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Method for preparing 1,1,1,3,3,3-hexafluoroisopropyl methyl ether through gas-phase methylation reaction

A technology of hexafluoroisopropyl methyl ether and hexafluoroisopropyl alcohol, applied in the field of gas-phase methylation reaction to prepare 1,1,1,3,3,3-hexafluoroisopropyl methyl ether, capable of Solve problems such as high cost, non-green chemical industry, and high energy consumption

Active Publication Date: 2020-01-31
ZHEJIANG RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method using methyl halide and dimethyl carbonate as raw materials requires the use of high temperature and high pressure reaction conditions, which consumes a lot of energy and costs in industrial applications, and does not belong to the category of green chemical industry.

Method used

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  • Method for preparing 1,1,1,3,3,3-hexafluoroisopropyl methyl ether through gas-phase methylation reaction
  • Method for preparing 1,1,1,3,3,3-hexafluoroisopropyl methyl ether through gas-phase methylation reaction
  • Method for preparing 1,1,1,3,3,3-hexafluoroisopropyl methyl ether through gas-phase methylation reaction

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Experimental program
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Effect test

Embodiment 1

[0045] Embodiment 1, the preparation of methylation catalyst

[0046] Get chromium nitrate 23.8g to be dissolved in 500ml distilled water, then add 52g ZSM-5 molecular sieve and carry out impregnation, now the mass ratio of main catalyst ZSM-5 molecular sieve and cocatalyst is 90%: 10%, impregnation temperature is 50 ℃, and impregnation time is After 10 hours, it was filtered, dried, pulverized, and pressed to form a catalyst precursor. The catalyst precursor was calcined at 400° C. for 10 hours in an inert gas atmosphere to obtain a methylation catalyst, coded as LW-1.

[0047] According to the preparation method described in this example, the soluble salt of the molecular sieve and the cocatalyst was changed to prepare the catalyst described in the following table 1:

[0048] Table 1

[0049]

Embodiment 2

[0051] Fill 20ml gas phase methylation catalyst LW-1 in the tubular reactor made of Monel alloy with an inner diameter of 1 / 2 inch and a length of 40cm, the reactor is heated to 200°C, and the liquid raw material mixture is passed into After the preheating is completed, in the mixing chamber, the molar ratio of 1,1,1,3,3,3-hexafluoroisopropanol and dimethyl carbonate is controlled to be 1:2, and the liquid raw material is vaporized in the mixing chamber and passed through the catalyst The reactor, the contact time is 6 seconds, the reaction product is collected in the cold trap after cooling. The composition of the collected product was analyzed with a gas chromatograph, and the reaction results are listed in Table 2.

Embodiment 3

[0053]Inner diameter is 1 / 2 inch, and the tubular reactor made of Monel alloy that length is 40cm is filled with 20ml gas-phase methylation catalyst LW-2, and the reactor is heated up to 220 ℃, and the liquid raw material mixture is passed into by using a sampling pump. After the preheating is completed, in the mixing chamber, the molar ratio of 1,1,1,3,3,3-hexafluoroisopropanol and dimethyl carbonate is controlled to be 1:2, and the liquid raw material is vaporized in the mixing chamber and passed through the catalyst The reactor, the contact time is 6 seconds, the reaction product is collected in the cold trap after cooling. The composition of the collected product was analyzed with a gas chromatograph, and the reaction results are listed in Table 2.

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Abstract

The invention provides a method for obtaining 1,1,1,3,3,3-hexafluoroisopropyl methyl ether through a gas phase methylation reaction of 1,1,1,3,3,3-hexafluoroisopropanol and dimethyl carbonate in the presence of a methylation catalyst, wherein the methylation catalyst comprises a molecular sieve and at least a cocatalyst selected from Cr, Al, Ni, Co, Fe, La, Zr, Zn and Mn. According to the invention, the preparation method has advantages of high conversion rate, high selectivity, environmental protection in operation, easy achieving, easy continuous large-scale production and the like.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and relates to a method for preparing 1,1,1,3,3,3-hexafluoroisopropyl methyl ether, in particular to a method for preparing 1,1, 1,3,3,3-Hexafluoroisopropylmethyl ether method. Background technique [0002] 1,1,1,3,3,3-Hexafluoroisopropylmethyl ether is an important hydrofluoroether compound, which can be used as a potential substitute for chlorofluorocarbons (CFCs). [0003] About the preparation method of 1,1,1,3,3,3-hexafluoroisopropyl methyl ether, following reports are arranged in the prior art: [0004] (1) U.S. Patent US3346448 and German Patent GB1250928 respectively reported using 1,1,1,3,3,3-hexafluoroisopropanol and dimethyl sulfate as raw materials and reacting with alkali to obtain 1,1,1, 3,3,3-Hexafluoroisopropyl methyl ether method; [0005] (2) Chinese patent CN102408317 reported that 1,1,1,3,3,3-hexafluoroisopropanol and methyl halide were used as raw materials and reacted un...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/12C07C41/16B01J29/48B01J29/70B01J29/72
CPCC07C41/16B01J29/48B01J29/7038B01J29/7276B01J29/7088C07C43/12
Inventor 李伟胡江平张迪刘冬鹏郭智恺
Owner ZHEJIANG RES INST OF CHEM IND CO LTD
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