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Novel process for synthesizing hexafluoroacetone

A technology of hexafluoroacetone and a new process, which is applied in the field of flame retardants, can solve the problems of high production cost, high price of hexafluoropropylene oxide, and limited use, and achieve high reaction yield, easy industrial production, and simple process Effect

Inactive Publication Date: 2020-07-10
张江南
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage is: due to the high price of hexafluoropropylene, the production cost is very high
(2) Oxidation method of perfluoroisobutylene: Due to the high toxicity of perfluoroisobutylene, its direct utilization is limited
(3) Hexafluoropropylene oxide rearrangement method: Due to the high price of hexafluoropropylene oxide, the use of this method is limited

Method used

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  • Novel process for synthesizing hexafluoroacetone

Examples

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Effect test

Embodiment 1

[0020] 210g (1mol) trifluoroacetic anhydride, 1200mL tetrahydrofuran and 2mol sodium fluoride were added to the reactor, reacted at 20°C for 3 hours, then 1.1mol potassium carbonate and 2.1mol sodium trifluoroacetate were added to the reactor, and the temperature was raised to 120 °C. ℃, stirring and reacting for 3 hours, cooling down, opening the reaction kettle, and distilling to obtain 435.3 g of the product hexafluoroacetone trihydrate. After testing, the HPLC purity was 96.3%, and the product yield was 93.1%.

Embodiment 2

[0022] 210g (1mol) trifluoroacetic anhydride, 1800mL dioxane and 2mol potassium fluoride were added in the reactor, reacted at 50°C for 1 hour, then added 1.1mol calcium carbonate and 2.1mol potassium trifluoroacetate in the reactor , heated to 70°C, stirred for 10 hours, cooled, opened the reactor, and distilled to obtain 438.3g of hexafluoroacetone trihydrate. After testing, the HPLC purity was 96.1%, and the product yield was 95.7%.

Embodiment 3

[0024] 210g (1mol) trifluoroacetic anhydride, 2000mL diethylene glycol dimethyl ether and 2.3mol cesium fluoride were added to the reaction kettle, reacted at 50°C for 2 hours, then 1.2mol cesium carbonate and 2.3mol trifluoride were added to the reaction kettle. Lithium fluoroacetate was heated to 80°C, stirred and reacted for 7 hours, cooled, opened the reaction kettle, and distilled to obtain 429.2 g of the product hexafluoroacetone trihydrate. After testing, the HPLC purity was 98.3%, and the product yield was 95.9%.

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Abstract

The invention discloses a novel process for synthesizing hexafluoroacetone. The novel process comprises the following steps: reacting trifluoroacetic anhydride with a metal fluoride in a solvent to obtain trifluoroacetyl fluoride, adding an alkaline salt and trifluoroacetate, and carrying out a coupling reaction on trifluoroacetate and trifluoroacetyl fluoride to obtain the product hexafluoroacetone. The product yield is 95% or above, and the product purity is higher than 96%.

Description

technical field [0001] The invention belongs to the field of flame retardants, and particularly relates to a new process for synthesizing hexafluoroacetone. Background technique [0002] Hexafluoroacetone (HFA, CF3COCF3, also known as 1,1,1,3,3,3-hexafluoroacetone) is an important intermediate of fluorine materials, CAS No. 684-16-2; English name Hexafluoroacetone; perfluoroacetone; molecular formula C3F6O; CF3CF2CFO, colorless gas; molecular weight 166.03 boiling point -27.28 ℃ molecular structure is: [0003] [0004] Hexafluoroacetone (HFA) is a fluorine-containing fine chemical with a wide range of uses. It can be used in aerospace, medicine and pesticides, textiles, microelectronics and synthetic materials, etc., especially as a raw material for synthesizing polymer materials in special fields. profound meaning. Among them, there have been larger industrial uses as a raw material for advanced solvents (eg, hexafluoroisopropanol) and as a monomer for high-performanc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/60C07C53/48C07C45/48C07C49/167
CPCC07C45/48C07C51/60C07C53/48C07C49/167
Inventor 张江南
Owner 张江南
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