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Catalyst for carbonylation of dimethyl ether to prepare methyl acetate and its preparation method and use

A methyl acetate and catalyst technology, applied in the field of catalytic chemistry, can solve the problems such as inability to selectively remove twelve-membered ring pore channels, easy collapse of molecular sieve structure, large mass transfer resistance and easy carbon deposition, etc. Reduced maintenance costs and long catalyst life

Active Publication Date: 2017-06-16
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, solid acid catalysts for dimethyl ether carbonylation are usually dealuminated by nitric acid or hydrochloric acid, which cannot selectively remove acid sites in the twelve-membered ring channels, lower crystallinity, easy collapse of molecular sieve structure, and mass transfer resistance. Disadvantages of easy carbon deposition and low catalyst life

Method used

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  • Catalyst for carbonylation of dimethyl ether to prepare methyl acetate and its preparation method and use
  • Catalyst for carbonylation of dimethyl ether to prepare methyl acetate and its preparation method and use
  • Catalyst for carbonylation of dimethyl ether to prepare methyl acetate and its preparation method and use

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Effect test

preparation example Construction

[0032] The present invention also provides the preparation method of above-mentioned catalyst:

[0033] For the catalyst containing the hydrogen type mordenite molecular sieve of silicon tetrachloride vapor dealumination, its main preparation steps are as follows:

[0034] a) contacting hydrogen-form mordenite with silicon tetrachloride vapor at 500-700° C. to obtain the hydrogen-form mordenite molecular sieve dealuminated by silicon tetrachloride vapor;

[0035] b) drying and calcining the hydrogen-type mordenite molecular sieve obtained in step a) after steam dealumination of silicon tetrachloride to obtain the catalyst for the carbonylation of dimethyl ether to produce methyl acetate.

[0036] The above-mentioned catalyst containing mesoporous, its main preparation steps are as follows:

[0037] a) contacting hydrogen-form mordenite with silicon tetrachloride vapor at 500-700° C. to obtain the hydrogen-form mordenite molecular sieve dealuminated by silicon tetrachloride va...

Embodiment 1

[0081] Example 1: Preparation of silicon tetrachloride vapor dealuminated mordenite molecular sieve

[0082] Weigh 1 g of hydrogen-type mordenite, fix both ends in a quartz tube with quartz wool, and let 273K saturated silicon tetrachloride vapor carried by nitrogen gas into it. The obtained solid sample is washed with deionized water, separated by filtration, dried and calcined to obtain the desired catalyst for carbonylation of dimethyl ether to produce methyl acetate. The temperature and time of silicon tetrachloride vapor treatment, the temperature and time of solid sample drying and roasting are shown in Table 1.

[0083] Table 1

[0084]

Embodiment 2

[0085] Embodiment 2: the reaction performance evaluation of catalyst

[0086] The 40-60 mesh sample obtained by tableting, crushing and sieving the catalyst powder obtained in Example 1 was used in the carbonylation of dimethyl ether to produce methyl acetate for performance measurement. 1.0 g of each catalyst was loaded into the reactor respectively, and the mixed gas of dimethyl ether, hydrogen, and carbon monoxide was passed through the reactor at a temperature of 200° C., a pressure of 2 MPa, and a gas volume flow rate of 1500 ml / g / h. Among them, the gas flow rate F(H 2 +DME)=16.4ml / min, DME / CO / H 2 =5 / 35 / 60 (volume ratio). The results of the catalyst reactions are listed in Table 2.

[0087] Table 2

[0088] catalyst Dimethyl ether conversion rate a (%)

Methyl acetate selectivity b (%)

life c (h)

1# 50.5 94.4 9.3 2# 48.1 94.3 8.0 3# 40.3 97.2 14.5 4# 44.2 98.8 17.8 5# 46.3 94.3 10.1 6# 44.5 96.5 20.1 ...

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Abstract

The invention provides a catalyst for preparing methyl acetate by carbonylation of dimethyl ether, a preparation method and application thereof. More specifically, the present invention provides a catalyst for the carbonylation of dimethyl ether to prepare methyl acetate, characterized in that the catalyst contains a hydrogen-type mordenite molecular sieve subjected to vapor dealumination of silicon tetrachloride, and its silicon and aluminum atoms Ratio=3:1~20:1. In the present invention, by using silicon tetrachloride vapor to contact mordenite, it can interact with the acid site in the twelve-membered ring channel without affecting the acid site in the eight-membered ring channel, and selectively remove the acid site in the twelve-membered ring channel. Aluminum can retain the acid site in the eight-membered ring pore, thereby improving the life and selectivity of the catalyst in the reaction of dimethyl ether carbonylation to prepare methyl acetate, thereby improving the yield of the reaction.

Description

technical field [0001] The invention belongs to the technical field of catalytic chemistry, and relates to the modification of mordenite and its application in dimethyl ether carbonylation reaction. 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 o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/18C07C69/14C07C67/37
Inventor 周慧朱文良刘红超刘勇倪友明刘中民孟霜鹤李利娜刘世平
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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