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Method for extracting citronellal from Litsea cubeba oil front distillate

A technology of litsea cubeba and citronellal, applied in the separation/purification of carbonyl compounds, organic chemistry, etc., can solve the problems of waste, etc., and achieve the effects of convenient operation, simple preparation process and high product purity

Active Publication Date: 2018-08-10
YONGZHOU SAMSHIANG FLAVOURS & FRAGRANCES CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Additionally, the growing demand for natural citral has resulted in more and more litsea cubeba head oil (pre-fraction of litsea cubeba oil) being wasted as a by-product

Method used

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  • Method for extracting citronellal from Litsea cubeba oil front distillate
  • Method for extracting citronellal from Litsea cubeba oil front distillate
  • Method for extracting citronellal from Litsea cubeba oil front distillate

Examples

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Effect test

Embodiment 1

[0042] A method for extracting citronellal from Litsea cubeba head oil of the present invention, wherein, used Litsea cubeba head oil is obtained through crude extraction and distillation from the fresh fruit of Litsea cubeba, and the specific extraction method is as follows:

[0043] (1) Rough extraction of litsea cubeba:

[0044] The picked Litsea cubeba fresh fruit is cleaned, and 150 kg of fresh fruit is weighed and placed in a retort tank in water, and water (225 kg) that is 1.5 times the weight of the Litsea cubeba fresh fruit is added. Use 4kg of pressure water vapor as the heating carrier, and use a 1000L multi-functional extraction device for extraction, adjust the temperature and steam pressure of the water distillation, and control the return flow at 150L / h;

[0045] After the distillation, the material in the distillation flask is filtered through a filter screen, and the remaining water in the flask is used as the water for the next feeding. The dried fruit in th...

Embodiment 2

[0059] A method for extracting citronellal from Litsea cubeba head oil of the present invention, wherein, used Litsea cubeba head oil is obtained through crude extraction and distillation from the fresh fruit of Litsea cubeba, and the specific extraction method is as follows:

[0060] (1) Rough extraction of litsea cubeba:

[0061] The picked Litsea cubeba fresh fruit is cleaned, and 150 kg of fresh fruit is taken by weighing and placed in a retort tank in water, and water (225 kg) that is 1.5 times the weight of the Litsea cubeba fresh fruit is added. Use 4kg of pressure water vapor as the heating carrier, and use a 1000L multi-functional extraction device for extraction, adjust the temperature and steam pressure of the water distillation, and control the return flow at 150L / h;

[0062] After the distillation is over, the material in the distillation is filtered through a filter screen, and the remaining water in the flask is used as the water for the next feeding. The dried...

Embodiment 3

[0073] A method for extracting citronellal from Litsea cubeba head oil of the present invention, wherein, used Litsea cubeba head oil is obtained through crude extraction and distillation from the fresh fruit of Litsea cubeba, and the specific extraction method is as follows:

[0074] (1) Rough extraction of litsea cubeba:

[0075]The picked Litsea cubeba fresh fruit is cleaned, and 150 kg of fresh fruit is taken by weighing and placed in a retort tank in water, and water (225 kg) that is 1.5 times the weight of the Litsea cubeba fresh fruit is added. Use 4kg of pressure water vapor as the heating carrier, and use a 1000L multi-functional extraction device for extraction, adjust the temperature and steam pressure of the water distillation, and control the return flow at 150L / h;

[0076] After the distillation is over, the material in the distillation is filtered through a filter screen, and the remaining water in the flask is used as the water for the next feeding. The dried ...

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Abstract

The invention discloses a method for extracting citronellal from Litsea cubeba oil front distillate. The method comprises: (1) pouring Litsea cubeba oil front distillate into a reaction container, controlling the temperature of the reaction system at 5-15 DEG C, adding a NaHSO3 aqueous solution in a dropwise manner, and carrying out an addition reaction on the NaHSO3 aqueous solution and the aldehyde ketone in the Litsea cubeba oil front distillate to obtain a solid product insoluble in the Litsea cubeba oil front distillate; (2) separating the solid product obtained in the step (1), adding anextractant, adding an acid solution in a dropwise manner, heating to a temperature of 68-72 DEG C under stirring, carrying out a reflux reaction, carrying out standing layering after completing the reaction, washing the organic layer, and drying to obtain citronellal crude oil; and (3) pouring the citronellal crude oil obtained in the step (2) into a rectification tower, and rectifying in three stages to respectively obtain methylheptenone, citronellal and citral. According to the present invention, the method has advantages of convenient operation, low cost, high efficiency and high productpurity, and can co-produce methylheptenone and citral.

Description

technical field [0001] The invention relates to the technical field of citronellal extraction, in particular to a method for extracting citronellal from litsea cubeba head oil. Background technique [0002] Citronellal is an important isolated spice with an intense, fresh, green citrus-like, slightly woody aroma. Citronellal is widely used in food flavors, to prepare citrus and cherry flavors, to prepare low-grade soap flavors, as a raw material for other flavors, and to synthesize other flavors such as hydroxycitronellal and menthol. There are two sources of citronellal, natural extraction and chemical synthesis. Because the synthetic citronellal brings in many uncertain impurities, the harm to the human body caused by the food flavor is unpredictable. [0003] Litsea cubeba oil has been used as a food additive for more than 30 years. Litsea cubeba oil contains citronellal, and the chemical components contained in it have not detected substances that are particularly harm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/78C07C47/21
CPCC07C45/78C07C47/21
Inventor 余杰坤张宁李维虎李鸿
Owner YONGZHOU SAMSHIANG FLAVOURS & FRAGRANCES CORP
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