Inorganic Aerogel Particle Preparation via Supercritical Spray Drying

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Solution Overview

Problem

Existing methods for preparing inorganic aerogels do not effectively merge the chemical gel formation step with the subsequent drying step, resulting in insufficient porosity and particle size in the final product.

Innovation Solution

A process involving spraying a composition suitable for forming an inorganic gel into supercritical carbon dioxide, followed by supercritical liquid extraction, where the ratio of spraying time to gelation time is controlled between 0.2 and 0.99, allowing for the production of aerogel particles with tailored particle characteristics, porosity, and pore size distribution.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If batch hydrolysis and condensation reactions are used to form gels, then gel formation occurs, but the resulting aerogels have insufficient porosity and particle size

Engineering Contradiction:
ImproveporosityVSAvoidgel formation process
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent replaces traditional batch chemical processing with a spray-drying system that uses fluid dynamics and mass transfer to achieve gel formation. The composition is sprayed into droplets that undergo rapid solvent exchange and gelation in the gas phase, eliminating the need for batch hydrolysis and condensation reactions while achieving superior porosity and particle size control

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

Solution Approach 2:

The patent changes the physical and chemical parameters of the system by controlling the spray droplet size, solvent composition, and environmental conditions during drying. By adjusting parameters such as spray temperature, humidity, and solvent volatility, the process achieves optimal porosity and particle characteristics that cannot be obtained through conventional batch methods

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If conventional drying methods are used after gel formation, then liquid removal occurs, but the aerogel structure collapses resulting in low porosity

Engineering Contradiction:
Improveaerogel structureVSAvoiddrying time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The patent performs preliminary action by forming the gel structure within the spray droplet before the drying process begins. The gelation occurs during the spray flight or immediately upon contact with the drying environment, creating a pre-formed network that resists collapse during subsequent solvent removal. This preliminary gel formation protects the aerogel structure while enabling rapid drying

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent combines gel formation and drying into a continuous spray-drying process rather than separate batch operations. The composition is sprayed as a continuous stream of droplets that simultaneously undergo solvent exchange and gelation, maintaining the aerogel structure throughout the process. This continuous action eliminates the need for prolonged drying times while preserving porosity

Inventive Principle:
Principle #20Continuity of useful action

3Manufacturing precision

If particle precipitation processes are used, then particles are formed, but the process complexity increases and particle size control is insufficient

Engineering Contradiction:
Improveparticle sizeVSAvoidprocess steps
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The spray-drying system performs multiple functions simultaneously: it atomizes the composition into droplets, provides rapid solvent exchange, induces gelation, and dries the particles all in one continuous process. This multi-functional approach replaces multiple separate unit operations required by conventional particle precipitation methods, reducing equipment complexity while achieving precise particle size control through spray parameter adjustment

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

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 highly porous and tailored aerogel particles with improved particle size and porosity, achieving high surface areas and pore volumes, suitable for applications such as thermal insulation and biomedical uses.

Implementation Method 1

spraying the composition (I) into supercritical carbon dioxide at a spraying time ts to obtain gel particles

Methodology Applied
Scientific EffectAnti-solvent effect: Supercritical Fluid

Implementation Method 2

drying the gel particles obtained in step (ii) by supercritical liquid extraction

Methodology Applied
Scientific EffectSupercritical liquid extraction: Supercritical Fluid Extraction

Data Source

PatentEP3221041B1Process for preparing a porous inorganic powder
Publication Date: 2020.02.26 BASF SE

AI summary

The present invention is directed to a process for preparing an inorganic aerogel, the process comprising the steps of providing a composition (I) suitable to form an inorganic gel with a gelation time tG, spraying the composition (I) into supercritical carbon dioxide at a spraying time ts to obtain gel particles, and drying the gel particles obtained in step (ii) by supercritical liquid extraction, wherein the ratio ts : tG is in the range of from 0.2 to 0.99. The present invention further is directed to the inorganic aerogel as such as well as the use of the inorganic aerogel according to the invention in particular for medical and pharmaceutical applications or for thermal insulation.