Polyimide Powder Thermo-Oxidative Stability

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Solution Overview

Problem

Current high-temperature polyimide moldings and powders have limitations in thermo-oxidative resistance, production complexity, and cost, particularly for applications requiring direct forming and hot compression molding processes.

Innovation Solution

Development of a polyimide powder with a specific composition of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride and a mixture of p-phenylenediamine, m-phenylenediamine, and 4,4'-diaminodiphenyl ether, optimized for direct forming and hot compression molding, which enhances thermo-oxidative resistance and reduces production costs.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If conventional polyimide powders (Vespel®, Meldin®, Plavis®, Upimol®) are used, then molded parts can be produced, but the powder is not available on the open market and production requires complex hot isostatic pressing processes

Engineering Contradiction:
Improvemanufacturing process complexityVSAvoidpolymer powder availability
Core Design Contradiction:
Ease of manufactureVSQuantity of substance

Solution Approach 1:

The patent uses readily available, inexpensive raw materials (BPDA, PMDA, p-PDA, m-PDA, ODA) that can be easily procured on the open market, replacing expensive proprietary polyimide powders. The simple synthesis process produces a functional equivalent that eliminates the need for complex hot isostatic pressing and proprietary powder sources.

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

Solution Approach 2:

The patent modifies the chemical composition parameters of the polyimide by using specific ratios of BPDA (60-100 mol%), PMDA (0-40 mol%), and diamines (p-PDA 30-70 mol%, m-PDA 10-40 mol%, ODA 5-20 mol%). These parameter changes enable the material to achieve desired properties while being producible through simpler processes.

Inventive Principle:
Principle #35Parameter changes

2Reliability

If block copolymer structures (P84® NT1 and NT2) are used, then powder is available on the market, but the production process is more complex than random copolymers and thermo-oxidative resistance can be improved only marginally

Engineering Contradiction:
Improvethermo-oxidative resistanceVSAvoidproduction process complexity
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent uses simple random copolymer synthesis instead of complex block copolymer production, achieving comparable or superior thermo-oxidative resistance through optimized monomer ratios. This approach uses readily available chemicals and straightforward polymerization processes, eliminating the need for complex block copolymer manufacturing.

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

Solution Approach 2:

The patent optimizes the compositional parameters of the random copolymer, specifically using BPDA content of 60-100 mol% and specific diamine ratios, to achieve high thermo-oxidative resistance without requiring block copolymer structures. The inherent viscosity range of 15-80 ml/g is controlled through these compositional parameters.

Inventive Principle:
Principle #35Parameter changes

3Temperature

If polyimides with higher PMDA content are used, then processing temperature can be adjusted, but thermo-oxidative resistance decreases significantly

Engineering Contradiction:
Improveprocessing temperatureVSAvoidthermo-oxidative resistance
Core Design Contradiction:
TemperatureVSReliability

Solution Approach 1:

The patent carefully controls the PMDA content parameter within 0-40 mol% (preferably 5-30 mol%, particularly preferably 10-20 mol%) to balance processing temperature requirements with thermo-oxidative resistance. This optimized parameter range allows sufficient processing flexibility while maintaining weight loss below 1.0% at 400°C.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates a composite polyimide system combining multiple dianhydrides (BPDA and PMDA) and multiple diamines (p-PDA, m-PDA, and ODA) in optimized ratios. This composite approach allows the material to achieve both adequate processing temperature and high thermo-oxidative resistance through synergistic effects of the different monomer components.

Inventive Principle:
Principle #40Composite materials

4Manufacturing precision

If existing polyimide formulations are used, then molded parts can be produced, but surface quality and edge integrity (small radii of curvature without chipping) are insufficient

Engineering Contradiction:
Improvesurface quality and edge integrityVSAvoidmoldability
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent optimizes the inherent viscosity parameter to 15-80 ml/g (particularly preferably 20-50 ml/g) through controlled monomer ratios and polymerization conditions. This viscosity optimization enables the powder to flow and pack properly during molding, producing high-quality surfaces and sharp edges without chipping, while maintaining ease of manufacture through direct forming and hot compression molding.

Inventive Principle:
Principle #35Parameter changes

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 new polyimide powder exhibits excellent thermo-oxidative resistance, allowing for extended service life at high temperatures and simplified, cost-effective production of moldings with improved mechanical properties and surface quality.

Implementation Method 1

The polyamic acid is introduced into the boiling aprotic dipolar solvent with stirring. The solvent preferably contains an acid or an amine as a catalyst and optionally a precipitation aid to catalyze the imidization reaction.

Methodology Applied
Scientific EffectThermal imidization: Phase Change

Implementation Method 2

When imidization has occurred, the polyimide precipitates as a fine precipitate

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Implementation Method 3

The resulting filter cake or concentrated suspension is then dried in step v) using conventional drying processes such as, but not to be limited to, thin-film evaporators, spray dryers, spray granulators, drying cabinets, horizontal, vertical dryers or heated filter suction filters.

Methodology Applied
Scientific EffectDrying: Evaporation

Data Source

PatentEP2886583B1Polyimide powder having high thermooxidative stability
Publication Date: 2018.10.17 EVONIK FIBERS

AI summary

The invention relates to molded bodies with high thermo-oxidative resistance, which can be produced using direct forming and hot compression molding processes, as well as a new polyimide powder for their production and a process for producing this polyimide powder.