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Polyimide precursor, polyimide having crosslinked structure, and production method therefor

A polyimide precursor, polyimide technology, applied in the direction of coating, can solve problems such as easy gelation, and achieve the effect of increasing solid content concentration and excellent bending resistance

Active Publication Date: 2020-05-29
UBE IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since gelation tends to occur when a cross-linked structure is introduced, it is limited to the form of a low-concentration polyamic acid solution, and thus has the problem of being subject to various restrictions in practical use.

Method used

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  • Polyimide precursor, polyimide having crosslinked structure, and production method therefor
  • Polyimide precursor, polyimide having crosslinked structure, and production method therefor
  • Polyimide precursor, polyimide having crosslinked structure, and production method therefor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0445] The present invention is further illustrated below by Examples and Comparative Examples. In addition, this invention is not limited to the following examples.

[0446] Embodiments of the invention of >

[0447] The raw materials used in each of the following examples are as follows.

[0448] [Tetracarboxylic acid (a)]

[0449] 3,3’,4,4’-Biphenyltetracarboxylic acid: s-BPTA

[0450] 2,3,3’,4’-Biphenyltetracarboxylic acid: a-BPTA

[0451] 4,4’-(4,4’-Isopropylidenediphenoxy)bis(phthalic acid): BPABP

[0452] 4,4’-(Hexafluoroisopropylidene)diphthalic acid: 6FDP

[0453] 4,4’-Oxydiphthalic acid: ODP

[0454] 3,3’,4,4’-Benzophenone tetracarboxylic acid: BTTA

[0455] [Compound (b) having 3 or more amino groups]

[0456] 1,3,5-tris(4-aminophenoxy)benzene: TAPOB

[0457] [chem 47]

[0458]

[0459] 4,4’,4”-Triaminotriphenylamine: TATPA

[0460] [chem 48]

[0461]

[0462] 2,4,4'-Triaminodiphenyl ether: TADE

[0463] [chem 49]

[0464]

[0465] 2,4,6-Triam...

Embodiment I-1

[0512] 1.015 molar equivalents (1.291 g) of s-BPTA (dihydrate) as tetracarboxylic acid (a), 0.03 molar equivalents (0.042 g) of TAPOB as compound (b) having 3 or more amino groups, and diamine ( C) 0.97 molar equivalents (1.000 g) of APB were added to a mortar, thoroughly ground and mixed to obtain a polyimide precursor powder. As a result of confirming this powder with a microscope, no particles having a particle diameter of 0.5 mm or more were found. Add DMAc in an amount (9.33 g) of a monomer concentration of 20% by mass as a solvent (D) to the powder, heat and dissolve at 50° C. to obtain a polyimide precursor solution (solid content 20%, viscosity 50 mPa· s).

[0513] The obtained polyimide precursor solution was applied to a glass substrate, dried at 120°C for 5 minutes, heated at 150°C and 200°C for 10 minutes each, and then heated at 250°C for 1 hour to perform imidization by heating. Amination was performed to obtain a polyimide / glass laminate. Next, after immersin...

Embodiment I-2～24

[0515] Except having changed each component into description in Table I-1, it carried out similarly to Example I-1, and produced the polyimide precursor powder and solution. In addition, in Examples I-23-24, NMP was used as a solvent (D). The polyimide precursor solution obtained obtained polyimide (film) by the same method as Example I-1. The measurement results of the characteristics of this polyimide are shown in Table I-1.

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Abstract

Provided is a polyimide precursor, polyimide having crosslinked structure, and production method therefor. This polyimide precursor includes: a tetracarboxylic acid (a) represented by formula (1), forexample; and an amine compound (b) having three or more amino groups and represented by formula (3), for example. Formula (1): X1 represents a direct bond or a divalent group. Formula (3): Z1 represents a trivalent or higher-valent group, Z2 represents a direct bond or a divalent group, R1 to R4 represent a monovalent group, n1 represents an integer of 3 or more, m1 and m3 represent an integer from 0 to 4, and m2 and m4 represent an integer from 0 to 3.

Description

[0001] This application is a divisional application, the original application number is 201680060718.7, the application date is October 19, 2016, and the invention name is "polyimide precursor, polyimide with cross-linked structure and its manufacturing method ". technical field [0002] The present invention relates to a polyimide precursor capable of easily producing a polyimide having a high crosslinking density, a polyimide having a crosslinked structure excellent in heat resistance and high temperature dimensional stability, and the like Manufacturing method. Moreover, another aspect of this invention relates to the polyimide precursor which can manufacture a highly heat-resistant polyimide easily, and its manufacturing method. Background technique [0003] In addition to its excellent heat resistance, polyimide is also superior to other engineering plastics in terms of mechanical properties and electrical properties. Due to its high reliability in space and aviation i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/18C09D179/08C08L79/08
CPCC08G73/1007C08G73/1039C08G73/1057C08G73/1078C08G73/1085C08J5/18C08J2379/08C09D179/08C08G73/10
Inventor 高泽亮一
Owner UBE IND LTD