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Preparation method of polybenzoxazole thin film

A polybenzoxazole and film technology, which is applied in the field of polybenzoxazole film preparation, can solve problems such as unfavorable industrialized large-scale production, unfavorable industrialized large-scale production, increase of three wastes, etc., and achieves easy recovery and recycling, and saves fixed assets. The effect of investment and simple operation steps

Inactive Publication Date: 2008-12-10
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The weak point of this method is: (1) water consumption is big, and resource waste is bigger; (2) waste water is more, is unfavorable for environmental protection; In addition, also increased waste water treatment cost
(3) The obtained 4,6-diaminoresorcinol / terephthalate is easily oxidized by air and affects the quality, which is not conducive to subsequent polymerization reactions
(4) The drying of 4,6-diaminoresorcinol / terephthalate must be vacuum-dried, which consumes a lot of energy
(5) Using polyphosphoric acid / P 2 o 5 The polymerization reaction in the system requires high requirements on the reaction equipment, and the follow-up treatment is difficult and expensive, which is not conducive to industrial scale production
[0008] The disadvantages of this method are: (1) the polymerization reaction is carried out at a low temperature of -10°C to 0°C, which consumes a lot of energy; (2) HCl is generated during the reaction and needs to be absorbed by propylene oxide, thereby increasing the cost. The increase in the three wastes has correspondingly increased the requirements for equipment, which is not conducive to large-scale industrial production

Method used

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  • Preparation method of polybenzoxazole thin film
  • Preparation method of polybenzoxazole thin film
  • Preparation method of polybenzoxazole thin film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 25.8 grams (0.1 moles) of 2,2-bis(3-amino-4-hydroxyphenyl) propane (B3A4HPP) into the polymerization bottle, add 400 milliliters of N-methyl-2-pyrrolidone (NMP), and feed Nitrogen, cooled to 5°C in an ice-water bath, stirred to make it completely dissolved, then added 21.8 grams (0.1 moles) of pyromellitic dianhydride (PMDA) powder, stirred and reacted for 3 hours, and viscous poly-o-hydroxyamide was obtained acid solution. Subsequently, cast the viscous poly-o-hydroxyamic acid solution into a uniform film, under the protection of nitrogen, heat up to 100°C and keep it for 2 hours; continue to heat up to 150°C, 200°C, 250°C, 300°C, 350°C The temperature points of ℃ and 400℃ were maintained for 1 hour; then the temperature was raised to 450℃, and after keeping for half an hour, the heating system was turned off, and after natural cooling to room temperature, the film was stripped to obtain a tough and transparent polybenzoxazole film. In the infrared spectrum absorp...

Embodiment 2

[0023] Add 25.8 grams (0.1 moles) of 2,2-bis(3-amino-4-hydroxyphenyl)propane (B3A4HPP) into the polymerization bottle, add 450 milliliters of N-methyl-2-pyrrolidone (NMP), and feed Nitrogen, ice-water bath cooling to 5 ° C, stirring, to make it completely dissolved, add 10.9 grams (0.05 moles) pyromellitic dianhydride (PMDA) powder and 14.7 grams (0.05 moles) 3,3',4,4' - Tetraformic acid biphenyl dianhydride (BPDA) powder, after stirring and reacting for 5 hours, a viscous poly-o-hydroxyamic acid solution was obtained. Subsequently, cast the viscous poly-o-hydroxyamic acid solution into a uniform film, under the protection of nitrogen, heat up to 100°C and keep it for 2 hours; continue to heat up to 150°C, 200°C, 250°C, 300°C, 350°C The temperature points of ℃ and 400℃ were maintained for 1 hour; then the temperature was raised to 450℃, and after keeping for half an hour, the heating system was turned off, and after natural cooling to room temperature, the film was stripped to...

Embodiment 3

[0025]12.9 g (0.05 mol) of 2,2-bis(3-amino-4-hydroxyphenyl)propane (B3A4HPP) and 18.3 g (0.05 mol) of 2,2-bis(3-amino-4-hydroxyphenyl) -1,1,1,3,3,3-hexafluoropropane (B3A4HPFP) was added to the polymerization bottle, 400 ml of N,N-dimethylacetamide (DMAc) was added, nitrogen gas was introduced, and the ice-water bath was cooled to 5 ℃, stirring, after making it completely dissolved, add 10.9 (0.05 mol) gram of pyromellitic dianhydride (PMDA) powder and 14.7 gram (0.05 mol) of 3,3',4,4'-tetracarboxylic biphenyl dianhydride (BPDA) powder, after stirring and reacting for 10 hours, a viscous poly-o-hydroxyamic acid solution was obtained. Subsequently, cast the viscous poly-o-hydroxyamic acid solution into a uniform film, and heat it up to 100°C, 150°C, 200°C, 250°C, 300°C, 350°C, and 400°C under the protection of nitrogen. The point was kept for 1 hour; then the temperature was raised to 450°C, and after keeping for half an hour, the heating system was turned off, and after natur...

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Abstract

The present invention discloses preparation process of polybenzoxazole film. The preparation process includes the following steps: 1. the reaction of aromatic di-o-amino phenol compound and aromatic binary anhydride in the molar ratio of 1 to 1 at 0-30 deg.c inside strong polar non-protonic organic solvent under nitrogen protection for 3-10 hr to obtain poly(o-hydroxy amino acid) solution; and 2. flow casting the poly(o-hydroxy amino acid) solution to form homogeneous film, heating to 100-300 deg.c under nitrogen protection to react for 4-8 hr, and further heating to 350-450 deg.c to react for 2.5-4 so as to obtain the polybenzoxazole film. The present invention has the beneficial effects of simple operation, environment friendship, low power consumption and easy recovering of organic solvent as reaction medium.

Description

technical field [0001] The invention relates to a method for preparing a high-temperature-resistant high-performance polymer film, in particular to a method for preparing a polybenzoxazole film. Background technique [0002] Polybenzoxazole has very good heat resistance, low temperature resistance, self-lubrication, radiation resistance, hydrolysis resistance and flame retardancy, and also has very good mechanical properties and dielectric properties. It can be applied to advanced structural composite materials, radome, fairing and empennage, ablation-resistant coatings, etc. for medium and hypersonic aircraft; it can also be applied to high-temperature and radiation-resistant materials for spacecraft, C-class electrical insulation materials, and electronic microelectronics In the field of FPC or PCB matrix materials, IC interlayer insulation materials, VLSI passivation coatings and α particle barrier coating materials, etc. [0003] U.S. Patent No. 5,276,128 discloses a pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J5/18C08G73/22C08G73/10
Inventor 虞鑫海赵炯心徐永芬
Owner DONGHUA UNIV
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