Method for preparing high purity (99.9 percent) 4,4'-difluorobenzophenone

A difluorobenzophenone, high-purity technology, applied in 4 fields, can solve problems such as inability to improve, and achieve the effect of mature recovery technology and mild synthesis process conditions

Inactive Publication Date: 2012-07-04
JINTAN CHUNFENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the existing synthesis technology of 4,4'-difluorobenzophenone, the purity of 4,4'-difluorobenzophenone monomer cannot be improved,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0019] Example 1:

[0020] Step 1: Put 275g (2.5mol) of 4-fluorotoluene into a 1000ml four-necked flask equipped with stirring, temperature juice, reflux spherical condenser and chlorine pipe, and add the initiator dibenzoyl peroxide ( BPO) Appropriate amount, heat to 90℃ and start to introduce liquid chlorine. Add initiator in the middle, react at 90℃~100℃ to the end, stop the chlorine for about 4 hours to 5 hours, and get 4-fluorotrichloro Toluene 515g, the yield is 96.5%;

[0021] In the second step, in a four-necked reaction flask equipped with stirring, temperature juice, reflux condenser and constant pressure dropping funnel, first add 320g (1.5mol) of 4-fluorotrichlorotoluene, and then add an appropriate amount of catalyst iron trichloride In the constant pressure dropping funnel, add 25.6g of water, start stirring, and when the temperature is raised to 90℃, start to drip water with ferric chloride, the reaction will start, control the dropping temperature at 90℃~105℃, abou...

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PUM

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Abstract

The invention discloses a method for preparing high purity (99.9 percent) 4,4'-difluorobenzophenone, wherein 4-fluorotoluene and liquid chlorine are taken as starting raw materials and then are processed through chlorination reaction, hydration reaction and condensation reaction, and high purity (99.9 percent) 4,4'-difluorobenzophenone is obtained finally. The method gives up the conventional synthetic route; 4-fluorotoluene is processed through chlorination, hydration and condensation firstly to obtain 4,4'-difluorobenzophenone, wherein the melting point of 4,4'-difluorobenzophenone ranges from 107 to 108 DEG C, and the purity of 4,4'-difluorobenzophenone is 99.9 percent; the purity of 4,4'-difluorobenzophenone exceeds the conventional technical standard (99.7 percent) of English ICI (Imperial Chemical Industries Ltd.); in the preparation technology of the method, the adopted raw materials are easy to get, the synthesis process conditions are mild, and almost no environment hazards can be caused. The method satisfies the technical requirements of special engineering plastic containing polyether-ether-ketone on monomers.

Description

Technical field: [0001] The present invention relates to the preparation of 4,4'-difluorobenzophenone, in particular to the preparation of high-purity (99.9%) 4,4'-difluorobenzophenone. Background technique: [0002] 4,4′-Difluorobenzophenone (DFBP) is an important monomer of special high-performance engineering plastics polyether ether ketone, polyether ether ketone is a semi-crystalline aromatic thermoplastic special engineering plastics, it is high temperature resistant, Engineering plastics with particularly excellent corrosion resistance and abrasion resistance were successfully developed in the late 1970s in the UK. The British ICI company adopted the diazonium salt method, using 4,4'-diaminodiphenylmethane and sodium nitrite as raw materials. The 4,4'-difluorobenzophenone with a purity of 99.7% can be obtained from the diazotization reaction, decomposition reaction and oxidation reaction, which provide the most important raw material for the polymerization of polyethe...

Claims

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Application Information

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IPC IPC(8): C07C49/813C07C45/46
Inventor 于锁荣
Owner JINTAN CHUNFENG CHEM
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