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Low water absorbable polyimide resin and process for its production

A technology of polyimide resin and polyimide film, applied in coating, instrument, transportation and packaging, etc., can solve the problems of insufficient anti-coloring property, poor moisture absorption dimensional stability and high water absorption rate

Active Publication Date: 2007-12-05
MITSUBISHI GAS CHEM CO INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method described in Patent Document 5 includes an imidization process at a high temperature, as in the conventional method, and therefore the anti-coloring property is insufficient. In addition, the polyimide resin films described in the two Patent Documents have high water absorption, Disadvantages of poor moisture absorption and dimensional stability

Method used

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  • Low water absorbable polyimide resin and process for its production
  • Low water absorbable polyimide resin and process for its production
  • Low water absorbable polyimide resin and process for its production

Examples

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preparation example Construction

[0043] The organic polar solvent used in the preparation method of the present invention is not particularly limited, but is preferably an aprotic organic polar solvent. For example, γ-butyrolactone, N,N-dimethylacetamide, N,N-dimethylformamide, N-methyl-2-pyrrolidone, dimethyl sulfoxide, p-chlorophenol, m-cresol, tetrahydrofuran, etc., among which the use of γ-butyrolactone and N,N-dimethylacetamide can improve colorlessness and transparency. These solvents may be used alone or in combination of two or more.

[0044] Next, the method for preparing the polyimide resin of the present invention and the method for preparing a polyimide film using the obtained organic polar solvent solution of the polyimide resin will be described.

[0045] Preparation of polyimide resin solution

[0046] Dissolving at least one imino group-forming compound in an organic polar solvent. It is preferable to dissolve 10 to 30 parts by weight of the imino group-forming compound relative to 100 par...

Embodiment

[0064] The present invention will be described in detail below by way of examples. However, the present invention is not limited to these Examples.

[0065] In addition, the physical properties of the polyimide resin and polyimide film obtained in the Example and the comparative example were measured by the method shown below.

[0066] (1) Logarithmic viscosity

[0067] A part of the polyimide resin solution was added to anhydrous methanol to precipitate the polyimide resin, which was filtered and separated from unreacted monomers. Vacuum drying at 80°C for 12 hours to obtain a polyimide, 0.1g of this polyimide was dissolved in 20ml of N-methyl-2-pyrrolidone, and was calculated according to the following formula with a Canon-Fenske viscometer The logarithmic viscosity (μ) at 30°C is given.

[0068] μ={1n(t s / t 0 )} / C

[0069] t s : Solvent flow time

[0070] t 0 : Flow time of dilute polymer solution

[0071] C: 0.5g / dL

[0072] (2) Glass transition temperature (Tg) ...

reference example 1

[0083] Reference Example 1 (Synthesis of 1,2,4,5-cyclohexanetetracarboxylic dianhydride)

[0084] Add 552 g of pyromellitic acid, 200 g of Rh catalyst (エヌイケムキヤツト (エヌ・イケムキャツト) ( Co., Ltd.), 1656 g of water, while stirring, replaced the air in the autoclave with hydrogen, raised the hydrogen pressure to 5.0 MPa, and raised the temperature to 60°C. The reaction was carried out under a hydrogen pressure of 5.0 MPa for 2 hours. The hydrogen in the autoclave was replaced with nitrogen, and the reaction liquid was taken out from the autoclave. The reaction solution was filtered while hot to separate the catalyst. Using a rotary evaporator, water was distilled off from the filtrate under reduced pressure, followed by concentration to precipitate crystals. The precipitated crystal was subjected to solid-liquid separation at room temperature and dried to obtain 481 g of 1,2,4,5-cyclohexanetetracarboxylic acid (85.0% yield).

[0085] Then, 481 g of the obtained 1,2,4,5-cyclohexanetet...

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PUM

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Abstract

Disclosed is a polyimide resin obtained by reacting a compound selected from 1,2,4,5-cyclohexanetetracarboxylic acid, acid dianhydrides thereof and reactive derivatives of them with a compound selected from diamines containing at least one phenylene group and an isopropylidene group and diisocyanates. Such a polyimide resin is colorless and has high heat resistance, high transparency and low water absorption.

Description

technical field [0001] The present invention provides a colorless and transparent low-absorption polyimide resin, a method for producing the same, a method for producing a film made of the polyimide, and a sealing material containing the polyimide resin. Background technique [0002] A polyimide resin is generally a heat-resistant resin obtained by dehydrating and cyclizing polyamic acid obtained by a condensation reaction of an aromatic tetracarboxylic anhydride and an aromatic diamine. Due to the rigidity of its molecular chain, resonance stability, and strong chemical bonds, polyimide resin has excellent resistance to thermal decomposition and resistance to chemical changes such as oxidation or hydrolysis, and has excellent mechanical properties and electrical properties. And flexibility, therefore, polyimide resins are widely used in fields such as electrical, electronic, automotive and aerospace industries as films, coatings, molded parts and insulating materials. [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08G18/34C08G18/76B29C41/12
CPCC08G2190/00C08G18/3846C08G18/765C08G73/10Y10T428/1091Y10T428/10C08G18/346Y10T428/1023C09K2323/00C09K2323/027G02F2202/28C08G61/12
Inventor 牧野嶋高史木原秀太
Owner MITSUBISHI GAS CHEM CO INC
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