Preparation method and catalytic application of graphene oxide immobilized tetra(4-hydroxyphenyl) manganese porphyrin catalytic material

A porphyrin catalytic material and hydroxyphenyl technology are applied in the field of preparation of graphene oxide-immobilized tetramanganese porphyrin catalytic materials, and can solve the problem of inconvenient recycling, low catalytic oxidation efficiency of ethylbenzene, and low catalytic efficiency of metal porphyrins. and other problems, to achieve the effect of environmental protection recycling, easy recycling and low cost

Inactive Publication Date: 2018-06-01
GUANGXI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention provides a preparation of graphene oxide-immobilized tetrakis (4-hydroxyphenyl) manganese porphyrin catalytic material in order to overcome...

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  • Preparation method and catalytic application of graphene oxide immobilized tetra(4-hydroxyphenyl) manganese porphyrin catalytic material
  • Preparation method and catalytic application of graphene oxide immobilized tetra(4-hydroxyphenyl) manganese porphyrin catalytic material
  • Preparation method and catalytic application of graphene oxide immobilized tetra(4-hydroxyphenyl) manganese porphyrin catalytic material

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preparation Embodiment 1

[0024] The preparation method of described graphene oxide immobilized tetrakis (4-hydroxyphenyl) manganese porphyrin catalytic material is made up of the following steps:

[0025] (1) Preparation of graphite oxide: Add 200 parts of concentrated sulfuric acid into a three-necked flask, put it in a cold trap and keep it for five minutes, then add 8 parts of graphite powder and 4 parts of sodium nitrate, let it react for 30 minutes, then slowly add high manganese 30 parts of potassium acid potassium, after reacting for 1 hour, take it out, wait for room temperature, continue to react in a water bath at 35°C for 1 hour, then add 500 parts of distilled water, continue to slowly add 150 parts of 5% hydrogen peroxide until the liquid turns yellow, and let it stand for stratification , remove the supernatant, wash with 1000 parts of 5% hydrochloric acid for several times until no sulfate ions are detected, and dry at 60°C for 48 hours to obtain graphite oxide;

[0026] (2) Preparation...

preparation Embodiment 2

[0029] The preparation method of described graphene oxide immobilized tetrakis (4-hydroxyphenyl) manganese porphyrin catalytic material is made up of the following steps:

[0030] (1) Preparation of graphite oxide: Add 250 parts of concentrated sulfuric acid into a three-necked flask, put it in a cold trap and keep it for five minutes, then add 10 parts of graphite powder and 5 parts of sodium nitrate, let it react for 30 minutes, then slowly add high manganese 38 parts of potassium acid potassium, after reacting for 1 hour, take it out, wait for room temperature, continue to react in a 35°C water bath for 1 hour, then add 625 distilled water, continue to slowly add 200 parts of 5% hydrogen peroxide until the liquid turns yellow, and let it stand for stratification. Remove the supernatant, wash with 1250 parts of 5% hydrochloric acid for several times until no sulfate ion is detected, and dry at 60°C for 48 hours to obtain graphite oxide;

[0031] (2) Preparation of graphene o...

preparation Embodiment 3

[0034] The preparation method of described graphene oxide immobilized tetrakis (4-hydroxyphenyl) manganese porphyrin catalytic material is made up of the following steps:

[0035](1) Preparation of graphite oxide: Add 300 parts of concentrated sulfuric acid into a three-necked flask, put it in a cold trap and keep it for five minutes, then add 12 parts of graphite powder and 6 parts of sodium nitrate, make it react for 30 minutes, then slowly add high manganese 45 parts of potassium acid potassium, after reacting for 1 hour, take it out, wait for room temperature, continue to react in a water bath at 35°C for 1 hour, then add 750 parts of distilled water, continue to slowly add 250 parts of 5% hydrogen peroxide until the liquid turns yellow, and let it stand for stratification , remove the supernatant, wash with 1500 parts of 5% hydrochloric acid for several times until no sulfate ion is detected, and dry at 60°C for 48 hours to obtain graphite oxide;

[0036] (2) Preparation ...

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Abstract

The invention relates to a preparation method and catalytic application of a graphene oxide immobilized tetra(4-hydroxyphenyl) manganese porphyrin catalytic material. The preparation method consists of the following steps: first, preparing graphite oxide by an improved Hermes method, preparing fluffy graphene oxide by microwave heating of the graphite oxide, then adding the fluffy graphene oxide into a tetra(4-hydroxyphenyl) manganese porphyrin solution dissolved by N,N-dimethylformamide, carrying out ultrasonic treatment at normal temperature for 6 hours, carrying out vacuum filtration, collecting filter cakes, and drying the filter cakes at 60 DEG C for 48 hours to obtain the required catalytic material. The catalytic material is applied to catalyzing oxygen to oxidize ethylbenzene to generate acetophenone and DL-1-phenylethanol; and under a reaction condition without adding any solvent or reducing agent, the conversion rate reaches 62.7%, and the yield of alcohol ketone is 42.0%. Inaddition, the catalyst can be reused for 5 times for cyclic catalysis, and still shows a good catalytic effect, and the catalyst has a practical application value and is an ideal biomimetic catalyst.

Description

technical field [0001] The invention belongs to the technical field of catalytic materials, in particular to a preparation method and catalytic application of graphene oxide immobilized tetrakis (4-hydroxyphenyl) manganese porphyrin catalytic material. Background technique [0002] The main products of ethylbenzene oxidation are acetophenone and DL-1-phenylethanol. Acetophenone is an important chemical raw material and an intermediate in the synthesis of other fragrances. It can be used in flavors, solvents and plastic plasticizers, and can also be used in pharmaceutical production. In industry, acetophenone can now be obtained from the by-products of phenol and acetone oxidized by cumene, and it can also be synthesized with benzene and acetyl chloride in the presence of ferric chloride, but this method will generate strong acid, which will cause corrosion to production equipment , while causing adverse effects on the environment. DL-1-phenylethyl alcohol is used in the or...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C29/50C07C33/22C07C45/36C07C49/78C07C27/12
CPCB01J31/1616B01J31/183B01J35/1014B01J35/1061B01J2231/70B01J2531/025B01J2531/72C07C29/50C07C45/36C07C33/22C07C49/78
Inventor 黄冠覃欢宴超郭勇安危素娟
Owner GUANGXI UNIV
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