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A method for preparing 2-phenylethanol by molecular distillation separation from biotransformation liquid

A molecular distillation and biotransformation technology, used in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of difficulty in two-phase separation, solvent residual refining cost, etc., and achieve simple production process and simple components. , the effect of pure fragrance

Active Publication Date: 2020-06-26
INST OF MICROBIOLOGY JIANGXI ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The organic solvent liquid-liquid extraction method usually uses alcohols, hydrocarbons and other compounds to extract, and then distills to obtain 2-PE. Disadvantages of high cost

Method used

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  • A method for preparing 2-phenylethanol by molecular distillation separation from biotransformation liquid
  • A method for preparing 2-phenylethanol by molecular distillation separation from biotransformation liquid
  • A method for preparing 2-phenylethanol by molecular distillation separation from biotransformation liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A method for preparing 2-phenylethanol by molecular distillation separation from biotransformation liquid, the steps are:

[0027] (1) Molecular distillation device preparation: VKL 70-5-WRS-T type scraped film short-path distillation equipment produced by German VTA company was selected; liquid nitrogen was added to the cold trap of the molecular distillation device as a cryogenic agent to prevent volatiles from entering the vacuum system ;The molecular distillation device also has a scraping film system, which can ensure the uniformity of the liquid film on the entire evaporation surface, and the surface of the liquid film is constantly updated, thus ensuring the residence time of the heated raw material on the evaporation surface;

[0028] (2) Molecular distillation once:

[0029] Material: 2-PE concentrate, in which 2-PE content is 850-920g / L, ethanol content is 40-120g / L;

[0030] Primary molecular distillation conditions: temperature 60-80°C, pressure 200-500mbar...

Embodiment 2

[0038] Example 2 Elution of 2-PE

[0039]The 2-PE in the biotransformation solution is adsorbed by HZ816 macroporous resin, and when there is 2-PE in the effluent, switch to another resin column; then the adsorbed resin column is saturated with ethanol to elute the product. The volume of the resin column is 7.3L, the wet apparent density of HZ816 macroporous resin is 0.65-0.75g / mL, and the particle size range is 0.315-1.25mm. First, replace the conversion solution in the resin column with pure water about 1.5-2 times the volume of the resin , mainly to remove the conversion liquid substrate L-phenylalanine remaining in the resin column, and then use 1.5 times the resin volume to elute with an ethanol solution with a mass percentage of 96%, and the elution flow rate is 2.0m 3 / (m 3 ×h), through 8 batches of ethanol elution, a total of 41.71L of ethanol eluate containing 2-PE was collected, and the 2-PE content was 84.13g / L, that is, 2-PE 3509.1g. The 2-PE-free ethanol solutio...

Embodiment 3

[0040] Example 3 Preparation of 2-PE Concentrate

[0041] Remove ethanol and water from the ethanol eluate in Example 2 by evaporating under reduced pressure, the evaporation conditions are: temperature is 60-75°C, evaporation pressure is 200-600mbar (vacuum degree); then measure the distillate and concentrate respectively 2-PE content and volume; 3.84L of 2-PE concentrate was collected, of which, the content of 2-PE was 898.1g / L, and the yield of 2-PE was 98.28%.

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Abstract

The invention discloses a method for preparing 2-phenylethanol from a biotransformation liquid through molecular distillation separation. The method comprises primary molecular distillation and secondary molecular distillation. According to the method, 2-PE biologically converted from yeast resting cells is used as a raw material, a conversion solution is adsorbed through macroporous resin, a 850-920 g / L 2-PE concentrated solution is obtained through ethanol elution and reduced pressure concentration, and the 2-PE concentrated solution is subjected to molecular distillation twice to obtain a high-purity product. Influences on 2-PE purity and yield are investigated according to technological parameters such as the distillation temperature, the feeding rate, the pressure and the rotating speed of a film scraping device. The purity of the produced 2-PE reaches 99.0% or above, an organic solvent can be completely recycled in the extraction and refining process, the method is simple in production process and environmentally friendly, high-purity 2-PE is obtained through efficient separation, industrial production is easy to achieve, and the method is a clean production process suitablefor industrial production.

Description

technical field [0001] The invention belongs to the technical field of biochemical preparation of 2-phenylethanol, and in particular relates to a method for preparing high-purity 2-phenylethanol from biotransformation liquid by using molecular distillation technology. Background technique [0002] 2-Phenylethyl alcohol (β-phenylethyl alcohol, 2-PE) is a kind of edible spice, which naturally exists in rose oil, neroli oil, geranium oil and other aromatic oils. Because it has a soft, pleasant and long-lasting rose aroma, It is widely used in daily chemical products in various food, medicine, cosmetics, tobacco, papermaking and other industries. It is the main raw material for preparing rose-flavored food additives and rose-flavored essences. [0003] Using yeast to catalyze the conversion of L-phenylalanine (L-Phe) to synthesize 2-PE is an effective way to industrially produce natural 2-PE. At present, many growing cells are used for fermentation at home and abroad, but there...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/80C07C33/22
CPCC07C29/80C07C33/22
Inventor 黄筱萍熊大维刘兰顾斌涛候安伟
Owner INST OF MICROBIOLOGY JIANGXI ACADEMY OF SCI
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