THF Purification via Polar Solvent Azeotrope Distillation

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Solution Overview

Problem

Existing distillation processes for purifying tetrahydrofuran (THF) are inadequate in reducing butyl methyl ether content to meet purity requirements, especially in THF obtained from gas phase hydrogenation of maleic anhydride or its derivatives, which affects further processing such as polytetrahydrofuran production.

Innovation Solution

A distillative purification process for THF is introduced, involving the use of a polar solvent, preferably methanol, added before distillation, which is carried out in a multistage distillation column with structured packing, to effectively lower butyl methyl ether content.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional distillation processes are used to purify THF, then the purification process is simple and economical, but the butyl methyl ether content cannot be reduced sufficiently to meet purity requirements

Engineering Contradiction:
ImproveTHF purityVSAvoiddistillation process complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

A polar solvent (entraining agent) is introduced as an intermediary substance to facilitate the separation of butyl methyl ether from THF. The polar solvent forms an azeotrope with butyl methyl ether, enabling its removal from the THF mixture through distillation. This mediator allows achieving high THF purity (greater than 99.9%) that cannot be obtained by conventional distillation alone.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The process changes the physical-chemical parameters of the distillation system by introducing a polar solvent that alters the relative volatility and azeotropic behavior of the mixture. By selecting a polar solvent with specific properties (higher polarity than THF, ability to form azeotropes with butyl methyl ether), the distillation parameters are optimized to achieve superior separation efficiency and meet the required purity specifications.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If multiple distillation columns are used to reduce butyl methyl ether content, then THF purity improves, but the process complexity and operational difficulty increase

Engineering Contradiction:
ImproveTHF purityVSAvoiddistillation process operation
Core Design Contradiction:
Manufacturing precisionVSEase of operation

Solution Approach 1:

The polar solvent acts as an entraining agent that simplifies the distillation operation by forming a distinct azeotropic layer with butyl methyl ether. This allows for easier phase separation and reduces the need for complex multi-column operations. The process can be implemented in a single distillation column with a side draw, making it more operationally simple while achieving the required purity levels.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Manufacturing precision

If conventional distillation is used for THF purification, then the process is economical, but it cannot achieve the required purity for further processing such as polytetrahydrofuran production

Engineering Contradiction:
ImproveTHF purityVSAvoidTHF yield
Core Design Contradiction:
Manufacturing precisionVSQuantity of substance

Solution Approach 1:

By changing the distillation parameters through the introduction of a polar solvent, the process achieves higher THF purity (greater than 99.9%) with optimized butyl methyl ether removal. The side draw operation allows for efficient withdrawal of the azeotropic layer containing butyl methyl ether and polar solvent, while maintaining high THF recovery in the distillate, thus balancing purity requirements with acceptable yield.

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

The process significantly reduces butyl methyl ether content in THF, achieving purities greater than 99.9% and less than 200 ppm of other oxygen-functionalized compounds, thereby meeting the required purity standards for further processing.

Implementation Method 1

The extent to which the distillation processes known from the prior art lower the butyl methyl ether content of the aqueous crude THF products... is not sufficient to be able to fulfill the purity requirements... The process according to the invention enables a pure THF in which the butyl methyl ether content has been distinctly lowered

Methodology Applied
Scientific EffectAzeotrope formation: Distillation

Implementation Method 2

For the recovery of pure THF from such crude products, DE-A 37 26 805 discloses a process for distillatively purifying crude aqueous THF in which the THF is passed through three distillation columns

Methodology Applied
Scientific EffectDistillation: Distillation

Data Source

PatentUS7598405B2Method for the distillative processing of tetrahydrofuran
Publication Date: 2009.10.06 BASF SE
  • US7598405B2 patent drawing

AI summary

The present invention provides a process for distillatively purifying tetrahydrofuran in the presence of a polar solvent.