Aspirating Agitator for Chlorinated Propane Synthesis

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

There is a need to improve the synthetic techniques for producing 1,1,1,3-tetrachloropropane, an important halogenated propane, as existing methods may not be efficient or effective in achieving high yields and product purity.

Innovation Solution

The process involves reacting carbon tetrachloride with ethylene in a tank reactor with an aspirating agitator, which transfers ethylene from the headspace back into the reaction mixture, and using an iron-based catalyst delivered through a continuously stirred slurry loop. Additionally, the chlorinated propane product is removed from a still zone within the reactor, and the crude product stream is purified using a distillation technique with a forced circulation reboiler to prevent fouling.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Object-affected harmful factors

If ethylene is fed as vapor through a dip tube or sponge-type gas diffuser, then polyvinyl chloride formation is reduced, but reaction efficiency and contact between reactants is insufficient

Engineering Contradiction:
Improvepolyvinyl chloride formationVSAvoidreaction efficiency
Core Design Contradiction:
Object-affected harmful factorsVSProductivity

Solution Approach 1:

The patent introduces an aspirating agitator as an intermediary device that uses a gas stream to actively transfer ethylene from the headspace back into the reaction mixture. This mediator enables efficient mass transfer without direct gas-liquid contact issues that cause polyvinyl chloride formation, thereby resolving the contradiction between reducing harmful byproducts and maintaining high reaction efficiency.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The aspirating agitator creates periodic circulation patterns where ethylene is continuously drawn from the headspace and reintroduced into the liquid phase. This periodic action ensures consistent reactant contact and maintains high reaction efficiency while preventing the continuous gas flow issues that lead to polyvinyl chloride formation.

Inventive Principle:
Principle #19Periodic action

2Productivity

If the reactor is agitated to provide adequate contact between liquid reactants and metallic iron surface, then reaction efficiency improves, but polyvinyl chloride formation increases

Engineering Contradiction:
Improvereaction efficiencyVSAvoidpolyvinyl chloride formation
Core Design Contradiction:
ProductivityVSObject-affected harmful factors

Solution Approach 1:

The patent segments the reactor into distinct zones: a liquid reaction mixture zone with controlled agitation for catalyst contact, and a vapor headspace zone. The aspirating agitator selectively transfers ethylene between these zones without requiring intense overall agitation, thus maintaining reaction efficiency while minimizing conditions that promote polyvinyl chloride formation.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The patent applies local quality by providing agitation specifically where needed - at the liquid-catalyst interface to ensure adequate contact - while using the aspirating mechanism to handle gas-phase ethylene transfer separately. This localized approach to agitation reduces overall mixing intensity and prevents excessive polyvinyl chloride formation while maintaining reaction efficiency.

Inventive Principle:
Principle #3Local quality

3Device complexity

If carbon tetrachloride and ethylene are reacted in a single reactor with continuous agitation, then synthesis is simplified, but temperature control and reactant contact become difficult

Engineering Contradiction:
Improvesynthesis process simplicityVSAvoidtemperature control
Core Design Contradiction:
Device complexityVSTemperature

Solution Approach 1:

The aspirating agitator serves multiple functions simultaneously: it provides mild mechanical agitation for reactant contact, creates vapor-liquid circulation for improved mass transfer, and facilitates heat distribution throughout the reaction mixture. This multi-functionality maintains synthesis simplicity while addressing temperature control challenges.

Inventive Principle:
Principle #6Universality (Multi-functionality)

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 approach enhances reaction efficiencies by ensuring adequate contact between reactants and catalysts, improves product yield and purity, and prevents fouling during distillation, thereby optimizing the production of chlorinated propanes.

Implementation Method 1

ethylene gas diffuses from the liquid reaction mixture into the headspace while agitating the reaction mixture

Methodology Applied
Scientific EffectGas diffusion: Diffusion

Implementation Method 2

transferring ethylene within the headspace back into the reaction mixture through a conduit within the mixing device that agitates the reaction mixture

Methodology Applied
Scientific EffectGas-liquid transfer: Absorption (physical)

Implementation Method 3

reacting carbon tetrachloride with vinyl chloride in the presence of an iron catalyst and tributylphosphate

Methodology Applied
Scientific EffectCatalysis: Catalysis

Implementation Method 4

The reactor effluent is distilled to recover catalyst and ultimately isolate the desired 1,1,1,3,3-pentachloropropane product

Methodology Applied
Scientific EffectDistillation: Distillation

Implementation Method 5

purified using a distillation technique with a forced circulation reboiler to prevent fouling

Methodology Applied
Scientific EffectForced convection: Forced Convection

Data Source

PatentEP4530279A1Method for producing halogenated propanes
Publication Date: 2025.04.02 OCCIDENTAL CHEMICAL CORP
  • EP4530279A1 patent drawingFigure 1
  • EP4530279A1 patent drawingFigure 2
  • EP4530279A1 patent drawingFigure 3

AI summary

A process of the type for producing chlorinated propanes by reacting carbon tetrachloride with ethylene within a tank reactor that includes a liquid reaction mixture and a headspace above the reaction mixture wherein ethylene gas diffuses from the liquid reaction mixture into the headspace while agitating the reaction mixture, the improvement comprising transferring ethylene within the headspace back into the reaction mixture through a conduit within the mixing device that agitates the reaction mixture.