Alkoxyamine Polymerization via Nitroxide Reducer

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Solution Overview

Problem

Conventional radical polymerization techniques require high temperatures, making it difficult to achieve polymerization at ambient or low temperatures, which is necessary for large-scale applications like wind turbine blades and multi-component adhesives, and results in increased viscosity and energy consumption.

Innovation Solution

A process involving the use of alkoxyamines in the presence of a nitroxide reducer to initiate polymerization at temperatures between -50°C and 80°C, allowing for the synthesis of block copolymers with rapid kinetics compatible with industrial applications.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Temperature

If conventional radical polymerization is carried out at high temperatures, then polymerization proceeds rapidly, but energy consumption increases and polymerization cannot be performed at ambient or low temperatures

Engineering Contradiction:
Improvepolymerization temperatureVSAvoidenergy consumption
Core Design Contradiction:
TemperatureVSUse of energy by moving object

Solution Approach 1:

The invention changes the temperature parameter from conventional high temperatures to low temperatures (0-80°C, preferably 20-50°C) by using alkoxyamine initiators with specific decomposition characteristics. This parameter change enables polymerization at ambient or low temperatures while maintaining industrial compatibility, directly resolving the contradiction between temperature reduction and energy consumption.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If block copolymer is prepared in a preliminary step, then block copolymer is obtained, but viscosity of the mixture increases significantly

Engineering Contradiction:
Improveblock copolymer synthesis controlVSAvoidmixture viscosity
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The invention applies preliminary action by pre-synthesizing the alkoxyamine initiator with controlled decomposition temperature characteristics before the main polymerization process. This preliminary preparation allows the initiator to remain stable during mixing and processing (low viscosity state) and then trigger controlled polymerization when activated, achieving both synthesis control and ease of manufacture.

Inventive Principle:
Principle #10Preliminary action

3Use of energy by moving object

If polymerization is carried out at room temperature or negative temperatures, then energy consumption is reduced, but polymerization kinetics become too slow for industrial applications

Engineering Contradiction:
Improveenergy consumptionVSAvoidpolymerization rate
Core Design Contradiction:
Use of energy by moving objectVSProductivity

Solution Approach 1:

The invention optimizes the initiator decomposition temperature parameter to match the desired polymerization temperature range (20-50°C). By selecting alkoxyamines with specific bond dissociation energies and thermal stability characteristics, the polymerization rate remains industrially acceptable (completion within minutes to hours) even at low temperatures, resolving the contradiction between energy savings and productivity.

Inventive Principle:
Principle #35Parameter changes

4Temperature

If alkoxyamine is used without nitroxide reducer, then polymerization cannot start at low temperatures, but adding nitroxide reducer enables low temperature polymerization initiation

Engineering Contradiction:
Improvepolymerization temperatureVSAvoidsystem composition
Core Design Contradiction:
TemperatureVSDevice complexity

Solution Approach 1:

The nitroxide reducer acts as an intermediary substance that facilitates the activation of alkoxyamine at low temperatures. It mediates the electron transfer process to generate radicals from the alkoxyamine C-O bond without requiring high thermal energy, enabling low temperature polymerization while adding only a simple functional component to the system.

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

Enables polymerization at low temperatures, reducing energy consumption, minimizing viscosity issues, and allowing for the synthesis of block copolymers in situ, which is favorable for applications such as coatings, adhesives, and composite materials.

Implementation Method 1

The invention relates to a process for the radical polymerization of alkoxyamines at low temperatures, typically at temperatures as low as minus 50°C in the presence of a nitroxide reducer

Methodology Applied
Scientific EffectElectron transfer: Redox Reactions

Data Source

PatentEP3233933B1Low-temperature radical polymerisation of alkoxyamines
Publication Date: 2019.11.06 ARKEMA FRANCE SA
  • EP3233933B1 patent drawingFigure 1~2
  • EP3233933B1 patent drawing
  • EP3233933B1 patent drawing

AI summary

The invention relates to a method for the radical polymerisation of alkoxyamines at low temperatures, typically at temperatures as low as - 50°C in the presence of a nitroxide-reducing agent.