In Situ Complex Coacervation Spray Drying Microcapsules

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Solution Overview

Problem

Conventional complex coacervation microencapsulation processes are cumbersome, resource-intensive, and challenging to scale up industrially due to multiple steps requiring pH adjustments, chemical cross-linking, and the use of toxic agents, limiting their commercial application.

Innovation Solution

The development of an in situ complex coacervation process during spray drying, known as the CoCo process, which collapses these steps into a single spray drying step, eliminating the need for chemical crosslinking agents and allowing for the formation of dry microparticles, fibers, or films by controlling pH through volatile bases or acids, facilitating industrial scalability.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional complex coacervation process is used with multiple steps including pH adjustments, shell-hardening, and chemical cross-linking, then microcapsule formation is achieved, but the process becomes cumbersome, resource-intensive, and difficult to scale up industrially

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

Solution Approach 1:

The patent combines multiple separate process steps (emulsification, coacervation, shell-hardening, and drying) into a single integrated spray drying step. The feed solution containing both polymers and cargo is atomized directly, and complex coacervation occurs in situ during the spray drying process, eliminating the need for separate handling steps and chemical crosslinking agents.

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The spray drying process serves multiple functions simultaneously: it acts as the emulsification step, the coacervation step, the shell-hardening step, and the drying step all in one operation. This multi-functional approach simplifies the overall process while maintaining microcapsule formation effectiveness.

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

2Strength

If chemical crosslinking agents are used to stabilize polymer associations, then shell hardening is achieved, but toxic agents such as formaldehyde or glutaraldehyde must be used which are incompatible with food systems

Engineering Contradiction:
Improveshell stabilityVSAvoidtoxicity
Core Design Contradiction:
StrengthVSObject-affected harmful factors

Solution Approach 1:

The patent converts the naturally occurring electrostatic attraction between oppositely charged polymers into a stabilizing force that eliminates the need for toxic chemical crosslinking agents. By controlling pH to induce charge reversal in one polymer, the process harnesses electrostatic forces to stabilize the microcapsule shell without introducing harmful chemicals.

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

Solution Approach 2:

The polymers themselves provide the stabilization mechanism through their inherent electrostatic interactions. The system uses the polymers' own charge properties to stabilize the microcapsule structure, eliminating the need for external crosslinking agents and making the process suitable for food applications.

Inventive Principle:
Principle #25Self-service

3Reliability

If conventional complex coacervation process with separate emulsification, coacervation, and drying steps is used, then microcapsule formation is achieved, but the process is time-consuming and not suitable for high-throughput production

Engineering Contradiction:
Improvemicrocapsule formationVSAvoidproduction throughput
Core Design Contradiction:
ReliabilityVSProductivity

Solution Approach 1:

The patent merges sequential process steps into a single concurrent operation. Spray drying simultaneously performs atomization, evaporation, and in situ complex coacervation, transforming a multi-step sequential process into a single high-throughput operation that can continuously produce microcapsules at industrial scales.

Inventive Principle:
Principle #5Merging (Combining)

4Stability of the object's composition

If multiple pH adjustments and incubation periods are performed in conventional complex coacervation, then proper polymer association is achieved, but the process requires precise adjustment of pH, concentrations and temperature taking hours to complete

Engineering Contradiction:
Improvepolymer associationVSAvoidprocess time
Core Design Contradiction:
Stability of the object's compositionVSLoss of time

Solution Approach 1:

The patent prepares the feed solution with pre-selected polymer concentrations and pH conditions optimized for in situ coacervation during spray drying. The volatile base is incorporated in advance, and upon atomization, the rapid pH change triggers immediate polymer association, eliminating the need for prolonged incubation periods and repeated pH adjustments.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent utilizes the phase transition of the volatile base (from liquid to vapor) during spray drying to drive the pH change that triggers polymer association. This phase transition provides a rapid, controlled mechanism for initiating coacervation without requiring gradual pH adjustments or extended incubation times.

Inventive Principle:
Principle #36Phase transitions

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 achieves efficient, energy-saving, and high-throughput microencapsulation with controlled release profiles and reduced toxicity, as demonstrated by up to 83% retention of d-limonene during encapsulation and stability over 72 days, with controllable particle sizes and pH-sensitive release properties.

Implementation Method 1

Complex Coacervation is a polymer phase separation process brought about by dissolving two ionic polymers in water at a pH where both polymers have the same charge (e.g., both are negatively charged) and then causing phase separation by dropping the pH so that one polymer maintains its negative charge, but the second polymer undergoes a charge reversal and becomes positively charged. The driving force for phase separation (complex coacervation) is electrostatic attraction.

Methodology Applied
Scientific EffectComplex coacervation: Coacervate

Implementation Method 2

The driving force for phase separation (complex coacervation) is electrostatic attraction.

Methodology Applied
Scientific EffectElectrostatic attraction: Electrostatics

Implementation Method 3

Spray-drying is an industrially ubiquitous unit operation; enabling complex coacervation by spray drying makes this process commercially feasible.

Methodology Applied
Scientific EffectEvaporation: Evaporation

Data Source

PatentUS11612870B2Microencapsulation of chemicals and bioactives by in situ complex coacervation during spray drying
Publication Date: 2023.03.28 RGT UNIV OF CALIFORNIA
  • US11612870B2 patent drawing
  • US11612870B2 patent drawing
  • US11612870B2 patent drawing

AI summary

An industrially scalable microcapsule, fiber or film forming process and formulations suitable for use in conventional spray drying systems are provided. The one-step spray drying process utilizes formulations of a first ionic polymer, a second ionic polymer with an isoelectric point (pI2) or acid dissociation constant (pKa2) that is greater than the isoelectric point (pI1) or acid dissociation constant (pKa1) of the first ionic polymer and a volatile base or volatile acid. Volatilization of the volatile base or acid of the spray formulation changes the pH of the solution and changes the charge of the second ionic polymer initiating electrostatic interactions with the first ionic polymer through complex coacervation. Microcapsules formed by the complex coacervation process can stabilize bioactive components as well as control the release of the bioactive components for a variety of applications.