Triblock Copolymer Purification via Methanol Trituration

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Solution Overview

Problem

The functionalization of aliphatic polyesters like polycaprolactone and polylactide through ring-opening polymerization is challenging due to multi-step syntheses and non-scaleable processes that result in poor yields and impurities, hindering the production of pure block copolymers for complex soft material applications.

Innovation Solution

A method involving heating a solution of crude block copolymer with an alcohol and then cooling it to promote precipitation, which effectively reduces impurities to 0-5 wt% and maintains polydispersity, molecular weight control, and structural integrity of the purified block copolymer.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If multi-step syntheses and non-scaleable processes are used for functionalization of caprolactones and lactides, then functionalized block copolymers can be produced, but the yields are poor and impurities are generated

Engineering Contradiction:

Improvefunctionalization processVSAvoidyield

Core Design Contradiction:

Ease of manufactureVSProductivity

Solution Approach 1:

The patent changes the physical parameters of the purification process by heating the solution to dissolve the crude block copolymer and then cooling it to precipitate the purified product. This temperature cycling enables effective separation of impurities while maintaining high yield and avoiding the need for multi-step syntheses

Inventive Principle:

Principle #35Parameter changes

Solution Approach 2:

The patent utilizes phase transition of the block copolymer between dissolved state (at elevated temperature) and precipitated state (at reduced temperature). This phase change mechanism allows for simple yet effective purification through heating and cooling cycles, eliminating complex multi-step synthesis procedures

Inventive Principle:

Principle #36Phase transitions

2Ease of manufacture

Engineering Contradiction:

Improvefunctionalization processVSAvoidpurity

Core Design Contradiction:

Ease of manufactureVSManufacturing precision

Solution Approach 1:

The patent extracts impurities from the crude block copolymer through selective dissolution and precipitation. The impurities remain in the solution phase while the purified block copolymer precipitates upon cooling, achieving effective separation and high purity without complex multi-step processes

Inventive Principle:

Principle #2Taking out (Extraction)

Solution Approach 2:

The patent uses an intermediary solvent system that enables selective dissolution of the crude block copolymer at elevated temperature. This intermediary medium facilitates the separation of impurities during the heating-cooling cycle, achieving high purity through a simple purification step

Inventive Principle:

Principle #24Intermediary (Mediator)

3Device complexity

If conventional purification methods are not used, then the process remains simple, but the amount of impurities in the block copolymer remains high

Engineering Contradiction:

Improvepurification processVSAvoidpurity

Core Design Contradiction:

Device complexityVSManufacturing precision

Solution Approach 1:

The patent employs a self-service purification mechanism where the block copolymer itself undergoes selective dissolution and precipitation. The material's own solubility characteristics at different temperatures drive the purification process, eliminating the need for complex external purification equipment or multi-step procedures

Inventive Principle:

Principle #25Self-service

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 method significantly reduces impurities in block copolymers while maintaining low polydispersity and controlled molecular weights, enhancing the purity and properties of the final polymer product.

Implementation Method 1

heating a solution containing a crude block copolymer and an alcohol

Methodology Applied

Scientific EffectHeating: Heating

Implementation Method 2

cooling the solution to promote precipitation

Methodology Applied

Scientific EffectCooling: Cooling

Implementation Method 3

cooling the solution to promote precipitation of a purified block copolymer

Methodology Applied

Scientific EffectPrecipitation: Precipitation

Data Source

PatentUS8952126B2Purification of functionalized triblock copolymers via methanol trituration

Publication Date: 2015.02.10 XEROX CORP

AI summary

A method of making a pure block copolymer includes forming a crude block copolymer; heating a solution of the crude block copolymer and alcohol; and cooling the solution to promote precipitation of a purified block copolymer, wherein an amount of impurities remaining in the purified block copolymer is from about 0 to about 5 wt % based on a total weight of the purified block copolymer; a ratio of a polydispersity index of the crude block copolymer to a polydispersity index of the purified block copolymer is from about 1.02 to about 1.25; a ratio of a molecular weight of the crude block copolymer to a molecular weight of the purified block copolymer is from about 0.75 to about 1.0; and a ratio of a number average molecular weight of the crude block copolymer to a number average molecular weight of the purified block copolymer is from about 0.65 to about 1.