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Method for synthesizing anethole by taking estragole oil as raw material

A technology of wormwood and anethole, applied in the field of synthesizing anethole, can solve the problems of low comprehensive utilization rate of anise oil, and achieve the effects of realizing reuse value, simple method and improving comprehensive utilization rate.

Inactive Publication Date: 2014-04-30
BEIJING FORESTRY UNIVERSITY
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  • Summary
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problem of low comprehensive utilization rate of anise oil, the present invention uses wormwood oil as a raw material to obtain a low-cost, high-yield synthesis method of anethole, whose purity of trans-anethole is as high as 96% or more

Method used

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  • Method for synthesizing anethole by taking estragole oil as raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Mix 6gKOH and 3gNaOH to prepare KOH / NaOH basic catalyst. Add the prepared catalyst into a stainless steel conical flask containing 120 g of wormwood oil (78.2% wormwood GC content), stir and reflux to rapidly raise the temperature to about 210°C, and continue the reaction for 2.5 hours. After the reaction is completed, cool to 70°C, add hot water to wash twice, let stand to separate layers, put the obtained oil layer in the refrigerator, and freeze and crystallize at 2°C, the crystallization time is 20h. The obtained crystals were crushed and separated using a centrifuge to obtain 75.7 g of anethole crude product.

[0021] The obtained crude anethole product was subjected to rectification and separation under the condition of vacuum degree of 99.4KPa and reflux ratio of 6:1, and the fraction between 123°C was collected to obtain 68.4g of the final product. 99.6%, of which trans-anethole content is 96.9%.

Embodiment 2

[0023] Take 10g KOH and 15g polyethylene glycol 1000 in a stainless steel flask, use an electric heating mantle to heat until completely melted and raise the temperature to 210°C, then add 154g wormwood oil (78.2% wormhole GC content) dropwise to the flask, reflux and The reaction was stirred for about 1.5h. After the reaction is completed, cool to 60°C, add hot water to wash twice, let stand to separate layers, put the obtained oil layer in the refrigerator, and refrigerate and crystallize at 2°C for 20 hours. The obtained crystals were crushed by adding 100 ml of ice-cold brine at -5°C, and separated using a centrifuge to obtain 115.1 g of anethole crude product.

[0024] The obtained crude anethole product was subjected to rectification and separation under the conditions of vacuum degree of 99.8KPa and reflux ratio of 7:1, and the fraction between 124°C was collected to obtain 104.4g of the final product, the relative effective yield of anethole was 86.7%, and the content ...

Embodiment 3

[0026] Take 10g of KOH and 100020g of polyethylene glycol in a three-necked stainless steel flask, heat it with an electric heating mantle until it is completely melted and raise the temperature to 150°C, then add 154g of wormwood oil (78.2% wormwood GC content) dropwise into the flask, reflux and The reaction was stirred for 1h. After completion of the reaction, cool to 80°C, add hot water to wash twice, stand to separate layers, put the obtained oil layer in the refrigerator, and refrigerate and crystallize at 2°C for 24 hours. The obtained crystals were crushed by adding 100 ml of ice-cold brine at -5°C, and separated by a centrifuge to obtain 106.8 g of anethole crude product.

[0027] The obtained crude anethole product was subjected to rectification and separation under the conditions of vacuum degree of 99.4KPa and reflux ratio of 6:1, and the fraction between 120°C was collected to obtain 97.8g of the final product, with a relative effective yield of 83.6% of anethole....

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Abstract

The invention relates to a method for synthesizing anethole by taking estragole oil as a raw material. The estragole oil is subjected to isomerization reaction in the presence of a basic catalyst, and is frozen, crystallized and separated, so as to obtain trans-anethole. The method is cheap in raw material and is simple and safe; meanwhile, the reuse value of a by-product is achieved, and the purity of the obtained anethole can be up to over 96% by optimization on rectification and extraction conditions, so that the method is applicable to industrial production.

Description

technical field [0001] The invention relates to a method for synthesizing anethole by using wormwood oil as a raw material, and belongs to the field of spice processing. Background technique [0002] Anethole, also known as anethole, anethole, etc., is divided into cis and trans isomers, and is the main component of star anise oil. Cis-anethole has a pungent and pungent odor and is toxic, so it is restricted to be used in small quantities. [0003] Trans-anethole has been confirmed by FEMA (No. 2086) as a food flavoring agent and flavoring agent. It is widely used in the food industry and is ingested in large quantities by the human body. It can also be widely used in the daily necessities industry and other industries as a masking agent. The structural formula of trans-anethole is as follows: [0004] [0005] In the prior art, natural anethole is mainly produced through an anise oil isolation method, such as the method for isolating high-purity anethole from anise oil...

Claims

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Application Information

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IPC IPC(8): C07C43/215C07C41/32
CPCC07C41/32C07C43/215
Inventor 刘六军邹志平
Owner BEIJING FORESTRY UNIVERSITY
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