Catalyst used for preparing methyl acetate through dimethyl ether carbonylation, preparation method and application thereof

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

Active Publication Date: 2015-06-10
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 t

Method used

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  • Catalyst used for preparing methyl acetate through dimethyl ether carbonylation, preparation method and application thereof
  • Catalyst used for preparing methyl acetate through dimethyl ether carbonylation, preparation method and application thereof
  • Catalyst used for preparing methyl acetate through dimethyl ether carbonylation, preparation method and application thereof

Examples

Experimental program
Comparison scheme
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

...

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Abstract

The invention provides a catalyst used for preparing methyl acetate through dimethyl ether carbonylation, a preparation method and an application thereof, more specifically, the invention provides the catalyst used for preparing methyl acetate through dimethyl ether carbonylation, the catalyst contains a silicon tetrachloride steam dealuminated hydrogen-mordenite molecular sieve, and silicon and aluminum atomic ratio is 3: 1-20: 1. According to the invention, silicon tetrachloride steam is contacted to mordenite for effecting acid site in 12-membered ring tunnel without influence of acid site in 8-membered ring tunnel, aluminum in 12-membered ring tunnel is selectively removed, and acid site in 12-membered ring tunnel is kept, so that life and selectivity of catalyst in a reaction for preparing methyl acetate through dimethyl ether carbonylation are increased, and reaction yield is increased.

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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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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