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Method for gas phase alkylation of phenol with methanol, mesoporous molecular sieve and preparation method and application thereof

A mesoporous molecular sieve and alkylation mesoporous technology, which is applied in molecular sieve catalysts, catalyst activation/preparation, preparation of organic compounds, etc., can solve the problem of low ortho selectivity and achieve remarkable results

Active Publication Date: 2013-05-08
BAOWU CHARCOAL MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the first aspect of the present invention is to propose a mesoporous molecular sieve catalyst for gas-phase alkylation of phenol-methanol to solve the technical problem that the current MCM-41 mesoporous molecular sieve is used for gas-phase alkylation of phenol-methanol, and the ortho selectivity is low

Method used

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  • Method for gas phase alkylation of phenol with methanol, mesoporous molecular sieve and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Weigh 0.722 grams (0.00617mol) NH 4 VO 3 and 0.261 g (0.00161 mol) C 2 h 2 o 4 4H 2 O, was added to 10.02 grams (0.556mol) of deionized water at room temperature, stirred and dissolved to obtain solution A; 2.520 grams (0.00624mol) of Fe(NO 3 ) 3 9H 2 O was added to the above solution A, stirred and dissolved to obtain solution B; weighed 10.061 grams of 20-40 mesh MCM-41, which was roasted at 823K for 8 hours, and placed in a container, then added the above solution B, and stirred evenly to obtain mixture C; Mixture C was dried at 378K for 12 hours, and then roasted at 823K for 8 hours to obtain solid D; sieve solid D, and sieve 20-40 mesh particles as phenol-methanol gas-phase alkylation Fe-V / MCM-41 catalyst.

[0042] Using Fe-V / MCM-41 as a catalyst, the ortho-selective performance of phenol-methanol gas-phase alkylation was investigated. At normal pressure, reaction temperature 713K, mass space velocity 0.8h -1 1. Under the reaction condition of methanol:ph...

Embodiment 2

[0044] Weigh 0.362 grams (0.00309mol) NH 4 VO 3 and 0.185 g (0.00114 mol) C 2 h 2 o 4 4H 2 O, was added to 10.05 grams (0.558mol) of deionized water at room temperature, stirred and dissolved to obtain solution A; weighed 5.013 grams (0.01241mol) of Fe(NO 3 ) 3 9H 2 Add O to the above solution A, stir and dissolve to obtain solution B; weigh 10.052 grams of 20-40 mesh MCM-41, which has been roasted at 823K for 8 hours, and place it in a container, then add the above solution B, and stir evenly to obtain mixture C; Mixture C was dried at 378K for 12 hours, and then roasted at 823K for 6 hours to obtain solid D; sieve solid D, and sieve 20-40 mesh particles for phenol-methanol vapor-phase alkylation of Fe-V / MCM-41 catalyst.

[0045] Using Fe-V / MCM-41 as catalyst, under normal pressure, reaction temperature 713K, mass space velocity 0.8h -1 1. Under the reaction condition of methanol:phenol=5:1 molar ratio, the reaction was carried out for 10 hours. The composition of th...

Embodiment 3

[0047] Weigh 1.445 grams (0.01235mol) NH 4 VO 3 and 0.718 g (0.00443 mol) C 2 h 2 o 4 4H 2 O, was added to 10.03 grams (0.557mol) of deionized water at room temperature, stirred and dissolved to obtain solution A; weighed 1.268 grams (0.00314mol) of Fe(NO 3 ) 3 9H 2 Add O to the above solution A, stir and dissolve to obtain solution B; weigh 10.032 grams of 20-40 mesh MCM-41, which has been roasted at 823K for 8 hours, and place it in a container, then add the above solution B, and stir evenly to obtain mixture C; Mixture C was dried at 378K for 12 hours, and then roasted at 823K for 6 hours to obtain solid D; sieve solid D, and sieve 20-40 mesh particles for phenol-methanol vapor-phase alkylation of Fe-V / MCM-41 catalyst.

[0048] Using Fe-V / MCM-41 as catalyst, under normal pressure, reaction temperature 713K, mass space velocity 0.8h -1 1. Under the reaction condition of methanol:phenol=5:1 molar ratio, the reaction was carried out for 10 hours, and the composition o...

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Abstract

The invention relates to a phenol alkylate mesoporous molecular sieve catalyst, preparation method thereof and application. The method for gas phase alkylation of phenol with methanol provided by the invention uses the mesoporous molecular sieve provided therein as a catalyst. The main body of the mesoporous molecular sieve of the invention is MCM-41 mesoporous molecular sieve, and the metallic active ingredient which is loaded on the main body is Fe-V active ingredient. The method for preparing a mesoporous molecular sieve of the invention comprises the step of dispersing and loading the Fe-V active ingredient on the MCM-41 mesoporous molecular sieve by means of an immersion method. The mesoporous molecular sieve provided by the invention is used as a catalyst during the process of gas phase alkylation of phenol with methanol. The method solves the technical problem of the existing MCM-41 mesoporous molecular sieve which has low ortho position selectivity during the process of gas phase alkylation of phenol with methanol.

Description

technical field [0001] The invention relates to a method for gas-phase alkylation of phenol and methanol, and also relates to a mesoporous molecular sieve, a preparation method of the mesoporous molecular sieve and an application of the mesoporous molecular sieve. Background technique [0002] The synthesis of o-cresol and 2,6-xylenol by vapor-phase alkylation of phenol and methanol is the most advanced and competitive process route in the world. It has been industrialized in developed countries, and its core technology is catalyst preparation. Recently, the emergence of mesoporous molecular sieves with adjustable pore size and acidity characteristics, high stability, and high specific surface area has brought new development opportunities for the gas-phase alkylation of phenol to methanol. [0003] The pore diameter of MCM-41 mesoporous molecular sieve can be adjusted between 1.5nm and 10nm, breaking through the previous limit of molecular sieve pore diameter not exceeding...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/78B01J37/04B01J37/08C07C39/07C07C37/16
Inventor 王仁远王焕煜朱春燕唐寄云
Owner BAOWU CHARCOAL MATERIAL TECH CO LTD