Chlorinated Alkane Purification via Segmented Synthesis

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Solution Overview

Problem

Current processes for producing high purity chlorinated alkane and alkene compounds face challenges due to impurity formation, which affects the yield and purity of fluorinated compounds, and require multiple steps and toxic starting materials, making them inefficient and environmentally harmful.

Innovation Solution

A process involving the chlorination of 1,1,1,3-tetrachloropropane to produce a mixture of 1,1,1,3,3-pentachloropropane and 1,1,1,2,3-pentachloropropane, followed by selective dehydrochlorination using a metal-containing catalyst, to achieve high purity 1,1,3,3-tetrachloropropene with controlled impurity profiles, reducing the need for toxic materials and simplifying production.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional multi-step processes are used to produce high purity chlorinated compounds, then purity can be achieved, but the process complexity and environmental harm increase due to toxic starting materials and multiple steps

Engineering Contradiction:
ImprovepurityVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The process segments the synthesis into two distinct stages: first producing a mixture of pentachloropropane isomers, then selectively dehydrochlorinating to obtain pure tetrachloropropene. This segmentation allows each stage to be optimized independently, reducing overall process complexity while maintaining high purity.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The method performs preliminary chlorination to produce a controlled mixture of pentachloropropane isomers before the final dehydrochlorination step. This preliminary action prepares the substrate in advance with the correct structural features needed for selective transformation, simplifying the subsequent purification process.

Inventive Principle:
Principle #10Preliminary action

2Productivity

If conventional processes are used, then fluorinated compounds can be produced, but impurity formation reduces yield and requires additional purification steps

Engineering Contradiction:
ImproveyieldVSAvoidimpurity formation
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The process changes key parameters including the ratio of starting materials (1,1,1,3,3-pentachloropropane to 1,1,1,2,3-pentachloropropane controlled between 3:7 to 7:3), temperature (50-150°C), and catalyst selection to achieve selective dehydrochlorination. These parameter optimizations maximize yield while minimizing impurity formation by favoring the desired reaction pathway.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

A metal-containing catalyst acts as an intermediary to facilitate selective dehydrochlorination of the pentachloropropane mixture. The catalyst mediates the reaction by lowering the activation energy for the desired transformation while being selective against side reactions, thereby improving both yield and purity.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Ease of manufacture

If selective dehydrochlorination is performed without metal catalysts, then the process is simpler, but the reaction efficiency and selectivity decrease

Engineering Contradiction:
Improveprocess simplicityVSAvoidreaction efficiency
Core Design Contradiction:
Ease of manufactureVSProductivity

Solution Approach 1:

Metal-containing catalysts serve as intermediaries that enable the dehydrochlorination reaction to proceed efficiently under milder conditions. The catalysts (such as Cu, Fe, Ni, Co, or their halides) mediate the bond breaking and forming processes, significantly improving reaction efficiency and selectivity compared to uncatalyzed thermal processes.

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

This process enables the production of highly pure chlorinated alkane isomers with controlled impurity profiles, simplifying the production of fluorinated compounds and reducing environmental impact by avoiding toxic starting materials and minimizing side reactions.

Implementation Method 1

subjecting the plurality of the resulting isomers stream to a selective dehydrochlorination step in which the first isomer is converted to 1,1,3,3-tetrachloropropene without the substantial dehydrochlorination of the second isomer, said selective dehydrochlorination being carried out in the liquid phase using a metal-containing catalyst

Methodology Applied
Scientific EffectCatalysis: Catalysis

Implementation Method 2

subjecting the reaction mixture to one or more distillation steps to produce a plurality of the resulting isomers stream, one or more single resulting isomer streams and optionally a 1,1,1,3-tetrachloropropane starting material stream

Methodology Applied
Scientific EffectDistillation: Distillation

Data Source

PatentEP3337777B1Process for producing c3 chlorinated alkane and alkene compounds
Publication Date: 2025.01.01 SPOLCHEMLE ZEBRA AS
  • EP3337777B1 patent drawingFigure 1~2
  • EP3337777B1 patent drawingFigure 3~4
  • EP3337777B1 patent drawingFigure 5~6

AI summary

A process for producing a reaction mixture comprising a plurality of C3 chlorinated alkane isomers comprising chlorinating a C3 chlorinated alkane starting material in a chlorination zone to produce the plurality of C3 chlorinated alkane isomers, the plurality of C3 chlorinated alkane isomers each having at least one more chlorine atom than the C3 chlorinated alkane starting material, wherein the concentration of the C3 chlorinated alkane starting material is controlled such that conversion of the C3 chlorinated alkane starting material to the plurality of C3 chlorinated alkane isomers, represented by the molar ratio of the C3 chlorinated alkane starting material : C3 chlorinated alkane isomers in the reaction mixture present in the chlorination zone, does not exceed about 40:60.