Composite Particles for Stable One-Part Epoxy Curing

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Solution Overview

Problem

Current epoxy resin curing compositions, whether two-part or one-part, face challenges in storage stability and efficient curing, with two-part systems requiring precise metering and having limited shelf-life, while one-part systems often have reduced shelf-life due to latent curing agents with high activation temperatures.

Innovation Solution

Development of composite particles with a porous polymeric core containing a curing agent or catalyst, coated with a fluoropolymer, which releases the curing agent or catalyst upon heating, allowing for a one-part formulation with improved storage stability and efficient curing with the epoxy resin.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Stability of the object's composition

If a two-part formulation is used with a curing agent and epoxy resin separated, then storage stability is improved (one year or more), but the system requires precise metering and careful mixing, and the epoxy resin must be used soon after mixing

Engineering Contradiction:
Improvestorage stabilityVSAvoidmixing operation
Core Design Contradiction:
Stability of the object's compositionVSEase of operation

Solution Approach 1:

The curing agent is segmented into discrete microcapsules with a shell structure, allowing it to be physically separated from the epoxy resin in storage while enabling controlled release upon mixing. The microcapsules break during mixing, releasing the curing agent uniformly throughout the epoxy resin without requiring precise metering.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The microcapsule shell acts as an intermediary that protects the curing agent during storage and transport, then selectively breaks down under mixing conditions to release the curing agent. This intermediary structure eliminates the need for precise metering while maintaining storage stability.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Ease of operation

If a one-part composition with a latent curing agent is used, then no mixing is required, but the shelf-life is significantly reduced compared to two-part formulations

Engineering Contradiction:
Improvemixing operationVSAvoidshelf-life
Core Design Contradiction:
Ease of operationVSDuration of action of stationary object

Solution Approach 1:

The curing agent is segmented into microcapsules that remain physically separated from the epoxy resin throughout storage. This segmentation prevents premature curing reactions, maintaining shelf-life comparable to two-part formulations, while the one-part formulation eliminates mixing operations.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The microcapsule shell provides a flexible barrier that maintains the integrity of the curing agent during storage. The shell is designed to break under mechanical stress during application, releasing the curing agent only when needed, thus preserving shelf-life while enabling one-part convenience.

Inventive Principle:
Principle #30Flexible shells and thin films

3Duration of action of stationary object

If a latent curing agent that is thermally activated is used, then shelf-life of 6 months or more is achieved, but the cure temperature is limited by the melting point of the curing agent which typically exceeds about 150°C or 170°C

Engineering Contradiction:
Improveshelf-lifeVSAvoidcure temperature
Core Design Contradiction:
Duration of action of stationary objectVSTemperature

Solution Approach 1:

The microcapsule shell composition and structure are optimized to enable curing at lower temperatures than the melting point of the latent curing agent. The shell material and thickness are adjusted to allow controlled release at reduced temperatures, expanding the range of applicable curing conditions while maintaining shelf-life.

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 composite particle system enables a one-part epoxy resin curing composition with enhanced storage stability and efficient curing, as the curing agent or catalyst is released upon heating, reacting with the epoxy resin to form a cured composition, thus overcoming the limitations of existing systems.

Implementation Method 1

a curing agent and/or curing catalyst for an epoxy resin positioned within the porous polymeric core particle

Methodology Applied
Scientific EffectAdsorption: Adsorption

Implementation Method 2

a fluoropolymer-containing coating layer around the porous polymeric core particle

Methodology Applied
Scientific EffectThermal insulation: Thermal Insulation

Implementation Method 3

the curing agent and/or curing catalyst is released upon heating

Methodology Applied
Scientific EffectThermal decomposition: Pyrolysis

Data Source

PatentEP3448923B1Composite particles for curing epoxy resin compositions and curable and cured epoxy resin compositions prepared using the particles
Publication Date: 2021.03.17 3M INNOVATIVE PROPERTIES CO
  • EP3448923B1 patent drawingFigure 1A~1B
  • EP3448923B1 patent drawingFigure 2~3A
  • EP3448923B1 patent drawingFigure 3B~4

AI summary

Composite particles are provided that can be used to cure epoxy resins. More particularly, the composite particles have a porous polymeric core particle, a curing agent and/or a curing catalyst for an epoxy resin positioned within the porous polymeric core particle, and a fluoropolymer-containing coating layer around the porous polymeric core particle. Additionally, curable compositions are provided that are mixtures containing an epoxy resin and the composite particles. The epoxy resin typically does not react until the curable composition is heated causing the release of the curing agent and/or curing catalyst from the composite particle. Further, cured compositions formed from the curable composition are provided.