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Fluoromethane production process and product

A technology of fluoromethane and methane, applied in the field of preparation of fluoromethane, can solve problems such as difficult separation

Active Publication Date: 2009-11-25
RESONAC CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since this reaction is an equilibrium reaction as shown in the following chemical equation (1), this method has problems in that it is necessary to increase the catalytic activity, and since HFC-41 (boiling point at atmospheric pressure is -78.5° C.) and hydrogen chloride which are close in boiling point are formed (The boiling point at atmospheric pressure is -84.9°C), which leads to the problem of difficult separation

Method used

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  • Fluoromethane production process and product

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Effect test

preparation Embodiment 1

[0041] 452g Cr(NO 3 ) 3 ·9H 2 O and 42g of In(NO 3 ) 3 ·NH 2 A solution of O (n is about 5) in 1.2L of purified water and 0.3L of 28% ammonia is added dropwise to a 10L container with 0.6L of purified water under stirring in about 1 hour, while controlling the flow rates of the two aqueous solutions So that the pH of the reaction solution is in the range of 7.5-8.5. The resulting hydroxide slurry was filtered and thoroughly washed with purified water, and then dried at 120°C for 12 hours. The obtained solid is pulverized, then mixed with graphite, and formed into flakes using a tablet machine. These flakes were burned at 400°C under a nitrogen stream for 4 hours to obtain a catalyst precursor. The catalyst precursor is charged into an inconel reactor, and then fluorinated (catalyst activation) is performed in a stream of hydrogen fluoride diluted with nitrogen under normal pressure at 350° C. and then in a stream of 100% hydrogen fluoride to prepare a catalyst.

preparation Embodiment 2

[0044] As the catalyst support, activated alumina (NST-7, Nikki Universal Co., Ltd.) is used here, which has a 50- The central pore size of the product contains at least 70% of the pores with a distribution of ±50% of the central size, has a pore volume of 0.5-1.6ml / g, and has a purity of 99.9% by mass or greater and a sodium content of not more than 100ppm.

[0045] In the 191.5g of chromium chloride (CrCl 3 ·6H 2 O) After adding 132 ml of purified water, the mixture is heated to 70-80°C in a hot water bath to dissolve. The solution was cooled to room temperature, and then 400 g of the above activated alumina was immersed in it until the solution was absorbed into the alumina. Next, the moistened alumina is dried on a hot water bath at 90°C until hardened. The hardened catalyst was dried in a hot air dryer with air circulation for 3 hours. Then the catalyst is charged into an inconel reactor, and fluorinated (catalyst activation) is performed in a stream of hydrogen fluoride dil...

preparation Embodiment 3

[0048] The catalyst was obtained according to the method of catalyst preparation example 2, except that 16.57g of zinc chloride (ZnCl 2 ) Was added to the catalyst preparation example 2 of example 2 as the second component.

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Abstract

To provide a method for efficiently producing HFC-41 having high purity and usable as an etching gas for semiconductor and provide a product produced by the method. The method for producing fluoromethane comprises reacting methyl chloride with hydrogen fluoride in gaseous phase in the presence of a fluorination catalyst to obtain a mixture containing the fluoromethane and hydrogen chloride, introducing the mixture into a distillation column, separating the fluoromethane and hydrogen chloride as a column top fraction and purifying the fluoromethane.

Description

[0001] Cross references to related applications [0002] This application is based on the submission of 35U.SC§111(a), according to 35U.SC§119(e)(1), it is entitled to the provisional application filed on September 24, 2004 under 35U.SC§111(b) 60 / 612,538 priority. Invention field [0003] The invention relates to a method for preparing fluoromethane (CH 3 F, hereinafter referred to as HFC-41) method. Background technique [0004] Hydrofluorocarbon (HFC) is characterized by its ozone depletion potential of 0, especially HFC-41, difluoromethane (CH 2 F 2 ) And trifluoromethane (CHF 3 ) Is a useful semiconductor etching gas. [0005] HFCs used as semiconductor etching gases must have high purity. More particularly, their acid component (hydrogen chloride, hydrogen fluoride, etc.) content is preferably not more than 1.0 ppm by mass, and their moisture content is preferably not more than 10 ppm by mass, more preferably not More than 5ppm by mass. [0006] Therefore, many methods have b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/20C07C19/08
CPCC07C17/206C07C17/383C07C19/08Y02P20/52
Inventor 大野博基新井龙晴
Owner RESONAC CORPORATION
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