Rutile Titanium Oxide Sol Synthesis via Hydrothermal Treatment

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

Existing methods for producing rutile titanium oxide sols face challenges such as impurity contamination, instability, and the need for solid-liquid separation, which affect the crystallinity and transparency of the final product.

Innovation Solution

A method involving the hydrothermal treatment of a titanium-containing aqueous solution with a tin salt, oxalic acid, and quaternary ammonium hydroxide, adjusting the molar ratios of tin, oxalic acid, and quaternary ammonium hydroxide to produce a single-phase rutile titanium oxide sol with a particle diameter of 5 nm to 100 nm, eliminating the need for solid-liquid separation and achieving high transparency.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Illumination intensity

If a solid phase method is used to produce rutile titanium oxide, then high refractive index is achieved, but particle diameter increases and transparency is impaired

Engineering Contradiction:
Improverefractive indexVSAvoidparticle diameter
Core Design Contradiction:
Illumination intensityVSLength of moving object

Solution Approach 1:

The patent employs hydrothermal treatment, a phase transition process involving heating an aqueous solution under pressure to form colloidal particles. This allows synthesis of rutile titanium oxide with controlled particle sizes (5-100 nm) that maintain both high refractive index and transparency, avoiding the particle growth issue of solid phase methods

Inventive Principle:
Principle #36Phase transitions

Solution Approach 2:

The patent controls particle diameter by adjusting hydrothermal treatment parameters (temperature, time, pH, precursor ratios) to produce fine particles in the 5-100 nm range. This parameter optimization enables simultaneous achievement of high refractive index and transparency by preventing excessive particle growth

Inventive Principle:
Principle #35Parameter changes

2Temperature

If existing wet methods are used to produce rutile titanium oxide sol, then low temperature synthesis is achieved, but impurities remain and solid-liquid separation is required

Engineering Contradiction:
Improvesynthesis temperatureVSAvoidpurity
Core Design Contradiction:
TemperatureVSManufacturing precision

Solution Approach 1:

The patent uses oxalic acid to selectively bind and remove impurity ions (such as alkali metals and tin) from the colloidal solution through complexation. This extraction process purifies the rutile titanium oxide sol without requiring solid-liquid separation, maintaining both low synthesis temperature and high purity

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

Oxalic acid acts as an intermediary agent that facilitates impurity removal by forming soluble complexes with impurity ions. This mediator enables purification in the liquid phase without needing filtration or centrifugation, achieving high purity while maintaining low temperature synthesis

Inventive Principle:
Principle #24Intermediary (Mediator)

3Temperature

If existing wet methods are used to produce rutile titanium oxide sol, then low temperature synthesis is achieved, but the process requires solid-liquid separation equipment

Engineering Contradiction:
Improvesynthesis temperatureVSAvoidprocess complexity
Core Design Contradiction:
TemperatureVSDevice complexity

Solution Approach 1:

The patent extracts impurities into solution phase using oxalic acid complexation, eliminating the need for solid-liquid separation equipment. The impurities remain dissolved in the aqueous phase while the purified rutile colloids stay dispersed, allowing direct filtration of the entire solution without intermediate separation steps

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent combines the purification function with the synthesis process itself. The oxalic acid treatment that removes impurities also stabilizes the colloidal particles, merging two separate operations (synthesis and purification) into one integrated process that eliminates equipment complexity

Inventive Principle:
Principle #5Merging (Combining)

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 a rutile titanium oxide sol with high transparency, refractive index, and improved stability, suitable for coating applications without impairing the base material's transparency, and exhibits excellent water, moisture, light, weather, heat, and wear resistance.

Implementation Method 1

performing hydrothermal treatment on the titanium-containing aqueous solution produced in the process (a) at 100°C to 200°C

Methodology Applied
Scientific EffectHydrothermal treatment:

Implementation Method 2

mixing a tin oxalate aqueous solution, a titanium alkoxide, oxalic acid, a quaternary ammonium hydroxide, and water

Methodology Applied
Scientific EffectHydrolysis: Hydrolysis

Data Source

PatentEP2676934B1Method for producing rutile-type titanium oxide sol
Publication Date: 2018.04.04 NISSAN CHEM CORP
  • EP2676934B1 patent drawing

AI summary

There is provided a method for efficiently producing a rutile titanium oxide sol that has excellent dispersibility, and has a particle diameter measured by dynamic light scattering of 5 nm to 100 nm. A method for producing a rutile titanium oxide sol having a particle diameter measured by dynamic light scattering of 5 nm to 100 nm, the method comprising: a process (a): mixing a tin oxalate aqueous solution, a titanium alkoxide, oxalic acid, a quaternary ammonium hydroxide, and water, while adjusting, per mole of titanium atoms, a proportion of tin atoms to be from 0.1 mol to 0.8 mol, a proportion of the oxalic acid to be from 0.01 mol to 5 mol, and a proportion of the quaternary ammonium hydroxide to be from 0.1 mol to 3.5 mol to prepare a titanium-containing aqueous solution having a concentration in terms of TiO2 of 0.1 % by mass to 15% by mass; and a process (b): performing hydrothermal treatment on the titanium-containing aqueous solution produced in the process (a) at 100°C to 200°C.