Spray Drying Synthesis of Nano CaCO3 Particles

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Solution Overview

Problem

Existing methods for synthesizing nanometric calcium carbonate particles often require high temperatures, hazardous chemical reactants, and surfactants, making them energy-intensive, unsafe, and difficult to scale up, while also resulting in contamination that complicates applications requiring pure particles.

Innovation Solution

A synthesis method using a Spray Dryer to control temperature, air humidity, and reactants flow, mixing stoichiometric ratios of NaHCO3 and CaCl2 solutions without surfactants, allowing for the production of pure calcium carbonate nanoparticles with controlled dimensions and form, using a spray dryer to atomize the solutions in a hot air flow and subsequent washing to remove byproducts.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Temperature

If conventional precipitation methods are used to synthesize calcium carbonate particles, then particle formation is achieved, but high temperatures (1000-1100°C) and hazardous chemical reactants are required

Engineering Contradiction:
Improvesynthesis temperatureVSAvoidenergy consumption and safety risks
Core Design Contradiction:
TemperatureVSObject-affected harmful factors

Solution Approach 1:

The invention changes the synthesis temperature parameter from conventional high temperatures (1000-1100°C) to a much lower range (20-100°C), and modifies the chemical environment by using ammonium carbonate instead of hazardous reactants like ammonium chloride and sodium carbonate. This parameter change resolves the contradiction by achieving particle formation at lower temperatures with safer chemicals.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention uses readily available, inexpensive materials such as ammonium carbonate, calcium chloride, and sodium bicarbonate that can be easily handled and disposed of, replacing expensive and hazardous materials. This principle addresses both the temperature and safety concerns by using benign, low-cost reactants.

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

2Stability of the object's composition

If surfactants are used to stabilize the mixture and reaction product, then particle stability is improved, but product purity is reduced due to contamination

Engineering Contradiction:
Improvemixture stabilityVSAvoidproduct purity
Core Design Contradiction:
Stability of the object's compositionVSLoss of substance

Solution Approach 1:

The invention uses ammonium carbonate as an intermediary substance that provides temporary stabilization during the reaction process without requiring persistent surfactant coverage. The ammonium carbonate decomposes to provide CO2 for carbonation while maintaining mixture stability, and its decomposition products are harmless, thus achieving both stability and purity.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The invention extracts or eliminates the need for traditional surfactants from the system by using the unique properties of ammonium carbonate and the spray drying process to achieve particle formation and stabilization without hydrophobic contaminants, thereby maintaining product purity.

Inventive Principle:
Principle #2Taking out (Extraction)

3Manufacturing precision

If laboratory synthesis methods with fine control of reaction conditions are used, then particle quality is improved, but scalability to large production is difficult

Engineering Contradiction:
Improveparticle dimension controlVSAvoidproduction scalability
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The invention replaces complex mechanical mixing and control systems with a spray drying process where atomization and rapid evaporation provide inherent mixing and uniformity. This substitution allows precise particle control through spray parameters rather than complex mechanical agitation, enabling easy scale-up.

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

Solution Approach 2:

The invention performs preliminary preparation of reactant solutions with precise stoichiometric ratios before the main reaction, and uses the spray drying process to immediately convert the reaction mixture into dry particles. This preliminary action with pre-mixed solutions followed by rapid processing enables both precision and scalability.

Inventive Principle:
Principle #10Preliminary action

4Manufacturing precision

If high shear mixing is used to prepare calcium carbonate particles, then particle formation is achieved, but energy consumption increases

Engineering Contradiction:
Improveparticle formationVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by moving object

Solution Approach 1:

The invention uses pneumatic spray atomization to replace mechanical high-shear mixing. The reactant solution is atomized into fine droplets using compressed air or gas flow, and the rapid evaporation and carbonation occur in the gas phase. This pneumatic approach achieves particle formation with much lower energy input compared to mechanical high-shear mixing.

Inventive Principle:
Principle #29Pneumatics and hydraulics

Solution Approach 2:

The invention exploits the phase transition from liquid to gas (evaporation of water) and from dissolved ions to solid precipitate (carbonation) to drive particle formation. The spray drying process uses heat to evaporate water, concentrating the reactants and triggering rapid carbonation, thereby achieving particle formation through phase changes rather than mechanical energy input.

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 method enables the production of pure, stable nanometric calcium carbonate particles without surfactants, reducing energy consumption and safety risks, and allows for scalable production with controlled particle dimensions and zeta potential, suitable for various industrial applications including biomedical uses.

Implementation Method 1

atomized in a hot air flow... The high temperature causes a rapid evaporation of the reaction mixture water

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 2

atomized in a hot air flow indicatively between 100 and 180°C temperature

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 3

The two solutions are then mixed and atomized in a hot air flow... the direct production of calcium carbonate in powder and of sodium chloride

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Data Source

PatentEP2796412B1Synthesis of nano-sized CaCO3 particles by spray dryer
Publication Date: 2021.05.12 UNIV DEL SALENTO
  • EP2796412B1 patent drawingFigure 1~2
  • EP2796412B1 patent drawingFigure 4~3
  • EP2796412B1 patent drawingFigure 6~7

AI summary

Method for preparing calcium carbonate comprising the steps of mixing an aqueous solution of NaHCO3 and an aqueous solution of CaCl2, then atomizing them in a pre-heated air flow, thereby obtaining calcium carbonate in powder form and sodium chloride. The calcium carbonate obtained comprises nanoparticles smaller than 200 nm.