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Method for preparing 1,2,3,4-tetrachloro-hexafluoro butane
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A technology of tetrachlorohexafluorobutane and hexafluorobutadiene, applied in 1 field, can solve problems such as slow reaction speed, increased by-products, and reactor corrosion
Inactive Publication Date: 2010-10-06
SINOCHEM LANTIAN +1
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Problems solved by technology
Although the yield of 1,2,3,4-tetrachlorohexafluorobutane prepared by this method is higher, about 90-98%, the reaction speed is slow, the reaction time is long, and a large amount of white Solid, that is, Lewis acid, increases by-products and severely corrodes the reactor
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Embodiment 1
[0033] Example 1 Preparation of 1,2,3,4-tetrachlorohexafluorobutane
[0034]In a 100ml three-neck flask, add 1g of ethyl acetate, 1g of water and 7g of 1-iodo-1,2-dichlorotrifluoroethane, stir well, control the reaction temperature at 20-25°C, and add zinc particles in batches within 1h 2g (3-6mm), react at a reaction temperature of 25°C for about 12h. After the reaction is completed, the reaction solution is poured out and washed with water, and the lower layer is separated to obtain 1,2,3,4-tetrachlorohexafluorobutane, 1- The conversion rate of iodine-1,2-dichlorotrifluoroethane was 99.1%, and the yield of 1,2,3,4-tetrachlorohexafluorobutane was 92.9%.
Embodiment 2
[0035] Example 2 Preparation of 1,2,3,4-tetrachlorohexafluorobutane
[0036] In a 100ml three-neck flask, add 1g of ethyl acetate and 7g of 1-iodo-1,2-dichlorotrifluoroethane, stir well, control the reaction temperature at 20-25°C, and add 2g of zinc particles in batches within 1h (3 -6mm), and reacted at a reaction temperature of 25°C for about 6 hours. After the reaction was completed, the reaction solution was poured out and washed with water, and the lower layer was separated to obtain 1,2,3,4-tetrachlorohexafluorobutane, 1-iodo-1 , the conversion rate of 2-dichlorotrifluoroethane was 99.0%, and the yield of 1,2,3,4-tetrachlorohexafluorobutane was 87.3%.
Embodiment 3
[0037] Example 3 Preparation of 1,2,3,4-tetrachlorohexafluorobutane
[0038] In a 100ml three-neck flask, add 1g of absolute ethanol and 7g of 1-iodo-1,2-dichlorotrifluoroethane, stir well, control the reaction temperature at 20-25°C, and add 2g of zinc particles in batches within 1.5h ( 3-6mm), and reacted at a reaction temperature of 25°C for about 6 hours. After the reaction was completed, the reaction solution was poured out and washed with water, and the lower layer was separated to obtain 1,2,3,4-tetrachlorohexafluorobutane, 1-iodo- The conversion rate of 1,2-dichlorotrifluoroethane was 97.3%, and the yield of 1,2,3,4-tetrachlorohexafluorobutane was 84.5%.
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Abstract
The invention discloses a method for preparing 1,2,3,4-tetrachloro-hexafluoro butane. In the presence of an oxygen-containing organic compound catalyst, 1-iodine-1,2,2-trifluoro-1,2-dichloroethane and zinc particles react to prepare 1,2,3,4-tetrachloro-hexafluoro butane, wherein the oxygen-containing organic compound catalyst is one or a combination of more of alcohol, ketone, ester, ether and amide; the added quantity of the oxygen-containing organic compound catalyst accounts for 5 to 50 weight percent of that of the 1-iodine-1,2,2-trifluoro-1,2-dichloroethane; the particle size of the zinc particles is of between 3 and 6 mm; and the added quantity of the zinc particles accounts for 10 to 50 weight percent of that of the 1-iodine-1,2,2-trifluoro-1,2-dichloroethane. The invention also provides a method for preparing hexachlorobutadiene from the 1,2,3,4-tetrachloro-hexafluoro butane. The hexachlorobutadiene can be used as a polymermonomer, an etching gas or the like.
Description
technical field [0001] The present invention relates to a kind of preparation method of 1,2,3,4-tetrachlorohexafluorobutane, especially 1-iodo-1,2,2-trifluoro-1,2-dichloroethane and zinc A method for preparing 1,2,3,4-tetrachlorohexafluorobutane from raw materials under the action of an oxygen-containing organic compound. Background technique [0002] Hexafluorobutadiene is not only a good polymermonomer, but also an excellent dry etching gas, capable of dry etching less than 100nm or even narrower width, with high selectivity and precision. In addition, the GWP of hexafluorobutadiene is only 290 (CO 2 100 years=1), the atmospheric lifetime is less than 2 days, is an environment-friendly etchant, and the preparation route of developing hexafluorobutadiene has far-reaching environmental protection significance and economic benefit. 1,2,3,4-Tetrachlorohexafluorobutane is a very important intermediate for the synthesis of hexafluorobutadiene, and its preparation routes are a...
Claims
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Application Information
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