Silicone Microsphere Production via Ultrasonic Spray Pyrolysis

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Solution Overview

Problem

Current methods for synthesizing silicone microspheres, such as emulsion polymerizations, face challenges in producing stable, micron-sized, spherical particles due to the low surface energy of silicone oligomers, leading to coalescence and agglomeration, resulting in large, polydisperse microspheres with limited control over size and composition.

Innovation Solution

The method involves nebulizing a silicone precursor solution into an aerosol, which is then exposed to light energy or heat in a reaction zone, allowing for the formation of silicone microspheres with controlled size and composition, reducing coalescence and aggregation through the use of ultrasonic spray pyrolysis.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If emulsion polymerizations are used to synthesize silicone microspheres, then polymerization can proceed, but the microspheres become large, polydisperse with diameters from 50 microns to hundreds of microns and exhibit multimodal size distribution

Engineering Contradiction:
Improvemicrosphere size controlVSAvoidmicrosphere size distribution
Core Design Contradiction:
Manufacturing precisionVSQuantity of substance

Solution Approach 1:

The continuous polymerization process is segmented into discrete droplet units, where each droplet acts as an independent microreactor. This segmentation prevents coalescence and aggregation by isolating oligomers in separate droplets, resulting in monodisperse microspheres with controlled sizes ranging from 0.1 to 30 microns rather than the large polydisperse spheres (50-1000 microns) produced by conventional emulsion polymerization.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The invention changes the physical state and surface properties of silicone oligomers by dispersing them in a nebulized aerosol form. This parameter change from bulk liquid to aerosol droplets increases surface area and prevents coalescence, enabling precise control over microsphere size distribution and producing uniform particles instead of the multimodal distribution observed in emulsion polymerization.

Inventive Principle:
Principle #35Parameter changes

2Productivity

If conventional synthesis methods are used, then production can be achieved, but the methods are cumbersome with low production rates and produce only large microspheres greater than 100 microns to 1 mm in diameter

Engineering Contradiction:
Improveproduction rateVSAvoidmicrosphere diameter
Core Design Contradiction:
ProductivityVSLength of moving object

Solution Approach 1:

The invention replaces cumbersome mechanical methods (grinding, dipping, manual fabrication) with a spray pyrolysis system that uses nebulization and thermal processing. This substitution enables continuous high-rate production of microspheres in the 0.1-30 micron range, overcoming the low productivity and large size limitations of conventional mechanical synthesis methods.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The invention utilizes phase transitions of the solvent (evaporation from liquid to vapor) during spray pyrolysis to drive microsphere formation. As the nebulized droplets pass through the heated reaction zone, solvent evaporation concentrates the oligomers and initiates polymerization, enabling rapid production of small microspheres without the size constraints of conventional methods.

Inventive Principle:
Principle #36Phase transitions

3Reliability

If silicone oligomers are used in emulsion polymerizations, then polymerization can occur, but the low surface energy causes coalescence and agglomeration during the process

Engineering Contradiction:
Improvepolymerization stabilityVSAvoidmicrosphere dispersion stability
Core Design Contradiction:
ReliabilityVSStability of the object's composition

Solution Approach 1:

The invention introduces a carrier gas and nebulization system as intermediaries between the silicone oligomers and the polymerization environment. The oligomers are dispersed in a solvent-containing aerosol, which acts as a mediator preventing direct contact and coalescence of oligomer droplets. This intermediary system maintains dispersion stability throughout polymerization, eliminating the coalescence problem inherent in direct emulsion polymerization of low-surface-energy silicones.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The spray pyrolysis process creates an inert atmospheric environment where nebulized droplets are rapidly vaporized and polymerized before coalescence can occur. The brief residence time in the heated zone and rapid solvent evaporation create conditions that prevent agglomeration, maintaining composition stability despite the inherently low surface energy of silicone oligomers.

Inventive Principle:
Principle #39Inert atmosphere (Inert environment)

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 approach enables the production of silicone microspheres with narrow size distributions and controlled diameters ranging from 0.1 to 30 microns, facilitating the creation of various types, including magnetic, fluorescent, and core-shell particles, with improved versatility and control compared to conventional methods.

Implementation Method 1

Upon exposure of the droplets to the light energy and/or the heat energy, the solvent evaporates and the one or more oligomeric dimethylsiloxanes are polymerized

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 2

Upon exposure of the droplets to the light energy and/or the heat energy, the solvent evaporates and the one or more oligomeric dimethylsiloxanes are polymerized

Methodology Applied
Scientific EffectPhotopolymerization: Photopolymerisation

Implementation Method 3

the one or more oligomeric dimethylsiloxanes are polymerized

Methodology Applied
Scientific EffectPolymerization:

Data Source

PatentUS9914106B2Method of producing silicone microspheres
Publication Date: 2018.03.13 THE BOARD OF TRUSTEES OF THE UNIV OF ILLINOIS
  • US9914106B2 patent drawing
  • US9914106B2 patent drawing
  • US9914106B2 patent drawing

AI summary

A method of making silicone microspheres comprises nebulizing a silicone precursor solution comprising one or more oligomeric dimethylsiloxanes, a catalyst and a solvent into an aerosol comprising a plurality of droplets. Each droplet comprises the silicone precursor solution. The droplets are entrained in a gas which is flowed through a reaction zone comprising light energy and/or heat energy. Upon exposure of the droplets to the light energy and/or the heat energy, the solvent evaporates and the one or more oligomeric dimethylsiloxanes are polymerized. Thus, silicone microspheres are formed from the droplets of the aerosol.