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Method for preparing citronellol from hydrogenated citral

A technology of citral and citronellol, which is applied in the field of hydrogenated citral preparation, can solve the problems that common catalysts cannot achieve effects, affect product yield and production efficiency, shorten the life of catalysts, etc. Rapid, selective effect

Pending Publication Date: 2022-03-08
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] CN102295531A improves the reaction conversion rate and reaction selectivity by improving the catalyst, but the realization of this effect depends on the specific catalyst type, common catalysts cannot achieve a considerable effect, and the reaction selectivity needs to be further improved
[0007] In the above-mentioned patents, the generation of excessive hydrogenation products cannot be avoided, and the problem of shortening the life of the catalyst with the increase in the number of times the catalyst is applied has not been solved, which seriously affects the product yield and production efficiency

Method used

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  • Method for preparing citronellol from hydrogenated citral
  • Method for preparing citronellol from hydrogenated citral
  • Method for preparing citronellol from hydrogenated citral

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0047] Preparation of citral raw materials with different metal ion contents

[0048] Add metal ion compound to the citral obtained by the above preparation and stir evenly to obtain citral raw material sample A, sample B, sample C and sample D of different metal ion content, add complexing agent ethylenediaminetetraacetic acid to sample B To reduce the metal ion content in citral, the test results are as follows.

[0049]

preparation example

[0051]Metal cobalt, nickel, molybdenum and aluminum are fused at high temperature according to the mass ratio of 25%, 30%, 5% and 40% respectively, the alloy is cooled to room temperature, pulverized, and alloy particles of 50-400 mesh are screened. Prepare 500 g of sodium hydroxide solution with a concentration of 20%, boil it, slowly add 100 g of alloy particles, continue to boil for 4 hours, and cool. Pour off the gray upper layer of turbid liquid, add water and wash it repeatedly at room temperature for 3 times. After standing still, the liquid layer is clear and transparent, and the pH value is less than 10. The prepared M2 catalyst has a cobalt content of 31% and a nickel content of 37% as detected by ICP, and is stored under the liquid level of the water seal for future use.

Embodiment

[0053] Transfer a certain amount of catalyst and citral to the autoclave, use nitrogen to replace the gas in the autoclave three times, use hydrogen to replace the nitrogen in the autoclave, adjust the hydrogen pressure to 3MPaA, start stirring, raise the temperature to 50°C for 5 hours, and use gas chromatography The conversion rate of citral was measured, and the citronellol product was obtained after removing the catalyst by filtration.

[0054]

[0055]

[0056] It can be seen from the above examples and comparative examples that when the metal ion content in the citral raw material is controlled within the range of 10ppm-100ppm, the catalyst activity can be adjusted to reduce excessive hydrogenation and improve selectivity.

[0057] Application example of catalyst

[0058] Repeat the conditions of Example 2, Example 4, Comparative Example 1 and Comparative Example 2, filter and recover the catalyst and apply mechanically, the reaction results are as follows:

[005...

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Abstract

The invention provides a method for preparing citronellol by hydrogenating citral, which comprises the following steps: providing a citral raw material, hydrogenating citral under the catalysis of a catalyst to obtain citronellol with high selectivity, and by controlling the mass content of metal ions in the citral raw material to be 10-100ppm, the selectivity of citronellol can be obviously improved, and the purity of citronellol is improved. And the problem that the service life of the catalyst is shortened along with increase of catalyst application times is solved.

Description

technical field [0001] The invention relates to the field of preparation of hydrogenated citral, in particular to a method for preparing citronellol by hydrogenated citral. Background technique [0002] Citronellol is an important spice raw material with a sweet floral smell, similar to the smell of roses. It is often used in rose and citrus flavors, and can be used to manufacture dihydrocitronellol, hydroxydihydrocitronellal raw materials. Citronellol can also be used in edible flavors, such as soft drinks, baked goods, candy, jelly pudding, etc., and is one of the bulk flavor raw materials. [0003] The citral molecule contains hydrogenated isolated C=C double bonds, C=O bonds and carbonyl-conjugated C=C double bonds, and the products that may be generated after hydrogenation are more complex. With the different catalysts and reaction conditions, the hydrogenation reaction may occur in different parts, and as the reaction time prolongs, the excessive hydrogenation produc...

Claims

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Application Information

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IPC IPC(8): C07C29/141C07C33/025B01J23/883
CPCC07C29/141B01J23/883C07C33/025Y02P20/584
Inventor 李康董菁于磊张永振黎源
Owner WANHUA CHEM GRP CO LTD
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