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Heterogeneous catalyst for synthesis of phenol, and preparation method and application thereof

A heterogeneous catalyst, phenol technology, applied in the preparation of organic compounds, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of low selectivity, low synthesis yield, use of The problem of short lifespan, etc., can achieve the effect of improving benzene conversion rate and phenol selectivity, good phenol selectivity and high reactivity

Inactive Publication Date: 2011-12-14
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a high activity and low selectivity for the existing catalysts used in the synthesis of phenol, which have the disadvantages of low synthesis yield or low selectivity, easy deactivation of heterogeneous catalysts, low stability, and short service life. Highly Selective Heterogeneous Catalysts for the Synthesis of Phenol

Method used

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  • Heterogeneous catalyst for synthesis of phenol, and preparation method and application thereof
  • Heterogeneous catalyst for synthesis of phenol, and preparation method and application thereof
  • Heterogeneous catalyst for synthesis of phenol, and preparation method and application thereof

Examples

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Effect test

example 1

[0029] Example 1: Cu II (salen)-PMo 11 Preparation of V / MCM-41 (salen=disalicylaldehyde ethylenediamine).

[0030] (1) 5-chloromethyl salicylaldehyde was prepared by literature method, and the yield was 40-60%. (Sun Zhenhua et al., Liaoning Chemical Industry, 2010, 39(5)461)

[0031] (2) 5-chloromethyl salicylaldehyde and allyl alcohol were refluxed in xylene for 24 hours in a molar ratio of 1:1 to obtain salicylaldehyde-5-methoxy allyl alcohol ether.

[0032] (3) Mix 1 gram of MCM-41 and 0.016mol 3-mercaptopropyltrimethoxysilane in dry toluene, and the concentration of 3-mercaptopropyltrimethoxysilane in dry toluene is 1.6mol / L. Mixture in N 2 Reflux for 48 hours under protection, filter the solid and perform Soxhlet extraction with dichloromethane for 24 hours to obtain SH-MCM-41. 1gSH-MCM-41, 5mmol salicylaldehyde-5-methoxy allyl alcohol ether, 5mmol 5-dimethylaminosalicylaldehyde, 5mmol ethylenediamine in CH 2 Cl 2 Mix in medium, react for 24h to get the loaded sale...

example 2

[0038] Example 2: Cu II (salen)-PMo 10 V 2 Preparation of / MCM-41 (salen=disalicylaldehyde ethylenediamine).

[0039] Steps (1)-(3) of this example are the same as steps (1)-(3) of Example 1.

[0040] The 4th step is: loading copper salen complex and H 5 PMo 10 V 2 o 40 React in anhydrous methanol acidified with HCl at a molar ratio of 1:1 for 24 h, filter, CH 2 Cl 2 Washed, vacuum dried, heterogeneous catalyst.

[0041] (5) Take the prepared Cu II (salen)-PMo 10 V 2 / MCM-41, benzene, 30%H 2 o 2 1. Add anhydrous acetonitrile into the three-necked flask at a mass ratio of 2:6:14:78, install a condenser tube and a thermometer, and use magnetic stirring. After the temperature rose to 65° C., reacted for 6 hours, filtered the catalyst, collected the filtrate, and analyzed by gas chromatography, the yield of phenol was 14.8%, and the selectivity was 90.5%.

[0042] (6) Take the prepared Cu II (salen)-PMo 10 V 2 / MCM-41 Benzene, Ascorbic Acid, Glacial Acetic Acid, ...

example 3

[0043] Example 3: Cu II (saloph)-PMo 11 Preparation of V / MCM-41 (saloph = salicylaldehyde ortho-phenylenediamine).

[0044] Steps (1)-(2) of this example are the same as steps (1)-(2) of Example 1.

[0045] Step (3) is: mix 1 gram of MCM-41, 0.016mol 3-mercaptopropyltrimethoxysilane in dry toluene, the concentration of 3-mercaptopropyltrimethoxysilane in dry toluene is 1.6mol / L. Mixture in N 2 Reflux for 48 hours under protection, filter the solid and perform Soxhlet extraction with dichloromethane for 24 hours to obtain SH-MCM-41. Mix 1 gram of SH-MCM-41 and 5 mmol of salicylaldehyde-5-methoxy allyl alcohol ether in xylene, and 1 gram of dried solid contains about 3 mmol of salicylaldehyde. Then add and dry the CH of 5-dimethylamino salicylaldehyde and o-phenylenediamine equimolar salicylaldehyde contained in the dry solid 2 Cl 2 The solution was stirred and reacted at room temperature for 24 hours to obtain the loaded saloph ligand, and the thermogravimetric results ...

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Abstract

The invention discloses a heterogeneous catalyst for the synthesis of phenol, and a preparation method and application thereof. The preparation method of the copper Schiff base / heteropoly acid supermolecular compound which is shown in formula (I) and loaded on a silicon-based molecular sieve comprises the functional group modification of a carrier, the preparation of a loaded copper Schiff base complex, the supermolecular combination of the copper complex loaded on the silicon-based molecular sieve and heteropoly acid and the like. In the formula (I), X3 is one of the following elements or groups: S, CONH-, OCO- and O. X1 / X2 is one of the following elements or groups: F, Cl, Br, I, NO2, R, C(CH3)3, COOR, OR and H. Y is NHR or NR2. Z is one of the following groups: -CH2-(CH2)n-CH2-C6H10 and C6H4, wherein n is 0 or 1. POM is H3+nPW12-nVnO40 or H3+nPMo12-nVnO40, wherein n is 1-3. R is CH3, C2H5 or C3H7. The compound can be used in the synthesis reaction for directly oxidizing benzene into phenol.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, and in particular relates to a heterogeneous catalyst for synthesizing phenol and its preparation method and application. Background technique [0002] Phenol is an important chemical raw material, which is widely used in the production of various polymer raw materials such as anti-aging agents, pharmaceutical intermediates, bisphenol A, phenolic resin, and nylon-6. The production method currently adopted is a three-step process for cumene. Benzene and propylene are catalyzed by Lewis acid to generate cumene, then cumene is oxidized to cumene hydroperoxide, and then decomposed under the action of sulfuric acid to obtain phenol and acetone. The main disadvantages of this process are low single-pass yield, a large amount of by-product acetone, and the explosive intermediate compound cumene hydroperoxide, which is not conducive to safe production. The direct oxidation of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/36C07C39/04C07C37/60
CPCY02P20/52
Inventor 陈丽娟向育君王鹏飞郝小礼冯涛
Owner HUNAN UNIV OF SCI & TECH
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