Separation and purification method of synthetic garlic oil

A technology for separation and purification of garlic oil, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as harm, toxic side effects, etc.

Inactive Publication Date: 2010-04-07
北京资源亚太饲料科技有限公司
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  • Abstract
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Problems solved by technology

At present, the synthetic garlic oil products have not been separated and purified, and most of them are used in feed additives and animal medicines, and there are also unscrupulous merchants who ...

Method used

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  • Separation and purification method of synthetic garlic oil

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Embodiment Construction

[0019] Synthesis:

[0020] Scheme 1: The synthetic product is mainly diallyl trisulfide.

[0021] Synthetic reaction principle:

[0022] CH 2 =CH-CH 2 -Cl+Na 2 S 2 o 3 ——CH 2 =CH-CH 2 S 2 o 3 Na+NaCl

[0023] 2CH 2 =CH-CH 2 S 2 o 3 Na+Na 2 S - CH 2 =CH-CH 2 -S-S-S-CH 2 -CH=CH 2 +2Na 2 SO 3

[0024] Specific steps:

[0025] 1. Add 205 kg of sodium thiosulfate (anhydrous) and 300 kg of water into a 1-ton reactor, close the feeding hole, start stirring, and heat to dissolve.

[0026] 2. After the sodium thiosulfate is dissolved, turn on the cooling water of the condenser, slowly add 90 kg of chloropropene, control the reaction temperature all the time, and react for 4 hours.

[0027] 3. Preparation of 1.0M potassium dihydrogen phosphate solution: Weigh 13.6 kg of potassium dihydrogen phosphate (anhydrous), dissolve in 100 kg of water, and stir evenly.

[0028] 4. Preparation of 1.0M sodium hydroxide solution: Weigh 4.0 kg of sodium hydroxide, dissolve in ...

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Abstract

The invention relates to a separation and purification method of synthetic garlic oil. The synthetic garlic oil contains 4-6 reaction products and unreacted reactants such as chloropropene and other components, wherein the useful components are diallyl disulfide and diallyl trisulfide, other components are useless, whereas chloropropene has stronger toxicity. The invention adopts an industrial chromatographic separation technology, the stationary phase is a T300 special chromatographic packing, the mobile phase is methanol and water, the ratio of which is 70:30, the flow rate is 280-300ml/min, the volume of a receiving bucket is 60L, and the total drip washing volume is 960L. After being detected by a high performance liquid chromatograph, the collected liquid is divided into four sections, wherein the second section and the third section can respectively obtain monomer pure products of the diallyl disulfide and the diallyl trisulfide by adding water and extracting; the contents of both the diallyl disulfide and the diallyl trisulfide are larger than 98%; and the monomer pure products of the diallyl disulfide and the diallyl trisulfide can replace natural garlic oil to be applied to the fields of medicines and foods, can also be used in animal feed additives and animal medicines, and have the advantages of environmental protection, safety and high efficiency. The cost of the synthetic garlic oil is only one tenth of the cost of the natural garlic oil and has considerable economic benefit.

Description

technical field [0001] The invention relates to an industrial chromatographic separation technology, specifically a method for separating and purifying a synthetic garlic oil product into diallyl trisulfide and diallyl disulfide. Background technique [0002] Garlic bulbs of Liliaceae plants contain a variety of functional active ingredients. Diallyl trisulfide (DATS) and diallyl disulfide (DDTS) are two of the most effective active ingredients identified so far. Diallyl trisulfide, which has the formula C 6 h 10 S 3 , has various pharmacological effects such as anti-tumor, prevention of cardiovascular and cerebrovascular diseases, anti-aging, anti-virus, anti-ulcer, and improving immunity of the body, and can be used to produce medical health products and allicin injections. Diallyl trisulfide is the main source of garlic aroma, so it is widely used in food as an additive to adjust food flavor; at the same time, diallyl trisulfide has great attraction to some animals suc...

Claims

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Application Information

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IPC IPC(8): C07C321/18C07C319/24C07C319/28
Inventor 莫少华刘钧贻徐国建曾清华
Owner 北京资源亚太饲料科技有限公司
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