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Method for producing 1,2,3,4-tetrachlorohexafluorobutane and method for purifying 1,2,3,4-tetrachlorohexafluorobutane

A technology of tetrachlorohexafluorobutane and its manufacturing method, which is applied in the field of purification 1 to achieve the effect of high yield and high safety

Active Publication Date: 2010-02-03
RESONAC CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, from this point of view, the method for producing 1,2,3,4-tetrachlorohexafluorobutane described in Patent Document 1 has a problem in terms of efficiently producing the target product industrially.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] In a reactor made of SUS304 (Teflon (registered trademark) lining) with an internal volume of 200 ml, 20 g of hydrogen fluoride was dissolved in 45 g of carbon tetrachloride as a solvent, and 5 g of 1 obtained in the above-mentioned raw material production example was added thereto, For 2,3,4-tetrachlorobutane, nitrogen gas was introduced at a pressure of 1.0 MPa, and after a leak test was performed, nitrogen gas was discharged, and the temperature was kept at 20° C. while stirring.

[0076] Then, utilize the gas introduction tube assembled in the autoclave to introduce 50% by volume fluorine gas diluted with nitrogen from the liquid phase at a pressure of 0.5 MPa to initiate the reaction, and discharge the gaseous phase from the gas phase of the autoclave after 2 hours at a pressure of 0.5 MPa. The pressure of MPa was introduced into 50% by volume of fluorine gas diluted with nitrogen, and the reaction was repeated. Finally, this operation was repeated 7 times to termin...

Embodiment 2

[0081] In a reactor made of SUS304 (Teflon (registered trademark) lining) with an internal volume of 200 ml, 10 g of hydrogen fluoride was dissolved in 45 g of carbon tetrachloride as a solvent, and 5 g of 1 obtained in was added thereto, For 2,3,4-tetrachlorobutane, nitrogen gas was introduced at a pressure of 1.0 MPa, and after a leak test was performed, nitrogen gas was discharged, and the temperature was kept at 20° C. while stirring. Then, the same operation was carried out under the same conditions as in Example 1, and the product containing the solvent was collected and analyzed by gas chromatography.

[0082] The analysis results are shown below.

[0083] Yield of 1,2,3,4-tetrachlorohexafluorobutane: 82.1%

[0084] The by-product is mainly pentachloropentafluorobutane, but compared with Example 1, the amount of by-product is reduced.

Embodiment 3

[0086] In a reactor made of SUS304 (lined with Teflon (registered trademark)) with an inner volume of 10 liters, 1000 g of hydrogen fluoride was dissolved in 2250 g of carbon tetrachloride as a solvent, and 250 g of the 1 obtained in the was added thereto. , 2,3,4-Tetrachlorobutane, nitrogen was introduced at a pressure of 1.0MPa, after a leak test was performed, nitrogen was discharged, and the temperature was kept at 20°C while stirring.

[0087] Then, the same operation was carried out under the same conditions as in Example 1, and the product containing the solvent was collected and analyzed by gas chromatography.

[0088] The analysis results are shown below.

[0089] Yield of 1,2,3,4-tetrachlorohexafluorobutane: 80.5%

[0090] Then, the solvent-containing product was introduced into a distillation column (theoretical number of stages: 25 stages), and low-boiling point component separation and high-boiling point component separation were performed to obtain 1,2,3,4-tetr...

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Abstract

Disclosed is a method for producing 1,2,3,4-tetrachlorohexafluorobutane, which is characterized in that 1,2,3,4-tetrachlorobutane is reacted with fluorine in the presence of a solvent containing hydrogen fluoride. The 1,2,3,4-tetrachlorobutane may be obtained by chlorination of 3,4-dichlorobutene-1. Also disclosed is a method for purifying the thus-obtained 1,2,3,4-tetrachlorohexafluorobutane. This method enables to commercially efficiently produce 1,2,3,4-tetrachlorohexafluorobutane, which is useful as a synthesis material for hexafluoro-1,3-butadiene that is used, for example, as an etchinggas for semiconductors, by using 1,2,3,4-tetrachlorobutane which has been conventionally discarded as a by-product of chloroprene.

Description

technical field [0001] The present invention relates to a production method and a purification method of 1,2,3,4-tetrachlorohexafluorobutane. More specifically, the present invention relates to a method for producing 1,2,3,4-tetrachlorohexafluorobutane useful as a synthetic raw material for hexafluoro-1,3-butadiene, etc., and for purifying 1,2 , the method of 3,4-tetrachlorohexafluorobutane, and the hexafluoro-1,3-butadiene have attracted people's attention as an etching gas for semiconductors and the like. Background technique [0002] 1,2,3,4-Tetrachlorohexafluorobutane is an important compound as a raw material for the synthesis of hexafluoro-1,3-butadiene, which is used in Etching gases used in semiconductor microfabrication are attracting attention. Conventionally, methods described in the following patent documents are known as methods for producing this 1,2,3,4-tetrachlorohexafluorobutane. [0003] (1) In JP-A-2006-342059 (Patent Document 1), it is described that b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/10C07C19/10
CPCC07C17/389C07C17/383C07C17/10C07C19/10C07C17/38
Inventor 大野博基大井敏夫佐佐木信利埜村清志
Owner RESONAC CORP
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