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Soluble polyimides containing phenolic hydroxyl group and preparation method and application thereof

A technology of soluble polyimide and polyimide film, which is applied in the field of chemical synthesis, can solve the problems of poor application, unresolved polyimide solubility and limitations, and improve the bonding performance or compatibility , good chemical solubility, and the effect of improving cyclization efficiency

Inactive Publication Date: 2017-05-24
NANXIONG MATERIAL PRODION BASE OF CHINESE ACADEMY OF SCI GUANGZHOU CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, none of the above research work has solved the problem that the application of polyimide is limited due to its poor solubility.

Method used

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  • Soluble polyimides containing phenolic hydroxyl group and preparation method and application thereof
  • Soluble polyimides containing phenolic hydroxyl group and preparation method and application thereof
  • Soluble polyimides containing phenolic hydroxyl group and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Embodiment 1: the preparation of polyimide film

[0067] (1) Add p-hydroxybenzaldehyde, aniline, and aniline hydrochloride in a molar ratio of 1:3:0.1 to the reaction flask, react at 120°C for 12 hours under nitrogen protection, and distill off excess aniline after cooling to room temperature. The residue was washed several times with water and recrystallized three times with ethanol, filtered, washed, and dried to obtain a purple-red product and 4,4'-diamino-4"-hydroxytriphenylmethane.

[0068] in N 2 Under protection, 2.90g (10mmol) 4,4'-diamino-4"-hydroxytriphenylmethane and 25.49g N-methyl-2-pyrrolidone were added to the reaction flask, stirred and dissolved, and 3.10g ( 10mmol) 4,4'-diphenyl ether dianhydride, then stirred and reacted for 0.5h, then added 4.25g xylene and catalyst (0.10gγ-valerolactone and 0.16g pyridine), heated to 180°C for reflux and azeotropic dehydration for 4h;

[0069] (2) Cool the mixed solution after reflux in step (1) to 30°C, then pour...

Embodiment 2

[0072] Embodiment 2: the preparation of polyimide film

[0073] (1) in N 2 Under protection, 2.90g (10mmol) 4,4'-diamino-4"-hydroxytriphenylmethane and 50.48g N-methyl-2-pyrrolidone were added to the reaction flask, stirred and dissolved, and 3.10g ( 10mmol) 4,4'-diphenyl ether dianhydride, then stirred and reacted for 0.5h, then added 8.41g xylene and catalyst (0.10gγ-valerolactone and 0.16g pyridine), heated to 180°C for reflux and azeotropic dehydration for 5h;

[0074] (2) Cool the mixed solution after reflux in step (1) to 25°C, then pour it into an aqueous methanol solution with a volume ratio of 0.1:1 (methanol:water) under high-speed stirring to precipitate the product, filter, wash, vacuum Dried to obtain soluble polyimide powder white powder containing phenolic hydroxyl group (Mn=96802, n=177);

[0075] (3) 1.00 g of dried soluble polyimide powder containing phenolic hydroxyl groups was dissolved in 9.00 g of N-methyl-2-pyrrolidone to obtain a polyimide solution; ...

Embodiment 3

[0077] Embodiment 3: the preparation of polyimide film

[0078] (1) in N 2 Under protection, 2.90g (10mmol) 4,4'-diamino-4"-hydroxytriphenylmethane and 34.56g N-methyl-2-pyrrolidone were added to the reaction flask, stirred and dissolved, and 3.10g ( 10mmol) 4,4'-diphenyl ether dianhydride, then stirred and reacted for 0.5h, then added 5.76g xylene and catalyst (0.10gγ-valerolactone and 0.16g pyridine), heated to 200°C and refluxed for azeotropic dehydration for 3h;

[0079] (2) Cool the mixed solution after reflux in step (1) to 20° C., then pour it into methanol under high-speed stirring to precipitate the product, filter, wash, and vacuum-dry to obtain soluble polyimide powder containing phenolic hydroxyl groups White powder (Mn=168138, n=307);

[0080] (3) 1.00 g of dried soluble polyimide powder containing phenolic hydroxyl group was dissolved in 5.67 g of N, N-dimethylformamide to obtain a polyimide solution;

[0081] (4) Put the polyimide solution under vacuum condit...

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Abstract

The invention belongs to the field of chemical synthesis and discloses soluble polyimides containing phenolic hydroxyl group and a preparation method and application thereof. The soluble polyimides containing phenolic hydroxyl group has a structure as shown in the formula (I). The invention also discloses a preparation method of the soluble polyimides containing phenolic hydroxyl group. By high temperature and by the use of a catalyst, cyclization efficiency is enhanced, and reaction time is shortened. As the obtained polyimides contain lots of flexible groups and large volume of phenyl ring side-group, the product has high molecular weight and is chemically soluble. The problem that polyimides have poor dissolvability and application of polyimides is limited is solved. On this basis, it is also easy to process a polyimide film, and the application range is widened. By introducing phenolic hydroxyl group into PI molecular chain, thermal property is not influenced, and compatibility or adhesive property of the polyimide material with other materials is improved. The product can be applied to electronic packaging, film materials and adhesives.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a soluble polyimide containing phenolic hydroxyl groups and a preparation method and application thereof. Background technique [0002] Polyimide refers to a class of polymers with imide rings in the main molecular chain, which can be divided into two categories: aromatic polyimides and aliphatic polyimides. Generally speaking, polyimide refers to aromatic polyimide. The existence of its bicyclic structure makes the heat resistance very good, and it can be used for a long time above 200°C. Very prominent in plastics. Polyimide materials have been widely used in aviation, aerospace, microelectronics, liquid crystal and other fields. [0003] In the 1950s, polyimide developed vigorously, and its commercialization and industrialization followed closely. The most representative ones were the Kapton film of DuPont in the United States and the Upilex film of Ube Industri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/18C08L79/08
Inventor 吕满庚王莹吴昆郑剑
Owner NANXIONG MATERIAL PRODION BASE OF CHINESE ACADEMY OF SCI GUANGZHOU CHEM
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