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Method for preparing hexafluoroacetone

A technology of hexafluoroacetone and hexafluoroisobutenol is applied in the field of preparation of industrial-scale hexafluoroacetone, and can solve the problems of increasing the manufacturing cost of the reaction vessel, increasing capital and labor costs, and the like

Inactive Publication Date: 2009-11-25
SHANGHAI 3F NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0036] Manufacture a feeding device that satisfies the above three conditions at the same time, there are difficulties in design and manufacture, which will inevitably increase the manufacturing cost of the reaction vessel, or need to modify the existing reaction vessel, increasing capital and labor costs

Method used

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  • Method for preparing hexafluoroacetone
  • Method for preparing hexafluoroacetone
  • Method for preparing hexafluoroacetone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] Add 110.4 grams (0.5M) of 1-methoxy-1-perfluoroisobutene (purity 96%) and 100 milliliters of acetonitrile (water content 150ppm) in 500 milliliters of three-necked flasks, add 51 grams under the condition of stirring and cooling (0.5M) triethylamine, and the mixture was kept at room temperature for 1.5 hours to obtain a reaction mixture of tetramethylammonium salt of hexafluoroisobutenol in a stable state for use.

[0081] Add 48.5 grams (0.7M) of sodium nitrite and 100 milliliters of acetonitrile (water content 150ppm) in a 500 milliliter three-necked flask at one time, connect the bubbler bottle (add liquid paraffin in the bubbler bottle) at the tail gas discharge port, Slowly add the above-mentioned tetramethylammonium salt reaction mixture of hexafluoroisobutenol in a steady state to the three-necked flask containing the acetonitrile dispersion of sodium nitrite at a controlled flow rate under vigorous stirring and cooling, Control the release rate of carbon dioxide...

Embodiment 2

[0090] Add 263 grams (1.1M) of 1-methoxy-2H-octafluoroisobutane (purity 95%) and 200 milliliters of acetonitrile (water content 150ppm) in a 1000 milliliter three-necked flask, add under stirring and cooling 222 g (2.2 M) of triethylamine, and the mixture was kept at room temperature for 1.5 hours to obtain a reaction mixture of tetramethylammonium salt of hexafluoroisobutenol in a stable state for use.

[0091] Add 111 grams (0.7M) of sodium nitrite and 300 milliliters of acetonitrile (water content 150ppm) at one time in 1000 milliliters of three-necked flasks, connect the bubble bottle (in the bubble bottle, add liquid paraffin) at the tail gas discharge port, Slowly add the above-mentioned tetramethylammonium salt reaction mixture of hexafluoroisobutenol in a steady state to the three-necked flask containing the acetonitrile dispersion of sodium nitrite at a controlled flow rate under vigorous stirring and cooling, Control the release rate of carbon dioxide and maintain th...

Embodiment 3

[0100] In a 1000 milliliter three-necked flask, such as 110.4 grams (0.5M) of 1-methoxy-1-perfluoroisobutene (purity 96%) and 80 milliliters of acetone (water content 200ppm), add 51 gram (0.5M) of triethylamine, and the mixture was kept at room temperature for 1.5 hours to prepare a reaction mixture of tetramethylammonium salt of hexafluoroisobutenol in a stable state for use.

[0101] Add 51 grams (0.7M) sodium nitrite and 50 milliliters of acetone (water content 200ppm) of 99.5% sodium nitrite and 50 milliliters of acetone (water content 200ppm) in 500 milliliters of three-necked flasks at one time, connect bubble bottle (in bubble bottle, add liquid paraffin) at tail gas discharge port, Slowly add the above-mentioned tetramethylammonium salt reaction mixture of hexafluoroisobutenol in a steady state to the three-necked flask containing the acetone dispersion of sodium nitrite at a controlled flow rate under vigorous stirring and cooling, Control the release rate of carbon ...

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Abstract

The invention provides a method for preparing hexafluoroacetone by perfluoroisobutylene or alcohol absorption liquid of the perfluoroisobutylene. The method sequentially comprises the following steps: firstly, in a reaction medium, the alcohol absorption liquid of the perfluoroisobutylene is reacted with tertiary amines to form middle stable state tetraalkylammonium salt of alcohol hexafluoroisobutene; secondly, nitrite of alkali metal or alkaline earth metal is dispersed in the reaction medium; thirdly, the obtained middle stable state tetraalkylammonium salt of the alcohol hexafluoroisobutene is mixed with dispersion liquid of the nitrite of the alkali metal or the alkaline earth metal to react to form oxime hexafluoroacetone; and fourthly, the oxime hexafluoroacetone is reacted with inorganic acid to form the hexafluoroacetone.

Description

technical field [0001] The invention relates to a method for preparing hexafluoroacetone on an industrial scale. Background technique [0002] In industry hexafluoroacetone ((CF 3 ) 2 CO) is an important fluorochemical used as an intermediate for example as a crosslinker in the manufacture of fluoroelastomer polymers. There are many methods for preparing hexafluoroacetone or its hydrate. For example, US Patent No. 4,960,947 (Sonoi et al.) mentions a method of thermally decomposing alcohol adducts of perfluoroisobutene to form hexafluoroacetone. [0003] Chinese patent application CN 1141623A submitted by U.S. 3M company discloses a kind of preparation method of hexafluoroacetone, and it comprises the steps: [0004] a) The steady-state hexafluoroisobutyryl carbanion alkyl ammonium salt is obtained from the alcohol adduct of perfluoroisobutene. Taking the methanol adduct of perfluoroisobutene as an example, the alkyl ammonium salt can be passed The following reaction pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/167C07C45/42
Inventor 应德雄粟小理周荣明
Owner SHANGHAI 3F NEW MATERIAL
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