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Preparation method of citronellol

A kind of technology of citronellol and citronellal, applied in the field of preparation of citronellol

Active Publication Date: 2013-07-03
广州百花香料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantage of this preparation method is that specially prepared catalysts have to be produced and used, and there is a risk of catalyst failure and having to be shut down and replaced at high cost
Not all companies can afford this high-cost and high-risk preparation method
At the same time, it is more dangerous to use pressurized hydrogenation process routes in cities, which also limits the use of such process routes.

Method used

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  • Preparation method of citronellol
  • Preparation method of citronellol

Examples

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preparation example Construction

[0019] The preparation method of citronellol of the present invention is characterized in that comprising the following steps:

[0020] (1) Put the solvent, reducing agent borohydride, antioxidant, and alkaline substances into the reduction pot and mix them, then perform pre-cooling treatment, and pre-cool to 0 O C~40 O During the time of C, citronellal is added dropwise in the described reducing pot, and dropwise process will control temperature at 0 O C~40 O C, after the dropwise addition, maintain at 0 O C~40 O Continue to react for 2 to 5 hours at a temperature of C;

[0021] (2) Recovering the solvent, washing with neutralizing water to obtain crude citronellol, and then performing vacuum distillation to obtain citronellol.

[0022] The present invention carries out the reaction equation of reduction reaction to citronellal as follows:

[0023]

[0024] Wherein the above-mentioned solvent adopts methanol or ethanol.

[0025] The above-mentioned borohydride is:...

Embodiment 1

[0034] Example 1: Pump 100Kg of methanol, 12Kg of reducing agent potassium borohydride, 0.33Kg of antioxidant B.H.T, 0.1Kg of 50%-80% potassium hydroxide into a clean and odorless reducing pot, and put 100Kg of qualified citronellal (above GC87%) Pull into the high slot. Start stirring, turn on freezing, and pre-cool to 0 O C~40 O C, drop citronellal at a constant speed, control the dropwise addition in 4 to 5 hours, and control the temperature of the dropping process at 0 O C~40 O c. After the dropwise addition, maintain the temperature at 15 O C~40 O C, continue to react for 2 to 5 hours, and the reaction ends. Confirm that the reducing pot of the equipment is open to the atmosphere, turn on the condensed water at the top of the tower and stir; then start to heat slowly, recover the methanol solvent, and control the recovery of methanol to account for 80%-90% of the amount of methanol injected, for the next batch of feeding. In order to avoid the recovered metha...

Embodiment 2

[0035] Example 2: Pump 70Kg of methanol, 30Kg of water, 12Kg of reducing agent potassium borohydride, 0.33Kg of antioxidant B.H.T, 0.1Kg of 50%-80% potassium hydroxide into a clean and odorless reducing pot, and put the qualified citronellal (GC87% Above) 100Kg pumped into the high slot. Start stirring, turn on freezing, and pre-cool to 0 O C~40 O C, drop citronellal at a constant speed, control the dropwise addition in 4 to 5 hours, and control the temperature of the dropping process at 0 O C~40 O c. After the dropwise addition, maintain the temperature at 15 O C~40 OC, continue to react for 2 to 5 hours, and the reaction ends. Confirm that the reduction pot of the equipment is open to the atmosphere (that is, the reduction pot is under normal pressure), turn on the condensed water at the top of the tower and stir; start to heat slowly, and the liquid temperature is required to be 120-122 ° C, and the top temperature is 70 ° C. Control the recovery of methanol to...

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PUM

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Abstract

The invention provides a preparation method of citronellol, comprising the following steps of: putting a solvent, a reducing agent of borohydride, an antioxidant and an alkaline substance in a reduction pot for mixing, then pre-cooling to 0-40 DEG C and dripping citronellal in the reduction pot, wherein the temperature is controlled within 0-40 DEG C in the dripping process, and continuing the reaction for 2-5 hours at the temperature of 0-40 DEG C after the dripping; and reclaiming the solvent, washing via neutralized water to obtain the crude citronellol and performing vacuum distillation to obtain the citronellol. Under the alkaline condition and by adopting the method of utilizing the borohydride to perform reduction reaction to the citronellal to obtain the target product citronellol, the invention has the advantages of simple preparation technology, secure production process and low raw material cost as the special catalyst is not needed and all the raw materials can be bought on the industrial market.

Description

technical field [0001] The invention relates to a preparation method of spices, in particular to a preparation method of citronellol. Background technique [0002] At present, in the fragrance industry, citronellol is an extremely important class of fragrance raw materials. Its rose and bay leaf-like fragrance is fresh and elegant, and it is a fragrance raw material widely used in rose and citronella fragrances. After years of use, the usage of citronellol is still flourishing and increasing year by year. Its current annual usage exceeds 5,000 tons. This product has always attracted the attention of major international flavor and fragrance companies. [0003] Traditionally, there is a method for hydrogenating citronellal to citronellol by catalytic hydrogenation or pressurized hydrogenation on a heterogeneous catalyst. In most cases, catalytic hydrogenation over heterogeneous catalysts is carried out using fixed-bed reactors to reap the advantages of continuous process oper...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C33/025C07C29/14
Inventor 高永芳焦亦正
Owner 广州百花香料股份有限公司