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Method for producing dry etching gas

一种气相、三氟甲基的技术，应用在氟代甲烷和3,3,3-三氟-2-丙酰氟领域，能够解决制造设备成本大、设备大、催化剂劣化等问题

Pending Publication Date: 2018-12-18
DAIKIN IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Among these methods, the method (1) is prone to catalyst degradation due to the large amount of water generated, and also has the disadvantage of being prone to corrosion because unreacted hydrogen fluoride and generated water generate hydrofluoric acid.
In the method of (2), in order to improve the reactivity of fluorination, it is necessary to add excess hydrogen fluoride, and if it is recycled and reused, the equipment will become huge and the cost of manufacturing equipment will be too high.
However, in this method, the yield is only 46%, and both alkali and acid are used in the reaction, so the reaction is complicated and corrosion resistance is required for the equipment, so it is not suitable as an industrial production method

Method used

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Examples

Experimental program
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Effect test

Embodiment 1～5

[0080] As a catalyst, γ-alumina (Al 2 o 3 )A (pore volume 0.45ml / g) (average particle diameter 3mm), which was filled in a heat-resistant and corrosion-resistant nickel-based alloy tubular reactor with an inner diameter of 15mm and a length of 650mm. This reaction tube was heated to 200° C., and 1,1,3,3,3-pentafluoro-2-trifluoromethylpropyl methyl ether as a raw material was supplied to the reaction tube. Table 1 shows the contact time: W / F (g·sec / cc) as the ratio of the catalyst amount W (g) to the feed rate F (cc / sec) of the raw material.

[0081] Table 1 shows the results of analyzing the gas effluent from the reaction tube by gas chromatography. The numerical values ​​described in Table 1 are component ratios (mol %) obtained by multiplying the area ratios of each peak obtained by gas chromatography by a coefficient for correcting the sensitivity of each gas.

[0082] However, each symbol described in Table 1 represents the following compounds.

[0083] CH 3 F: fluoro...

Embodiment 6

[0094] By passing the thermally decomposed gas obtained in Example 4 through a 5% by weight KOH aqueous solution, 99.5% of the gas components become CH 3 F. From this result, it was confirmed that 3,3,3-trifluoro-2-(trifluoromethyl)propionyl fluoride can be separated and removed by bringing the generated gas after thermal decomposition into contact with an aqueous alkali solution. By further cooling and recovering the separated gas, and performing rectification, CH with a purity of 99.99% can be obtained 3 F.

Embodiment 7

[0096] Under the same conditions as in Examples 1 to 5, the reaction tube was heated to 150°C, and 1,1,3,3,3-pentafluoro-2-trifluoromethylpropyl methyl ether as a raw material was supplied to in the reaction tube.

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Abstract

Provided is a method for safely producing fluoro-methane and 3,3,3-trifluoro-2-(trifluoromethyl)propanoyl fluoride ((CF3)2CHCOF), which are useful as a dry etching gas or the like, with high purity atlow cost. By a method for thermally decomposing 1,1,3,3,3-pentafluoro-2-trifluoromethylpropylmethyl ether in a vapor state in the presence of a catalyst, the aimed fluoro-methane and 3,3,3-trifluoro-2-(trifluoromethyl)propanoyl fluoride can be obtained with high starting material conversion rate and high selectivity by a simple process wherein a thermal decomposition reaction is carried out in avapor state using a low-cost starting material.

Description

[0001] This case is filed on November 12, 2013 , the application number is 201380059241.7 (PCT / JP2013 / 080563) , A divisional application of the patent application titled "Manufacturing Method of Dry Etching Gas". technical field [0002] The present invention relates to a method capable of simultaneously producing fluoromethane and 3,3,3-trifluoro-2-(trifluoromethyl)propionyl fluoride, which are useful as dry etching gases. Background technique [0003] Hydrofluorocarbons are useful as etching gases for microfabrication of semiconductors, liquid crystals, etc., especially fluoromethane (CH 3 F) is attracting attention as an etching gas for forming the most advanced fine structure. [0004] As a method for producing fluoromethane, for example, the following methods are known. [0005] (1) A method of reacting methanol and hydrogen fluoride using a catalyst (Patent Document 1). [0006] (2) A method of reacting methyl chloride and hydrogen fluoride using a catalyst (Pat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/361C07C17/383C07C41/06C07C51/58C07C51/64
CPCC07C17/361C07C17/383C07C41/06C07C51/58C07C51/64C07C19/08C07C53/50C07C43/12C07B61/00C07C17/38
Inventor 中村新吾江藤友亮大塚达也福本可奈子内藤真人
Owner DAIKIN IND LTD
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