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Fluoromethane production process and product

A technology for fluoromethane and methane, which is applied in the field of preparing fluoromethane and can solve problems such as difficulty in separation

Active Publication Date: 2007-08-22
株式会社力森诺科
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  • Summary
  • Abstract
  • Description
  • Claims
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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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preparation Embodiment 1

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

preparation Embodiment 2

[0044] As a catalyst support, activated alumina (NST-7, Nikki Universal Co., Ltd.) is used here, which has a central pore diameter of 50-400mm, contains at least 70% of pores with a central size distribution of ±50%, and has It has a pore volume of 0.5-1.6 ml / g, and has a purity of 99.9% by mass or more and a sodium content of not more than 100 ppm.

[0045] In 191.5g of chromium chloride (CrCl 3 ·6H 2 O) After adding 132 ml of purified water, the mixture was 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 therein until the solution was absorbed into the alumina. Next, the wetted alumina was dried to harden in a hot water bath at 90°C. The hardened catalyst was dried in an air circulating hot air dryer for 3 hours. The catalyst was then loaded into an Inconel reactor and subjected to fluorination treatment (catalyst activation) at 330° C. under normal pressure in a ...

preparation Embodiment 3

[0048] Obtain the catalyst according to the method of catalyst preparation example 2, the difference is that 16.57g of zinc chloride (ZnCl 2 ) was added as the second component to the catalyst preparation example 2 of Example 2.

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Abstract

Methyl chloride and hydrogen fluoride are reacted in a gas phase in the presence of a fluorination catalyst and the resulting mixture, containing fluoromethane and hydrogen chloride, is fed to a distillation column for separation and purification of the fluoromethane and hydrogen chloride as the overhead fraction. It is thus possible to efficiently produce high purity HFC-41 which is suitable for use as a semiconductor etching gas.

Description

[0001] Cross References to Related Applications [0002] This application is based on 35 U.S.C. §111(a) filed pursuant to 35 U.S.C. §119(e)(1) to claim provisional application 60 / 612,538 filed September 24, 2004 under 35 U.S.C. §111(b) priority. field of invention [0003] The present invention relates to a kind of preparation fluoromethane (CH 3 F, hereinafter referred to as HFC-41) method. Background technique [0004] Hydrofluorocarbons (HFCs) are characterized by their zero ozone depletion potential, 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, and 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 Greater than 5ppm mass. [0006] Therefore, many m...

Claims

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Application Information

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IPC IPC(8): C07C17/20C07C19/08
CPCC07C17/206C07C17/383C07C19/08Y02P20/52
Inventor 大野博基新井龙晴
Owner 株式会社力森诺科
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