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Synthesis of biphenyl type polyimide resin with phenyl ethyne dead-end

A technology of biphenyl type polyimide and phenylacetylene is applied in the synthesis field of biphenyl type polyimide resin, which can solve the problem of high cost and achieve the effects of low cost, good thermal stability and mechanical properties

Inactive Publication Date: 2005-03-23
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore in recent years based on the resin of the phenylacetylene end capping of biphenyl, development is very fast, mainly also be to research its application (US Patent, 5493002; 5567800; 6133401; 6350817, document, journal of compositematerials, 2002,36 (19), 2255,), which involves a large number of relatively expensive 3,4-biphenyl dianhydrides that have not yet been commercialized, which also makes the final cost of the resin higher

Method used

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  • Synthesis of biphenyl type polyimide resin with phenyl ethyne dead-end
  • Synthesis of biphenyl type polyimide resin with phenyl ethyne dead-end

Examples

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Effect test

Embodiment 1

[0016] Example 1 Add 0.1mol (32.6g) of 4,4'-biphenyldianhydride, 0.1mol (32.6g) of 1,6-hexanediamine (23.2g, 0.2mol) and 0.1mol (24.8g) of phenylacetylene phthalic anhydride to N, N' - In dimethylformamide (3000ml), after stirring and reacting at room temperature for 12h, add 0.4mol (40g) of dehydrating agent acetic anhydride and 0.04mol (4g) of catalyst triethylamine to continue stirring for 12h, then pour it into a large amount of ethanol , a pale yellow precipitate was precipitated, and the precipitate was collected by filtration, washed thoroughly with ethanol, and dried to obtain 73 g of phenylacetylene-capped polyimide resin.

Embodiment 2

[0018] Add 0.2mol (65.2g) of 3,4'-biphenyldianhydride, 0.3mol (32.4g) of p-phenylenediamine and 0.2mol (49.6g) of phenylacetylene phthalic anhydride to N,N'-dimethylformamide ( 300mL), stirred and reacted at room temperature for 12h, added 1.5mol (153g) of dehydrating agent acetic anhydride and 1mol (101g) of catalyst triethylamine and continued to stir for 12h, then poured it into a large amount of ethanol, precipitated, and collected the precipitate by filtration , and fully washed with ethanol, and dried to obtain phenylacetylene-capped polyimide resin.

Embodiment 3

[0020] Add 0.1mol (32.6g) of 3,3'-biphenyldianhydride, 0.11mol (11.9g) of m-phenylenediamine and 0.02mol (5g) of phenylacetylene phthalic anhydride to N,N'-dimethylformamide (110ml ), after stirring and reacting at room temperature for 12 hours, add 0.44 mol (44 g) of dehydrating agent acetic anhydride and 0.44 mol (44 g) of catalyst triethylamine to continue stirring and reacting for 12 hours, then pour it into a large amount of ethanol, precipitate out, and collect the precipitate by filtration , and fully washed with ethanol, and dried to obtain phenylacetylene-capped polyimide resin.

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Abstract

A process for synthesizing the phenylacetylene dead-end biphenylpolyimide resin with high thermal stability and mechanical performance and low viscosity of molten body includes such steps as proportionally adding diphenyldianhydride, bibasic amine and phenylacetylene phenylanhydride to polar solvent, stirring while reacting, adding acetic anhydride and triethylamine, stirring while reacting, depositing, washing the deposit and drying.

Description

technical field [0001] The invention belongs to the synthesis method of biphenyl type polyimide resin endcapped by phenylacetylene. Background technique [0002] Thermosetting polyimide is a kind of advanced composite material matrix resin, which has high thermal oxidation resistance, mechanical properties and high glass transition temperature, and has very important applications in the field of aerospace materials. Phenylacetylene phthalic anhydride-terminated polyimide resin has very low melt viscosity and is expected to be used in resin transfer molding (RTM) forming process, which is characterized by high efficiency and low cost, and can process various complex composite materials parts. In recent years, NASA has gradually applied it to polyimide resin for RTM. Biphenyl polyimide resin has a high glass transition temperature and high mechanical properties, and has a very wide range of uses, and its performance is obviously due to Polyimide resins based on ketone anhydr...

Claims

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Application Information

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IPC IPC(8): C08G73/10
Inventor 王震刘燕峰杨慧丽高连勋丁孟贤
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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