Polyimide precursor, polyimide, and materials to be used in producing same

A polyimide precursor, polyimide technology, applied in the field of polyimide, can solve problems such as reducing color, and achieve the effects of high glass transition temperature, excellent transparency, and high heat resistance

Active Publication Date: 2013-07-31
UBE IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these documents only describe the synthesis of 2,2',3,3'-biphenyltetracarboxylic acid and 2,2',3,3'-biphenyltetracarboxylic dianhydride, without describing or suggesting any purification of 2 , 2 ', 3, 3'-biphenyltetracarboxylic dianhydride to reduce the color method

Method used

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  • Polyimide precursor, polyimide, and materials to be used in producing same
  • Polyimide precursor, polyimide, and materials to be used in producing same
  • Polyimide precursor, polyimide, and materials to be used in producing same

Examples

Experimental program
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preparation example Construction

[0107] 6. The method for preparing a co-polyimide precursor according to item 5, wherein the solvent used has a purity of 99.8% or higher (purity measured by GC analysis).

[0108] 7. The method for preparing the solution composition of the copolymerization-polyimide precursor described in item 5 or 6, comprising making the tetracarboxylic acid component and the diamine component so that the molar ratio of the excess diamine component react to obtain a polyimide precursor; and in an amount approximately corresponding to the excess molar number of the diamine, further add a carboxylic acid derivative to the obtained polyimide precursor so that the tetracarboxylic acid and the The total molar ratio of the carboxylic acid derivative components is approximately equal to the molar ratio of the diamine components.

[0109] 8. Co-polyimide having a unit structure represented by general formula (A5) and a unit structure represented by general formula (A6):

[0110]

[0111] Among ...

Embodiment

[0586] The present invention will now be described in more detail based on the following Examples and Comparative Examples. However, the present invention is not limited to the following examples.

[0587] >

[0588] In each of the following examples, evaluation was performed based on the following method.

[0589] Evaluation of Polyimide Precursors

[0590] [Solid content of varnish]

[0591] Weigh 1 gram of the polyimide precursor solution and put it into an aluminum dish, and heat it in a hot air circulation box at 200° C. for 2 hours to remove the non-solid content. The solids content of the varnish (residual mass % after heating) was determined from the residual substance.

[0592] [rotational viscosity]

[0593] Polyimide precursor solution at 25°C temperature and 20sec -1 The viscosity at a shear rate of 0 was determined using a TV-22E-type rotational viscometer manufactured by Toki Sangyo Co., Ltd.

[0594] [logarithmic viscosity]

[0595] The logarithmic visco...

Embodiment A1

[0620] In a reaction vessel, 10.82 g (0.0947 mol) of trans-1,4-diaminocyclohexane (hereinafter referred to as t-DACH) was charged and dissolved in 313.0 g of N,N-diaminocyclohexane dehydrated using molecular sieves. Methylacetamide (hereinafter referred to as t-DMAc). To this solution, 26.48g (0.090mol) 3,3',4,4'-biphenyltetracarboxylic dianhydride (hereinafter referred to as s-BPDA) and 1.394g (0.0047mol) 2,3 were gradually added, 3',4'-biphenyltetracarboxylic dianhydride (hereinafter may be referred to as a-BPDA), and the resulting mixture was heated to 120°C. When it was determined that the salt started to dissolve for 5 minutes, the mixture was rapidly cooled to room temperature and maintained at room temperature for 8 hours with stirring, thereby obtaining a uniform and viscous co-polyimide precursor solution composition.

[0621] The obtained polyimide precursor solution composition was applied on a glass substrate by heating at 120°C for 1 hour, at 150°C for 30 minutes...

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Abstract

Disclosed is a novel copolyimide precursor for producing a highly transparent polyimide. This copolyimide precursor comprises unit structures represented by general formula (A1) and unit structures represented by general formula (A2). In general formula (A1), R1 is a hydrogen atom or a C1-4 alkyl group; and R2 and R3 are each independently a hydrogen atom, a C1-6 alkyl group, or a C3-9 alkylsilyl group, while in general formula (A2), R4 is a hydrogen atom or a C1-4 alkyl group; R5 and R6 are each independently a hydrogen atom, a C1-6 alkyl group, or a C3-9 alkylsilyl group; and X is a tetravalent group except the groups represented by formulae (A3).

Description

technical field [0001] The present invention relates to polyimides having high transparency, high mechanical strength and low coefficient of linear thermal expansion, and to polyimide precursors suitable for preparing said polyimides. Background technique [0002] In recent years, with the advent of an advanced information society, optical materials such as optical fibers and optical waveguides in the field of optical communications, and liquid crystal alignment films and color filter protective films in the field of displays have been developed. Particularly low, in the field of displays, research has been conducted on plastic substrates that are lightweight and have excellent flexibility as a substitute for glass substrates, and displays that can be bent or rolled up have been actively developed. Therefore, there is a need for higher performance optical materials that can be used for such purposes. [0003] Typically, polyimides are yellowish-brown in nature due to intram...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
CPCC07D307/89C08G73/1007C08G73/1067C08G73/1082C08L79/08C09D179/08C08G73/1042C08G73/1075C08L2201/08C08L2201/10C08G73/10C08G73/00
Inventor 高泽亮一冈卓也小滨幸德中川美晴久野信治幸田政文中山刚成中山知则
Owner UBE IND LTD
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