Alkaline-Earth Fluoride Nanoparticle Synthesis via Charge Transfer Complex

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Solution Overview

Problem

Current processes for producing alkaline-earth element fluoride nanoparticles are hindered by the use of toxic and corrosive anhydrous hydrogen fluoride, slow reaction times, and the need for hazardous handling and treatment of gaseous effluents, while also requiring the use of organic solvents that can contaminate the final product, making them unsuitable for industrial-scale production and medical applications.

Innovation Solution

A process involving the reaction of an alkaline-earth element salt with a charge transfer complex, using non-toxic solvents like water or ethanol, to produce colloidal suspensions of functionalized nanoparticles with controlled size and stability, eliminating the need for anhydrous hydrogen fluoride and enabling safer, faster, and more efficient production.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If anhydrous hydrogen fluoride is used to produce fluoride nanoparticles, then the reaction can proceed, but the process becomes hazardous and requires special handling equipment

Engineering Contradiction:
Improveease of manufactureVSAvoidharmful factors
Core Design Contradiction:
Ease of manufactureVSObject-affected harmful factors

Solution Approach 1:

The patent uses ammonium bifluoride as an intermediary substance to deliver fluoride ions without requiring anhydrous HF gas. The ammonium bifluoride decomposes in situ to release fluoride, acting as a safe mediator that eliminates the need for handling toxic gaseous HF while maintaining the chemical reaction pathway.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The invention changes the physical and chemical parameters of the fluoride source from gaseous anhydrous HF to solid ammonium bifluoride dissolved in aqueous or alcoholic solution. This parameter change transforms the process from hazardous to safe, while also enabling standard laboratory equipment to be used instead of specialized corrosion-resistant equipment.

Inventive Principle:
Principle #35Parameter changes

2Productivity

If the reaction is conducted with anhydrous hydrogen fluoride, then fluoride nanoparticles can be synthesized, but the reaction time becomes excessively long

Engineering Contradiction:
ImproveproductivityVSAvoidloss of time
Core Design Contradiction:
ProductivityVSLoss of time

Solution Approach 1:

The patent changes the reaction medium from anhydrous conditions to aqueous or alcoholic solutions, and modifies the fluoride source to ammonium bifluoride. These parameter changes dramatically accelerate the reaction rate, reducing synthesis time from days to hours or minutes, thereby improving productivity without sacrificing product quality.

Inventive Principle:
Principle #35Parameter changes

3Ease of manufacture

If organic solvents are used in the synthesis process, then the reaction can proceed, but the final product becomes contaminated with organic residues

Engineering Contradiction:
Improveease of manufactureVSAvoidpurity of product
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The invention changes the solvent system to aqueous or alcoholic solutions that can be easily removed by evaporation or drying, leaving no harmful organic residues. The use of water or ethanol as solvents, combined with the decomposition of ammonium bifluoride, enables the production of high-purity fluoride nanoparticles suitable for medical and optical applications.

Inventive Principle:
Principle #35Parameter changes

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 allows for the direct production of stable, functionalized alkaline-earth element fluoride nanoparticles with sizes less than 100 nm, achieving high dry extract concentrations and ensuring chemical purity, stability, and safety, making them suitable for industrial-scale production and medical applications such as dental treatments.

Implementation Method 1

the reaction of an alkaline-earth element salt with a charge transfer complex

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

produce colloidal suspensions of functionalized nanoparticles

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Implementation Method 3

colloidal suspensions of functionalized alkaline-earth element fluoride nanoparticles

Methodology Applied
Scientific EffectColloidal suspension: Colloid

Implementation Method 4

dispersing the functionalized or non-functionalized alkaline-earth element fluoride nanoparticles

Methodology Applied
Scientific EffectDispersion: Dispersion (of waves)

Data Source

PatentEP3538258B1Colloidal suspension of functionalised nanoparticles of a fluoride of an alkaline-earth element
Publication Date: 2021.08.04 MATHYM
  • EP3538258B1 patent drawingFigure 1a~2a
  • EP3538258B1 patent drawingFigure 2b~6a
  • EP3538258B1 patent drawingFigure 6b~7b

AI summary

The invention relates to a method for preparing a colloidal suspension of functionalised nanoparticles of a fluoride of an alkaline-earth element, which comprises the following steps: preparing a corresponding alkaline-earth element salt solution; preparing a solution of a charge-transfer complex of formula (I) (formula I) by reacting an amide of formula (II) with a source of fluoride ions, wherein: Ra and Rb, identical or different, are a 5- or 6-member (C1-C6)alkyl, (C3-C7)cycloalkyl, phenyl or heterocycloalkyl group, or else Ra and Rb are connected to one another and form an alkylene chain, comprising 2 to 6 carbon atoms, and Rc is a hydrogen atom or a 5- or 6-member (C1-C6)alkyl, (C3-C7)cycloalkyl, phenyl or heterocycloalkyl group, or else Rb and Rc are connected to one another and form an alkylene chain, comprising 2 to 5 carbon atoms; placing the corresponding alkaline-earth element salt solution and the solution of the charge-transfer complex of formula (I) in contact in a solvent or mixture of solvents; reacting the mixture obtained in step (c), optionally by heating, so as to obtain a colloidal suspension of nanoparticles of a fluoride of an alkaline-earth element.