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Method for extracting alpha and beta-unsaturated ketone from illicium verum rectifying kettle residual liquor

A star anise, unsaturated technology, applied in the field of recycling useful substances, can solve the problems of high cost and complicated synthesis process, and achieve the effect of improving grade, improving aroma and reducing miscellaneous gas

Active Publication Date: 2016-02-10
黎芷杉
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Problems solved by technology

[0004] The α, β-unsaturated ketones reported in the public literature are mainly synthesized from aldehydes, ketones, alcohols and alkenes as starting materials, which require different raw materials and catalysts, but many synthetic processes are complex and costly, so from natural plants Extracting α, β-unsaturated ketones is a good direction

Method used

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  • Method for extracting alpha and beta-unsaturated ketone from illicium verum rectifying kettle residual liquor
  • Method for extracting alpha and beta-unsaturated ketone from illicium verum rectifying kettle residual liquor
  • Method for extracting alpha and beta-unsaturated ketone from illicium verum rectifying kettle residual liquor

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Embodiment 1

[0034] Take 100 g of star anise residue, add 300 ml of ethyl acetate, stir at room temperature for 2 hours, filter off the insoluble matter to obtain the filtrate, weigh 100 g of column chromatography silica gel, add to the filtrate, and mix the sample;

[0035] Weigh 820g column chromatography silica gel column, and use pure cyclohexane, cyclohexane: ethyl acetate = 50:1, 10:1, 5:1, 1:1 mixed solvent gradient elution, each bottle flow Tap liquid 250ml;

[0036] Each fraction was detected by thin-layer chromatography, and the combined bottle numbers were as follows: HY-1 (1-26 bottles), HY-2 (27-32 bottles), HY-3 (33-37 bottles), HY-4 ( 38-50 bottles), HY-5 (51-77 bottles), HY-6 (78-81 bottles), HY-7 (82-88 bottles), HY-8 (89-99 bottles), HY-9 (100 bottles -109 bottles), HY-10 (110-127 bottles);

[0037] Distill HY-7 to remove the solvent under reduced pressure to obtain 5.1g of viscous material, mix the sample with 10g of silica gel for column chromatography, weigh 120g of ...

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Abstract

The invention provides a method for recycling usable materials from waste of spice of natural plants, and particularly relates to a method for extracting alpha and beta-unsaturated ketone from illicium verum rectifying kettle residual liquor. The method comprises the steps that after the illicium verum rectifying kettle residual liquor is dissolved, 1,4-bi(4-methoxyphenyl)-3-butene-2-keto is obtained after two-time column chromatography on silica gel, one-time gel column chromatography and ethyl acetate recrystallization. Industrial waste is further extracted and utilized, and the usable material alpha and beta-unsaturated ketone is separated out from the industrial waste.

Description

technical field [0001] The invention relates to the technical field of extracting spices from natural plants, in particular to a method for recovering useful substances from wastes of extracting spices from natural plants. Background technique [0002] Star anise is a Magnoliaceae plant, and its Latin name (IlliciumverumHooK.f.) is an evergreen tree. It is a special aromatic plant in my country, mainly distributed in Guangxi, Guangdong, Guizhou, Yunnan and other provinces. Guangxi is the main production area of ​​star anise in my country, and its output accounts for 85% of the country and 70% of the world. The star anise tree has become one of the important economic tree species in the local mountainous areas. Star anise and star anise oil are excellent food seasonings that people like to use. Star anise oil has a spicy aroma of star anise, also known as star anise. In addition to being used as a seasoning spice, it is widely used in food industry, brewing industry, beverage...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/255C07C45/78A24B15/30
Inventor 林葵黄岛平韦英亮黄和明张思敏谢集照徐慧陈秋虹黄文琦
Owner 黎芷杉
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