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Preparation method of novel high-barrier polyimide material

A technology of polyimide and new material, applied in the field of preparation of new high-barrier polyimide material, can solve the problems of limitation, polyimide material does not have high-barrier performance, etc.

Inactive Publication Date: 2019-01-18
孝感寰誉新材科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The polyimide materials prepared by the above inventions and prior art do not have high barrier properties and limit its application in fields such as FOLED substrate materials and solar cells

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method of a new high-barrier polyimide material, the preparation technical scheme is as follows:

[0019] According to the number of parts by mass, add 43 parts of condensed ring diamine monomer and 450 parts of N-methylpyrrolidone into the reaction kettle, under the protection of nitrogen, after stirring evenly, control the temperature at 25 ° C, and then add 38 parts of thickened The cyclic dianhydride monomer was added to the reactor in 3 times within 50 minutes. After the addition, the temperature was controlled at 25°C, and the reaction was continued for 18 hours with stirring; after the reaction was completed, 150 parts of xylene and 1.5 parts of catalyst, 0.1 part Methyleneoxybicyclic oxazolidine, 0.03 parts poly[[octahydro-5-(methoxycarbonyl)-5-methyl-4,7-methylene-1H-indene-1,3-diyl]- 1,2-ethylenediyl], 0.03 parts of 2-bromo-spiro[9H-fluorene-9,9'-[9H]xanthene], 0.2 parts of 5-boronic acid pinacol ester indole-2- Put the ketone into the reaction ...

Embodiment 2

[0027] A preparation method of a new high-barrier polyimide material, the preparation technical scheme is as follows:

[0028] According to the number of parts by mass, add 39 parts of condensed ring diamine monomer and 400 parts of N-methylpyrrolidone into the reaction kettle, under the protection of nitrogen, after stirring evenly, control the temperature at 20°C, and then add 26 parts of thickened The cyclic dianhydride monomer was added to the reactor in 3 times within 40 minutes. After the addition, the temperature was controlled at 20°C, and the stirring reaction was continued for 15 hours. After the reaction was completed, 100 parts of xylene and 0.5 parts of catalyst, 0.05 parts of Methyleneoxybicyclic oxazolidine, 0.01 part poly[[octahydro-5-(methoxycarbonyl)-5-methyl-4,7-methylene-1H-indene-1,3-diyl]- 1,2-ethylenediyl], 0.01 part of 2-bromo-spiro[9H-fluorene-9,9'-[9H]xanthene], 0.1 part of 5-boronic acid pinacol ester indole-2- Put the ketone into the reaction kettl...

Embodiment 3

[0036] A preparation method of a new high-barrier polyimide material, the preparation technical scheme is as follows:

[0037]According to the number of parts by mass, add 48 parts of condensed ring diamine monomer and 500 parts of N-methylpyrrolidone into the reaction kettle, under the protection of nitrogen, after stirring evenly, control the temperature at 30°C, and then add 48 parts of thickened The cyclic dianhydride monomer was added to the reactor in 3 times within 60 minutes. After the addition, the temperature was controlled at 30°C, and the reaction was continued for 20 hours with stirring; after the reaction was completed, 200 parts of xylene and 2.5 parts of Methyleneoxybicyclic oxazolidine, 0.2 parts poly[[octahydro-5-(methoxycarbonyl)-5-methyl-4,7-methylene-1H-indene-1,3-diyl]- 1,2-ethylenediyl], 0.06 parts of 2-bromo-spiro[9H-fluorene-9,9'-[9H]xanthene], 0.7 parts of 5-boronic acid pinacol ester indole-2- Put the ketone into the reaction kettle, control the tem...

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Abstract

The invention relates to the field of material preparation, in particular to a preparation method of a novel high-barrier polyimide material. According to the preparation method of the novel high-barrier polyimide material, disclosed by the invention, a fused-ring diamine monomer is prepared from 2,7-dibromopyrene and 4-aminobenzeneboronic acid hydrochloride under an alkali condition; a polymerization reaction is performed on the diamine monomer and a fused-ring dianhydride monomer to obtain a polyamic acid solution; then, a water-carrying agent and a catalyst are added, a polyimide slurry isprepared by a one-step method, and the slurry is prepared into a film to obtain the novel high-barrier polyimide material. By the preparation method, through introduction of fused-ring structures intoa main chain of polyimide, molecular chains of the polyimide are more tightly packed, the rigidity is improved, movement of the molecular chains is limited, and the free volume of a polymer is reduced, so that a gas passage is difficultly formed in the polymer, and thus the barrier property of the polyimide material is effectively improved.

Description

technical field [0001] The invention relates to the field of material preparation, in particular to a preparation method of a new high-barrier polyimide material. Background technique [0002] Polyimide materials are widely used in aerospace, electronic devices, precision machinery, and microelectronics because of their excellent high temperature resistance, mechanical properties, corrosion resistance, and electrical properties. Therefore, their preparation methods have attracted widespread attention. [0003] CN105461925A discloses a polyimide containing a carbazole structure and its preparation method and application. This type of polyimide material uses aromatic diamine with high planarity and carbazole structure and various tetra-acid dianhydrides as raw materials, and prepares polyimide powder by thermal imidization or chemical imidization material or film. Due to the high planarity and strong rigidity of the lowest energy state structure of the diamine monomer, the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
CPCC08G73/1067C08G73/1057
Inventor 谷灿波王金霞
Owner 孝感寰誉新材科技有限公司
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