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Thermoplastic polyimide resin with low thermal expansion coefficient and preparation method thereof

A technology of polyimide resin and low thermal expansion coefficient, which is applied in the field of thermoplastic polyimide resin with low thermal expansion coefficient and its preparation, can solve the problems of complex preparation process, solvent corrosion resistance, degradation of hydrolysis resistance, etc. Improve the effect of thermoplastic

Active Publication Date: 2020-06-05
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product prepared by this material is in the form of a thin film, and the preparation process is complicated. After the introduction of Si-O, the solvent corrosion resistance and hydrolysis resistance will decrease.

Method used

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  • Thermoplastic polyimide resin with low thermal expansion coefficient and preparation method thereof
  • Thermoplastic polyimide resin with low thermal expansion coefficient and preparation method thereof
  • Thermoplastic polyimide resin with low thermal expansion coefficient and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation method (add catalyst) of low coefficient of thermal expansion thermoplastic polyimide resin is as follows:

[0032] Under the protection of nitrogen, add 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl (9.6072g, 30.0mmol) and 25mL of N,N-dimethylacetamide to the reaction flask at room temperature Stir to dissolve, then add trimethylchlorosilane (3.2592g, 30.0mmol), pyridine (2.1350g, 27.0mmol) and 4-dimethylaminopyridine (0.3665g, 3.0mmol), stir at room temperature for 15 minutes, then cool to 0 ℃, add isophthaloyl dichloride (4.0929, 20.16mmol) and 4,4-biphenyldianhydride (2.5420g, 8.64mmol), then add 25mL of N,N-dimethylacetamide, naturally warm to room temperature, Stir for 12 hours, then add phthalic anhydride (0.3554g, 2.4mmol) to cap, continue to react for 2 hours, then add a mixture of acetic anhydride (120mmol) and pyridine (60mmol), and react at 80°C for 2 hours. Drop the reaction solution into ethanol to obtain fibrous polyimide precipitates, and...

Embodiment 2

[0034] The preparation method (do not add catalyst) of low coefficient of thermal expansion thermoplastic polyimide resin is as follows:

[0035]Under the protection of nitrogen, add 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl (9.6072g, 30.0mmol) and 25mL of N,N-dimethylacetamide to the reaction flask at room temperature Stir to dissolve, then cool to 0°C, add isophthaloyl dichloride (4.0929, 20.16mmol) and 4,4-biphenyldianhydride (2.5420g, 8.64mmol), add 25mL of N,N-dimethylethane Amide, naturally warmed to room temperature, stirred for 12 hours, then added phthalic anhydride (0.3554g, 2.4mmol) capping, continued to react for 2 hours, then added a mixture of acetic anhydride (120mmol) and pyridine (60mmol), and reacted at 80°C for 2 hours. Hour. Drop the reaction solution into ethanol to obtain fibrous polyimide precipitates, and dry to obtain polyimide powder. See Table 1 for performance measurements.

Embodiment 3

[0037] Under the protection of nitrogen, add 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl (9.6072g, 30.0mmol) and 25mL of N,N-dimethylacetamide to the reaction flask at room temperature Stir to dissolve, then add trimethylchlorosilane (3.2592g, 30.0mmol), pyridine (2.1350g, 27.0mmol) and 4-dimethylaminopyridine (0.3665g, 3.0mmol), stir at room temperature for 15 minutes, then cool to 0 ℃, add isophthaloyl dichloride (1.7542g, 8.64mmol) and 4,4-biphenyl dianhydride (5.9315g, 20.16mmol), add 25mL of N,N-dimethylacetamide, naturally warm to room temperature , stirred for 12 hours, then added phthalic anhydride (0.3554g, 2.4mmol) to block, continued the reaction for 2 hours, then added a mixture of acetic anhydride (120mmol) and pyridine (60mmol), and reacted at 80°C for 2 hours. Drop the reaction solution into ethanol to obtain fibrous polyimide precipitates, and dry to obtain polyimide powder. See Table 1 for performance measurements.

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Abstract

The invention discloses a thermoplastic polyimide resin with a low thermal expansion coefficient and a preparation method thereof, wherein the resin has the following structural formula. The inventionalso discloses a preparation method of the resin, wherein 4,4'-diamino-2,2'-bis(trifluoromethyl)biphenyl, isophthaloyl dichloride and 4,4-biphenyl dianhydride are taken as polymerization monomers, and the resin is prepared by reaction in a solvent. According to the invention, a structure containing amido bonds is introduced into a polyimide system; therefore, by means of the interaction force ofintramolecular hydrogen bonds, the thermoplasticity is improved through a meta-position asymmetric structure, so that the molecular structure simultaneously has the two advantages of thermoplasticityand low thermal expansion coefficient, the melt index is 0.1-2 g / 10 min, thermoplastic processing can be met, and the thermal expansion coefficient is 20-40 ppm / K.

Description

technical field [0001] The invention relates to the technical field of thermoplastic polyimide resins, in particular to a thermoplastic polyimide resin with low thermal expansion coefficient and a preparation method thereof. Background technique [0002] Thermoplastic polyimide (TPI) is developed on the basis of traditional thermosetting polyimide (PI). Polyimide (PI) refers to a class of hetero Cyclopolymer is one of the organic polymer materials with the best comprehensive properties. It has many excellent characteristics such as corrosion resistance, fatigue resistance, damage resistance, impact resistance, and high thermal decomposition temperature. It is one of the varieties with the highest thermal stability among polymers so far. It has been widely used in many high-tech fields such as aerospace, aviation, space, automobile, microelectronics, nanometer, medical equipment, etc., and is called "problem-solving expert" and "golden plastic". [0003] However, PI has the...

Claims

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Application Information

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IPC IPC(8): C08G73/14
CPCC08G73/14
Inventor 王冰柯陈国飞娜菲莎.穆什塔奇方省众
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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