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Polyimide precursor, resin composition, and method for producing resin film

A technology of polyimide precursor and resin composition, which is applied in the direction of chemical instruments and methods, synthetic resin layered products, layered products, etc., and can solve the problems of insufficient transparency, areas where transparency is difficult to use, and visible light regions Problems such as low light transmittance

Active Publication Date: 2018-05-11
ASAHI KASEI KK
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, conventional polyimide resins, including the polyimides described in the above documents, are colored brown or yellow due to their high density of aromatic rings, and therefore have low light transmittance in the visible light region, making it difficult to use them in applications requiring transparency. sexual domain
For example, the polyimide of the above-mentioned Non-Patent Document 1 obtained from 3,3',4,4'-biphenyltetracarboxylic dianhydride and p-phenylenediamine has a high yellowness index (YI value) at a film thickness of 10 μm. To 40 or more, it is not sufficient in terms of transparency

Method used

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  • Polyimide precursor, resin composition, and method for producing resin film
  • Polyimide precursor, resin composition, and method for producing resin film
  • Polyimide precursor, resin composition, and method for producing resin film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0361] Put 96g of N-methyl-2-pyrrolidone (NMP) in a 500ml detachable flask replaced by nitrogen, and put 17.71g (77.6mmol) of 4-aminophenyl-4-aminobenzoate (APAB) and 4.82 g (19.4 mmol) of 4,4'-diaminodiphenylsulfone (DAS), and stirred to dissolve APAB and DAS. Then, 29.42 g (100 mmol) of biphenyl-3,3',4,4'-tetracarboxylic dianhydride (BPDA) was added, and polymerization reaction was carried out under stirring at 80° C. for 3 hours under nitrogen flow. Then, it cooled to room temperature, said NMP was added, and it adjusted so that the solution viscosity might become 51000 mPa*s, and obtained the NMP solution (henceforth varnish) P-1 of polyamic acid. The weight average molecular weight (Mw) of the obtained polyamic acid was 65000.

Embodiment 2～21 and comparative example 1～5

[0363] In the above-mentioned Example 1, the input amount (molar ratio) of the raw materials, the type of solvent used, the polymerization temperature and the polymerization time were changed to record in Table 1 respectively, except that it was operated in the same manner as in Example 1 to obtain the varnish P- 2~P-26.

[0364] Table 1 shows together the weight average molecular weight (Mw) of the polyamic acid contained in each varnish.

[0365] [Table 1]

[0366]

[0367] The abbreviations of the components in Table 1 have the following meanings, respectively.

[0368] BPDA: 3,3’,4,4’-Biphenyltetracarboxylic dianhydride

[0369] PMDA: pyromellitic dianhydride

[0370] TAHQ: p-phenylene bis(trimellitic monoester anhydride)

[0371] APAB: 4-Aminophenyl-4-aminobenzoate

[0372] ATAB: 2-Methyl-4-aminophenyl-4-aminobenzoate

[0373] BABB: [4-(4-aminobenzoyl)oxyphenyl]4-aminobenzoate

[0374] BAFL: 9,9-bis(aminophenyl)fluorene

[0375] BFAF: 9,9-bis(4-amino-3-fluoroph...

Embodiment 22

[0391] Put N-methyl-2-pyrrolidone (NMP) (moisture content 250 mass ppm) in an amount corresponding to a solid content of 17% by weight in a 500 ml detachable flask replaced with nitrogen, immediately after opening the 18 L can, and put Add 5.71 g (25.0 mmol) of 4-aminophenyl-4-aminobenzoate (APAB, purity 99.5%, manufactured by Junyoshi Pharmaceutical Co., Ltd.), and stir to dissolve APAB. Then, 7.36 g (25.0 mmol) of biphenyl-3,3',4,4'-tetracarboxylic dianhydride (BPDA, purity 99.5%, manufactured by MANAC Inc.) was added, and the mixture was heated at 80° C. under a nitrogen stream for 3 The polymerization reaction was carried out under stirring. Then, it cooled to room temperature, said NMP was added, and the solution viscosity was adjusted so that it might become 51000 mPa*s, and the NMP solution (henceforth also referred to as varnish) P-27 of polyamic acid was obtained. The weight average molecular weight (Mw) of the obtained polyamic acid was 128000, and content of the mo...

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Abstract

Provided is a polyimide precursor comprising a structural unit L represented by formula (1) (in the formula, X1 represents a tetravalent group having 4-32 carbon atoms, each of R1, R2, and R3 independently represents a monovalent organic group having 1-20 carbon atoms, n represents 0 or 1, and each of a, b, and c is an integer of 0-4) and a structural unit M represented by formula (2) (in the formula, X2 represents a tetravalent group having 4-32 carbon atoms) such that 1 / 99 <= (number of moles of structural unit L / number of moles of structural unit M) <= 99 / 1 is satisfied.

Description

technical field [0001] The present invention relates to a method for producing a polyimide precursor, a resin composition, and a resin film for use in the production of a substrate such as a flexible device. Background technique [0002] Generally, in applications requiring high heat resistance, a polyimide resin film is used as the resin film. Conventional polyimide resins are prepared by polymerizing aromatic carboxylic acid dianhydrides and aromatic diamines to produce polyimide precursors, which are thermally imidized at high temperatures or chemically imidated using catalysts. High heat-resistant resin produced by imidization. [0003] Polyimide resin is an insoluble and infusible super heat-resistant resin with excellent properties such as thermal oxidation resistance, heat resistance, radiation resistance, low temperature resistance, and chemical resistance. Therefore, polyimide resins are used in a wide range of fields including electronic materials. Examples of a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/16B32B27/34C08J5/18C08K5/5415C08L79/08H05K1/03
CPCH05K1/0346C08K5/5415B32B27/34C08G73/16C08J5/18C08G73/1025C08L79/08C08J2379/08H05K1/03G09F9/301
Inventor 米谷昌树清水建树金田隆行
Owner ASAHI KASEI KK
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