Polyimide Film Monomer Quantification via Hydrolysis

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Solution Overview

Problem

Conventional methods for analyzing the monomer composition of polyimide films, such as Pyrolysis GC-MS and derivatization followed by GC/MS, face challenges like complex data interpretation and limited quantitative analysis capabilities, particularly due to the difficulty in extracting and identifying monomer components.

Innovation Solution

A method involving hydrolysis of polyimide films with a strong base, followed by the addition of DMAc solvent and ultrasonication, and subsequent analysis using HPLC, which allows for the simultaneous derivatization and quantitative analysis of diamine and acid dianhydride monomers without a separate methyl derivatization step.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If Pyrolysis GC-MS or derivatization with TMAH is used to analyze monomer composition, then monomer components can be identified, but data interpretation becomes difficult due to complicated pyrolysis products

Engineering Contradiction:

Improvemonomer composition analysis capabilityVSAvoiddata interpretation complexity

Core Design Contradiction:

Measurement precisionVSDevice complexity

Solution Approach 1:

The patent extracts and analyzes only the necessary monomer components (dianhline and acid dianhydride) through selective hydrolysis, avoiding the generation of complicated pyrolysis products. This extraction approach isolates the target analytes from the complex polyimide matrix without creating additional interfering substances, thereby simplifying data interpretation while maintaining analysis capability

Inventive Principle:

Principle #2Taking out (Extraction)

Solution Approach 2:

The patent introduces hydrolysis as an intermediary step that converts the polyimide film into soluble monomer components that can be directly analyzed by HPLC. This intermediary transformation avoids the complex direct pyrolysis pathway and provides a cleaner analytical route with simpler data interpretation

Inventive Principle:

Principle #24Intermediary (Mediator)

2Measurement precision

If derivatization with TMAH is performed to analyze polyimide film, then monomer components can be identified, but derivatization of dianhydride does not easily occur, making it difficult to identify monomer components

Engineering Contradiction:

Improvemonomer component identificationVSAvoidderivatization efficiency

Core Design Contradiction:

Measurement precisionVSEase of manufacture

Solution Approach 1:

The patent changes the chemical parameters by using hydrolysis conditions (strong base, elevated temperature) that facilitate the cleavage of imide bonds and release of monomer components. This parameter change transforms the recalcitrant polyimide structure into reactive monomers that can be easily detected, overcoming the derivatization efficiency problem

Inventive Principle:

Principle #35Parameter changes

Solution Approach 2:

The patent performs preliminary hydrolysis treatment to break down the polyimide into monomer components before analysis. This preliminary action converts the difficult-to-analyze polyimide into easily detectable monomers, eliminating the need for difficult derivatization reactions

Inventive Principle:

Principle #10Preliminary action

3Quantity of substance

If hydrolysis method is used for extraction of diamine and methanolysis method for extraction of acid dianhydride, then monomer components can be extracted, but only qualitative analysis is possible

Engineering Contradiction:

Improvemonomer extraction capabilityVSAvoidquantitative analysis capability

Core Design Contradiction:

Quantity of substanceVSMeasurement precision

Solution Approach 1:

The patent merges the extraction and quantification steps by using HPLC with appropriate detection (UV-Vis or fluorescence) to simultaneously achieve both extraction of monomer components and their quantitative analysis. This combined approach eliminates the limitation of qualitative-only analysis while maintaining effective monomer extraction

Inventive Principle:

Principle #5Merging (Combining)

Solution Approach 2:

The patent substitutes the traditional separate extraction and analysis methodology with a unified HPLC-based system that provides both extraction and quantitative measurement capabilities in an integrated platform, enabling precise quantification

Inventive Principle:

Principle #28Mechanics substitution (Replace mechanical system)

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

This approach enables accurate and universal quantitative analysis of monomer content in polyimide films, providing a calibration curve-based method with an error of +/-15% or less and an average RSD of 5% or less, overcoming the limitations of previous qualitative analysis methods.

Implementation Method 1

a) hydrolyzing a polyimide film prepared by using at least one diamine and acid dianhydride with a strong base

Methodology Applied

Scientific EffectHydrolysis: Hydrolysis

Implementation Method 2

b) adding DMAc (dimethylacetamide) solvent to the solution containing the hydrolyzed polyimide film and performing ultrasonication of the solution to dissolve it

Methodology Applied

Scientific EffectUltrasonication: Ultrasonic Vibration

Data Source

PatentUS11549920B2Method for quantitative analysis of monomers in polyimide film

Publication Date: 2023.01.10 LG CHEM LTD

AI summary

An analysis method is provided, wherein a measurement sample containing a diamine and an acid dianhydride can be obtained without a separate methyl derivatization process. The analysis method includes pretreating a polyimide film including the polyimide which is a poorly soluble polymer with DMAc after hydrolysis, and determining an amount of monomers contained in the polyimide film.