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Dimethyl ether carbonylation catalyst and preparation method and application thereof

A technology of dimethyl ether and carbonylation, which is applied in the direction of physical/chemical process catalysts, carbon monoxide or formate reaction preparation, molecular sieve catalysts, etc., can solve the problems of easy blockage of molecular sieves, unfavorable reactivity of butene isomerization reaction, etc. To achieve the effect of improving activity and stability

Active Publication Date: 2018-01-05
ZHENGZHOU TOBACCO RES INST OF CNTC
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Problems solved by technology

[0005] The Chinese invention patent with the publication number of CN 101475432A discloses a method for the selectivity of butene double bond isomerization reaction. The method of pre-carbon deposition is used to prepare a pre-carbon-deposited aluminosilicate catalyst to improve the isomerization of butene double bonds. However, the starting point of this patent is that the strong acid sites in the pores are covered by pre-carbon deposition, while the weak acid sites that play a role in isomerization are not covered, and the molecular sieves are easily blocked in the preparation method of pre-carbon deposition catalysts The orifice is unfavorable to the reactivity of the subsequent butene isomerization reaction

Method used

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  • Dimethyl ether carbonylation catalyst and preparation method and application thereof
  • Dimethyl ether carbonylation catalyst and preparation method and application thereof

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Embodiment 1

[0034] The preparation method of the catalyst of the dimethyl ether carbonylation of the present embodiment, such as figure 1 shown, including the following steps:

[0035] 1) Converting mordenite molecular sieves into hydrogen-type mordenite by ammonia exchange method, filling hydrogen-type mordenite in a fixed-bed reactor, and heating to 400° C. for 1 hour activation under nitrogen atmosphere;

[0036] 2) After activation, lower the temperature to 350° C. and feed propylene into the catalyst bed for catalytic reaction. When the conversion rate of propylene is lower than 5%, stop feeding the substrate, and use nitrogen to purge the catalyst bed to lower the temperature to obtain precursor A ;

[0037] 3) Mix the precursor A obtained in step 2) with the dispersant deionized water, place it in a planetary ball mill at a speed of 200 rpm for 12 hours, and then filter, wash and dry it. The mass ratio of deionized water to precursor A is is 30:1.

Embodiment 2

[0039] The preparation method of the catalyst of the dimethyl ether carbonylation of the present embodiment comprises the following steps:

[0040] 1) Converting mordenite molecular sieves into hydrogen-type mordenite by ammonia exchange method, filling hydrogen-type mordenite in a fluidized bed reactor, and heating to 500° C. for activation for 1 h under a nitrogen atmosphere;

[0041] 2) After activation, feed 1-butene and p-xylene to the catalyst bed at 500°C for catalytic reaction, the molar ratio of 1-butene and p-xylene is 1:1, and 1-butene and p-xylene When the conversion rate of toluene is lower than 5%, the substrate feeding is stopped, and the catalyst bed is purged with helium to lower the temperature to obtain the precursor A;

[0042] 3) Mix the precursor A obtained in step 2) with the dispersant deionized water, place it in a planetary ball mill and mill it at a speed of 350 rpm for 8 hours, then filter, wash and dry it. The mass ratio of deionized water to precu...

Embodiment 3

[0044] The preparation method of the catalyst of the dimethyl ether carbonylation of the present embodiment comprises the following steps:

[0045] 1) Converting mordenite molecular sieves into hydrogen-type mordenite by ammonia exchange method, filling hydrogen-type mordenite in a fluidized bed reactor, and heating to 450° C. for activation for 2 hours under a nitrogen atmosphere;

[0046] 2) After activation, keep 450 DEG C to feed isopentene into the catalyst bed for catalytic reaction, and when the conversion rate of isopentene is lower than 5%, stop feeding the substrate, and use helium to blow down the catalyst bed to lower the temperature. Get precursor A;

[0047] 3) Mix the precursor A obtained in step 2) with the dispersant methanol, place it in a planetary ball mill and mill it at a speed of 300rpm for 8 hours, then filter, wash and dry it. The mass ratio of methanol to precursor A is 1:1 .

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Abstract

The invention relates to a dimethyl ether carbonylation catalyst and a preparation method and application thereof, and belongs to the technical field of chemical catalysis. The preparation method of the dimethyl ether carbonylation catalyst comprises the following steps that firstly, a catalytic reaction is conducted on an activated hydrogen type molecular sieve and micromolecule organic substances at the temperature of 300-600 DEG C, the reaction is stopped when the conversion rate of the micromolecular organic substances is lower than 5%, and a precursor A is obtained, wherein the moleculardynamic diameter of the micromolecular organic substances is 0.4-0.7 nm; secondly, the precursor A is mixed with a dispersing agent, ball milling is conducted to obtain mixed slurry, and then solid-liquid separation, washing and drying are conducted to obtain the catalyst, wherein the dispersing agent is any one or more of water, methanol and ethyl alcohol. The dimethyl ether carbonylation catalyst obtained through the method has high selectivity and long service life in the process of preparing methyl acetate.

Description

technical field [0001] The invention relates to a catalyst for carbonylation of dimethyl ether, a preparation method and application thereof, and belongs to the technical field of chemical catalysis. Background technique [0002] Methyl acetate (methyl acetate) is widely used in textile, perfume and pharmaceutical industries, and is an important intermediate of organic raw materials. The downstream products mainly include acetic acid, acetic anhydride, methyl acrylate, vinyl acetate, acetamide, etc. In China, the production of methyl acetate is mainly the traditional esterification method. This method has the problems of complex separation of product and catalyst, expensive and scarce precious metal rhodium, and iodides cause severe corrosion to equipment. Solid acid catalyzed carbonylation of dimethyl ether to produce methyl acetate is a novel route. The catalyst used in the process is a solid catalyst, which is easy to separate without corrosion and can solve the problem ...

Claims

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Application Information

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IPC IPC(8): B01J29/18B01J29/65C07C67/37C07C69/14
Inventor 王金棒高健韩丽程多福高运谦邱纪青汪志波张仕华郑路刘亚丽程彪
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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