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Polyimide as well as preparation method and application thereof

A technology of polyimide and polycondensation reaction, applied in the field of polyimide and its preparation, can solve the problems of low optical transmittance of flexible materials, poor solubility, and increase the difficulty of production of flexible materials

Inactive Publication Date: 2017-12-22
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Polyimide (Polyimide, referred to as PI) is a class of polymers containing imide rings in the main chain. Due to its good mechanical properties, high temperature resistance and radiation resistance, it has been widely used in flexible display materials. However, there are also some problems in the process of manufacturing flexible display materials, mainly as follows: 1), the solubility of existing polyimide materials is poor, which increases the difficulty of production of flexible materials; 2), Existing polyimide materials have light or dark colors, resulting in low optical transmittance of flexible materials

Method used

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  • Polyimide as well as preparation method and application thereof
  • Polyimide as well as preparation method and application thereof
  • Polyimide as well as preparation method and application thereof

Examples

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preparation example Construction

[0067] The invention provides a kind of preparation method of polyimide, comprises the following steps:

[0068] The dianhydride compound and the diamine compound are subjected to a polycondensation reaction in the presence of a catalyst to obtain a polyimide;

[0069] The dianhydride compound is 2,3,2',3'-dicyclohexyl tetracarboxylic dianhydride, 3,4,3',4'-dicyclohexyl ether tetracarboxylic dianhydride, 2,3,3', 4'-Dicyclohexyl ether tetracarboxylic dianhydride, 2,3,2',3'-Dicyclohexyl ether tetracarboxylic dianhydride, 1,4-bis(3,4-dicarboxycyclohexyl)cyclohexyl Dianhydride, 2,5,7,10-decalin tetracarboxylic dianhydride, 4,4'-didecalinyl-1,1',8,8'-tetracarboxylic dianhydride, bis(3,4 - dicarboxycyclohexyl)methane dianhydride or 2,2-bis(3,4-dicarboxycyclohexyl)hexafluoropropane dianhydride;

[0070] Described polyimide comprises the repeating unit with formula (I) structure:

[0071]

[0072] In formula (I), R 1 One of the following structures:

[0073]

[0074] R 2 I...

Embodiment 1

[0142] Preparation of 2,3,2',3'-dicyclohexyltetracarboxylic dianhydride:

[0143](1) Add 69g of zinc powder, 7.67g of nickel bromide, and 32.21g of triphenylphosphine into 132ml of N,N-dimethylacetamide, stir until dark brown at 60°C, add 132ml of N,N-di 200g of 3-chlorophthalamide solution in methylacetamide was maintained at 60-80°C for 6h, the catalyst was filtered off, washed several times with dilute hydrochloric acid, and recrystallized with ethanol to obtain 143g of tetraester.

[0144] (2) Add 5g of tetraester and 0.5g of rhodium / activated carbon catalyst (Acros, Rhodium on activated carbon, 5%Rh) into a 250ml autoclave, then add 40ml of THF, at a temperature of 120°C and a hydrogen pressure of 2 to 5Mpa under magnetic stirring After reacting for 5 to 8 hours, the catalyst was filtered off, and then THF was evaporated to obtain the hydrogenated tetraester.

[0145] (3) Dissolve 5 g of the obtained hydrogenated tetraester in 25 ml of methanol, add 40 g of 20 wt % sodiu...

Embodiment 2

[0149] 1) Preparation of polyimide:

[0150] Under nitrogen protection, 0.7276g 2,3,2',3'-dicyclohexyl tetracarboxylic dianhydride, 0.4756g 4,4'-diaminodiphenyl ether and 0.2898g benzoic acid were added to the polymerization bottle, and then 4.81 g m-cresol, heated to 90°C and stirred until completely dissolved. After dissolution, the temperature was raised to 180°C for 20 hours. After the reaction, m-cresol was added to dilute and the temperature was lowered to 100°C, and the solution was poured into ethanol to obtain a white filamentous solid. Soxhlet extraction was performed with ethanol. After extraction, dry at 100° C. under vacuum to obtain polyimide.

[0151] The polyimide that present embodiment makes has following structure:

[0152]

[0153] Infrared spectrum analysis is carried out to the above-mentioned polyimide that makes, the result is as follows: figure 2 as shown, figure 2 It is the polymer infrared spectrogram provided by Example 2 of the present i...

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Abstract

The invention belongs to the field of high molecular materials, and particularly relates to polyimide as well as a preparation method and application thereof. The polyimide provided by the invention comprises a repetitive unit having a structure as shown in the formula (I) (as shown in the description), wherein in the formula (I), R1 is one of following structures( as shown in the description), and R2 is a residue after removing two aminos from a diamine compound. Experimental results indicate that the polyimide provided by the invention is transparent, the ultraviolet absorption cut-off wavelength of the polyimide is 291-320nm, and the optical transmissivity of the polyimide at 450nm is 75-90%; the polyimide has favorable solubility in resorcinol, N-methylpyrrolidinone, N,N-dimethylacetamide and the like, and the polyimide can partially dissolve in chloroform and the like; besides, the vitrification transition temperature of the polyimide is 200 DEG C or above, and the 5% hot zero gravity of the polyimide is 400 DEG C or above; and besides, the inherent viscosity of the polyimide is more than 0.30dL / g, and the film forming property of the polyimide is good.

Description

[0001] This application is a divisional application with an application date of January 7, 2016, an application number of 201610007792.4, and an invention titled "a polyimide and its preparation method and application". technical field [0002] The invention belongs to the field of polymer materials, and in particular relates to a polyimide and its preparation method and application. Background technique [0003] In recent years, with the rapid development of optoelectronic materials, such as the replacement of materials in the fields of display, storage, waveguide and solar cells, traditional components processed or shaped by inorganic materials have been difficult to meet the processing and use needs of users. Therefore, flexible display materials made of high molecular polymers that can be stretched, bent, folded and restored to their original state are gradually leading a new round of optoelectronic material revolution. [0004] Polyimide (Polyimide, referred to as PI) i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/18C08L79/08
CPCC08G73/1007C08G73/1021C08G73/1078C08J5/18C08J2379/08C08L79/08C08L2201/08C08L2201/10C08L2203/16
Inventor 阎敬灵胡小凡王震刘敬峰孟祥胜范卫锋
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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