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Polyamide acid imide obtained by end-group exchange and preparation thereof

A technology of polyamide-imide and terminal group, which is applied in the field of polyamide-imide and its preparation, can solve the problems of low-molecular-weight end-group-blocked PAI, affect the growth of PAI molecular chain, and limit the application of PAI, so as to broaden the use Range, storage stability, simple polymerization process effect

Inactive Publication Date: 2009-05-20
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The blocking and unblocking temperatures of these compounds without electron-withdrawing groups are relatively high. Even in the presence of catalysts, they often need to be deblocked at a temperature above 150 ° C or even higher, and diisocyanates are easy to be deblocked at high temperatures. Under self-polymerization or cross-linking, this affects the growth of PAI molecular chains
Therefore, the preparation of such compounds can only obtain end-blocked PAI with lower molecular weight, which limits the application of PAI in some respects.

Method used

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  • Polyamide acid imide obtained by end-group exchange and preparation thereof
  • Polyamide acid imide obtained by end-group exchange and preparation thereof
  • Polyamide acid imide obtained by end-group exchange and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Add 20g (0.0799mol) of diphenylmethane diisocyanate (MDI) and 22.6g (0.176mol) of p-chlorophenol into 120ml of toluene to dissolve, add 0.02g of tri-n-butylamine dropwise under stirring, and then react at a temperature of 40°C After 24 hours, a white precipitate was formed in the system, which was filtered, and the precipitate (referred to as BMDI) was collected and dried.

[0045] Dissolve 1.92g (0.01mol) of trimellitic anhydride with 60ml of N-methylpyrrolidone, then add 10.14g (0.02mol) of BMDI and dropwise add 0.0101g of tri-n-butylamine, then react at 80°C for 0.5h, then raise the temperature to 120°C Continue to react at ℃ for 3h, pour the reaction solution into 2000ml tap water to precipitate, filter to obtain p-chlorophenol-terminated polyamideimide (referred to as PAI-1) and dry it.

[0046] Dissolve 2g of PAI-1 and 0.02g of phenol with 40.4ml of N-methylpyrrolidone, add 0.002g of tri-n-butylamine, then raise the temperature to 80°C for 3 hours, pour the reacti...

Embodiment 2

[0048] Add 12.79g (0.0799mol) of p-phenylene diisocyanate (PPDI) and 24.5g (0.176mol) of p-nitrophenol into 120ml of benzene to dissolve, add 0.1279g of tri-n-butylamine dropwise under stirring, and then at a temperature of 40°C After 20 hours of reaction, a white precipitate was formed in the system, which was filtered, and the precipitate (referred to as BPPDI) was collected and dried.

[0049] Dissolve 1.92g (0.01mol) of trimellitic anhydride with 31ml of N-dimethylformamide (DMF), then add 4.22g (0.01mol) of BPPDI and dropwise add 0.0844g of stannous octoate, then react at 90°C for 1h, then The temperature was raised to 130° C. to continue the reaction for 5 h, the reaction solution was poured into 2000 ml tap water to precipitate, filtered, and p-nitrophenol-terminated polyamideimide (referred to as PAI-1) was obtained and dried.

[0050] Dissolve 2g of PAI-1 and 0.2g of benzyl alcohol in 22ml of N-methylpyrrolidone, add 0.02g of tri-n-butylamine, then raise the temperatu...

Embodiment 3

[0052] Add 20g (0.0799mol) of diphenylmethane diisocyanate (MDI) and 24.5g (0.176mol) of p-nitrophenol into 120ml of toluene to dissolve, add 0.4g of stannous octoate dropwise under stirring, and then react at a temperature of 30°C After 14 hours, a white precipitate was formed in the system, which was filtered, and the precipitate (referred to as BMDI) was collected and dried.

[0053] Dissolve 1.92g (0.01mol) of trimellitic anhydride with 59ml of dimethyl sulfoxide (NMSO), then add 15.85g (0.03mol) of BMDI and dropwise add 0.317g of stannous octoate, then react at 70°C for 2h, then heat up to The reaction was continued at 120°C for 8 hours, the reaction solution was poured into 2000ml of tap water to precipitate, filtered, and p-nitrophenol-terminated polyamideimide (referred to as PAI-1) was obtained and dried.

[0054] Dissolve 2g of PAI-1 and 0.04g of caprolactam in 13.5ml of N,N-dimethylformamide (DMF), add 0.04g of stannous octoate, then raise the temperature to 80°C fo...

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Abstract

The invention discloses polyamide imide which is obtained by the exchange of terminal groups. The structural general formula of the polyamide imide is showed on the right, wherein, X in the formula is the remanent part of diisocyanate removed diisocyanato; the R' is the remanent structure of a compound containing active hydrogen removed hydrogen and the limiting viscosity number thereof is 0.1dL / g to 0.4dL / g. The invention also discloses a preparation method of the polyamide imide. As the polyamide imide provided by the invention which is obtained by the exchange of terminal groups not only has a great variety of terminal groups, thus being capable of obtaining polyamide imide which cannot be obtained through direct terminating method, but also has a higher molecular weight, stable storage and is characterized by simple preparation and low cost, and the polyamide imide disclosed by the invention can greatly widen the application range of the polyamide imide.

Description

technical field [0001] The invention belongs to the technical field of polyamide-imide and its preparation method, and in particular relates to a polyamide-imide obtained by terminal group exchange and its preparation method. Background technique [0002] Polyimide (PI) is a class of high-performance polymers containing imide rings in the main chain, among which the research on fully aromatic polyimide has attracted much attention. Due to its excellent thermal stability, mechanical properties, chemical inertness, dielectric properties, and radiation resistance, PI has been widely used in aerospace, electronics industries, etc. in commercial forms such as films, coatings, fibers, plastics, adhesives, and resin-based composites. High-tech fields have been widely used. However, due to its rigid molecular structure and strong intermolecular forces, traditional aromatic polyimides are usually insoluble and infusible, which brings great difficulties to the processing of materials...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/14
Inventor 杨刚周鸿飞
Owner SICHUAN UNIV
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