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Platinum catalyst loaded on aminated graphene and preparation method thereof

A technology for amination of graphene and platinum catalysts, which is applied in the preparation of amino compounds, catalyst activation/preparation, catalysts for physical/chemical processes, etc., and can solve the problems that the reduction catalyst cannot remove the reaction heat in time, high-temperature sintering activity, and metal accumulation. , to reduce solvent consumption, improve selectivity, and reduce recovery costs

Pending Publication Date: 2021-10-15
SINOPEC NANJING RES INST OF CHEM IND CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the present invention is to provide a method for preparing a platinum catalyst supported on aminated graphene, which is used to catalyze the hydrogenation of nitrobenzene to prepare p-aminodiphenylamine, and is intended to solve the problem that the reduction catalyst cannot be shifted in time in the existing production of p-aminodiphenylamine Take away the heat of reaction, leading to metal accumulation, high temperature sintering and reduced activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The natural flake graphite is soaked in a sulfuric acid solution with a content of 10%, boiled and refluxed for 8.0h to separate the solid from the liquid, wash the solid phase with water, and the solid phase obtained is the pretreated natural flake graphite; the pretreated natural flake graphite is added to the In concentrated sulfuric acid, stir and mix thoroughly, add potassium permanganate to the mixed solution for 3.0 hours, add deionized water for 1.0 hours, then add hydrogen peroxide solution for 1.0 hours to obtain graphite oxide solution; ultrasonically Peel off for 0.5h and filter, wash the solid phase with deionized water until the filtrate is neutral, and dry the solid phase in vacuum at 110°C for 2h to obtain graphene oxide; ultrasonically disperse graphene oxide in ethylene glycol and ethylenediamine solution for 15h to obtain amination Graphene: add chloroplatinic acid solution with a content of 10% to impregnate the aminated graphene for 10 hours, use a h...

Embodiment 2

[0036] Natural flake graphite is soaked in the nitric acid solution that content is 10%, after boiling and refluxing for 1.5h, solid-liquid separation is carried out, and the solid phase is washed with water, and the obtained solid phase is natural flake graphite after pretreatment; the natural flake graphite after pretreatment is added to In concentrated sulfuric acid, stir and mix thoroughly, add potassium permanganate to the mixed solution for 2.5 hours, add deionized water for 1.5 hours, then add hydrogen peroxide solution for 0.5 hours to obtain graphite oxide solution; ultrasonically Peel off for 1.0h and filter, wash the solid phase with deionized water until the filtrate is neutral, dry the solid phase at 110°C in vacuum for 2h to obtain graphene oxide; ultrasonically disperse graphene oxide in ethylene glycol and ethylenediamine solution for 8h to obtain amination Graphene: add chloroplatinic acid solution with a content of 15% to the aminated graphene and impregnate i...

Embodiment 3

[0040] Natural flake graphite is soaked in the hydrochloric acid solution that content is 10%, after boiling and refluxing for 3.0h, solid-liquid separation is carried out, and the solid phase is washed with water, and the obtained solid phase is natural flake graphite after pretreatment; the natural flake graphite after pretreatment is added to In concentrated sulfuric acid, stir and mix thoroughly, add potassium permanganate to the mixed solution for 3.5 hours, add deionized water for 0.5 hours, then add hydrogen peroxide solution for 1.5 hours to obtain graphite oxide solution; ultrasonically Peel off for 1.0h and filter, wash the solid phase with deionized water until the filtrate is neutral, dry the solid phase at 110°C in vacuum for 2h to obtain graphene oxide; ultrasonically disperse graphene oxide in ethylene glycol and ethylenediamine solution and react for 12h to obtain amination Graphene: add chloroplatinic acid solution with a content of 32% to impregnate the aminat...

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Abstract

The invention discloses a preparation method of a platinum catalyst loaded on aminated graphene, the preparation method comprises the following steps: pretreating natural crystalline flake graphite, oxidizing the pretreated natural crystalline flake graphite to prepare graphite oxide, performing ultrasonic exfoliation on the graphite oxide to obtain graphene oxide, aminating the graphene oxide to obtain aminated graphene, and adding a platinum salt solution into the aminated graphene to prepare the platinum catalyst loaded on the aminated graphene. The problems of sintering deactivation, large catalyst loss, more impurities in hydrogenation liquid and reduced production capacity caused by local overheating of the catalyst due to the fact that the reduction catalyst cannot timely remove reaction heat in the existing p-aminodiphenylamine production can be solved. The catalyst has the advantages of high activity, high selectivity, good stability, long service life and good application prospect when being used for catalyzing nitrobenzene process hydrogenation to prepare p-aminodiphenylamine.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a platinum catalyst supported on aminated graphene and a preparation method thereof, which are used to catalyze the hydrogenation of nitrobenzene to prepare p-aminodiphenylamine. Background technique [0002] p-aminodiphenylamine (also known as RT base, 4-aminodiphenylamine) is an important organic intermediate, widely used in rubber additives, dyes, textiles, printing and pharmaceutical industries, etc., mainly as anti-aging for p-phenylenediamine rubber Agent intermediates are used to prepare rubber antioxidants 4010NA, 6PPD, etc. [0003] There are more than ten kinds of synthetic methods for p-aminodiphenylamine, such as aniline method, formanilide method, carboanilide method, diphenylamine method, and nitro method. At present, the processes used for industrial production at home and abroad mainly include diphenylamine method and nitro method , the prepara...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/18B01J23/42B01J31/02B01J35/00B01J37/02C07C209/36C07C209/38C07C211/54
CPCB01J21/18B01J23/42B01J31/0238B01J37/0207C07C209/38C07C209/36B01J35/393C07C211/54
Inventor 吴其建陈永平刘卓管成年洪庆军刘权魏鹏辉秦涛
Owner SINOPEC NANJING RES INST OF CHEM IND CO LTD
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