Polyglycerol Ester Purification via Basic Solution Refining

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Solution Overview

Problem

The existing methods for preparing polyglycerol fatty acid esters face challenges in achieving high yields and efficient purification, particularly due to emulsion formation during alkaline refining, which results in significant losses of polyglycerol fatty acid esters, and the inefficiency of dry refining methods that depend on granulometry and mixing intensity.

Innovation Solution

A process involving the use of metallic catalysts like tetrabutyl titanate is introduced, which facilitates efficient esterification and subsequent purification by refining with basic solutions, followed by solvent removal and separation under controlled pressure and temperature conditions, ensuring high yields of polyglycerol fatty acid esters without compromising the product.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If alkaline refining is used to purify polyglycerol fatty acid esters, then the purification process can remove excess fatty acid, but emulsion formation occurs resulting in significant losses of polyglycerol fatty acid esters

Engineering Contradiction:
Improvepurification qualityVSAvoidpolyglycerol fatty acid ester loss
Core Design Contradiction:
Manufacturing precisionVSLoss of substance

Solution Approach 1:

The patent introduces a specific basic solution (aqueous sodium hydroxide or potassium hydroxide solution with 5-20% concentration) as an intermediary medium to facilitate the separation of excess fatty acid from polyglycerol fatty acid esters. This basic solution acts as a mediator that reacts with excess fatty acid to form water-soluble salts, enabling efficient separation without causing emulsion formation that leads to product loss. The basic solution concentration and composition are carefully controlled to optimize the separation process while minimizing product loss.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Ease of manufacture

If dry refining methods are used to remove excess fatty acid, then the process can be simpler, but the method depends on granulometry and mixing intensity making it inefficient

Engineering Contradiction:
Improveprocess simplicityVSAvoidrefining efficiency
Core Design Contradiction:
Ease of manufactureVSProductivity

Solution Approach 1:

The patent replaces the mechanical-based dry refining method (which relies on granulometry and mixing intensity) with a chemical-based wet refining method using basic solutions. Instead of relying on mechanical mixing and particle size characteristics, the process uses chemical reactions between the basic solution and excess fatty acid to form water-soluble salts that can be easily separated. This substitution of mechanical action with chemical action significantly improves refining efficiency while maintaining process simplicity.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

3Productivity

If metallic catalysts are used to accelerate esterification, then reaction speed increases, but the process requires additional purification steps to remove catalyst residues

Engineering Contradiction:
Improvereaction speedVSAvoidpurification process complexity
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The patent employs metallic catalysts (such as zinc, manganese, cobalt, or titanium compounds) that are used in small quantities and can be easily removed through the basic solution refining process. These catalysts act as short-living components that facilitate the esterification reaction and then are eliminated in the purification step along with excess fatty acid. The basic solution effectively removes catalyst residues, so while catalysts are introduced, they do not permanently complicate the process as they are disposed of in the refinement stage.

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

4Manufacturing precision

If complete esterification is achieved to produce full esters, then product quality improves, but reaction time and energy consumption increase

Engineering Contradiction:
Improveesterification completenessVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by stationary object

Solution Approach 1:

The patent optimizes the esterification process by carefully controlling parameters such as the molar ratio of polyglycerol to fatty acid (typically 1:1.05 to 1:1.2), reaction temperature (100-200°C), and catalyst concentration. By adjusting these parameters, the process achieves complete esterification (full esters with hydroxyl value < 5 mg KOH/g) while minimizing energy consumption and reaction time. The use of efficient metallic catalysts and optimized basic solution refinement allows the process to reach complete conversion without excessive energy input.

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

This approach significantly improves the yield of polyglycerol fatty acid esters to over 90% by minimizing emulsion-related losses and optimizing reaction conditions, using non-toxic components and reducing reaction time, while maintaining product quality.

Implementation Method 1

a catalyst is added to the reaction mixture which has at least one metallic compound which contains at least the metals manganese, zinc, cobalt or titanium

Methodology Applied
Scientific EffectCatalysis: Catalysis

Implementation Method 2

refining with basic solution, preferably with dilute aqueous sodium or potassium hydroxide until fatty acid salts are formed

Methodology Applied
Scientific EffectNeutralization reaction: Redox Reactions

Implementation Method 3

an example of a centrifugal separator is a decanter centrifuge

Methodology Applied
Scientific EffectCentrifugal separation: Centrifugal Separation

Data Source

PatentUS11414370B2Process for preparing polyglycerol ester of fatty acids
Publication Date: 2022.08.16 IOI OLEO GMBH

AI summary

A process is described for the preparation of polyglycerol fatty acid esters from a reaction mixture to which a metallic catalyst is added, as well as to a method for the purification of an intermediate synthesis product which contains excess fatty acid in addition to polyglycerol fatty acid esters. Compared with the prior art, a significantly improved yield and a higher process speed is obtained along with more economic use of raw materials, auxiliary materials, solvents and energy.