Method for preparing hexafluorobutadiene from iodine and chlorine

A technology of hexafluorobutadiene and hexafluorobutane, which is applied in the field of hexafluorobutadiene preparation, can solve the problems of long reaction time, many side reactions, low catalytic efficiency, etc., and achieves a long reaction time and many side reactions. Effect

Inactive Publication Date: 2017-01-18
ZHEJIANG BRITECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, the oxygen-containing organic compounds used as solvents in the prior art will cause low catalytic efficiency, slow reaction speed, long reaction time and many side reactions. It is necessary to find more efficient organic solvents

Method used

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  • Method for preparing hexafluorobutadiene from iodine and chlorine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Preparation of metal complex ionic liquid solvent:

[0033] Add 100Kg ethanol, 0.05Kg vitamin B12 (Vitamin B12), 0.2Kg 1-ethyl ethyl ether-3-methylimidazolium tetrafluoroborate in 500L reactor, 1Kg boron trifluoride ether solution, add Mix in the reaction kettle at room temperature for 20 hours to prepare the metal complex ionic liquid solvent;

[0034] (2) Preparation of iodine monochloride:

[0035] Add 100Kg iodine in a 500L reactor, the reaction temperature is 58°C, iodine is sublimated, chlorine gas is introduced, the molar ratio of chlorine gas and iodine is 1.2:1, the reaction end point is that the solid is completely transformed into a liquid, and the obtained liquid is distilled to obtain monochloride iodine products.

[0036] (3) Preparation of 1,2-dichloro-2-iodo-1,1,2-trifluoroethane:

[0037] In the 500L reactor, add 100Kg iodine monochloride, iodine monochloride, chlorotrifluoroethylene is put into reactor with mol ratio 1.2: 1, adds the metal compl...

Embodiment 2

[0043] (1) Preparation of metal complex ionic liquid solvent:

[0044] Add 100Kg1,4-dioxane, 0.01Kg vitamin B12 (Vitamin B12), 0.05Kg 1-ethyl ethyl ether-3-methylimidazole tetrafluoroborate, 0.5Kg tri The boron fluoride ether solution was added to the reaction kettle and mixed at room temperature for 10 hours to obtain the metal complex ionic liquid solvent;

[0045] (2) Preparation of iodine monochloride:

[0046] Add 100Kg iodine in a 500L reactor, the reaction temperature is 55°C, iodine is sublimated, chlorine gas is introduced, the molar ratio of chlorine gas and iodine is 1.1:1, the reaction end point is that the solid is completely transformed into a liquid, and the obtained liquid is distilled to obtain monochloride iodine products.

[0047] (3) Preparation of 1,2-dichloro-2-iodo-1,1,2-trifluoroethane:

[0048] In the 500L reactor, add 100Kg iodine monochloride, iodine monochloride, chlorotrifluoroethylene is put into reactor with mol ratio 1.1: 1, adds the metal co...

Embodiment 3

[0054] (1) Preparation of metal complex ionic liquid solvent:

[0055] Add 60Kg tetrahydrofuran, 40Kg propanol, 0.1Kg vitamin B12 (VitaminB12), 0.5Kg 1-ethyl ethyl ether-3-methylimidazolium tetrafluoroborate, 2Kg boron trifluoride ether in 500L reactor solution, added to the reactor at room temperature and mixed for 40 hours to obtain the metal complex ionic liquid solvent;

[0056] (2) Preparation of iodine monochloride:

[0057] Add 100Kg iodine in a 500L reactor, the reaction temperature is 70°C, iodine is sublimated, chlorine gas is introduced, the molar ratio of chlorine gas and iodine is 1.5:1, the end point of the reaction is that the solid is completely transformed into a liquid, and the obtained liquid is distilled to obtain monochloride iodine products.

[0058] (3) Preparation of 1,2-dichloro-2-iodo-1,1,2-trifluoroethane:

[0059] In the 500L reactor, add 100Kg iodine monochloride, iodine monochloride, chlorotrifluoroethylene is put into reactor with mol ratio 1....

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Abstract

The invention relates to a method for preparing hexafluorobutadiene from iodine and chlorine. The method comprises the following steps: preparing a metal coordinated ionic liquid solvent, and reacting iodine with chlorine to prepare iodine monochloride; reacting iodine monochloride with chlorotrifluoroethylene in the presence of the metal coordinated ionic liquid solvent to prepare 1,2-dichloro-2-iodo-1,1,2-trifluoroethane; carrying out a reaction on the 1,2-dichloro-2-iodo-1,1,2-trifluoroethane in the presence of the metal coordinated ionic liquid solvent under the catalysis of zinc powder to obtain 1,2,3,4-tetrachloro-1,1,2,3,4,4-hexafluorobutane; and reacting the 1,2,3,4-tetrachloro-1,1,2,3,4,4-hexafluorobutane with zinc powder in the presence of the metal coordinated ionic liquid solvent to generate hexafluorobutadiene.

Description

technical field [0001] The invention relates to a method for preparing hexafluorobutadiene, in particular to a method for preparing hexafluorobutadiene using iodine and chlorine gas as raw materials. Background technique [0002] In recent years, the market demand for C4F6 in the etching process of the semiconductor industry has continued to grow. It can replace CF4 for dry process of KrF laser sharp etching semiconductor capacitor pattern. C4F6 has many advantages in etching at the 0.13nm technical level. Compared with CF8, it has a higher selectivity ratio to photoresist and silicon nitride. When used, it can improve the stability of etching, increase the etching rate and uniformity, and thus improve the product quality. Excellent rate. C4F6 is anisotropic, can produce ideal aspect ratio in silicon and silicon oxide etching, and protects sidewall when etching to form polymer film (photoresist). The greenhouse effect index (GWP) of C4F6 is almost zero, and it can replace...

Claims

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Application Information

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IPC IPC(8): C07C17/23C07C21/20
CPCC07C17/04C07C17/23C07C17/269C07C19/12C07C19/10C07C21/20Y02P20/54
Inventor 陈刚张晓东李军周井森王宁陈立峰钱红东花永紧徐建仙
Owner ZHEJIANG BRITECH CO LTD
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