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Preparation method of 3-fluorophthalic anhydride

A kind of technology of fluorophthalic anhydride and chlorophthalic anhydride, applied in the field of preparation of 3-fluorophthalic anhydride

Active Publication Date: 2013-04-03
QUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the above-mentioned methods, potassium fluoride is used as the fluorinating reagent, which will produce a large amount of solid waste, the main components of which are potassium chloride produced by the exchange of fluorine and chlorine and unreacted excess potassium fluoride

Method used

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  • Preparation method of 3-fluorophthalic anhydride
  • Preparation method of 3-fluorophthalic anhydride

Examples

Experimental program
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Effect test

Embodiment 1

[0029] In a 500mL four-neck flask, add 100g of 3-chlorophthalic anhydride and 100mL of hydrogen fluoride pyridine complex, protect it with nitrogen, stir the reaction at 100-160°C, monitor the reaction progress by GC, when the conversion rate of 3-chlorophthalic anhydride reaches 98.0% When above, stop the reaction; pour the reaction liquid into 2000mL ice water, stir and mix thoroughly, precipitate the solid, filter, rinse the solid with ice water, and dry in vacuo to obtain 82.6g of crude product of 3-fluorophthalic anhydride; 160 mL of n-heptane was fully washed, filtered, and vacuum-dried to obtain 76.4 g of pure 3-fluorophthalic anhydride, with a yield of 84.0% and a melting point of 158-160°C.

Embodiment 2

[0031] In a 500mL four-neck flask, add 100g of 3-chlorophthalic anhydride and 100mL of hydrogen fluoride pyridine complex, protect it with nitrogen, stir the reaction at 120-140°C, monitor the reaction progress by GC, when the conversion rate of 3-chlorophthalic anhydride reaches 98.0 % above, terminate the reaction; pour the reaction solution into 4000mL ice water, stir and mix thoroughly, precipitate the solid, filter, rinse the solid with ice water, and dry in vacuo to obtain 81.8g of crude 3-fluorophthalic anhydride; Wash thoroughly with 200mL of n-pentane, filter, and vacuum-dry to obtain 75.8g of pure 3-fluorophthalic anhydride, with a yield of 83.3% and a melting point of 159-161°C.

Embodiment 3

[0033] In a 500mL four-neck flask, add 100g of 3-chlorophthalic anhydride and 100mL of hydrogen fluoride triethylamine complex, protect it with nitrogen gas, stir the reaction at 100-180°C, monitor the reaction progress by GC, when the conversion rate of 3-chlorophthalic anhydride When it reaches above 98.0%, the reaction is terminated; the reaction solution is poured into 2000mL ice water, fully stirred and mixed, the solid is precipitated, filtered, the solid is rinsed with ice water, and vacuum-dried to obtain 79.8g of crude 3-fluorophthalic anhydride; 160 mL of toluene and 200 mL of n-pentane were fully washed, filtered, and vacuum-dried to obtain 71.1 g of pure 3-fluorophthalic anhydride, the yield was 78.2%, and the temperature was 159-161 ° C.

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Abstract

The invention discloses a preparation method of 3-fluorophthalic anhydride, which is characterized in that an organic complex of hydrogen fluoride is used as a fluorination reagent and homogeneous fluorination is performed on 3-chlorophthalic anhydride to prepare the 3-fluorophthalic anhydride. The preparation method sequentially comprises the following steps: 1) fluorination reaction: adding the 3-chlorophthalic anhydride and the fluorination reagent into a four-neck flask, reacting under a nitrogen gas protective atmosphere, monitoring the reaction progress through gas phase chromatography, and terminating the reaction when the 3-chlorophthalic anhydride conversion rate is up to 98.0% or above; 2) post treatment of the reaction solution, namely pouring the reaction solution into ice water, precipitating solids, sufficiently stirring and mixing, filtering, leaching the solids with ice water, and drying in vacuum to obtain a crude 3-fluorophthalic anhydride product; and 3) purification: sufficiently washing the crude product with a certain amount of aromatic hydrocarbon and long-carbon-chain alkane sequentially, performing vacuum filtration, and drying in vacuum to obtain the purified 3-fluorophthalic anhydride product, wherein the melting point of the purified 3-fluorophthalic anhydride product is 159-161 DEG C. According to the invention, the preparation method for producing 3-fluorophthalic anhydride has the advantages of high fluorination efficiency, good product purity, high yield, environment friendliness and the like.

Description

(1) Technical field [0001] The present invention relates to a preparation method of 3-fluorophthalic anhydride, in particular provides a method for preparing 3-fluorophthalic anhydride by using an organic complex of hydrogen fluoride as a fluorination reagent. (2) Background technology [0002] Polyimide (PI) is a class of polymer materials with imide repeating units on the molecular chain. The performance of polyimide depends to a large extent on the structure of monomers. Synthesizing monomers with certain special structures can give polyimide materials corresponding characteristics through their polymerization. Fluorophthalic anhydride, as the key intermediate, has better reactivity than chlorophthalic anhydride, and can be used to synthesize monomers with special structures, and the industrialization of each important monomer will bring polyimides The rapid development of materials. As one of the fluorinated phthalic anhydrides, 3-fluorophthalic anhydride can be used i...

Claims

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Application Information

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IPC IPC(8): C07D307/89
Inventor 吕亮吴雪妹王玉林陈剑君吾国强
Owner QUZHOU UNIV
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