Fluorination Catalyst Regeneration Using Nitrogen Trifluoride

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Solution Overview

Problem

Existing methods for activating and reactivating metal oxide-based fluorination catalysts used in fluorinating substrates like chlorinated compounds with hydrogen fluoride face issues such as catalyst deactivation due to water by-products, corrosion, and reduced catalyst life, necessitating the development of more effective activation and regeneration procedures that avoid water generation.

Innovation Solution

The use of nitrogen trifluoride (NF3) as a source of reactive fluorine to activate and reactivate metal oxide-based fluorination catalysts, either in situ or ex situ, in conjunction with other substances like HF, HCl, or chlorocarbons, to restore catalytic activity without producing water.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If oxygen is co-fed continuously or intermittently during fluorination reaction or reactivation to oxidize and remove carbonaceous deposits, then catalyst activity is maintained, but water and carbon dioxide are produced as by-products that damage and deactivate the catalyst

Engineering Contradiction:
Improvecatalyst activityVSAvoidwater by-product
Core Design Contradiction:
ReliabilityVSObject-generated harmful factors

Solution Approach 1:

The invention changes the chemical parameters of the reactivation process by replacing oxygen with nitrogen trifluoride (NF3) as the reactivating agent. This parameter change transforms the reaction chemistry from oxidation to fluorination, eliminating water production while maintaining catalyst activity through fluorine-based regeneration of the catalyst surface.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

Nitrogen trifluoride serves as an intermediary substance that mediates the reactivation process. Instead of using oxygen that produces harmful water by-products, NF3 acts as a fluorine source that regenerates the catalyst without generating damaging substances, thus mediating between the need for reactivation and the avoidance of water-induced deactivation.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Reliability

If oxygen is used to remove carbonaceous deposits from catalyst surface, then catalyst activity is restored, but corrosion or erosion of fluorination equipment occurs due to water presence

Engineering Contradiction:
Improvecatalyst activityVSAvoidequipment corrosion
Core Design Contradiction:
ReliabilityVSObject-affected harmful factors

Solution Approach 1:

The invention changes the chemical environment parameter by substituting oxygen-based reactivation with nitrogen trifluoride-based reactivation. This eliminates the formation of water that causes corrosion, while still achieving catalyst regeneration through fluorine incorporation into the catalyst structure.

Inventive Principle:
Principle #35Parameter changes

3Reliability

If traditional activation methods are used to prepare fluorination catalysts, then catalyst is activated, but water is generated that damages and deactivates the catalyst due to phase changes

Engineering Contradiction:
Improvecatalyst activationVSAvoidcatalyst life
Core Design Contradiction:
ReliabilityVSDuration of action of stationary object

Solution Approach 1:

The invention fundamentally changes the activation process parameters by using nitrogen trifluoride instead of water-based or oxygen-based activation methods. This parameter change eliminates water generation during activation, preventing the phase change-induced damage that shortens catalyst life, while still achieving the necessary activation of the catalyst for fluorination reactions.

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

NF3 effectively reactivates spent catalysts, maintaining or exceeding initial fluorination efficiency by reacting with the catalysts at controlled temperatures, thereby extending their useful life and preventing corrosion, while avoiding the drawbacks of water-based activation methods.

Implementation Method 1

contacting the spent or depleted fluorination catalyst with an agent that is a source of reactive fluorine comprising NF3

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

The fluorination catalyst has been used to catalyze the fluorination of a chlorinated compound such as a chloroolefin or chloroalkane using HF

Methodology Applied
Scientific EffectCatalysis: Catalysis

Data Source

PatentEP2950926B1Activation and regeneration of fluorination catalysts
Publication Date: 2020.02.19 ARKEMA INC

AI summary

A fluorination catalyst such as a chromium oxide-based fluorination catalyst may be activated or reactivated by contacting the catalyst. with a source of reactive fluorine, for example nitrogen trifluoride (NF3) or fluorine (F2). Fluorinated compounds may be prepared by the gas phase reaction of hydrogen fluoride (HF) with various substrates such as chlorinated compounds. A number of metal oxide-based catalysts have been developed for this purpose.