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Preparation method of nerolin

A technology of nerol ether and nerol, which is applied in the field of preparation of daily fragrances, can solve the problems of low product purity, limited product application scope, many by-products, etc., and achieves high product purity, easy purification and few by-products. Effect

Active Publication Date: 2014-12-24
HUNAN PROVINCE HONGJIANG HUAGUANG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The method of producing nerolidol in foreign countries mainly uses nerolidol as raw material and uses peroxide to oxidize. In this method, there are many by-products and low product purity, so the range of application of the product is limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] (1) Photosensitive oxidation of nerol to generate peroxy nerol: add a certain amount of nerol to the photosensitive reactor, then add 96% methanol with 1.5 times the volume of nerol, and 0.5% chlorophyll of nerol mass Powder, magnetically stirred at 250 rpm, stirred evenly, and then poured oxygen into the above-mentioned prepared solution, so that the flow rate of oxygen was controlled at 0.5m3 / h, and the pressure in the reactor was kept at 0.15 kg. Iodine tungsten light illumination, control the reaction temperature at 45 ° C, make the reaction continue for 25 hours, to obtain peroxynerol;

[0015] (2) Recovering the solvent: heating the oxide in the reactor to 40-50°C, recovering 60% of methanol under reduced pressure, and obtaining the nerolidol concentrated solution for later use;

[0016] (3) Reduction of nerol peroxide to nerolidol: Add distilled water with 2.5 times the volume of nerol and sodium sulfite with 1.2 times the mass of nerol into the reaction kettle, ...

Embodiment 2

[0021] (1) Photosensitive oxidation of nerol to generate peroxy nerol: add a certain amount of nerol to the photosensitive reactor, then add 97% methanol twice the volume of nerol, and chlorophyll with 1.2% nerol mass Powder, magnetically stirred at 300 rpm, stirred evenly, and then poured oxygen into the above-mentioned prepared solution, so that the flow rate of oxygen was controlled at 0.8m3 / h, and the pressure in the reactor was kept at 0.3 kg. Iodine tungsten light illumination, control the reaction temperature at 45 ℃, make the reaction continue for 30 hours, to obtain peroxynerol;

[0022] (2) Solvent recovery: heat the oxide in the reaction kettle to 40-50°C, recover 65% methanol under reduced pressure, and obtain nerolidol concentrate for use;

[0023] (3) Reduction of nerol peroxide to nerolidol: add distilled water with 3.5 times the volume of nerol and sodium sulfite with 1.25 times the mass of nerol into the reaction kettle, react while stirring, and control the r...

Embodiment 3

[0028] (1) Photosensitive oxidation of nerol to generate peroxy nerol: add a certain amount of nerol to the photosensitive reactor, then add 98.5% methanol with 2.5 times the volume of nerol, and 1.5% chlorophyll of nerol mass Powder, magnetically stirred at 280 rpm, stirred evenly, and then passed oxygen into the above-mentioned prepared solution, so that the flow rate of oxygen was controlled at 1.2m3 / h, and the pressure in the reactor was kept at 0.35 kg. Iodine tungsten light illumination, control the reaction temperature at 46 ℃, make the reaction continue for 28 hours, to obtain peroxynerol;

[0029] (2) Recovering the solvent: heating the oxide in the reactor to 40-50°C, recovering 60% of methanol under reduced pressure, and obtaining the nerolidol concentrated solution for later use;

[0030] (3) Reduction of nerol peroxide to nerolidol: add distilled water with 3.5 times the volume of nerol and sodium sulfite with 1.35 times the mass of nerol into the reaction kettle,...

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Abstract

The invention discloses a preparation method of nerolin. In order to overcome the defects that an existing preparation method of the nerolin has many byproducts, low product purity and limited production application, the preparation method comprises the following steps: generating nerol peroxide by carrying out photosensitized oxidation on nerol; recycling a solvent; reducing the nerolin peroxide into dinerol; inducing the dinerol by acid to generate nerolin; and purifying the nerolin. The preparation method is used for preparing nerolin, and is high in raw material conversion ratio, short in process route, gentle in reaction condition, energy-saving and environment-friendly, few in byproduct and high in product purity, so that an applied range of the nerolin is expanded, and the benefits are remarkably improved. According to the test and detection results, the mass fraction of the nerolin is 96%-98.5%, and the yield of the nerolin is 78-83.5%.

Description

technical field [0001] The invention relates to a preparation method of daily spices, in particular to a preparation method of nerolidol with nerol as the main raw material. Background technique [0002] Nerolido is naturally present in pomelo juice, white wine, rose oil, and geranium oil. It is a raceme and has a strong floral aroma, a scent like neroli oil, and a fresh green scent. Colorless to yellow liquid, insoluble in water, soluble in ethanol and other organic solvents, with high application value, widely used in the preparation of medicinal herbs, vegetables, cucumbers, tropical fruits, tea and other food flavors. [0003] The method for producing nerolidol abroad mainly takes nerolidol as raw material and uses peroxide to oxidize. In this method, there are many by-products and low product purity, so the range of application of the product is limited. Therefore, it is of great significance to develop a green synthesis process of nerolithin and obtain high-purity ner...

Claims

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Application Information

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IPC IPC(8): C07C43/20C07C41/01
CPCC07C29/132C07C41/01C07C407/00C07C407/003C07C409/04C07C33/02C07C43/202
Inventor 刘洪生付志雄石磊杨芳
Owner HUNAN PROVINCE HONGJIANG HUAGUANG BIOTECH
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