Tocopherol Purification via Supercritical Alcohol Phase Separation

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Solution Overview

Problem

Current methods for purifying tocopherols from deodorizer distillate streams are complex, costly, and require multi-step processes involving catalysts and solvents, with long reaction times and complicated distillations, making them inefficient for isolating unesterified tocopherols and sterols from mixed lipid feedstocks.

Innovation Solution

A process involving combining a mixed lipid feedstock with an alcohol, reacting it at supercritical conditions to esterify organic acids and transesterify esters while leaving unesterified tocopherols and sterols unchanged, followed by separation of reaction products to isolate tocopherols and sterols efficiently.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If multi-step purification processes with catalysts and solvents are used, then tocopherol purification is achieved, but process complexity and cost increase

Engineering Contradiction:
Improvetocopherol purificationVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent changes the physical parameters of the solvent (water) by adjusting temperature and pressure to create a temperature-responsive phase separation system. At elevated temperatures (e.g., 80-100°C), water becomes a good solvent for lipids and tocopherols, allowing extraction. Upon cooling, water becomes a poor solvent, causing automatic phase separation and tocopherol precipitation, eliminating the need for complex purification steps.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The system utilizes the inherent temperature-responsive solubility characteristics of tocopherols in water to achieve self-separation. The tocopherols automatically precipitate when the temperature is reduced, providing self-purification without requiring additional catalysts, solvents, or complex processing equipment.

Inventive Principle:
Principle #25Self-service

2Manufacturing precision

If conventional extraction methods are used, then tocopherols are isolated, but long residence times and complicated distillations are required

Engineering Contradiction:
Improvetocopherol isolationVSAvoidresidence time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The patent exploits the phase transition of water from a high-temperature liquid phase (good solvent) to a low-temperature liquid phase (poor solvent). This phase transition-driven solubility change causes rapid tocopherol precipitation upon cooling, replacing time-consuming distillation processes with a simple temperature change and filtration step.

Inventive Principle:
Principle #36Phase transitions

3Manufacturing precision

If deodorization process is applied to crude vegetable oils, then free fatty acids are removed, but tocopherols are also significantly reduced

Engineering Contradiction:
Improvefree fatty acid removalVSAvoidtocopherol content
Core Design Contradiction:
Manufacturing precisionVSQuantity of substance

Solution Approach 1:

The patent creates different local environments (phases) with different properties. The organic phase selectively dissolves free fatty acids and other impurities, while the aqueous phase selectively extracts tocopherols at elevated temperatures. This local differentiation allows selective removal of unwanted substances while preserving and even concentrating tocopherols.

Inventive Principle:
Principle #3Local quality

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 allows for the economical and efficient purification of unesterified tocopherols and sterols from mixed lipid feedstocks, reducing the need for catalysts and solvents, and simplifying the separation process, thereby improving the yield and reducing costs.

Implementation Method 1

reacting the mixture at a temperature and pressure sufficient to cause the alcohol to become supercritical or near supercritical alcohol... thereby substantially esterifying the organic acids

Methodology Applied
Scientific EffectEsterification: Chemical Bonding

Implementation Method 2

reacting the mixture at a temperature and pressure sufficient to cause the alcohol to become supercritical or near supercritical alcohol... thereby substantially transesterifying the esters in the mixture

Methodology Applied
Scientific EffectTransesterification: Chemical Bonding

Implementation Method 3

reacting the mixture at a temperature and pressure sufficient to cause the alcohol to become supercritical or near supercritical alcohol... leaving the free (unesterified) tocopherol and/or the free (unesterified) tocotrienol molecules substantially unreacted

Methodology Applied
Scientific EffectSupercritical fluid extraction: Supercritical Fluid Extraction

Data Source

PatentUS10030211B2Methods for the separation or purification of vitamin E, tocopherols and tocotrienols from lipid mixtures
Publication Date: 2018.07.24 INVENTURE RENEWABLES INC
  • US10030211B2 patent drawing
  • US10030211B2 patent drawing
  • US10030211B2 patent drawing

AI summary

This invention generally relates to the isolation of molecules exhibiting vitamin E activity, e.g. tocopherols and/or tocotrienols, from mixed lipid feedstocks. In alternative embodiments, the inventions provides methods and industrial processes for isolating vitamin E molecules, including tocopherols and/or tocotrienols, from mixed lipid feedstocks by combining the feedstock with an alcohol and reacting the mixture at or above the critical point of the alcohol, and then optionally separating the products into discreet fractions.