Titanium Oxide Fine Particles Hydrolysis Control

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Solution Overview

Problem

Conventional methods for producing titanium oxide fine particles with high purity and small primary particle diameter result in agglomerated particles with large diameters, leading to reduced transparency, UV-blocking ability, reactivity, and catalyst activity.

Innovation Solution

Controlling the pH and temperature ranges during the hydrolysis of titanium(oxy)chloride in an aqueous solvent, and conducting the hydrolysis in two steps, with the addition of titanium(oxy)chloride and an alkali, to produce titanium oxide fine particles with small primary and agglomerated particle diameters.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If titanium tetrachloride is hydrolyzed in a liquid phase using conventional methods, then high purity titanium oxide fine particles with small primary particle diameter can be produced, but the primary particles agglomerate to form agglomerated particles with large diameter

Engineering Contradiction:
Improveprimary particle diameterVSAvoidagglomerated particle diameter
Core Design Contradiction:
Manufacturing precisionVSLength of stationary object

Solution Approach 1:

The patent applies preliminary action by controlling the hydrolysis process conditions (pH 2-4, temperature 40-80°C, specific TiCl4 concentration) before agglomeration occurs. This preliminary control of hydrolysis parameters prevents excessive agglomeration during particle formation, resulting in smaller agglomerated particle diameters while maintaining high purity and fine primary particle sizes.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent employs parameter changes by systematically optimizing multiple hydrolysis parameters including pH (maintained at 2-4), temperature (40-80°C), titanium tetrachloride concentration (0.1-10%), and hydrolysis time. These parameter changes control the rate of particle formation and agglomeration, achieving smaller agglomerated particles without sacrificing primary particle fineness or purity.

Inventive Principle:
Principle #35Parameter changes

2Length of stationary object

If the agglomerated particle diameter is large, then the transparency and UV-blocking ability are reduced

Engineering Contradiction:
Improveagglomerated particle diameterVSAvoidtransparency and UV-blocking ability
Core Design Contradiction:
Length of stationary objectVSReliability

Solution Approach 1:

By changing the hydrolysis parameters (pH 2-4, temperature 40-80°C, controlled TiCl4 concentration), the patent achieves smaller agglomerated particle diameters that maintain good transparency and UV-blocking performance. The optimized parameters prevent excessive agglomeration that would otherwise scatter light and reduce these functional properties.

Inventive Principle:
Principle #35Parameter changes

3Length of stationary object

If the agglomerated particle diameter is large, then the reactivity with barium, lithium, or the like is reduced when producing titanium composite oxide

Engineering Contradiction:
Improveagglomerated particle diameterVSAvoidreactivity
Core Design Contradiction:
Length of stationary objectVSReliability

Solution Approach 1:

The patent applies preliminary action by controlling the hydrolysis process to form particles with optimal agglomeration characteristics before they are used in composite oxide production. The pre-controlled small agglomerated particle diameter (5-50 μm) ensures high reactivity with barium, lithium, and other metals during subsequent processing, while maintaining the handling advantages of fine particles.

Inventive Principle:
Principle #10Preliminary action

4Length of stationary object

If the agglomerated particle diameter is large, then dispersing and carrying a catalyst component on the titanium oxide fine particles is difficult

Engineering Contradiction:
Improveagglomerated particle diameterVSAvoiddispersibility
Core Design Contradiction:
Length of stationary objectVSEase of manufacture

Solution Approach 1:

The patent employs parameter changes in the hydrolysis process to achieve an optimal balance between particle size and dispersibility. By controlling pH, temperature, and concentration parameters, the resulting agglomerated particles have sufficient small diameter to allow easy dispersing and catalyst component carrying, while still maintaining the structural integrity needed for handling and processing.

Inventive Principle:
Principle #35Parameter changes

5Length of stationary object

If the agglomerated particle diameter is large, then the ability of adsorbing a component to be treated is reduced to decrease catalyst activity

Engineering Contradiction:
Improveagglomerated particle diameterVSAvoidadsorption ability and catalyst activity
Core Design Contradiction:
Length of stationary objectVSReliability

Solution Approach 1:

The patent employs parameter changes to optimize the hydrolysis conditions, achieving small agglomerated particle diameters that provide large specific surface areas. This increased surface area enhances the ability to adsorb treatment components and supports high catalyst activity, while the controlled agglomeration maintains particle stability and ease of handling.

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

The method produces titanium oxide fine particles with improved reactivity, dispersibility, and adsorption capabilities, making them suitable for catalyst carriers, photocatalysts, and composite oxides like barium and lithium titanates.

Implementation Method 1

conducting the hydrolysis of titanium(oxy)chloride in an aqueous solvent

Methodology Applied
Scientific EffectHydrolysis: Hydrolysis

Data Source

PatentEP3656740B1Method for producing titanium oxide fine particles
Publication Date: 2023.04.12 ISHIHARA SANGYO KAISHA LTD
  • EP3656740B1 patent drawingFigure 1~3
  • EP3656740B1 patent drawingFigure 4~6
  • EP3656740B1 patent drawingFigure 7~9

AI summary

Provided are: titanium oxide fine particles having small primary particle diameters and small agglomerated particle diameters; and a method for producing titanium oxide fine particles. The BET diameters of the titanium oxide fine particles are 1-50 nm; the agglomerated particle diameters thereof are 1-200 nm; and the (agglomerated particle diameter)/(BET diameter) ratio is 1-40. Titanium (oxy)chloride is hydrolyzed in an aqueous solvent, while controlling the pH range and the temperature range. Preferably, titanium (oxy)chloride is subjected to a primary hydrolysis in an aqueous solvent, and a secondary hydrolysis is subsequently carried out, while adding titanium (oxy)chloride thereto.