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A kind of method for preparing p-benzoquinone

A p-benzoquinone and solvent technology, applied in the field of preparation of p-benzoquinone, can solve the problems of corrosion equipment, long reaction time, complicated process, etc., and achieve the effects of reducing equipment corrosion, high atom utilization rate, and good product selectivity

Active Publication Date: 2021-01-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the method for industrially synthesizing p-benzoquinone is mainly catalytic oxidation, mainly including aniline oxidation and phenol catalytic oxidation, but the process is complicated, a large amount of waste residue is produced by-product, serious pollution, corrosion equipment, high cost, and difficult to large-scale production (p-benzoquinone Research Progress on Synthetic Methods of Diphenols. Liu Yingxin, Li Xinxue, Wei Xionghui. Chemical Bulletin, 2004,67(12):869-875)
In recent years, a large number of studies on the preparation of p-benzoquinone by electrochemical oxidation of benzene as raw material have been carried out at home and abroad, but the conversion rate of benzene is low, the energy consumption is high, a large amount of benzene needs to be separated and recycled, the reaction time is long, and the electrode and diaphragm The lifespan is still difficult to meet the needs of industrial production (research progress on p-benzoquinone synthesis methods. Sui Lingling, Li Sen, Zhang Di. Liaoning Chemical Industry, 2012, 11:032)

Method used

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  • A kind of method for preparing p-benzoquinone
  • A kind of method for preparing p-benzoquinone
  • A kind of method for preparing p-benzoquinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] This example is used to illustrate the preparation method of the titanium-silicon molecular sieve used in the present invention.

[0059] Under stirring conditions, mix ethyl orthosilicate, tetrapropylammonium hydroxide, tetrabutyl titanate and deionized water to obtain a molar ratio of SiO 2 : Structure directing agent: TiO 2 :H 2 O=1:0.2:0.025:50 mixture. Press SiO again 2 The molar ratio to silylating agent is 1:0.1, SiO 2 The weight ratio of the natural polymer compound is 1:0.1, add quaternized cellulose and N-phenyl-3-aminopropyltrimethoxysilane to the titanium-silicon molecular sieve precursor gel mixture, and stir evenly Finally, the obtained silylating agent and the titanium-silicon molecular sieve precursor treated with the modified natural polymer compound were transferred to a pressure-resistant stainless steel reaction kettle; under stirring conditions, heated to 170°C and crystallized under autogenous pressure for 24 hours.

[0060] After the stainles...

Embodiment 2

[0062] This example is used to illustrate the preparation method of the titanium-silicon molecular sieve used in the present invention.

[0063] Under stirring conditions, mix propyl orthosilicate, tetraethylammonium hydroxide, tetraethyl titanate and deionized water to obtain a molar ratio of SiO 2 : Structure directing agent: TiO 2 :H 2 O=1:0.01:0.01:16 mixture. Press SiO again 2 The molar ratio to silylating agent is 1:0.04, SiO 2 The weight ratio of the natural polymer compound is 1:0.05. Add cellulose and trimethylchlorosilane to the titanium-silicon molecular sieve precursor gel mixture. After stirring evenly, the obtained silylating agent and natural polymer compound are treated The titanium-silicon molecular sieve precursor was transferred to a pressure-resistant stainless steel reactor; under stirring conditions, it was heated to 190°C and crystallized under autogenous pressure for 48h.

[0064] After the stainless steel pressure-resistant reactor was lowered to ...

Embodiment 3

[0066] This example is used to illustrate the preparation method of the titanium-silicon molecular sieve used in the present invention.

[0067] Under stirring conditions, mix silica gel, tetrabutylammonium hydroxide, tetrapropyl titanate and deionized water to obtain a molar ratio of SiO 2 : Structure directing agent: TiO 2 :H 2 O=1:1:0.03:90 mixture. Press SiO again 2 The molar ratio to silylating agent is 1:0.18, SiO 2 The weight ratio of the natural polymer compound is 1:0.2. Add tapioca cationic starch and N-phenyl-3-aminopropyltrimethoxysilane to the titanium-silicon molecular sieve precursor gel mixture. After stirring evenly, put The titanium-silicon molecular sieve precursor treated with the obtained silylating agent and the modified natural polymer compound was transferred to a pressure-resistant stainless steel reaction kettle; under stirring conditions, it was heated to 120° C. and crystallized under autogenous pressure for 8 hours.

[0068] After the stainles...

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Abstract

The invention discloses a method for preparing p-benzoquinone. The method comprises the following steps: enabling benzene, an oxidizing agent and a catalyst to be reacted in presence of a solvent, wherein the catalyst is a titanium silicalite molecular sieve catalyst, the particle size of the titanium silicalite molecular sieve is 250-350nm, the relative crystallinity is 45-150%, and the specific surface area is 600-1000m<2> / g. The method is mild in reaction conditions, high in product selectivity, high in reaction rate and less in by-products.

Description

technical field [0001] The invention relates to a method for preparing p-benzoquinone. Background technique [0002] p-Benzoquinone is golden yellow prism, has strong oxidizing property, can sublimate and distill with water vapor, is soluble in hot water, ethanol and ether, and is an important fine chemical raw material with broad application prospects , used in the synthesis of intermediates in dyes, flame retardants, pharmaceuticals, rubber antioxidants, pesticides, dyes, electrodes and other industries. [0003] At present, the method for industrially synthesizing p-benzoquinone is mainly catalytic oxidation, mainly including aniline oxidation and phenol catalytic oxidation, but the process is complicated, a large amount of waste residue is produced by-product, serious pollution, corrosion equipment, high cost, and difficult to large-scale production (p-benzoquinone Research progress on synthesis methods of diphenols. Liu Yingxin, Li Xinxue, Wei Xionghui. Chemical Bullet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C50/04C07C46/04
CPCC07C46/04C07C50/04
Inventor 武杰林民朱斌彭欣欣王宝荣
Owner CHINA PETROLEUM & CHEM CORP