Nerol and geraniol preparation method

A technology for geraniol and nerol, which is applied in the field of preparation of nerol and geraniol, can solve the problems of high product impurities, reduced profitability, low product price, etc., and achieves low requirements for production equipment and easy separation and purification. , the effect of low production cost

Active Publication Date: 2018-12-07
WANHUA CHEM GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In summary, the above-mentioned method for preparing nerol and geraniol has a long process flow, low yield, high cost and more impurities in the prepared product, and poor fragrance, which limits the application of the product in the downstream essence, so the product price is relatively low. Inexpensive, reduces profitability

Method used

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  • Nerol and geraniol preparation method
  • Nerol and geraniol preparation method
  • Nerol and geraniol preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 3 L of steel balls with a diameter of 5 cm into a 10 L vertical ball mill reactor, then add 1.33 kg of sodium hydroxide, 1.00 kg of paraformaldehyde, and 2.5 g of tetrabutylphosphine bromide. Start the ball mill and turn on the heating to 70°C to preheat the material. After grinding for 10 minutes, remove the hot water from the jacket. Through the feeding port, add 5.07kg of citral into the ball mill reactor in 3 batches. At this time, the reaction is exothermic, and the temperature is lowered by cooling water to maintain the reaction at 65-75°C. After the addition of citral, the grinding reaction was continued for 3 hours to ensure that the conversion of citral was complete. Tracking method: Take out a small amount of reaction materials, add water to dissolve, extract once with ethyl acetate, and analyze the upper layer by gas chromatography.

[0034] Stop grinding, transfer the material to a vibrating screen to separate the slurry and steel balls, and use 15kg o...

Embodiment 2

[0036] Add 3 L of steel balls with a diameter of 3 cm into a 10 L vertical ball mill reactor, then add 1.20 kg of sodium hydroxide, 1.00 kg of paraformaldehyde, and 0.45 g of benzyltriphenylphosphine chloride. Start the ball mill and turn on the heating to 100°C to preheat the material. After grinding for 10 minutes, remove the hot water from the jacket. Through the feeding port, add 4.5kg citral to the ball mill reactor in 3 batches. At this time, the reaction is exothermic, and the temperature is lowered by cooling water to maintain the reaction at 95-100°C. After the addition of citral, the grinding reaction was continued for 1 hour to ensure that the conversion of citral was complete. Tracking method: with embodiment 1.

[0037] Stop grinding, transfer the material to a vibrating sieve to separate the slurry and steel balls, and use 26kg of 1,2-dichloroethane to rinse the steel balls during the sieving process. Transfer the slurry to a centrifuge, turn on the centrifuge...

Embodiment 3

[0039] Add 3 L of steel balls with a diameter of 5 cm into a 10 L vertical ball mill reactor, then add 1.5 kg of sodium hydroxide, 1.00 kg of paraformaldehyde, and 5.5 g of benzyltrimethylphosphine bromide. Start the ball mill and turn on the heating to 30°C to preheat the material. After grinding for 10 minutes, remove the hot water from the jacket. Through the feeding port, add 5.5kg of citral to the ball mill reactor in 3 batches. At this time, the reaction is exothermic, and the temperature is lowered by cooling water to maintain the reaction at 30-40°C. After the addition of citral, the grinding reaction was continued for 5 hours to ensure that the conversion of citral was completed. Tracking method: with embodiment 1.

[0040]Stop grinding, and transfer the material to the vibrating screen to separate the slurry and steel balls. Transfer the slurry to stop grinding, transfer the material to a vibrating sieve to separate the slurry and steel balls, and wash the steel b...

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Abstract

The invention discloses a nerol and geraniol solid-phase method production technology. The technology adopts citral, paraformaldehyde and sodium hydroxide as raw materials, adds quaternary phosphoniumsalt as an auxiliary agent, and performs a solid-phase reaction in a ball mill reactor. After completion of the reaction, the obtained slurry is subjected to sieving, centrifugation, washing, and finally distilled to obtain nerol and geraniol products. The process is the green and solid-phase synthesis process, the product is easy to separate and purify, and the by-product sodium formate is highin purity and can be directly sold. The process overcomes the disadvantages of more step, low yield, large amount of three wastes, and many impurities in products in a traditional process route, and has industrial value.

Description

technical field [0001] The invention relates to a preparation method of nerol and geraniol, in particular to a solid-phase production process of nerol and geraniol. Background technique [0002] Geraniol and nerol are very important flavoring and flavoring agents, which are widely used in food and daily chemical flavors. [0003] In the existing synthetic methods, geraniol and nerol need to be separated by rectification after multi-step synthesis, the route is long, the yield is low and the price is expensive. For example, Liu Xianzhang et al. (Forest Products Chemistry and Industry, 1989, 9(4), 11-19) synthesized myrcene (as shown in the following formula 1), followed by hydrogen chloride addition, esterification, and hydrolysis to obtain geraniol and neroli Alcohol mixture, and then separated by rectification to obtain pure product. [0004] [0005] Formula 1, synthesis of nerol and geraniol by myrcene [0006] For another example, Yang Shaoxiang et al. (Chemical Re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/14C07C33/02
CPCC07B2200/09C07C29/14C07C33/02
Inventor 信勇谢硕张永振何勇黎源李广琼孙钦鹤李晶姜庆梅
Owner WANHUA CHEM GRP CO LTD
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