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Method for producing decafluorobiphenyl

A technology of decafluorobiphenyl and pentafluorobenzoic acid is applied in the field of preparation of decafluorobiphenyl, can solve the problems of low yield, high cost of raw materials, unworkable industrialization routes, etc., and achieves high yield, low production cost, Easy-to-use effects

Inactive Publication Date: 2010-12-22
江苏华达化工集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has a low yield and a high reaction temperature, which must reach 240°C, and also produces a large amount of waste water
[0005] 2. Journal of the American Chemical Society, No. 132(8), 2522~2523; In 2010, the by-product of decafluorobiphenyl was generated by reacting styrene with pentafluorotoluene. The yield of this method was low, only 13%.
The disadvantage is that the cost of raw materials is high, the price of pentafluoroiodobenzene or pentafluorobromobenzene is expensive, and the industrialization route is not feasible

Method used

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  • Method for producing decafluorobiphenyl
  • Method for producing decafluorobiphenyl

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Weigh 50 g of pentafluorobenzoic acid, grind it, and put 12.6 g of catalyst copper oxide (molar ratio: pentafluorobenzoic acid:catalyst = 1.5:1), stir evenly, and put it into the reactor. Slowly start stirring, and slowly raise the temperature to 240°C, with an average of 0.8~1°C per minute. Obtained white solid: 37g, content 97%, calculated by pentafluorobenzoic acid, pure yield: 91.1%.

[0020] Take 50g of the product with a content of 97%, put it in a reactor, add (product: solvent weight ratio = 1:1) ethanol, heat up to 70 degrees to completely dissolve, cool to normal temperature, filter, and dry to obtain a solid: 45g, Sampling analysis content: 98.4%.

Embodiment 2

[0021] Example 2: The basic implementation steps are the same as the first paragraph of Example 1, except that the amount of catalyst copper oxide is changed to 21g (molar ratio: pentafluorobenzoic acid:catalyst=0.9:1), and the white solid is obtained: 37.5g, content 97.5%, based on pentafluorobenzoic acid, the pure yield is: 92.8%.

Embodiment 3

[0022] Example 3: The basic implementation steps are the same as the first paragraph of Example 1, except that the amount of catalyst copper oxide is changed to 10.5g (molar ratio: pentafluorobenzoic acid:catalyst=1.8:1), and a white solid is obtained: 32g, content 97%, based on pentafluorobenzoic acid, the pure yield is: 78.8%.

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Abstract

The invention discloses a method for producing decafluorobiphenyl, belonging to the field of a preparation method for the decafluorobiphenyl and comprising the following steps of: (1) reacting: evenly stirring reaction raw materials: penta fluoro benzoic acid and a catalyst and then feeding; (2) distilling: gradually heating to the centigrade temperature of 200-260 DEG C, and distilling to obtain a product; and (3) refining: refining the product to obtain a refined product. The invention has the advantages that 1. an environmental-protection synthesis method is provided; 2. a solid-solid reaction system adopted in the invention does not need reaction solvents, does not generate waste water and has low production cost; and moreover, reaction is carried out in one container in one step. The method has the advantages of simple and convenient operation and high product yield and ensures that the scale production becomes possible.

Description

technical field [0001] The invention relates to a preparation method of decafluorobiphenyl, more specifically a method for producing decafluorobiphenyl by using pentafluorobenzoic acid as a raw material and adding a catalyst. Background technique [0002] As fluorine-containing liquid crystal materials are more and more widely used and the market prospect is getting better and better, decafluorobiphenyl, as a key raw material of liquid crystal materials, plays an increasingly important role in the production of liquid crystal materials. [0003] At present, the synthesis methods of decafluorobiphenyl mainly include the following types, and there is no report on the synthesis of this substance in China: [0004] 1. Volume 100 of "Chem.Ber", pages 3016-3023, describes the method of preparing decafluorobiphenyl by reacting sodium pentafluorobenzoate and copper acetate with water as the medium. The yield of this method is low, and the reaction temperature is relatively high...

Claims

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Application Information

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IPC IPC(8): C07C25/18C07C17/363
Inventor 徐光辉刘军周豪恽海顺
Owner 江苏华达化工集团有限公司
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