Polyimide precursor, preparation method and resin composition and application thereof

A technology of polyimide precursor and resin composition, which is applied in the field of resin composition, polyimide precursor and preparation, can solve the problem that the main chain flexibility and aromatic ring side groups are not compatible, cracking, carboxyl group pair amide group autocatalytic cracking and other problems, to achieve the effect of easy self-degradation, prolonged storage time, and inhibition of self-degradation

Pending Publication Date: 2019-06-28
SHENZHEN INST OF ADVANCED TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ionic liquid that this method provides can make the polyimide prepolymer of generation carry out complete imidization reaction at low temperature, make the polyimide of preparation be colorless and have very high transparency, but still There is a problem with autocatalytic cleavage of carboxyl to amide groups
[0004] CN108640846A discloses a flexible aromatic diamine monomer containing aromatic ring side groups and its preparation method. The purpose of the present invention is to solve the main chain flexibility and aromatic rin

Method used

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  • Polyimide precursor, preparation method and resin composition and application thereof
  • Polyimide precursor, preparation method and resin composition and application thereof
  • Polyimide precursor, preparation method and resin composition and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0058] This embodiment prepares the polyimide precursor through the following steps

[0059]

[0060] (1) 43.624 g (200 mmol) of pyromellitic dianhydride, 57.002 g (401 mmol) of glycidyl methacrylate and 0.220 g of hydroquinone dried in a dryer at 160°C for 24 hours were dissolved in 394 g of N-methylpyrrolidone In , after adding a catalytic amount of 1,8-diazabicycloundecene, it was stirred at room temperature (25° C.) for 24 hours to perform esterification, thereby obtaining a pyromellitic acid-glycerol methacrylate solution.

[0061] (2) Add 195.564 g of the solution obtained in step (1) to a 0.5 L flask equipped with a stirrer and a thermometer, and then add 25.9 g of thionyl chloride dropwise using a dropping funnel under ice cooling to keep the temperature of the reaction solution below 10°C. g (217.8 mmol). After the dropwise addition of thionyl chloride was completed, the reaction was carried out under ice cooling for 2 hours to obtain an acid chloride solution of ...

Embodiment 2

[0065] This embodiment prepares the polyimide precursor through the following steps

[0066]

[0067] (1) 58.844 g (200 mmol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride, 57.002 g (401 mmol) of glycidyl methacrylate, and hydroquinone dried in a dryer at 160°C for 24 hours 0.220g was dissolved in 350g N,N-dimethylformamide, after adding a catalytic amount of 1,8-diazabicycloundecene, stirred at room temperature (25°C) for 24 hours to carry out esterification, thereby A 3,3',4,4'-biphenyltetracarboxylic dianhydride-glycerol methacrylate solution was obtained.

[0068] (2) Add 213.52 g of the solution obtained in step (1) to a 0.5 L flask equipped with a stirrer and a thermometer, and then add 26.5 g of thionyl chloride dropwise using a dropping funnel under ice cooling to keep the temperature of the reaction solution below 10°C. g (222.5 mmol). After the dropwise addition of thionyl chloride was completed, the reaction was carried out under ice cooling for 2.5 hours to...

Embodiment 3

[0071] This embodiment prepares the polyimide precursor through the following steps

[0072]

[0073] (1) Dissolve 43.624 g (200 mmol) of pyromellitic dianhydride, 12.802 g (401 mmol) of methanol, and 0.220 g of hydroquinone dried in a dryer at 160°C for 24 hours in 353 g of dimethyl sulfoxide, and add a catalytic amount The 1,8-diazabicycloundecene was stirred at room temperature (25° C.) for 24 hours to perform esterification, thereby obtaining a pyromellitic acid-methyl ester solution.

[0074] (2) Add 172.55 g of the solution obtained in step (1) to a 0.5 L flask equipped with a stirrer and a thermometer, and then add 24.8 g of thionyl chloride dropwise using a dropping funnel under ice cooling to keep the temperature of the reaction solution below 10°C. g (208.9 mmol). After the dropwise addition of thionyl chloride was completed, the reaction was carried out under ice cooling for 2 hours to obtain an acid chloride solution of PMDA. Next, using a dropping funnel, a sol...

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Abstract

The invention provides a polyimide precursor, a preparation method and a resin composition and an application thereof. The polyimide precursor has a structure as shown in a formula I. The polyimide precursor achieves a purpose of inhibiting self degradation effectively as protons in carboxyl are constrained by forming ester groups by carboxyl in polyimide, so that the storage time is prolonged. Compared with existing polyimide which has the defects that the highest thermal imidization temperature of polyimide reaches 400 DEG C to waste resources and the imidization degree of polyimide in a solution cannot be controlled and is easy to self-degraded, the polyimide precursor has more obvious advantages. A formed curing film has a relatively low dielectric property, is convenient to store a room temperature, is low in stress, and high in adaptability and wide in application range.

Description

technical field [0001] The invention belongs to the field of polymer materials, and relates to a polyimide precursor, a preparation method, a resin composition and applications thereof. Background technique [0002] Polyimide is currently the best heat-resistant polymer material that has been industrialized. Due to its superior comprehensive performance, it is widely used in high-tech applications such as films, coatings, plastics, composite materials, foam plastics, fibers, and photoresists. fields are widely used. However, the traditional synthesis route of polyimide (PI), that is, the process of obtaining PI products through further high-temperature imidization of polyamic acid (PAA) precursors, still has shortcomings. Studies in recent years have suggested that the easy degradation of PAA is mainly due to the autocatalytic cracking of the amide group by the ortho carboxyl group in PAA, and the anhydride produced is hydrolyzed by the water in the solvent, making it unabl...

Claims

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Application Information

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IPC IPC(8): C08G73/12C08G73/10C08F283/04C08F222/20C08J5/18C08L79/08
Inventor 张国平黄超孙蓉李金辉
Owner SHENZHEN INST OF ADVANCED TECH
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