Polyaspartic Acid Reflux Cooling Process

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Solution Overview

Problem

The production of polyaspartic acid via thermal polycondensation with acidic catalysts like phosphoric acid or methanesulfonic acid often results in highly viscous condensation phases that caking occurs, leading to process interruptions and laborious product purification, especially when using small amounts of catalyst.

Innovation Solution

A process involving reflux cooling without distilling water, achieving a degree of conversion of aspartic acid between 1% to 10%, followed by polycondensation with simultaneous water distillation, and subsequent hydrolysis with a base to produce polyaspartic acid, allowing for continuous operation and reduced catalyst usage.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Loss of substance

If small amounts of acidic catalyst (1 to 25 mol%) are used in polycondensation, then catalyst recovery cost is reduced, but highly viscous to very hard condensation phases prone to clumping occur that cannot be stirred or kneaded

Engineering Contradiction:
Improvecatalyst recovery costVSAvoidstirring and kneading ability
Core Design Contradiction:
Loss of substanceVSEase of operation

Solution Approach 1:

The patent applies preliminary action by conducting a pre-condensation step at lower temperature (100-220°C) before the main polycondensation. This preliminary treatment prevents the formation of hard, clumping condensation phases during the subsequent high-temperature polycondensation, maintaining stirrability and kneadability throughout the process while using only 1-25 mol% catalyst.

Inventive Principle:
Principle #10Preliminary action

2Stability of the object's composition

If phosphoric acid is used as both catalyst and solvent, then polycondensation is well-controlled, but product purification becomes complex requiring washing and acid recovery

Engineering Contradiction:
Improvepolycondensation controlVSAvoidpurification process complexity
Core Design Contradiction:
Stability of the object's compositionVSDevice complexity

Solution Approach 1:

The patent segments the use of phosphoric acid into two distinct stages: first as catalyst/solvent during pre-condensation, then as catalyst only during polycondensation. The pre-condensation phase uses phosphoric acid to control the reaction, while the subsequent polycondensation phase eliminates the need for extensive purification by using the acid solely as a catalyst that can be easily removed.

Inventive Principle:
Principle #1Segmentation

3Ease of operation

If condensation is interrupted to break up clumped solid polycondensate, then mixing ability is restored, but productivity decreases due to process interruptions

Engineering Contradiction:
Improvemixing abilityVSAvoidprocess continuity
Core Design Contradiction:
Ease of operationVSProductivity

Solution Approach 1:

The patent performs preliminary action by conducting pre-condensation at lower temperature before main polycondensation, which prevents the formation of clumped, non-stirrable solid polycondensate. This eliminates the need to interrupt the process for breaking up clumps, allowing continuous operation and maintaining high productivity throughout the polycondensation.

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

This method prevents caking issues, enables continuous polycondensation, and facilitates easier product recovery, improving process efficiency and reducing labor in catalyst recovery, while producing polyaspartic acid suitable for applications in cleaning and detergent compositions.

Implementation Method 1

Heating the mixture according to (a) under reflux without distillation of water at a reaction temperature of 100 to 220°C

Methodology Applied
Scientific EffectReflux cooling: Distillation

Implementation Method 2

Polycondensation of the reaction mass according to (b) with simultaneous distillation off water at 170 to 250°C

Methodology Applied
Scientific EffectDistillation: Distillation

Implementation Method 3

Hydrolysis of the polycondensates according to (c) with the addition of a base

Methodology Applied
Scientific EffectHydrolysis: Hydrolysis

Data Source

PatentEP3347405B1Method for the preparation of polyaspartic acid under reflux
Publication Date: 2022.11.09 BASF SE
  • EP3347405B1 patent drawing
  • EP3347405B1 patent drawing
  • EP3347405B1 patent drawing

AI summary

The invention relates to a method for producing polyaspartic acid under reflux cooling, compositions containing polyaspartic acid obtained by said method, and the use of polyaspartic acids obtained by said method in rinsing agents, washing agents, and cleaning agents.