Activator for chemical combination of phenol by benzene hydroxide radical and the application method

An application method and catalyst technology, applied in the direction of physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve the problem of low phenol yield, loss of active components, and catalyst failure Reuse and other issues to achieve a single product, reduce pollution, and save raw materials

Inactive Publication Date: 2007-09-12
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to avoid the danger caused by the mixture of molecular oxygen and explosive reducing gas (hydrogen or carbon monoxide), there are many reports on catalysts for benzene hydroxylation reaction in mild ascorbic acid liquid phase reaction system, such as heteropoly compound catalysts, supported copper , vanadium catalysts, but these catalysts all have the disadvantages that active components will be lost during the reaction process, the catalyst cannot be reused, and the yield of phenol is low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Preparation of Molecular Sieve-Supported Transition Metal Phthalocyanine Catalyst FePc-MCM-41

[0023] The first step: mix 1g MCM-41 molecular sieve with 10g of 5% FeSO 4 The aqueous solution was mixed, refluxed at 70°C for 24 hours, filtered, dried, and calcined at 500°C for 2 hours to obtain a powder material.

[0024] The second step: mix the powder obtained in the first step with 3.7g of phthalic anhydride, 6g of urea and 0.2g of ammonium molybdate, slowly heat up in an oil bath, and constantly stir the mixture. When the state of the mixture changes from liquid to After solidification, raise the reaction temperature to 240°C and keep it warm for 24 hours. After cooling, alternately boil and wash with dilute sodium carbonate and hydrochloric acid for 10 times, filter while hot until the filtrate is basically colorless, and then wash with ethanol until it is almost free. color, FePc-MCM-41 was obtained after drying.

Embodiment 2

[0026] Preparation of Molecular Sieve Supported Transition Metal Phthalocyanine Catalyst V / CuPc-SBA-15

[0027] Step 1: Mix 1g of SBA-15 molecular sieve with 10g of NH at the same time 4 VO 3 and 1% CuSO 4 The aqueous solution was mixed, refluxed at 90°C for 24 hours, filtered, dried, and calcined at 550°C for 4 hours to obtain a powder material.

[0028] The second step: mix the powder obtained in the first step with 7.4g of phthalic anhydride, 12g of urea and 0.5g of ammonium molybdate, slowly heat up in an oil bath, and constantly stir the mixture. When the state of the mixture changes from liquid to After solidification, raise the reaction temperature to 250°C and keep it warm for 4 hours. After cooling, alternately boil and wash with dilute sodium carbonate and hydrochloric acid for 10 times, and filter while hot until the filtrate is basically colorless. It was washed with ethanol until it was almost colorless, and V / CuPc-SBA-15 was obtained after drying.

Embodiment 3

[0030] Preparation of Molecular Sieve Supported Transition Metal Phthalocyanine Catalyst MnPc-Y

[0031] The first step: 1g Y molecular sieve and 10g content are 6% Mn(NO 3 ) 2 The aqueous solution was mixed, refluxed at 30°C for 12 hours, filtered, dried, and calcined at 500°C for 6 hours to obtain a powder material.

[0032] The second step: mix the powder obtained in the first step with 0.74g of phthalic anhydride, 2.4g of urea and 0.1g of ammonium molybdate, slowly heat up in an oil bath, and constantly stir the mixture. When the state of the mixture changes from liquid to After it is solid, raise the reaction temperature to 300°C and keep it warm for 8 hours. After cooling, it is boiled and washed 8 times with dilute sodium carbonate and hydrochloric acid alternately, and filtered while it is hot until the filtrate is basically colorless, and then washed with ethanol until Basically colorless, MnPc-Y can be obtained after drying.

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PUM

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Abstract

The present invention discloses one kind of catalyst for hydroxylating benzene to synthesize phenol and its application method. The catalyst with molecular sieve as carrier is prepared through soaking the carrier to support salt of transition metal, roasting, mixing with phthalic anhydride, urea and ammonium molybdenate, and in-situ solid phase synthesis. It is used in the oxidation of benzene dissolved in solvent comprising acetic acid and water with oxygen as oxidant in the presence of reductant ascorbic acid to synthesize phenol. The catalyst of the present invention has no loss of active components, easy separation from the reaction system, mild reaction condition, high yield of target product phenol and other advantages.

Description

technical field [0001] The invention relates to a catalyst and its application method, in particular to a catalyst for synthesizing phenol by hydroxylation of benzene and its application method. Background technique [0002] Phenol is a very important chemical raw material. It is the precursor for the production of bisphenol A, phenolic resin, caprolactam, nylon-6, detergents, adhesives, antioxidants and many other chemical products. Therefore, the market demand for phenol The quantity is very large, among various chemical products, its output ranks in the top ten. At present, the methods used in the industrial production of phenol are all indirect synthesis methods, that is, first reacting benzene to produce intermediate products, and then reacting the intermediate products to produce phenol. The indirect method of synthesizing phenol is low in yield due to a large amount of raw material consumption, resulting in high cost and serious environmental pollution. Therefore, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J31/26B01J37/02C07C39/04C07C37/58
CPCY02P20/52
Inventor 单永奎顾颖颖华春燕侯亚伟孟静赵新华
Owner EAST CHINA NORMAL UNIV
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