Continuous Diene Elastomer Synthesis Using Lithium Amide

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Solution Overview

Problem

Conventional continuous polymerization processes with a single reactor struggle to achieve both high monomer conversion and high levels of living polymer chains when initiated with lithium amide, leading to suboptimal polymer properties for tire applications.

Innovation Solution

A continuous synthesis process using multiple reactors in series, where the mass conversion in the first reactor is less than 70%, with subsequent reactors receiving reinjected solutions to achieve total mass conversion greater than 70% and a high rate of living polymer chains greater than 90%, utilizing lithium amide as an initiator and controlling parameters like temperature and residence time.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If a single reactor is used for continuous polymerization with lithium amide initiator, then the process is simple and continuous, but it cannot achieve both high monomer conversion and high level of living polymer chains simultaneously

Engineering Contradiction:
Improvemonomer conversionVSAvoidlevel of living polymer chains
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The polymerization process is divided into multiple continuous stirred-tank reactors (CSTRs) connected in series. Each reactor operates at a controlled conversion rate, with the first reactor maintaining conversion below 70% to preserve living chains, while subsequent reactors continue polymerization to achieve overall high conversion. This segmentation allows simultaneous achievement of high conversion and high living chain levels.

Inventive Principle:
Principle #1Segmentation

2Productivity

If mass conversion in the first reactor is increased to improve productivity, then more monomer is converted, but the level of living polymer chains decreases

Engineering Contradiction:
Improvemonomer conversion in first reactorVSAvoidlevel of living polymer chains
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The first reactor is deliberately operated at partial conversion (less than 70%) rather than complete conversion. This partial action preserves a high proportion of living polymer chains (greater than 90%) by preventing excessive chain termination that would occur at higher conversions. The remaining monomer conversion is then completed in subsequent reactors.

Inventive Principle:
Principle #16Partial or excessive action

3Reliability

If multiple reactors in series are used to achieve high conversion and high living polymer chains, then polymer quality improves, but process complexity increases

Engineering Contradiction:
Improvelevel of living polymer chainsVSAvoidnumber of reactors
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

Each reactor in the series performs the same basic function (anionic polymerization with lithium amide initiator), but operates at different conversion stages. This multi-functionality allows the system to achieve both high conversion and high living chain levels without requiring fundamentally different reactor types or complex process changes in each unit.

Inventive Principle:
Principle #6Universality (Multi-functionality)

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 process enables the production of diene elastomers with high monomer conversion and living polymer chains, enhancing their mechanical properties and reducing hysteresis, thereby improving tire performance and reducing rolling resistance.

Implementation Method 1

continuous synthesis of a diene elastomer by means of n reactors r1 to rn, equipped with an internal stirring system... supplied with an input solution comprising a solvent, one or more monomers, an anionic polymerization initiator chosen from lithium amides

Methodology Applied
Scientific EffectAnionic polymerization: Chemical Bonding

Implementation Method 2

the mass conversion C1 in the first reactor being less than 70%, the polymerization being continued in such a manner so that the total mass conversion at the outlet of the last reactor is greater than 70%

Methodology Applied
Scientific EffectPolymerization reaction: Chemical Bonding

Data Source

PatentEP3558512B1Method for the continuous synthesis of a diene elastomer with lithium amide initiator
Publication Date: 2021.07.21 MICHELIN & CO (CIE GEN DES ESTAB MICHELIN)
  • EP3558512B1 patent drawing
  • EP3558512B1 patent drawing
  • EP3558512B1 patent drawing

AI summary

The invention concerns a method for the continuous synthesis of a diene elastomer by means of n reactors r1 to rn, equipped with an internal stirring system, that are assumed to be perfectly stirred, arranged in series, n varying from 2 to 15, preferably from 2 to 9, the reactor r1 being supplied with an inlet solution comprising a solvent, one or more monomers, an anionic polymerisation initiator chosen from the lithium amides and a polar agent, the mass conversion C1 in the first reactor being less than 70%, the total mass conversion Cn at the outlet of the reactor rn being greater than or equal to 70%.