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Two fluoric dianhydride monomers and preparation method thereof

A dianhydride monomer and monomer technology, applied in the field of dianhydride monomer and its preparation of hyperbranched polyimide, can solve the problems of solvent waste, large amount of solvent, low solid content, etc., and achieve easy operation , Improve light transmittance, simple synthesis route

Inactive Publication Date: 2010-05-12
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the large amount of solvent used in the reaction process and low solid content, if the reaction solution is directly poured into acid or other solutions to precipitate the product, it will cause a great waste of solvent

Method used

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  • Two fluoric dianhydride monomers and preparation method thereof
  • Two fluoric dianhydride monomers and preparation method thereof
  • Two fluoric dianhydride monomers and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Embodiment 1: the process of synthesizing 4,4'-(2-(3'-trifluoromethyl-phenyl)-1,4-phenoxy)-phthalic anhydride

[0040]In a 500ml three-neck flask equipped with mechanical stirring, a nitrogen port with a thermometer, and a spherical condenser, add 30.30 grams (0.12mol) of 2-(3'-trifluoromethyl-phenyl)-1,4-terephthalene Phenol, 42.56 grams (0.30mol) of 4-nitrophthalonitrile, 49.68 grams (0.36mol) of potassium carbonate, 240ml N, N-dimethylacetamide (solid content is 51.1%), nitrogen flow, start stirring , reacted for two days, then slowly raised the temperature to 50-80°C, reacted for 2 hours, stopped heating, and continued to stir for a period of time, and stopped stirring after returning to room temperature to end the reaction. The output is in deionized water; then the product is washed repeatedly with deionized water until the water is colorless, filtered by suction, and dried in vacuum to obtain a yellow powder, namely 4,4'-(2-(3'-trifluoromethyl -55.86 g of -pheny...

Embodiment 2

[0046] The method is the same as in Example 1, and the amount of 2-(3', 5'-bistrifluoromethyl-phenyl)-1,4-hydroquinone is changed to 38.40 grams (0.12mol), 42.56 grams (0.3mol ) 4-nitrophthalonitrile, 49.68 grams (0.36mol) of potassium carbonate, 240ml N, N-dimethylacetamide (solid content is 54.4%) is packed into the nitrogen port with thermometer, mechanically stirred , in a 500ml three-neck flask with a spherical condenser, blow nitrogen, start stirring, react for two days, then slowly raise the temperature to 50-80°C, react for 2 hours, stop heating, continue stirring for a while, stop stirring when the room temperature is restored, and end reaction. The material is discharged in deionized water; then the product is washed repeatedly with deionized water until the water is colorless, filtered by suction, and dried in vacuum to obtain a yellow powder, namely 4,4'-(2-(3',5'-di 62.40 g of trifluoromethyl-phenyl)-1,4-phenoxy)-1,1',2,2'-phthalonitrile.

[0047] Put the above ...

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Abstract

The invention provides two fluoric dianhydride monomers and a preparation method, belonging to the technical field of organic compound and preparation thereof. The fluoric dianhydride monomers are 4,4'-(2-(3'- trifluoromethyl-phenyl)-1,4-phenoxy)-phthalic anhydride and 4,4'-(2-(3',5'- Di(trifluoromethyl)-phenyl)-1,4-phenoxy)-phthalic anhydride. The preparation method is as follows: taking 2-(3'-trifluoromethyl-phenyl)-1,4-hydroquinone or 2-(3',5'-Di(trifluoromethyl)-phenyl)-1,4-hydroquinone as a raw material to prepare tetranitrile monomer; hydrolyzing the tetranitrile monomer under backflow of the mixed solution of potassium hydroxide, water and alcohol to prepare tetracid monomer; and refluxing, dehydrating and recrystallizing on the tetracid monomer to obtain the product. The invention has the advantages of simpler synthesis route, stable raw material monomer at room temperature, easy separation of products and lowered cost; the product can be applied in the field of preparing polyimide hyperbranched waveguide materials.

Description

technical field [0001] The invention belongs to the technical field of organic compounds and their preparation, and specifically relates to two novel dianhydride monomers containing fluorine, large side groups and ether bonds which can be used to prepare hyperbranched polyimides and a preparation method thereof. Background technique [0002] Diether dianhydride is a commonly used monomer for the synthesis of ether anhydride polyimide (PI) in the past, but bisether dianhydride containing fluorine, large side groups and ether bonds important monomer. By introducing large side groups and ether bonds, the solubility of polyimide materials can be improved, and the introduction of trifluoromethyl groups can improve the light transmittance of materials and reduce the dielectric constant, especially for optical waveguide materials, which can reduce the material The absorption loss in the communication band, and the introduction of large side groups can reduce the birefringence valu...

Claims

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Application Information

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IPC IPC(8): C07D307/89
Inventor 姜振华刘禹关绍巍张云鹤张海博王永鹏
Owner JILIN UNIV
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