Stereocomplex PLA Particle Formation via Twin-Screw Extrusion

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Solution Overview

Problem

Current methods for manufacturing stereocomplex polylactic acid (sc-PLA) particles are inefficient and costly, particularly due to the use of supercritical fluids, and lack scalability for industrial production, with a need for a process that can produce particles with a mean volume diameter below 1 mm in commercially available equipment.

Innovation Solution

A process involving extruding a melt comprising 30-70 wt.% PDLA and 70-30 wt.% PLLA through an sc-PLA formation zone in a twin-screw extruder, operated at temperatures above the melting point of PDLA and PLLA but below 220°C, followed by a finishing zone at temperatures below 160°C, without a die head, to produce stereocomplex particles with a mean volume diameter below 0.75 mm.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If supercritical fluid is used to manufacture sc-PLA particles, then stereocomplex formation is increased, but process complexity and investment cost increase

Engineering Contradiction:
Improvestereocomplex formationVSAvoidprocess complexity
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The invention removes the supercritical fluid component from the process entirely, extracting only the essential function of achieving stereocomplex formation through simpler means - specifically through controlled melt mixing and crystallization in a twin-screw extruder without requiring supercritical CO2 or other complex fluid systems

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The invention replaces expensive, complex supercritical fluid equipment with standard, readily available extrusion equipment that is already widely used in the polymer industry, significantly reducing investment costs while maintaining production capability

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

2Reliability

If supercritical fluid is used to manufacture sc-PLA particles, then stereocomplex formation is increased, but investment cost increases

Engineering Contradiction:
Improvestereocomplex formationVSAvoidinvestment cost
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The invention replaces expensive, complex supercritical fluid equipment with standard, readily available extrusion equipment that is already widely used in the polymer industry, significantly reducing investment costs while maintaining production capability

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

Solution Approach 2:

The invention uses a twin-screw extruder, which is a multi-functional piece of equipment already standard in polymer processing, to perform multiple functions including mixing, heating, extruding, and particle formation, eliminating the need for specialized supercritical fluid equipment

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

3Ease of manufacture

If conventional extrusion method is used, then process simplicity is maintained, but particle size reduction below 1 mm is difficult

Engineering Contradiction:
Improveprocess simplicityVSAvoidparticle size
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The invention changes the temperature parameters during extrusion - specifically maintaining the barrel temperature above the melting point of PDLA and PLLA but below 220°C, and the finishing zone below 160°C - to enable spontaneous particle size reduction to below 0.75 mm through controlled crystallization

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention performs preliminary mixing of PDLA and PLLA in the melt state before extrusion, ensuring homogeneous distribution of the two polymers, which facilitates uniform particle formation and size reduction during the extrusion process

Inventive Principle:
Principle #10Preliminary action

4Manufacturing precision

If multiple processing steps are used to produce sc-PLA particles, then particle quality is improved, but production time increases

Engineering Contradiction:
Improveparticle qualityVSAvoidproduction time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The invention combines multiple processing steps - mixing, melting, extrusion, and particle formation - into a single continuous extrusion process, eliminating the need for separate grinding or size reduction steps and enabling single-step conversion of polymer pellets to sub-millimeter particles

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The invention employs continuous extrusion processing where the melt is continuously formed, extruded, and solidified into particles without interruption, maintaining continuous production flow and eliminating downtime between processing steps

Inventive Principle:
Principle #20Continuity of useful action

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 efficient and continuous production of high-quality sc-PLA particles with a mean volume diameter below 0.75 mm, eliminating the need for a grinding step and allowing for single-step conversion of polymer pellets to free-flowing sub-millimeter-sized powder, suitable for industrial-scale production.

Implementation Method 1

extruding a melt comprising 30-70 wt. % of PDLA and 70-30 wt. % of PLLA through an sc-PLA formation zone in a twin-screw extruder

Methodology Applied
Scientific EffectShear stress: Shear Stress

Implementation Method 2

operated at a barrel temperature of above the melting temperature of the PDLA and PLLA and below 220° C.

Methodology Applied
Scientific EffectMelting: Melting

Implementation Method 3

the sc-PLA formation zone is operated at a barrel temperature of above the melting temperature of the PDLA and PLLA and below 220° C.

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 4

the finishing zone is operated at a barrel temperature below 160° C.

Methodology Applied
Scientific EffectCooling: Cooling

Implementation Method 5

Upon proper mixing of PLLA and PDLA, co-crystallization can result in a specific racemic crystal type called stereocomplex polylactic acid (sc-PLA)

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentUS12024627B2Process for manufacturing particles comprising polylactic acid
Publication Date: 2024.07.02 PURAC BIOCHEM BV

AI summary

A process for manufacturing particles including a stereocomplex of poly-D-lactide (PDLA) and poly-L-lactide (PLLA), including the steps of: extruding a melt including 30-70 wt. % of PDLA and 70-30 wt. % of PLLA through an sc-PLA formation zone in a twin-screw extruder, wherein the formation zone is operated at a barrel temperature above the melting temperature of the PDLA and PLLA and below 220° C.; wherein the sc-PLA formation zone is followed by a finishing zone which is operated at a barrel temperature below 160° C.; wherein the finishing zone is followed by the end of the extruder which has a die-head resistance of 0; and recovering solid stereocomplex particles from the end of the extruder. The stereocomplex particles find use in various applications, e.g., in fracking fluids, as filler, as nucleating agent, in particular in the molding of semi-crystalline PLA, or as a starting material for the manufacture of sc-PLA products.