PMDETA Purification by By-Product Derivatization Before Distillation

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Solution Overview

Problem

The separation of intermediate products such as N,N,3-trimethyl-1-imidazolidineethanamine (DMAEMI) from pentamethyl diethylenetriamine (PMDETA) is challenging due to their similar boiling points, making distillation inefficient.

Innovation Solution

A process involving the addition of a reactive compound with a C=O moiety, such as aldehydes, ketones, or carboxylic acid derivatives, to react with by-products, followed by distillative separation to obtain pure PMDETA.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If distillation is used to separate by-products from PMDETA, then separation is attempted, but the similar boiling points make distillation inefficient

Engineering Contradiction:
Improvepurity of PMDETAVSAvoidseparation efficiency
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent changes the chemical parameter of the by-products by reacting them with a reactive compound to form derivatives with different boiling points. This transforms the separation problem from one of physical property similarity to one of chemical property difference, enabling efficient distillation separation.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The reactive compound acts as an intermediary substance that selectively reacts with by-products to convert them into separable derivatives. This intermediary enables the separation process by creating a chemical distinction between the by-products and the desired PMDETA product.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Manufacturing precision

If a reactive compound is added to convert by-products, then by-products are converted into separable derivatives, but additional process steps are required

Engineering Contradiction:
Improvepurity of PMDETAVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The reactive compound is added to the crude reaction mixture before distillation, performing the conversion of by-products in advance. This preliminary chemical modification simplifies the subsequent distillation step by pre-differentiating the boiling points of components that would otherwise be difficult to separate.

Inventive Principle:
Principle #10Preliminary action

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

Achieves a purity of ≥ 99% PMDETA by effectively converting by-products into derivatives that can be separated through distillation, reducing the presence of impurities like DMAEMI.

Implementation Method 1

adding a compound reactive with the by-products; reacting the by-products with the reactive compound to obtain derivatives of the by-products

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

distillative separation of PMDETA from the derivatives obtained in step c) to obtain pure PMDETA

Methodology Applied
Scientific EffectDistillation: Distillation

Data Source

PatentEP4700012A1Process for the purification of pentamethyl diethylenetriamine
Publication Date: 2026.02.25 BASF SE
  • EP4700012A1 patent drawing
  • EP4700012A1 patent drawing
  • EP4700012A1 patent drawing

AI summary

A process for the purification of pentamethyl diethylenetriamine (PMDETA) comprising one or more by-products selected from the group consisting of N,N,N",N"-tetramethyldiethylenetriamine, N,N,N'-trimethyl-N'-[2-(methylamino)ethyl]ethane-1,2-diamine and N,N,3-trimethyl-1-imidazolidineethanamine, comprising the steps: a) providing a crude PMDETA mixture comprising one or more of the by-products; b) adding a compound reactive with the by-products; c) reacting the by-products with the reactive compound to obtain derivatives of the by-products; d) distillative separation of PMDETA from the by-product derivatives obtained in step c) to obtain pure PMDETA.