1,2,3,4-Tetrachlorohexafluorobutane Production via HF Solvent Fluorination

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Solution Overview

Problem

Current processes for producing 1,2,3,4-tetrachlorohexafluorobutane face challenges such as low yield due to side reactions, excessive fluorination, and the need for high reaction temperatures, which hinder industrial efficiency and product purity.

Innovation Solution

Reacting 1,2,3,4-tetrachlorobutane with fluorine in the presence of a solvent containing hydrogen fluoride, controlling reaction conditions like temperature and pressure, and using distillation and alkaline treatment to separate and refine the product.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If 1,2,3,4-tetrachlorobutane is reacted with fluorine in a liquid phase using conventional solvents, then the reaction can proceed, but side reactions occur and yield decreases due to C—C cleavage and excessive fluorination

Engineering Contradiction:
Improveyield of 1,2,3,4-tetrachlorohexafluorobutaneVSAvoidside reactions (C—C cleavage and excessive fluorination)
Core Design Contradiction:
ProductivityVSObject-generated harmful factors

Solution Approach 1:

The invention changes the chemical composition parameter of the solvent system by using hydrogen fluoride-containing solvents (such as HF-BF3 complex, HF-SbF5 complex, or mixtures with perfluorinated solvents) instead of conventional solvents. This parameter change modifies the reaction environment to suppress C—C bond cleavage and excessive fluorination, thereby reducing side reactions and improving yield.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention introduces hydrogen fluoride as an intermediary substance that mediates the fluorination reaction. Hydrogen fluoride acts as a catalyst and reaction medium that facilitates the controlled introduction of fluorine atoms while preventing uncontrolled C—C bond breaking and excessive fluorination, thus improving selectivity and yield.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Productivity

If high reaction temperature is used to maintain liquid phase reaction, then the reaction proceeds, but side reactions increase and product purity decreases

Engineering Contradiction:
Improvereaction rateVSAvoidproduct purity
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The invention changes the temperature parameter by conducting the reaction at lower temperatures (−50°C to +50°C, preferably −30°C to +20°C) compared to conventional high-temperature processes. This temperature reduction suppresses thermal side reactions and C—C cleavage while maintaining acceptable reaction rates through the catalytic effect of hydrogen fluoride-containing solvents.

Inventive Principle:
Principle #35Parameter changes

3Ease of manufacture

If conventional solvents are used for fluorination reaction, then the reaction can proceed, but solvent separation and recovery processes are required, increasing process complexity

Engineering Contradiction:
Improvesimplicity of processVSAvoidsolvent separation and recovery system
Core Design Contradiction:
Ease of manufactureVSDevice complexity

Solution Approach 1:

The invention applies the self-service principle by using 1,2,3,4-tetrachlorohexafluorobutane (the product itself) as the solvent for the fluorination reaction. This eliminates the need for separate solvent removal and recovery systems, as the product serves its own function as the reaction medium, thereby simplifying the overall process and reducing equipment complexity.

Inventive Principle:
Principle #25Self-service

4Device complexity

If product is used as solvent to avoid separation, then process simplification is achieved, but reverse reaction becomes more likely due to Gibbs free energy considerations

Engineering Contradiction:
Improvesolvent separation systemVSAvoidreaction direction control
Core Design Contradiction:
Device complexityVSReliability

Solution Approach 1:

The invention introduces hydrogen fluoride as a chemical intermediary that shifts the reaction equilibrium toward the product side. By using hydrogen fluoride-containing solvents, the reaction environment is modified to favor forward fluorination, suppressing the reverse reaction despite the product serving as the solvent medium.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The invention changes the chemical composition parameter of the reaction medium by incorporating hydrogen fluoride, which alters the thermodynamic parameters of the system. This composition change affects the Gibbs free energy landscape, making the forward reaction more favorable and suppressing reverse reactions even when the product acts as the solvent.

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 enhances the yield and purity of 1,2,3,4-tetrachlorohexafluorobutane, reduces side reactions, and allows for the economic and efficient production of the compound.

Implementation Method 1

reacting 1,2,3,4-tetrachlorobutane with fluorine in the presence of a solvent containing hydrogen fluoride

Methodology Applied
Scientific EffectCatalysis: Catalysis

Implementation Method 2

a reaction liquid containing 1,2,3,4-tetrachlorohexafluorobutane produced by reacting 1,2,3,4-tetrachlorobutane with fluorine in the presence of the solvent containing hydrogen fluoride is introduced into a distillation column to separate at least a part of 1,2,3,4-tetrachlorohexafluorobutane from the reaction liquid

Methodology Applied
Scientific EffectDistillation: Distillation

Implementation Method 3

the separated 1,2,3,4-tetrachlorohexafluorobutane is brought into contact with an alkaline substance and/or water

Methodology Applied
Scientific EffectNeutralization: Redox Reactions

Data Source

PatentUS8293955B2Production process for 1,2,3,4-tetrachlorohexafluorobutane and refining process
Publication Date: 2012.10.23 RESONAC CORP

AI summary

The production process for 1,2,3,4-tetrachlorohexafluorobutane of the present invention is characterized in that 1,2,3,4-tetrachlorobutane is reacted with fluorine in the presence of a solvent containing hydrogen fluoride. The 1,2,3,4-tetrachlorobutane may be obtained by chlorination of 3,4-dichlorobutene-1. Further, the present invention provides as well a process of refining 1,2,3,4-tetrachlorohexafluorobutane obtained in the manner described above. According to the present invention, 1,2,3,4-tetrachlorohexafluorobutane which is useful, for example, as a synthetic raw material for hexafluoro-1,3-butadiene used as an etching gas for semiconductors can industrially efficiently be produced by using 1,2,3,4-tetrachlorobutane which is a by-product of chloroprene and which has so far been disposed.