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Synthesis of mesoporous catalyst for synthesizing phenol through direct hydroxylation of benzene

A catalyst and chemical synthesis technology, applied in the field of preparation of mesoporous catalysts, can solve problems such as low activity and difficult separation of products

Inactive Publication Date: 2018-12-07
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved in the present invention is to develop a three-dimensional ordered mesoporous silica KIT-6 as a carrier to support acetyl Vanadyl acetonate [VO(acac) 2 ] of heterogeneous catalysts

Method used

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  • Synthesis of mesoporous catalyst for synthesizing phenol through direct hydroxylation of benzene
  • Synthesis of mesoporous catalyst for synthesizing phenol through direct hydroxylation of benzene
  • Synthesis of mesoporous catalyst for synthesizing phenol through direct hydroxylation of benzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Dissolve 10 parts by mass of mesoporous silica (KIT-6) and 5 parts by mass of APTES in toluene, and stir for 4 hours at 80°C under nitrogen protection;

[0027] (2) After the reaction, it was preliminarily washed with toluene, and then stirred and refluxed with toluene at 100°C for 2 hours, and filtered, washed and dried to obtain ammonia-functionalized mesoporous silica (KIT-6-NH 2 );

[0028] (3) 3 parts by mass of VO(acac) 2 and 5 parts by mass of KIT-6-NH 2 Dissolved in toluene, stirred and refluxed at 120°C for 20 hours, cooled, filtered, washed and dried to obtain ammonium-functionalized mesoporous silica-supported vanadyl acetylacetonate material (KIT-6-NH 2 -V);

[0029] (4) Add 0.1 parts by mass of catalyst to the acetonitrile-acetic acid solution mixed with 4.5 parts by mass of benzene and 20 parts by mass of 30 wt% hydrogen peroxide, and react at 70°C for 6h;

[0030] (5) After the reaction is completed, the catalyst is separated. The liquid phase co...

Embodiment 2

[0032] (1) Dissolve 10 parts by mass of mesoporous silica (KIT-6) and 5 parts by mass of APTMS in toluene, and stir for 2 hours at 120°C under nitrogen protection;

[0033] (2) After the reaction, it was preliminarily washed with toluene, then stirred and refluxed with toluene at 80°C for 1 h, and filtered, washed and dried to obtain ammonia-functionalized mesoporous silica (KIT-6-NH 2 );

[0034] (3) 3 parts by mass of VO(acac) 2 and 5 parts by mass of KIT-6-NH 2 Dissolved in toluene, stirred and refluxed at 100°C for 24 hours, cooled, filtered, washed and dried to obtain ammonium-functionalized mesoporous silica-supported vanadyl acetylacetonate material (KIT-6-NH 2 -V);

[0035](4) Add 0.35 parts by mass of catalyst to the acetonitrile-acetic acid solution mixed with 4.5 parts by mass of benzene and 20 parts by mass of 30 wt% hydrogen peroxide, and react at 50°C for 4h;

[0036] (5) After the reaction is completed, the catalyst is separated. The liquid phase components...

Embodiment 3

[0038] (1) Put 10 parts by mass of mesoporous silica (KIT-6) and 5 parts by mass of APTES in acetonitrile, and stir for 2 hours at 100°C under nitrogen protection;

[0039] (2) After the reaction, it was preliminarily washed with acetonitrile, and then stirred and refluxed with acetonitrile at 100°C for 2 hours, then filtered, washed and dried to obtain ammonia-functionalized mesoporous silica (KIT-6-NH 2 );

[0040] (3) 3 parts by mass of VO(acac) 2 and 5 parts by mass of KIT-6-NH 2 Dissolved in acetonitrile, stirred and refluxed at 110°C for 24h, cooled, filtered, washed and dried to obtain ammonium-functionalized mesoporous silica-supported vanadyl acetylacetonate material (KIT-6-NH 2 -V);

[0041] (4) Add 0.4 parts by mass of catalyst to the acetonitrile-acetic acid solution mixed with 4.5 parts by mass of benzene and 20 parts by mass of 30 wt% hydrogen peroxide, and react at 60°C for 6h;

[0042] (5) After the reaction is completed, the catalyst is separated. The liq...

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Abstract

The invention relates to a catalyst for synthesizing phenol through direct hydroxylation of benzene and a preparation method thereof. Ammonia functionalization mesoporous silica is used as a carrier of the catalyst, and vanadiumoxy acetylacetonate is used as an active component of the catalyst. The catalyst is applied to the reaction of synthesizing the phenol through the direct hydroxylation of the benzene under the condition of hydrogen peroxide; when the reaction temperature is 50-70 DEG C, the reaction time is 4-6h, the conversion rate of benzene is 15-20%, the selectivity of phenol is 96-99%, and the yield of final phenol is 14-20%. Compared with the conventional catalyst for catalytic reaction, the catalyst has the advantages of being simple in product separation, relatively high incatalytic activity and the like.

Description

technical field [0001] The invention belongs to the field of heterogeneous catalysis, and in particular relates to a preparation method of a mesoporous catalyst used in the direct hydroxylation of benzene to synthesize phenol. Background technique [0002] Phenol is an important chemical raw material, mainly used in the synthesis of phenolic resin. In addition, phenol also has important uses in the synthesis fields of medicine, dyestuff, rubber and pesticide. At present, more than 95% of the phenol in the world is mainly synthesized through the three-step cumene method. This method has higher energy consumption, and the one-way yield of phenol is low (<5%), and co-product acetone in equimolar amounts is also present, and the equipment is corroded more seriously during the reaction process. In order to solve these problems, researchers have made many new attempts and proposed a series of new synthesis processes. Among them, the direct hydroxylation of benzene to phenol ...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C39/04C07C37/60
CPCB01J31/2213B01J2231/70B01J2531/0258B01J2531/56C07C37/60C07C39/04Y02P20/52
Inventor 许杰洪颖马丁阳程明杰薛冰李永昕
Owner CHANGZHOU UNIV
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