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Preparation method of hydroxycitronellal and adopted catalyst

A technology of hydroxycitronellal and catalyst, which is applied to the preparation of carbon-based compounds, the preparation of organic compounds, and catalysts for physical/chemical processes. It can solve the problems of high energy consumption, low selectivity, and low conversion rate, and achieve raw material conversion. High efficiency, high purity and yield, and the effect of inhibiting side reactions

Active Publication Date: 2022-04-08
SHANDONG NHU PHARMA +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The invention provides a method for preparing hydroxycitronellal by direct hydration reaction of citronellal. In the preparation method of hydroxycitronellal, a new catalyst is adopted, and under mild reaction conditions, high conversion rate and high selectivity are achieved. Hydroxycitronellal has been obtained, which solves the technical problems of low conversion rate, low selectivity and high energy consumption in the prior art, and has a good industrial application prospect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] In the three-necked flask, first add 200mL of absolute ethanol, and then add 0.1mol of Fe(NO 3 ) 3 9H 2 O, 0.08 mol of PdCl 2 2H 2 O, 0.2mol of 9,18-dithiobenzo-20-crown-6 ligand, start stirring, heat, and reflux for 2 hours until the precipitate no longer precipitates, cool, and stand still. Filter and wash repeatedly with absolute ethanol for 3 to 4 times, and place the obtained solid powder in a vacuum drying oven for storage for later use. Marked as 1# Catalyst.

Embodiment 2~44

[0056] According to the method of Example 1, the types and proportions of the added metal salt 1, metal salt 2 and ligands were changed to obtain the following catalysts (Table 1).

[0057] Table 1 Catalysts and preparation parameters corresponding to Examples 2-44

[0058] Example serial number metal salt 1 metal salt 2 Ligand The molar ratio of Catalyst number 2 Fe(NO 3 ) 3 9H 2 o

Embodiment 45

[0063] Example 45 Preparation of Hydroxycitronellal

[0064] The hydration reaction was carried out in a 500ml reactor, replaced by nitrogen three times, citronellal (154.25g), water and catalyst (Examples 1-44 and Comparative Examples 1, 2, 3) were added in sequence, and the reaction was kept at normal pressure. After the reaction, the gas chromatograph was used to analyze the reaction solution, and the conversion rate of citronellal and the selectivity of hydroxycitronellal were calculated. The results are shown in Table 2 below.

[0065] Table 2 Preparation of hydroxycitronellal

[0066] serial number catalyst no 香茅醛 : n 水

[0067] a The catalyst used in Comparative Example 3 is only the ligand: 9,18-dithiobenzo-20-crown-6.

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Abstract

The invention discloses a preparation method of citronellal hydroxylaldehyde and an adopted catalyst, and the preparation method comprises the following steps: under the action of a metal coordination catalyst, citronellal and water are subjected to a direct hydration reaction, and after the reaction is finished, post-treatment is performed to obtain the citronellal hydroxylaldehyde, the metal coordination catalyst is prepared by the following method: dissolving a metal salt 1, a metal salt 2 and a ligand in an alcohol solvent, heating and stirring for reaction, and after the reaction is finished, standing, filtering, washing and drying to obtain the metal coordination catalyst. According to the preparation method, a novel metal coordination catalyst is adopted to catalyze the reaction, the conversion rate of raw materials is high, side reactions are effectively inhibited, and the purity and yield of the product are improved.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of hydroxycitronellal and a catalyst used. Background technique [0002] Hydroxycitronellal, the chemical name is 3,7-dimethyl-7-hydroxyoctanal, the pure product is a viscous colorless liquid, with delicate and pleasant lily of the valley and lily-like floral aroma, sweet and powerful, Widely used in daily chemical flavors, often used as spices, to prepare clove, lily and other floral flavors for cosmetics; also used as a stabilizer for food flavors, to prepare lemon, cherry, citrus and other food flavors, and can play a role in reconciliation. It is an important bulk spice, and now the world's annual demand has reached thousands of tons. [0003] The synthesis of hydroxycitronellal mainly contains two methods according to the difference of starting materials: the one, using citronellol as raw material, successively obtain product through ...

Claims

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Application Information

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IPC IPC(8): C07C45/64C07C47/19B01J31/22
Inventor 籍晓飞马慧娟于明马啸孙荣钦范玉雪樊国涛朱全东
Owner SHANDONG NHU PHARMA
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