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Preparation method of crosslinking poly(p-phenylenebenzobisoxazole) film

A technology of polyphenylene benzene and dioxazole, which is applied in the field of preparation of cross-linked polyphenylene benzobisoxazole films, can solve the problems of difficulty in controlling film thickness and shape, large shrinkage and the like, and achieves no The effect of complex residue, small shrinkage and controllable shape

Active Publication Date: 2016-04-20
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the large volume shrinkage of the film during the drying process, it is difficult to control the thickness and shape of the film by this method

Method used

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  • Preparation method of crosslinking poly(p-phenylenebenzobisoxazole) film
  • Preparation method of crosslinking poly(p-phenylenebenzobisoxazole) film
  • Preparation method of crosslinking poly(p-phenylenebenzobisoxazole) film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1: Synthesis of aromatic polyamide precursors with side methyl groups and phenolic hydroxyl groups

[0031] Into a 250ml three-neck flask, under nitrogen protection, first add 2.28g of 2-methyl-4,6-diaminoresorcinol dihydrochloride (0.01mol), 100ml of dry N-methylpyrrolidone and 2.5ml of dry pyridine After stirring for 10 minutes at 15°C, add 2.03g of terephthaloyl chloride, stir for 1 minute, then add 1.6ml of dry pyridine, stir for 2 hours at 15°C, pour into 200ml of water, filter, and dry to obtain 2.87g of yellow-green Solid (100% yield). n is 58.

[0032] The polyamide precursor synthesized above was tested by IR and 1 HNMR detection, for the target product, IR and 1 HNMR analysis result is as follows:

[0033] IR (KBr, cm -1 ): 3410, 3271, 1640, 1537, 1244, 863; 1 HNMR (CDCl 3 , 400MHz, δ(ppm)): 10.06(s, 2H), 8.97(s, 2H), 8.10(m, 4H), 7.38(s, 1H), 2.16(s, 3H).

Embodiment 2

[0034] Embodiment 2: the preparation of cross-linked polyamide film

[0035] The polyamide synthesized above was stirred and dissolved in dimethyl sulfoxide at 100°C to prepare a solution with a concentration of 5%, and was coated on a glass plate or an aluminum plate by a solution casting method, or coated on a glass plate by a spin coating method The quartz plate was then continuously treated at 60° C., 70° C., 80° C., 100° C. and 120° C. for 1 hour each to obtain a polyamide film.

[0036] The polyamide film was placed on a hot stage at 350° C. for 1 hour in a nitrogen atmosphere to obtain a cross-linked PBO film, which was insoluble in non-cross-linked PBO solvents, such as methanesulfonic acid and concentrated sulfuric acid.

[0037] The cross-linked PBO film prepared above was detected by IR and ultraviolet-visible light. IR analysis results are as follows: IR (KBr, cm -1 ): 3427, 2927, 1624, 1364, 1062; in the ultraviolet-visible light absorption spectrum, the absorpt...

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Abstract

The invention discloses a preparation method of a crosslinking poly(p-phenylenebenzobisoxazole) film and belongs to the field of high polymer materials. The method comprises the steps that 2-methyl-4,6-diamido-resorcinol cystamine dihydrochloride and paraphthaloyl chloride are subjected to a reaction, and aromaticity polyamide with a methyl pendant group and a phenolic hydroxyl group is prepared; then the aromaticity polyamide is dissolved in a nonprotic polarity organic solvent to obtain a solution with a certain concentration, a substrate is coated with the solution, and heating is carried out to enable the solvent to evaporate to obtain a polyamide film; the polyamide film is treated at the high temperature to obtain the crosslinking poly(p-phenylenebenzobisoxazole) film. According to the method, extrusion forming is omitted, the presoma polyamide is dissolved in the organic solvent, the polyamide film with the certain thickness can be well prepared after the solvent is evaporated, the thickness of the crosslinking PBO film is controllable, and the film from nanoscale to microscale can be conveniently prepared. The preparation method can be applied to preparing photochromic devices, photovoltaic cells, organic light emitting diodes and other photoelectric devices, can also be used for a high-temperature resistance coating, and can well meet market requirements.

Description

technical field [0001] The invention relates to a preparation method of a cross-linked polyphenylene benzobisoxazole film, which belongs to the field of polymer materials. Background technique [0002] As an aromatic heterocyclic conjugated polymer, polyphenylene benzobisoxazole (PBO) is not only used for structural materials with high strength, high modulus and high temperature resistance, but also has unique photoelectric properties, and can also be used for photochromic , photovoltaic cells, organic light-emitting diodes and DNA fluorescence detection and other photoelectric functional devices. [0003] Alkyl or halogen atoms are introduced into the main chain of PBO, and chemical crosslinks can be formed between molecular chains after high temperature treatment, which improves the mechanical properties of PBO materials. "Polymer" 1997, 38, page 621 records that 2-methyl terephthalic acid and 2,5-dimethyl terephthalic acid are used as polymerized monomers respectively, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32C08G69/28C08G73/22C08J5/18
CPCC08G69/28C08G69/32C08G73/22C08J5/18C08J2377/10C08J2379/04
Inventor 郭凯郑世军李旭阳魏爱卿李自法
Owner ZHENGZHOU UNIV
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