Vitamin E Rectification and Acetylation for High-Purity Recovery

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Solution Overview

Problem

Current processes for purifying vitamin E (VE) and vitamin E acetate (VEA) suffer from high product loss, complex and costly separation methods, and inability to produce high-purity 'pharma grade' quality, requiring additional purification steps and recycling, which complicates the production of both 'technical grade' and 'pharma grade' products.

Innovation Solution

A process involving rectification columns with structured packings, where vitamin E is purified before acetylation, allowing for the production of all four end products (VE-TG, VEA-TG, VE-PG, VEA-PG) in variable proportions, with minimal product loss and simplified process engineering, eliminating the need for recycling by achieving high purity through sharp separation in fewer columns.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Loss of substance

If thin-film evaporator is used to remove low-boiling substances, then separation of low boilers is achieved, but product loss increases and device complexity increases

Engineering Contradiction:
Improveproduct lossVSAvoidapparatus complexity
Core Design Contradiction:
Loss of substanceVSDevice complexity

Solution Approach 1:

The invention extracts and removes low-boiling substances (phytadienes) from the crude VEA product stream before the main purification process. By taking out these impurities early through a simple distillation step, the subsequent short-path evaporators operate more efficiently with reduced load, minimizing product loss and reducing the complexity of the vacuum system required.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The process performs preliminary removal of low-boiling substances before the main purification stage. This preliminary action reduces the burden on the subsequent evaporation and condensation system, allowing operation at higher pressures and reducing the complexity of the vacuum system while minimizing product loss.

Inventive Principle:
Principle #10Preliminary action

2Manufacturing precision

If multiple evaporation and condensation stages are used for purification, then product purity increases, but device complexity and operational complexity increase

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

Solution Approach 1:

The purification process is segmented into distinct functional stages: (1) preliminary removal of low-boiling substances, (2) main purification by evaporation and condensation, and (3) final polishing. This segmentation allows each stage to be optimized independently, achieving high purity while managing device complexity through modular design.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The process applies partial condensation rather than complete condensation in the condenser system. By condensing only the necessary portion of the vapor stream, the process achieves sufficient purification while reducing the complexity of the condensation system and minimizing the need for extensive recycling operations.

Inventive Principle:
Principle #16Partial or excessive action

3Loss of substance

If recycling streams are implemented to minimize product loss, then product recovery increases, but process complexity increases

Engineering Contradiction:
Improveproduct recoveryVSAvoidprocess complexity
Core Design Contradiction:
Loss of substanceVSDevice complexity

Solution Approach 1:

The process selectively discards the condensate stream containing low-boiling substances and acetic acid residues, which cannot be economically reused. Meanwhile, it recovers and returns to the process the portion of condensed vapor that contains valuable VEA product. This selective discarding and recovering approach minimizes product loss while avoiding the complexity of fully recycling all streams.

Inventive Principle:
Principle #34Discarding and recovering

4Manufacturing precision

If complete separation of low-boiling substances is achieved, then product purity increases, but energy consumption and operational complexity increase

Engineering Contradiction:
Improveproduct purityVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by moving object

Solution Approach 1:

The process implements partial separation of low-boiling substances rather than complete separation. The preliminary distillation step removes the bulk of low-boiling impurities, and the subsequent evaporation-condensation process achieves final purification. This partial action approach achieves sufficient product purity while significantly reducing energy consumption compared to complete separation methods.

Inventive Principle:
Principle #16Partial or excessive 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 process achieves high purity (>97% VEA content) with reduced product loss and operational complexity, enabling flexible production of different product qualities while minimizing waste and recycling, thus meeting stringent 'pharma grade' quality requirements efficiently.

Implementation Method 1

purification of vitamin E and vitamin E acetate preferably by distillation, for example rectification

Methodology Applied
Scientific EffectVapor-liquid equilibrium: Distillation

Implementation Method 2

The vapour stream produced in a thin-film evaporator contains substantially phytadienes, vitamin E acetate and residues of acetic acid and acetic anhydride and is virtually completely condensed in a downstream condenser system

Methodology Applied
Scientific EffectCondensation: Condensation

Implementation Method 3

A thin-film evaporator usually operated at about 1 mbar and intended for removing the low boilers

Methodology Applied
Scientific EffectEvaporation: Evaporation

Data Source

PatentUS8183396B2Process for the working-up of a vitamin E- and vitamin E-acetate- containing mixture or products stream
Publication Date: 2012.05.22 DSM IP ASSETS BV
  • US8183396B2 patent drawing
  • US8183396B2 patent drawing
  • US8183396B2 patent drawing

AI summary

The invention relates to a process for the working-up of a vitamin E (VE)- and/or vitamin E acetate (VEA)-containing product stream, which is substantially characterized by purification of a vitamin E-containing product stream, acetylation of at least a part of the purified vitamin E and purification of at least a part of the acetylated vitamin E, the purification of vitamin E and vitamin E acetate preferably being effected by distillation, for example rectification. A preferred process according to the invention is characterized in that a vitamin E-containing product stream is fed to a first rectification column (105), low-boiling products and unspecified isomers of vitamin E being taken off at the top (105a) of this first rectification column virtually without loss of useful substance, and a purified, vitamin E-containing stream being taken off at the side (105b) and/or at the bottom (105c) of the rectification column (105), at least a part of the side take-off or of the bottom take-off or at least a part of the side and bottom take-off is passed, for acetylation of vitamin E, into an acetylation stage (111), at least a part of the product stream emerging from the acetylation stage is passed into a second rectification column (115) or is taken off as useful product having a purity of ≧92% by weight, and in a second rectification column, the VEA useful product is obtained as a side take-off having a purity of ≧97% by weight.