Polyimide Resin Production via Low-Temperature Imidization

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Solution Overview

Problem

Conventional methods for producing polyimide resin at lower temperatures result in degraded heat resistance and mechanical properties, and increased dielectric constant, making it difficult to achieve polyimide products with excellent properties without high-temperature heat treatment.

Innovation Solution

Using a specific amide-based solvent, such as N,N,2-trimethylpropione amide, to react tetracarboxylic acid dianhydride and diamine components, allowing for the production of polyamic acid that is then heated between 120°C to 350°C to form a polyimide resin with improved heat resistance and mechanical properties while maintaining a low dielectric constant.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Strength

If heat-treatment at high temperature of about 300°C is performed to form polyimide resin, then heat resistance and mechanical properties are improved, but the method cannot be applied to heat-sensitive materials and increases processing complexity

Engineering Contradiction:

Improveheat resistance and mechanical propertiesVSAvoidapplicability to heat-sensitive materials

Core Design Contradiction:

StrengthVSAdaptability or versatility

Solution Approach 1:

The patent changes the chemical composition parameters of the polyamic acid precursor by selecting specific tetracarboxylic acid dianhydride and diamine components, which enables the polymer to achieve excellent heat resistance and mechanical properties after heat-treatment at lower temperatures (100-200°C) while maintaining adaptability to heat-sensitive materials

Inventive Principle:

Principle #35Parameter changes

2Adaptability or versatility

If heat-treatment at lower temperature of around 200°C is performed to form polyimide resin, then applicability to heat-sensitive materials is improved, but heat resistance and mechanical properties degrade and dielectric constant increases

Engineering Contradiction:

Improveapplicability to heat-sensitive materialsVSAvoidheat resistance and mechanical properties

Core Design Contradiction:

Adaptability or versatilityVSStrength

Solution Approach 1:

The patent performs preliminary action by carefully selecting and combining specific tetracarboxylic acid dianhydride and diamine components to form a polyamic acid precursor with optimized molecular structure and composition, which enables the final polyimide resin to achieve excellent properties even after low-temperature heat-treatment

Inventive Principle:

Principle #10Preliminary action

Solution Approach 2:

Inventive Principle:

Principle #35Parameter changes

3Ease of manufacture

If conventional solvents like NMP or DMF are used to produce polyamic acid, then ease of manufacture is improved, but the resulting polyimide resin cannot achieve excellent properties at lower heat-treatment temperatures

Engineering Contradiction:

Improveease of producing polyamic acid solutionVSAvoidheat resistance and mechanical properties

Core Design Contradiction:

Ease of manufactureVSStrength

Solution Approach 1:

The patent uses propyleneglycol monomethylether acetate as an intermediary solvent that facilitates the polymerization reaction between tetracarboxylic acid dianhydride and diamine components, enabling the formation of polyamic acid with optimized structure that can be converted to high-performance polyimide resin at lower temperatures

Inventive Principle:

Principle #24Intermediary (Mediator)

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

The method enables the production of polyimide resin with excellent heat resistance and mechanical properties, including tensile elongation, and a low dielectric constant, even when heat-treated at lower temperatures, thereby overcoming the limitations of conventional high-temperature processing.

Implementation Method 1

a polyamic acid resulting from the reaction of a tetracarboxylic acid dianhydride component and a diamine component in a solvent

Methodology Applied

Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

heating at from 120°C to 350°C a polyamic acid resulting from the reaction of a tetracarboxylic acid dianhydride component and a diamine component

Methodology Applied

Scientific EffectThermal imidization: Heat Treatment

Data Source

PatentEP2907838B1Method of producing polyimide resin, method of producing polyimide coating, method of producing polyamic acid solution, polyimide coating, and polyamic acid solution

Publication Date: 2019.11.27 TOKYO OHKA KOGYO CO LTD

AI summary

Provided is a method of producing a polyimide resin that produces a polyimide resin excellent in heat resistance and mechanical properties and having a low dielectric constant even when heat-treated at a lower temperature. The method of producing a polyimide resin according to the present invention includes heating at from 120°C to 350°C a polyamic acid resulting from the reaction of a tetracarboxylic acid dianhydride component and a diamine component in a solvent comprising at least a compound (A) represented by the general formula (1), in which R1 represents a hydrogen atom or a hydroxyl group, R2 and R3 independently represent a hydrogen atom or a C1 to C3 alkyl group, and R4 and R5 independently represent a C1 to C3 alkyl group.