Tocopherol Purification via Acid-Activated Bleaching Earth

Solution Overview

Problem

The existing methods for producing protected tocopherols result in high levels of impurity, particularly free tocopherol, which are not effectively reduced, especially under thermal stress conditions, making it challenging to achieve the desired purity levels for commercial applications.

Innovation Solution

Contacting tocopherol with acid-activated bleaching earth before the protection reaction significantly reduces the impurity level of free tocopherol, achieving high purity and quality in the production of protected tocopherols, such as tocopheryl acetates, even under thermal stress.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional methods are used to produce protected tocopherols, then the production process is simple, but the impurity level of free tocopherol remains high (above 0.5%)

Engineering Contradiction:

Improvepurity of protected tocopherolVSAvoidcomplexity of production process

Core Design Contradiction:

Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent applies preliminary action by treating the tocopherol starting material with acid-activated bleaching earth before the protection reaction. This pre-treatment step removes impurities from the tocopherol before it undergoes acetylation, preventing the formation of excessive free tocopherol impurity in the final product. The bleaching earth treatment is performed in advance to ensure high purity without complicating the main protection reaction process.

Inventive Principle:

Principle #10Preliminary action

2Stability of the object's composition

If thermal stress is applied to protect tocopherols (e.g., rectification processes), then the stability of tocopherols is improved, but the level of free tocopherol impurity increases

Engineering Contradiction:

Improvestability of protected tocopherolVSAvoidpurity of protected tocopherol

Core Design Contradiction:

Stability of the object's compositionVSManufacturing precision

Solution Approach 1:

The patent applies preliminary action by treating the tocopherol starting material with acid-activated bleaching earth before the protection reaction. This pre-treatment step removes impurities from the tocopherol before it undergoes acetylation, preventing the formation of excessive free tocopherol impurity in the final product. The bleaching earth treatment is performed in advance to ensure high purity without complicating the main protection reaction process.

Inventive Principle:

Principle #10Preliminary action

Solution Approach 2:

The patent converts the potentially harmful effect of thermal stress, which normally increases free tocopherol impurity, into a beneficial outcome. By pre-treating with acid-activated bleaching earth, the system can withstand thermal stress during rectification while maintaining low impurity levels. The thermal stress that would normally be harmful is now tolerated because the starting material has been pre-purified, converting the harmful thermal effect into an acceptable processing condition that still achieves high purity product.

Inventive Principle:

Principle #22Blessing in disguise (Convert harm into benefit)

3Manufacturing precision

If bleaching earth is used to refine oils and fats, then the odor and color are improved, but the tocopherol content is significantly reduced due to adsorption

Engineering Contradiction:

Improvequality of oil and fatVSAvoidtocopherol content

Core Design Contradiction:

Manufacturing precisionVSQuantity of substance

Solution Approach 1:

The patent applies preliminary action by treating the tocopherol starting material with acid-activated bleaching earth before the protection reaction. This pre-treatment step removes impurities from the tocopherol before it undergoes acetylation, preventing the formation of excessive free tocopherol impurity in the final product. The bleaching earth treatment is performed in advance to ensure high purity without complicating the main protection reaction process.

Inventive Principle:

Principle #10Preliminary action

Solution Approach 2:

The patent applies parameter changes by using acid-activated bleaching earth with specific properties (acid treatment) rather than conventional bleaching earth. The acid activation modifies the surface properties of the bleaching earth to reduce tocopherol adsorption while maintaining its ability to remove impurities. This parameter change in the bleaching earth treatment allows for purification without significant tocopherol loss.

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 method efficiently reduces the impurity level of free tocopherol by more than 30% by weight, often below 0.5%, ensuring highly purified protected tocopherols suitable for pharmaceutical and food applications, maintaining low impurity levels even after thermal rectification processes.

Implementation Method 1

contacting the tocopherol used for its preparation with acid activated bleaching earth leads to a remarkably reduction of said impurity

Methodology Applied

Scientific EffectAdsorption: Adsorption

Data Source

PatentEP2882729B1Protected tocopherol with reduced content of free tocopherol

Publication Date: 2016.09.21 DSM IP ASSETS BV

AI summary

The present invention relates to a method of preparing a protected tocopherol with a reduced content of free tocopherol, comprising the step of contacting the tocopherol used for the preparation of the protected tocopherol in neat or in the form of a highly concentrated solution with an acid activated bleaching earth. The method is rather efficient in removal of substantial amounts of this impurity.