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Preparation method of high-purity difluorobenzophenone

A difluorobenzophenone, high-purity technology, applied in 4 fields, can solve the problems of complicated preparation process, low yield of difluorobenzophenone, and high impurity content, and achieves simple synthesis process, improved yield, and high purity improved effect

Inactive Publication Date: 2018-10-02
江苏万隆化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the problems of low yield of 4,4'-difluorobenzophenone, high impurity content and complicated preparation process, the present invention provides a method for preparing high-purity difluorobenzophenone, which includes The following preparation steps:

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] A kind of preparation method of high-purity difluorobenzophenone of the present invention specifically comprises the steps:

[0014] 1. Under the irradiation of ultraviolet light, add 10 parts by mass of p-fluorotoluene into the reaction kettle, and feed 50 parts by mass of chlorine gas into the reaction kettle, heat up to 60°C, add 5 parts by mass of benzophenone and stir evenly, keep warm After 0.8h to the complete reaction of the raw materials, cooling to obtain p-fluorobenzotrichlorotoluene;

[0015] 2. Stir 10 parts by mass of p-fluorobenzotrichloride and 20 parts by mass of 2,6-dichlorofluorobenzene prepared in step 1, and add 5 parts by mass of ferric chloride to react the three to obtain 4,4 Crude '-difluorobenzophenone.

[0016] 3. 5 parts by mass of the crude product of 4,4'-difluorobenzophenone were dissolved in 60 parts by mass of an ethanol solution with a mass percent concentration of 30% after vacuum distillation, and multi-stage cooling and fractional c...

Embodiment 2

[0019] A kind of preparation method of high-purity difluorobenzophenone of the present invention specifically comprises the steps:

[0020] 1. Under the irradiation of ultraviolet light, add 25 parts by mass of p-fluorotoluene into the reaction kettle, and feed 70 parts by mass of chlorine gas into the reaction kettle, raise the temperature to 68°C, add 10 parts by mass of benzophenone and stir evenly, keep warm After 0.8h to the complete reaction of the raw materials, cooling to obtain p-fluorobenzotrichlorotoluene;

[0021] 2. Stir 20 parts by mass of p-fluorobenzotrichloride and 50 parts by mass of 2,6-dichlorofluorobenzene prepared in step 1, and add 15 parts by mass of aluminum trichloride to react the three to obtain 4,4 Crude '-difluorobenzophenone.

[0022] 3. The obtained 10 parts by mass of 4,4'-difluorobenzophenone crude product was subjected to vacuum distillation and then dissolved in 90 parts by mass of an ethanol solution with a mass percent concentration of 90...

Embodiment 3

[0025] A kind of preparation method of high-purity difluorobenzophenone of the present invention specifically comprises the steps:

[0026] 1. Under the irradiation of ultraviolet light, add 15 parts by mass of p-fluorotoluene into the reaction kettle, and feed 60 parts by mass of chlorine gas into the reaction kettle, heat up to 68°C, add 7 parts by mass of benzophenone and stir evenly, keep warm After 0.8h to the complete reaction of the raw materials, cooling to obtain p-fluorobenzotrichlorotoluene;

[0027] 2. Stir 15 parts by mass of p-fluorobenzotrichloride and 30 parts by mass of 2,6-dichlorofluorobenzene prepared in step 1 evenly, add 5 parts by mass of aluminum trichloride and 5 parts by mass of methylbenzene, and the reaction system Crude 4,4'-difluorobenzophenone was obtained.

[0028] 3. The obtained 7 parts by mass of 4,4'-difluorobenzophenone crude product was subjected to vacuum distillation and dissolved in 75 parts by mass of an ethanol solution with a concen...

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Abstract

The invention discloses a preparation method of high-purity difluorobenzophenone. According to the method, p-fluorotoluene, chlorine, 2,6-dichlor fluorbenzene, an ethanol solution and diphenyl ketoneare taken as raw materials, the raw materials are subjected to chlorination reaction, multistage cooling and fractional crystallization, finally a target product 4,4'-difluorobenzophenone is obtained.The purity of the product is improved, and meets the purity requirement of composite polyether-ether-ketone (PEEK). In the method, the raw materials are easy to get, the composite technology is simple, and the yield of the 4,4'-difluorobenzophenone is improved, so that the method has a broad application prospect and industrial value.

Description

technical field [0001] The invention relates to a preparation method of difluorobenzophenone, in particular to a preparation method of high-purity 4,4'-difluorobenzophenone. Background technique [0002] 4,4'-Difluorobenzophenone (4,4'-DFBP) is a well known chemical intermediate that is known to be useful in the preparation of, for example, PAEK polymers such as PEEK and PEK . At the same time, 4,4'-DFBP is an important intermediate in the synthesis of fluorine-containing drugs flunarizine, lomerizine, and almitrigine in medicine. In the chemical and military fields, polyetheretherketone (PEEK) is a special Polymer Materials. It has physical and chemical properties such as high temperature resistance and chemical corrosion resistance. It is a kind of high temperature resistant structural material and electrical insulation material. It can be combined with glass fiber or carbon fiber to prepare reinforcement materials; 4,4'-difluorobenzophenone In the preparation process o...

Claims

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Application Information

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IPC IPC(8): C07C45/45C07C49/813
CPCC07C17/14C07C45/45C07C49/813C07C25/13
Inventor 郁红明
Owner 江苏万隆化学有限公司