High-χ Diblock Copolymer Purification via Selective Precipitation

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Solution Overview

Problem

Current methods for preparing high-X diblock copolymers are inefficient in removing homopolymer contaminants, leading to impurities that hinder their use in directed self-assembly applications, which require high purity and precise control of composition.

Innovation Solution

A process involving the formation of micelles in a solvent mixture containing diblock copolymers and homopolymers, followed by micellar aggregation and separation, allows for the isolation of pure diblock copolymers with specific molecular weights and compositions, ensuring less than 5 wt% homopolymer contamination.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If complex purification procedures are used to remove homopolymer contaminants, then purity of diblock copolymer is improved, but process complexity and time consumption increase

Engineering Contradiction:
Improvepurity of diblock copolymerVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent utilizes selective precipitation through solvent addition, which induces phase separation between the diblock copolymer and homopolymer contaminants. By adding a non-solvent to the polymer solution, the diblock copolymer precipitates while homopolymers remain in solution, enabling efficient separation without complex equipment or multiple purification steps.

Inventive Principle:
Principle #36Phase transitions

Solution Approach 2:

The patent extracts homopolymer contaminants from the diblock copolymer mixture by selective dissolution. The homopolymers are selectively dissolved in the solvent system, allowing them to be separated from the precipitated diblock copolymer, thereby achieving high purity through a simple extraction-based purification process.

Inventive Principle:
Principle #2Taking out (Extraction)

2Manufacturing precision

If multiple purification steps are implemented to achieve high purity, then homopolymer contamination is reduced, but yield and production efficiency decrease

Engineering Contradiction:
Improvepurity of diblock copolymerVSAvoidyield of diblock copolymer
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The single-step selective precipitation method achieves both high purity and high yield by utilizing phase separation. The diblock copolymer selectively precipitates while homopolymers remain dissolved, allowing for complete separation in one step without the need for repeated purification that would cause material loss and reduce overall yield.

Inventive Principle:
Principle #36Phase transitions

3Loss of time

If conventional purification methods are used, then processing time is reduced, but purity and composition control are insufficient

Engineering Contradiction:
Improvepurification timeVSAvoidcomposition control
Core Design Contradiction:
Loss of timeVSManufacturing precision

Solution Approach 1:

The patent achieves rapid purification with excellent composition control through selective precipitation. By carefully controlling the solvent composition and addition rate, the method enables fast separation while maintaining precise control over the purity and molecular weight distribution of the recovered diblock copolymer, outperforming conventional methods in both speed and precision.

Inventive Principle:
Principle #36Phase transitions

Data Source

PatentUS9169383B2Preparation, purification and use of high-X diblock copolymers
Publication Date: 2015.10.27 DUPONT ELECTRONICS INC
  • US9169383B2 patent drawing
  • US9169383B2 patent drawing
  • US9169383B2 patent drawing

AI summary

This invention relates to the preparation and purification of high-X (“chi”) diblock copolymers. Such copolymers contain two segments (“blocks”) of polymers with significantly different interaction parameters and can be used in directed self-assembly applications.