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Method for preparing graphene dispersion liquid by utilizing pyrenyl benzoic acid polyether ester parent reagent

A graphene dispersion, pyrene-based benzoic acid technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements and other directions, can solve the problems of graphene structure being easily destroyed and stable, and achieve the effect of wide source of raw materials

Active Publication Date: 2014-05-07
中科悦达(上海)材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the problems in the prior art that the graphene structure is easily destroyed and the stability of the graphene liquid phase dispersion system is poor, and to provide a method for preparing graphene sulfonate by using pyrenylbenzoic acid polyether ester amphiphile. method of dispersion

Method used

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  • Method for preparing graphene dispersion liquid by utilizing pyrenyl benzoic acid polyether ester parent reagent
  • Method for preparing graphene dispersion liquid by utilizing pyrenyl benzoic acid polyether ester parent reagent

Examples

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Embodiment 1

[0021] (1) Dissolve 8g of polyethylene glycol monomethyl ether (Mn=750) and 1.75g ​​of p-aminobenzoic acid in the solvent THF, transfer the above solution to a 100mL round bottom flask, and then add 1mL of concentrated sulfuric acid to it, A precipitate formed and was heated to reflux for 30 minutes. Then transfer the reaction mixture into a 250mL beaker, add 10% sodium carbonate to pH ≈ 9, filter with suction, wash, extract twice with ether, and purify to obtain product A. 3g of A, 40ml of water, 40% 20mmolHBr and a certain amount of 30% 20mmolH 2 o 2 Mix well at room temperature, and purify to obtain product B. Dissolve 1.00 g of B and 0.25 g of 1-boronic acid pyrene in the solvent THF, add 40 ml of Na 2 CO 3 aqueous solution. Then 0.10 g of tetrakis(triphenylphosphine) palladium was added thereto, the mixture was vigorously stirred under a nitrogen atmosphere, heated to reflux for 24 hours, the mixture was layered, the aqueous phase layer was washed twice with dichloro...

Embodiment 2

[0024] (1) Dissolve 8g of polyethylene glycol monomethyl ether (Mn=1000) and 1.64g of p-aminobenzoic acid in the solvent THF, transfer the above solution to a 100mL round bottom flask, and then add 1mL of concentrated sulfuric acid to it, A precipitate formed and was heated to reflux for 30 minutes. Then transfer the reaction mixture into a 250mL beaker, add 10% sodium carbonate to pH ≈ 9, filter with suction, wash, extract twice with ether, and purify to obtain product A. 3.00g of A, 40ml of water, 40% 20mmolHBr and a certain amount of 30% 20mmolH 2 o 2 Mix well at room temperature, and purify to obtain product B. Dissolve 1.00 g of B and 0.25 g of 1-boronic acid pyrene in the solvent THF, add 40 ml of Na 2 CO 3aqueous solution. Then 0.10 g of tetrakis(triphenylphosphine) palladium was added thereto, the mixture was vigorously stirred under a nitrogen atmosphere, heated to reflux for 24 hours, the mixture was layered, the aqueous phase layer was washed twice with dichlor...

Embodiment 3

[0027] (1) Dissolve 8g of polyethylene glycol monomethyl ether (Mn=550) and 2.19g of p-aminobenzoic acid in the solvent THF, transfer the above solution to a 100mL round bottom flask, and then add 1mL of concentrated sulfuric acid to it, A precipitate formed and was heated to reflux for 30 minutes. Then transfer the reaction mixture into a 250mL beaker, add 10% sodium carbonate to pH ≈ 9, filter with suction, wash, extract twice with ether, and purify to obtain product A. 3.00g of A, 40ml of water, 40% 20mmolHBr and 30% 24mmolH 2 o 2 Mix well at room temperature, and purify to obtain product B. Dissolve 1.00 g of B and 0.93 g of 1-boronic acid pyrene in the solvent THF, add 40 ml of Na 2 CO 3 aqueous solution. Then 0.10 g of tetrakis(triphenylphosphine) palladium was added thereto, the mixture was vigorously stirred under a nitrogen atmosphere, heated to reflux for 24 hours, the mixture was layered, the aqueous phase layer was washed twice with dichloromethane, and purifi...

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Abstract

The invention relates to a method for preparing a graphene dispersion liquid by utilizing a pyrenyl benzoic acid polyether ester parent reagent. The method comprises the steps: with methoxy polyethylene glycol, p-aminobenzoic acid and 1-pyrenylboronicacid as raw materials, carrying out esterification reaction to obtain p-aminobenzoic acid polyether ester of a hydrophilic long chain, then introducing HBr which is reacted with the 1-pyrenylboronicacid to prepare 3, 5-dibromo benzoic acid methoxy polyethylene glycol, and carrying out reaction on the 3, 5-dibromo benzoic acid methoxy polyethylene glycol and the pyrenylboronicacid to synthesize amphoteric (hydrophilic and oleophylic) graphite remover; and dissolving the compound and graphene in a H2O / Et solution, carrying out twice ultrasonic treatment, standing, and carrying out centrifugation to obtain the stable a graphene dispersion liquid. With the adoption of the method, as the graphene does not need oxidation reduction, the destructive effect on a graphene structure is very small, and the unique electric and thermal conductivities of the graphene can be fully exerted; as the prepared dispersion liquid has good aqueous phase stability, an effective way is provided for the application of the graphene in the field of composites.

Description

technical field [0001] The present invention relates to a kind of method that utilizes pyrenylbenzoic acid polyether lipid amphiphile to prepare graphene dispersion liquid, specifically relates to the synthesis of a kind of pyrenylbenzoic acid polyether lipid amphiphile and utilizes it to prepare stable graphene dispersion liquid Methods. Background technique [0002] Graphene is a new type of carbon material with a single atomic layer two-dimensional conjugated structure, and its theoretical specific surface area is as high as 2630m 2 / g. For a long time, the scientific community has theorized that single-layer graphene crystals cannot exist stably. Until 2004, the team led by Professor Geim of the University of Manchester successfully prepared single-layer graphene for the first time, which not only allowed scientists to re-understand graphene, but more importantly, it made people realize that graphene and fullerene and carbon nano Compared with nano-carbon materials su...

Claims

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Application Information

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IPC IPC(8): C01B31/04C08G65/48C01B32/194
Inventor 董海军徐德善蔡铜祥
Owner 中科悦达(上海)材料科技有限公司
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