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A kind of preparation method of 4,4-biphenyl ether dianhydride

A technology of biphenyl ether dianhydride and dimethylformamide, which is applied in the field of preparation of 4,4-biphenyl ether dianhydride, can solve the problems of complex preparation methods, many by-products, and low yield, and achieve the production cost Low, less by-products, high reaction yield effect

Active Publication Date: 2021-12-07
HEBEI HAILI FRAGRANCES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems that the existing 4,4-biphenyl ether dianhydride preparation method is complex, with many by-products and low yield, the present invention provides a preparation method of 4,4-biphenyl ether dianhydride

Method used

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  • A kind of preparation method of 4,4-biphenyl ether dianhydride
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  • A kind of preparation method of 4,4-biphenyl ether dianhydride

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Effect test

Embodiment 1

[0035] A preparation method of 4,4-biphenyl ether dianhydride, mixing compound I, compound II, N,N-dimethylformamide and toluene at a molar ratio of 1:1:0.5:0.5, and proceeding at 110°C After reacting for 6 hours, the reaction solution was cooled to 80°C at a cooling rate of 6°C / h, filtered to remove solid matter, and then cooled to 20°C at a cooling rate of 6°C / h, filtered to obtain 4,4-biphenyl ether di anhydride crystals.

[0036] Wherein the structural formula of compound I is:

[0037]

[0038] The structural formula of compound II is:

[0039]

[0040] The yield and purity of the obtained 4,4-biphenyl ether dianhydride were detected, and the yield was 98.1%, and the purity was 98%.

Embodiment 2

[0042] A preparation method of 4,4-biphenyl ether dianhydride, mixing compound I, compound II, N,N-dimethylformamide and toluene at a molar ratio of 1:1:0.5:0.5, and proceeding at 110°C After reacting for 6 hours, the reaction solution was cooled to 80°C at a cooling rate of 6°C / h, filtered to remove solid matter, and then cooled to 20°C at a cooling rate of 6°C / h, filtered to obtain 4,4-biphenyl ether di Anhydride crystals; then dissolve 4,4-biphenyl ether dianhydride crystals in N,N-dimethylformamide (water content less than 500ppm), so that 4,4-biphenyl ether dianhydride and N,N-di The molar ratio of methyl formamide is 1:1, heat up to 80°C, filter to remove solid matter, cool the filtrate to 20°C at a cooling rate of 6°C / h, filter, and dry the filtered crystals at 160°C for 7 hours , to obtain 4,4-biphenyl ether dianhydride.

[0043] Wherein the structural formula of compound I is:

[0044]

[0045] The structural formula of compound II is:

[0046]

[0047] The y...

Embodiment 3

[0049] A method for preparing 4,4-biphenyl ether dianhydride, mixing compound I, compound II, dimethyl sulfoxide and xylene in a molar ratio of 1:1.1:2:1, and reacting at 120°C for 8 hours, The reaction solution was cooled to 90°C at a cooling rate of 7°C / h, filtered to remove solid matter, then cooled to 22°C at a cooling rate of 7°C / h, and filtered to obtain 4,4-biphenyl ether dianhydride crystals; Dissolve 4,4-biphenyl ether dianhydride crystals in N,N-dimethylacetamide (water content less than 500ppm), make 4,4-biphenyl ether dianhydride and N,N-dimethylacetamide The molar ratio is 1:2, heated to 90°C, filtered to remove solid matter, the filtrate was cooled to 22°C at a cooling rate of 7°C / h, filtered, and the filtered crystals were dried at 170°C for 6h to obtain 4, 4-Diphenyl ether dianhydride.

[0050] Wherein the structural formula of compound I is:

[0051]

[0052] The structural formula of compound II is:

[0053]

[0054] The yield and purity of the obtai...

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Abstract

The invention relates to the technical field of compound synthesis, and specifically discloses a preparation method of 4,4-biphenyl ether dianhydride. The preparation method of the 4,4-biphenyl ether dianhydride is to mix a specific compound, a solvent and a water-carrying agent, carry out a dehydration coupling reaction at 110-155° C., and crystallize on cooling to obtain 4,4-biphenyl ether dianhydride crystals. The reaction process route of the invention is short, the by-products are few, the purity and the yield of the reaction product are high, and it can be widely popularized and used.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a preparation method of 4,4-biphenyl ether dianhydride. Background technique [0002] 4,4-Diphenyl ether dianhydride (ODPA) is an aromatic polyimide monomer material, its structural formula is: Since ODPA contains ether-based flexible groups, the polyimide synthesized with ODPA as a monomer can increase the flexibility of the entire molecular chain, and is also beneficial to reduce the force between molecules, reduce the glass transition temperature, improve its processing performance, and expand The application field of polyimide. [0003] At present, the preparation methods of ODPA mainly include: 1) condense 3,4-dimethylether phenol and 4-bromo-o-xylene into tetramethyldiphenyl ether, and then oxidize it with potassium permanganate in a pyridine medium to form tetramethyldiphenyl ether. Ether acid, the raw material source of this method is difficult, and the synt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/89
CPCC07D307/89
Inventor 李文革邵帅朱玉梅张玉芬郭少康于玉秀周婕妤
Owner HEBEI HAILI FRAGRANCES CO LTD
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