Batch Esterification Pressure Staging for Higher Throughput

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Solution Overview

Problem

Existing batch processes for preparing ester-based plasticizers are costly and inefficient, lacking optimization through process condition control, leading to energy consumption and reduced productivity.

Innovation Solution

A method controlling reactor pressure in two stages during the esterification reaction, with initial pressure of 0.3 to 1.0 barg and final pressure of 0 to 0.5 barg, and adjusting pressure based on reaction conversion rates to minimize reflux and optimize reaction duration.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If small-scale manual preparation methods are used, then flexibility and simplicity are maintained, but productivity and manufacturing efficiency are insufficient

Engineering Contradiction:
Improvemanufacturing efficiencyVSAvoidprocess complexity
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The preparation method is divided into distinct sequential steps: dissolving the ester in water, adding the salt, stirring, filtering, and concentrating. This segmentation allows each step to be optimized independently while maintaining overall process simplicity and enabling scalable production from small to large scales.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The method utilizes changes in physical parameters (solubility, temperature, concentration) to achieve separation and purification. By adjusting these parameters systematically, the process maintains simplicity while significantly increasing productivity compared to manual methods.

Inventive Principle:
Principle #35Parameter changes

2Productivity

If conventional preparation methods are used, then basic production is achieved, but time consumption is excessive and efficiency is low

Engineering Contradiction:
Improvepreparation efficiencyVSAvoidtime consumption
Core Design Contradiction:
ProductivityVSLoss of time

Solution Approach 1:

The method performs preliminary dissolution of the ester in water before adding the salt, which facilitates easier separation and reduces subsequent processing time. This preliminary action streamlines the overall process and significantly reduces total time consumption while maintaining high efficiency.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The preparation process continues without interruption through sequential steps of dissolving, adding salt, stirring, filtering, and concentrating. This continuous workflow eliminates idle time between operations and maximizes preparation efficiency.

Inventive Principle:
Principle #20Continuity of useful action

3Manufacturing precision

If detailed separation and purification steps are implemented, then product purity is improved, but process complexity and time consumption increase

Engineering Contradiction:
Improveproduct purityVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The method extracts the target compound from the reaction mixture by dissolving it in water and then precipitating it through salt addition. This simple extraction approach achieves effective purification without requiring complex multi-step separation procedures, maintaining low process complexity while improving product purity.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

Water acts as an intermediary solvent that facilitates separation between the ester-based material and impurities. The salt serves as another intermediary that triggers precipitation. These intermediaries enable effective purification through simple, low-complexity operations.

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 approach enhances productivity and energy efficiency by reducing reaction time and minimizing reflux, while ensuring high conversion rates and uniform product quality.

Implementation Method 1

dissolving the ester in water

Methodology Applied
Scientific EffectDissolution: Solvation

Implementation Method 2

adding the salt to the solution

Methodology Applied
Scientific EffectSalting out: Precipitation

Data Source

PatentEP4219440B1Batch preparation method for ester-based material
Publication Date: 2026.05.06 LG CHEM LTD
  • EP4219440B1 patent drawingFigure 1

AI summary

The present invention provides a method for preparing an ester-based material, the method including a step in which in a batch reactor, under a catalyst, at least one polycarboxylic acid selected from the group consisting of a terephthalic acid, a phthalic acid, an isophthalic acid, a cyclohexane dicarboxylic acid, a cyclohexane tricarboxylic acid, a trimellitic acid, and citric acid reacts with at least one mono-alcohol having 3 to 12 alkyl carbon atoms, wherein pressure in the reactor is configured such that the pressure at the early stage is 0.3 barg to 1.0 barg and the pressure at the latter stage is 0 barg to 0.5 barg, the pressure at the early stage being greater than the pressure at the latter stage, and the early and latter stages are divided based on any one of the time points when reaction conversion rate is 30% to 90%, and when the method is applied, the productivity of an ester-based material may increase and energy consumption in processes may be reduced.