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Method for preparing maleimide stop end type polyimide resin

A technology of polyimide resin and maleimide, applied in the preparation of maleimide-terminated polyimide resin, the application field of adhesive-free two-layer flexible copper clad laminate, can Solve the problems of limited application, poor impact resistance and stress cracking resistance, and achieve the effects of reduced requirements for equipment and environmental conditions, low production costs, and simple processes

Active Publication Date: 2009-12-23
华烁电子材料(武汉)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This new type of polymer material made by modifying certain chemicals called Maleimides (Malehydrides) was developed earlier but it still had some drawbacks like poor water resistance or instability during use due to its hydrophobicity when mixed into other materials. To solve this problem, researchers have been working on improving these properties through various methods including introducing specific groups onto Matsumoto' s catalyst residues or adding different types of substituents around them. These modifications resulted in improved physical characteristics without affecting their original function.

Problems solved by technology

This patented technical problem addressed in this patents relates to improving flexibility and durability when producing an adhesion-less double-ply flexible coated liquid crystal display panel (LCD). Current solutions involve adding polymerizable monomers like diacid chloroacrylate(BCMA)-based copolymerized acids onto the surfaces of both layers during fabrication processes. These modifications result in decreased strengths over time due to reduced solubility of BCMA and improved stability against UV ray exposures. Additionally, current biaxially oriented plastic films require expensive special facilities and strict environment control regulations. Therefore there exists a demand for new types of compositions containing less volatile components while maintaining their good physical characteristics and compatibility with existing systems without compromising their quality.

Method used

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  • Method for preparing maleimide stop end type polyimide resin
  • Method for preparing maleimide stop end type polyimide resin
  • Method for preparing maleimide stop end type polyimide resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 24.03 grams (0.12 moles) of 3,4'-diaminodiphenyl ether, 3.92 grams (0.04 moles) of maleic anhydride and 29.42 grams (0.10 mol) was successively added to NMP (229 milliliters), under nitrogen protection, after stirring at room temperature for 10 hours, 0.24 moles of dehydrating agent acetic anhydride (22.65 milliliters), 0.24 moles of dehydration catalyst triethylamine (33.47 milliliters) and NMP 153 milliliters, reacted at 50°C for 7 hours, and poured it into a large amount of absolute ethanol stirred at high speed to obtain a precipitate. The obtained precipitate was thoroughly washed successively with absolute ethanol and absolute ether, and vacuum-dried to obtain 47.16 g of maleimide-terminated polyimide resin.

[0035] Take by weighing 30 grams of the above-mentioned maleimide-terminated polyimide resin and 3 grams of diallyl bisphenol A, mix the two, dissolve in NMP (158 milliliters), and fully stir to form a homogeneous solution . Coat this solution on a copper ...

Embodiment 2

[0037] With 4,4'-diaminodiphenyl ether 50.06 grams (0.25 mole), maleic anhydride 9.81 grams (0.10 mole) and 3,3',4,4'-diphenyl ether tetraacid dianhydride 62.13 grams ( 0.20 mole) was successively added in DMAc (488 milliliters), under the protection of nitrogen, after stirring at room temperature for 12 hours, add 0.75 moles (70.77 milliliters) of dehydrating agent acetic anhydride, 0.50 moles (69.73 milliliters) of dehydration catalyst triethylamine and DMAc 325 milliliters were reacted at 70° C. for 4 hours, and poured into a large amount of high-speed stirring absolute ethanol to obtain a precipitate. The obtained precipitate was washed thoroughly with anhydrous ethanol and anhydrous ether successively, and vacuum-dried to obtain 99.26 g of maleimide-terminated polyimide resin.

[0038] Take by weighing 80 grams of the above-mentioned maleimide-terminated polyimide resin and 13 grams of diallyl bisphenol A, after the two are mixed, be dissolved in DMAc (425 milliliters), f...

Embodiment 3

[0040] 4,4'-diaminodiphenylsulfone (4,4'-DDS) 86.90 grams (0.35 moles), maleic anhydride 9.81 grams (0.10 moles) and 2,2'-bis(3,4-di Carboxyphenyl) 133.27 grams (0.30 moles) of hexafluoropropane tetra-acid dianhydride were successively added to DMF (920 milliliters), under nitrogen protection, after stirring at room temperature for 16 hours, 1.40 moles (132.10 milliliters) of dehydrating agent acetic anhydride were added , 0.14 mol (19.52 milliliters) of dehydration catalyst triethylamine and 613 milliliters of DMF were reacted at 60° C. for 6 hours, and poured into a large amount of dehydrated ethanol stirred at high speed to obtain a precipitate. The obtained precipitate was thoroughly washed successively with absolute ethanol and absolute ether, and then vacuum-dried to obtain 200.00 g of maleimide-terminated polyimide resin.

[0041] Take by weighing 100 grams of the above-mentioned maleimide-terminated polyimide resin and 6 grams of diallyl bisphenol A, mix the two, disso...

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Abstract

The invention relates to a method for preparing maleimide stop end type polyimide resin, comprising the following steps: diamine, maleic anhydride and tetracarboxylic dianhydride are sequentially added to a polar solvent according to a molar ratio of (n+1):2:n to have the solid content of 25 plus or minus 1 percent (gram/milliliter) and then stirred for 8-24 hours at room temperature under the protection of nitrogen to generate intermediate polyamide acid, then a dehydrating agent acetic anhydride, a dehydrating catalytic agent triethylamine and the polar solvent are added into the intermediate polyamide acid so that the solid content is reduced to 15 percent (gram/milliliter) and then chemical imidization for 4-6 hours is conducted under the temperature of 30 DEG C-80 DEG C, then reaction liquid is poured into anhydrous ethanol which is stirred at high speed to obtain deposits, and the deposits are sequentially and sufficiently washed by the anhydrous ethanol and anhydrous ether and then dried in vacuum so as to obtain the maleimide stop end type maleimide polyimide resin, or heat dehydration cyclizing is conducted on the generated intermediate polyamide acid under the action of entrainer ortho-dichlorobenzene and chlorobenzene or methylbenzene to obtain outcomes of the maleimide stop end type maleimide polyimide resin.

Description

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Claims

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Application Information

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Owner 华烁电子材料(武汉)有限公司
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