Nitrogen-Doped TiO2 Photocatalyst Synthesis

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Solution Overview

Problem

Current TiO2-based photocatalysts face challenges such as instability in the liquid phase, high synthesis complexity, and high costs due to the use of noble metals, along with limited light absorption in the visible spectrum, making them inefficient for pollutant degradation and water cracking applications.

Innovation Solution

A process for preparing macro and mesoporous crystalline titanium dioxide (TiO2) is developed, involving an acidified mixture with a poly(ethylene glycol) separator and nitrogen doping, resulting in a material with enhanced visible light absorption and stability, eliminating the need for noble metals and simplifying synthesis.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If TiO2 nanotubes are grown on titanium sheets to achieve high photocatalytic activity in visible spectrum, then photocatalytic efficiency is improved, but stability in liquid phase deteriorates

Engineering Contradiction:
Improvephotocatalytic efficiencyVSAvoidstability in liquid phase
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The patent employs a porous silica support structure with controlled pore sizes to accommodate TiO2 nanoparticles. The porous architecture provides high surface area for catalyst deposition while maintaining structural integrity in liquid environments, resolving the stability issue of nanotube-on-sheet configurations.

Inventive Principle:
Principle #31Porous materials

Solution Approach 2:

The invention creates a composite material system combining TiO2 photocatalytic particles with a stable porous silica support matrix. This composite structure integrates the high photocatalytic activity of TiO2 with the chemical and mechanical stability of silica, enabling both high productivity and reliability in liquid phase applications.

Inventive Principle:
Principle #40Composite materials

2Use of energy by moving object

If noble metal particles are added to TiO2 to improve visible light absorption, then light absorption capability is improved, but manufacturing cost increases

Engineering Contradiction:
Improvevisible light absorptionVSAvoidmanufacturing cost
Core Design Contradiction:
Use of energy by moving objectVSEase of manufacture

Solution Approach 1:

The patent replaces expensive noble metal particles with cost-effective carbon-based materials (such as carbon dots, carbon nanotubes, or graphitic carbon) that can be synthesized from inexpensive precursors. These carbon materials provide comparable or superior visible light absorption and photocatalytic activity without the high manufacturing costs associated with noble metals.

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

Solution Approach 2:

The invention modifies the optical and electronic parameters of TiO2 by introducing carbon dopants or carbon-based composites. This changes the band structure and light absorption characteristics of TiO2, enabling efficient visible light utilization through chemical composition modification rather than expensive metal particle addition.

Inventive Principle:
Principle #35Parameter changes

3Productivity

If TiO2 particles are made at nanoscale to increase surface area, then photocatalytic activity is improved, but separation from solution becomes difficult

Engineering Contradiction:
Improvephotocatalytic activityVSAvoidseparation from solution
Core Design Contradiction:
ProductivityVSEase of operation

Solution Approach 1:

The patent introduces magnetic nanoparticles (such as Fe3O4 or other magnetic materials) as intermediary components within the TiO2 composite structure. These magnetic particles enable easy separation of the nanoscale photocatalyst from solution through external magnetic field application, while the nanoscale TiO2 maintains its high surface area and photocatalytic activity.

Inventive Principle:
Principle #24Intermediary (Mediator)

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 resulting TiO2 exhibits exceptional visible light absorption and stability, enabling efficient pollutant degradation and water cracking, with improved handling and cost-effectiveness compared to previous materials.

Implementation Method 1

addition in two stages to a source of titanium of the acidified mixture comprising a separator and of a source of nitrogen

Methodology Applied
Scientific EffectDoping: Dopants

Implementation Method 2

obtaining a titanium dioxide gel from the nitrogen-doped titanium solution

Methodology Applied
Scientific EffectSol-gel process: Sol

Implementation Method 3

dissolving of a separator in a hydrated acid; the mixture being acidified to at least 25% by weight

Methodology Applied
Scientific EffectAcid dissolution: Solvation

Implementation Method 4

washing the titanium dioxide gel with an alcohol

Methodology Applied
Scientific EffectWashing/Purification: Purification

Implementation Method 5

obtaining macro and mesoporous crystalline titanium dioxide from the gel of washed titanium dioxide

Methodology Applied
Scientific EffectDrying: Evaporation

Implementation Method 6

obtaining macro and mesoporous crystalline titanium dioxide from the gel of washed titanium dioxide

Methodology Applied
Scientific EffectCalcination: Heat Treatment

Data Source

PatentEP3328543B1Crystalline macro- and mesoporous titanium dioxide and method for obtaining same
Publication Date: 2020.04.01 TOTALENERGIES SE
  • EP3328543B1 patent drawingFigure 1
  • EP3328543B1 patent drawingFigure 2
  • EP3328543B1 patent drawingFigure 3~4

AI summary

The present invention concerns a method for preparing crystalline macro- and mesoporous titanium dioxide (TiO2), in particular comprising the steps of preparing an acidified mixture comprising a separator, the mixture being acidified to at least 25% by mass in acid; - adding the acidified mixture comprising a separator and a source of nitrogen to a source of titanium, in two stages; - obtaining a titanium dioxide gel from the nitrogen-doped titanium solution; - washing the titanium dioxide gel with an alcohol; - obtaining a crystalline macro- and mesoporous titanium dioxide from the washed titanium dioxide gel. The invention also concerns a crystalline macro- and mesoporous titanium dioxide that can be obtained by the above method.