthesis tower, gas-phase catalyzed to obtain adiponitrile, hydrogen, carbon dioxide and water, cool adiponitrile and collect hydrogen Then add 5g of nickel acetate, under the condition of temperature at 90°C and pressure of 0.05MPa, conduct closed reaction for 8 hours, and react to obtain caprolactam; then add 0.5L of hydrogen gas, add 1g of palladium acetate, at the condition of temperature at 60°C and pressure of 120KPa Next, after reacting for 3 hours, let it stand still for 10 hours to obtain aromatic nitrile graphene microcrystals; then add 5L of deionized water, and adjust the pH value of the solution to 7.5, and precipitate palladium hydroxide will be generated in the solution, and the precipitate will be filtered Finally, heat the reactant to 100°C to remove the raw material moisture, cool to below 40°C, add 1....

Embodiment 2

[0049] 4L acetic acid and 1L ammonia water are heated to 260°C and pass through the DPZSM-5 molecular sieve (the loading capacity of dibutyl phosphate is 3%) synthesis tower, gas-phase catalyzed to obtain adiponitrile, hydrogen, carbon dioxide and water, cool adiponitrile and collect hydrogen Then add 6g of nickel acetate, under the conditions of temperature at 90°C and pressure of 0.5MPa, conduct a closed reaction for 9 hours, and react to obtain caprolactam; then add 2L of hydrogen, add 1.2g of palladium acetate, at a temperature of 100°C and a pressure of 150KPa Next, after reacting for 4 hours, let it stand for 12 hours to obtain aromatic nitrile graphene microcrystals; then add 7L deionized water, and adjust the pH value of the solution to 7.5, and precipitate palladium hydroxide will be generated in the solution, and the precipitate will be filtered Finally, heat the raw material to 100°C to remove the raw material moisture, cool to below 40°C, add 1.5L hydrazine hydrate ...

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Abstract

The invention discloses a method for preparing aromatized cyanation graphene. The method comprises the steps of obtaining adiponitrile, hydrogen, carbon dioxide and water from acetic acid and ammonia water through gas phase synthesis reaction by means of a molecular sieve synthetic tower, conducting cooling to obtain adiponitrile oily liquid and collecting hydrogen; adding nickel acetate to obtain caprolactam through synthesis; adding palladium acetate and introducing hydrogen to obtain aromatized cyanation graphene microcrystal through reaction; adding deionized water, separating out metallic palladium through hydrolysis, and separating out water through heating; reducing the temperature to 40 DEG C, then adding hydrazine hydrate to substitute metallic nickel, conducting filtration to obtain metallic nickel and solid carbon, eluting the solid with alcohols solvent, making elution solution return to a reactor, and then increasing the temperature to separate out alcohol, ammonium acetate and acethydrazide to obtain the aromatized cyanation graphene. Acetic acid and ammonia water are taken as basic materials, nickel acetate serves as a graphene microcrystal adsorbent and an electrolusis electrode, palladium acetate serves as an electrode and graphene microcrystal sediment loader of nickel acetate, and then the aromatized cyanation graphene can be synthesized to the maximum extent.

Description

technical field [0001] The invention relates to the field of graphene, in particular to an aromatic nitrile 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. 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. Most of these methods have the problem of low graphene yield and difficult to realize commercialization. [0004] Therefore, only by finding a way to achieve large-scale prod...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/10
CPCC07C231/10C07C231/12C07C253/22C07D223/10C08G69/00C07C255/04C07C237/22
Inventor 李新勇
Owner 重庆中安材料科技有限公司