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A kind of synthetic method of hexafluorobisphenol A

A synthetic method and technology of hexafluorobisphenol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of complex preparation methods and high equipment requirements

Active Publication Date: 2022-07-26
湖南有色郴州氟化学有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The above-mentioned preparation methods are relatively complicated and require high equipment

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  • A kind of synthetic method of hexafluorobisphenol A

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[0019] The invention provides a kind of synthetic method of hexafluorobisphenol A, comprising the following steps:

[0020] a) reacting hexachloroacetone and phenol under a Lewis acid catalyst to obtain hexachlorobisphenol A;

[0021] b) subjecting the hexachlorobisphenol A to a fluorination reaction with hydrogen fluoride to obtain hexafluorobisphenol A.

[0022] The present invention reacts hexachloroacetone and phenol under Lewis acid catalyst to obtain hexachlorobisphenol A. The present invention carries out the reaction of hexachloroacetone and phenol under nitrogen protection. The present invention carries out the reaction of hexachloroacetone and phenol in the reactor. In the present invention, hexachloroacetone, phenol and Lewis acid catalyst are added into the reaction kettle to be sealed and stirred. In the present invention, the molar ratio of the hexachloroacetone and phenol is 1:0.5˜1:5. The Lewis acid catalyst is selected from one or more of anhydrous hydroge...

Embodiment 1

[0031] Under nitrogen protection, add phenol 94.1g (1.0mol), hexachloroacetone 132.4g (0.5mol) and aluminum trichloride 66.7g (0.5mol) respectively to the reaction kettle, seal the reaction kettle and open stirring, heat to 150 ° C to react 15 hours. After the reaction was completed, it was lowered to room temperature, 100 mL of dichloromethane was added and stirred, the released reaction solution was washed with water three times, extracted again, the organic phases were combined, dried over anhydrous sodium sulfate, and the solvent was removed under reduced pressure to obtain 192.4 g of crude hexachlorobisphenol A. , the purity is 95.3%, the yield is 84.3%, and the crude hexachlorobisphenol A is directly used in the next reaction without further processing;

[0032] Under nitrogen protection, the prepared 200g hexachlorobisphenol A crude product and 2.7g antimony pentachloride were respectively added to the reaction kettle, cooled to below 10°C with an ice bath, and then int...

Embodiment 2

[0035] Under nitrogen protection, 94.1g (1.0mol) of phenol and 132.4g (0.5mol) of hexachloroacetone were added to the reactor respectively, and 210.6g (10.5mol) of hydrogen fluoride was introduced into the reactor after cooling to below 10°C with an ice bath. Turn on stirring, heat to 120°C and react for 10 hours. After the reaction was finished, it was lowered to room temperature, and the reaction solution was passed into a container equipped with 1000 mL of water to precipitate a solid, filter the precipitated solid and washed with water, and after drying, 202.5 g of HCB A crude product was obtained, the purity was 98.1%, and the yield was 98.1%. 91.3%, the crude hexachlorobisphenol A is directly used in the next reaction without further processing;

[0036] Under nitrogen protection, the prepared 200g hexachlorobisphenol A crude product and 4.1g antimony trifluoride were respectively added to the reaction kettle, cooled to below 10°C with an ice bath, and then introduced in...

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Abstract

The invention provides a method for synthesizing hexafluorobisphenol A, comprising the following steps: a) reacting hexachloroacetone and phenol under a Lewis acid catalyst to obtain hexachlorobisphenol A; b) combining hexachlorobisphenol A with hydrogen fluoride A fluorination reaction is carried out to obtain hexafluorobisphenol A. The method uses Lewis acid as a catalyst to change the electronic reaction characteristics of phenol, so that the para-carbon atom of phenol and the carbonyl group of hexachloroacetone undergo an addition and elimination reaction, instead of the oxygen atom of phenol and hexachloroacetone. The intermediate hexachlorobisphenol A is obtained by the nuclear substitution reaction, and then the hexachlorobisphenol A is fluorinated to obtain the hexafluorobisphenol A. The method replaces hexafluoroacetone and hexafluoropropylene oxide with hexachloroacetone, which is cheap, easy to obtain and less toxic, as raw materials, has lower requirements on equipment, is beneficial to safe production and reduces production cost, and is the synthesis of hexafluorobisphenol A. The method provides new ideas. The hexafluorobisphenol A prepared by the method has higher yield and higher purity.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for synthesizing hexafluorobisphenol A. Background technique [0002] Bisphenol AF, also known as hexafluorobisphenol A, organic chemical name 2,2-bis(4-hydroxyphenyl)hexafluoropropane, is an important product in organic fluorine materials, widely used in polymer modification and fluorine-containing materials Synthesis of polymers. [0003] At present, the raw materials for the synthesis of bisphenol AF reported in the literature are mainly hexafluoropropylene oxide gas, hexafluoroacetone gas and hexafluoroacetone trihydrate. Patent DE3046604 reported that using anhydrous hydrogen fluoride as solvent and catalyst, hexafluoropropylene oxide was isomerized into hexafluoroacetone, and then reacted with phenol to prepare bisphenol AF, and the reaction required high pressure. Patent JP29449293A reports that under the condition that the amount of trifluoromethanesu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/62C07C37/20C07C39/367
CPCC07C37/62C07C37/20C07C39/367
Inventor 王刚彭智敏李志鹏尹德美张振华
Owner 湖南有色郴州氟化学有限公司