Polyimide containing benzimidazole unit and preparation method thereof

A technology of polyimide and benzimidazole, applied in the field of polyimide containing benzimidazole unit and its preparation, can solve problems such as thermal performance decline, achieve low cost, expand application scope, reduce regularity and interaction effect of force

Inactive Publication Date: 2012-07-25
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

PI is usually structurally modified by introducing flexible structural units, large side groups, twisted and non-coplanar structures, or breaking the symmetry and regularity of molecular chains by copolymerization, but it usually leads to a decline in thermal properties.

Method used

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  • Polyimide containing benzimidazole unit and preparation method thereof
  • Polyimide containing benzimidazole unit and preparation method thereof
  • Polyimide containing benzimidazole unit and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Synthesis of diamine monomer 3,3',5,5'-four substituent structure aromatic diamine

[0024] Add 30.4g (0.25mol) 2,6-dimethylaniline (or 2,6-dichloroaniline or 2,6-difluoroaniline), after being heated to 120 DEG C, dropwise add 17.8ml (0.12mol) benzaldehyde (or formaldehyde) and 5ml mass fraction 36~38% concentrated hydrochloric acid through the constant pressure dropping funnel in half an hour again, in After continuing to stir at this temperature for half an hour, the temperature of the reaction system was raised to reflux, and the temperature was lowered to 80° C. after the reaction was continued for 10 hours, and the reaction system was poured into 200 ml of 10% potassium hydroxide aqueous solution to terminate the reaction. After the obtained crude product was dried, it was further separated and purified by silica gel column chromatography to obtain a white crystal powdery diamine compound with a yield of about 80%. The diamine monomer is 3,3',5,5'-tetrasubstit...

Embodiment 2

[0029] The synthesis of 3,3',5,5'-tetrachloro-4,4'-diaminophenylmethane is the same as in Example 1.

[0030] In a 250ml three-necked round-bottomed flask equipped with a mechanical stirrer, water separator, condenser and nitrogen protection, the diamine monomer 3,3',5,5'-tetrachloro- 4,4'-diaminophenylmethane and BIA are mixed and added, and then the dianhydride monomer BPDA and 500ml NMP solvent in an equimolar amount to the total molar amount of the two diamine monomers, the solid content in the solution is 12% . After reacting and stirring at 120°C for 1 hour, continue to heat up to 200°C, keep the reaction temperature for 10 hours to obtain a viscous polymer solution, cool down to about 150°C, then pour the reaction solution into 500ml of ethanol to settle to end the reaction, and obtain a fibrous polymer solution. or strip-shaped polymer samples, the polymer was further rinsed twice with 1:1 ethanol and acetone, then suction-filtered, and vacuum-dried at 80°C for 10 h t...

Embodiment 3

[0033] The synthesis of 3,3',5,5'-tetrafluoro-4,4'-diaminophenyltoluene is the same as in Example 1.

[0034] In a 250ml three-necked round-bottomed flask equipped with a mechanical stirrer, water separator, condenser and nitrogen protection, the diamine monomer 3,3',5,5'-tetrafluoro- 4,4'-diaminophenyltoluene and BIA are mixed and added, and then the dianhydride monomer BTDA and 500ml DMAC solvent in an equimolar amount to the total molar amount of the two diamine monomers, the solid content in the solution is 10% . After reacting at 120° C. and stirring for 1 hour, the temperature was continued to rise to 190° C., and the reaction temperature was kept at 190° C. for 9 hours to obtain a viscous polymer solution. Cool down to about 150°C, then pour the reaction solution into 500ml of ethanol to settle to end the reaction, to obtain a fibrous or strip-shaped polymer sample, further wash the polymer twice with 1:1 ethanol and acetone, and then suction filter , vacuum drying at...

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Abstract

The invention relates to polyimide containing a benzimidazole unit and a preparation method thereof. The polyimide has the following structural formula. The preparation method comprises the following steps of: firstly, performing the reaction on 2,6-disubstituted aniline and aldehyde under the acidic condition to generate a diamine compound 3,3',5,5'-tetra-substituted aromatic diamine; and then, after mixing the synthesized aromatic diamine and a heterocyclic diamine monomer 6-aminophenyl-2-aminobenzimidazole according to a certain ratio, performing the reaction on the mixture and a dianhydride monomer in an organic solvent to obtain the polyimide. The polyimide provided by the invention has excellent solubility property, can be dissolved in conventional solvents such as NMP (N-methyl-2-pyrrolidone) and DMAc (dimethyl acetamide), has excellent heat resistance and mechanical property and has excellent thermal properties of glass-transition temperature of over 410 DEG C, decomposition temperature of over 500 DEG C and the like.

Description

technical field [0001] The invention belongs to the field of polyimide and its preparation, in particular to a polyimide containing benzimidazole units and its preparation method. Background technique [0002] Polyimide (PI) is a kind of polymer material containing imide rings in the main chain of polymer molecules. It has excellent mechanical, dielectric, insulation, radiation resistance, corrosion resistance, high and low temperature resistance and other excellent properties. Widely used in aerospace, electrical, microelectronics and chemical industries. Due to the strong rigidity of the PI molecular chain itself and the strong interaction between the molecular chains, the common type of PI neither melts nor dissolves until the decomposition temperature, which makes its processing and molding difficult. Improving the processability of polyimide and maintaining its excellent heat resistance is one of the current research hotspots. Structural modification of PI is usually ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
Inventor 张清华程曾汉王鑫宇王亚平吉亚丽夏清明陈大俊
Owner DONGHUA UNIV
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