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A kind of preparation method of hydroxycitronellal

A technology of hydroxycitronellal and impregnation, which is applied in the field of fragrance chemistry and fine chemicals, can solve the problems of high polymer reaction and easy deactivation of catalysts, achieve high catalytic activity, avoid mist entrainment, and simplify the process flow Effect

Active Publication Date: 2021-12-03
SHANDONG NHU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a preparation method of hydroxycitronellal, which reduces the reaction temperature, improves the reaction conversion rate and yield, and solves the problems of easy deactivation of the catalyst and many reactive polymers, and is suitable for industrial production and catalytic systems. Can be recycled, environmentally friendly

Method used

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  • A kind of preparation method of hydroxycitronellal

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Embodiment 1

[0033] Embodiment 1 A kind of preparation method of hydroxycitronellal

[0034] Step 1, preparation of solid dehydrogenation catalyst:

[0035] Using zeolite as the carrier, the supported dehydrogenation catalyst was prepared by impregnation method, in which, the CuO loading rate in the zeolite was 7%, the ZnO loading rate was 2%, the NiO loading rate was 1%, and the K 2 The O loading rate is 0.1%; the above-mentioned zeolite loaded dehydrogenation catalyst is filled in a fixed bed with a pipe diameter of 7 cm, and the filling height is 5 m.

[0036] Step 2. Reaction

[0037] Configure 300g of hydroxycitronellol in the reaction kettle, enter the fixed bed after heating and vaporization, heat the fixed bed with heat transfer oil, control the reaction temperature at 200°C, the vacuum degree of the reaction system is 15kpa, and the mass space velocity is set at 5h -1 ;

[0038] The fixed bed top extraction fluid produced by the above reaction system is cooled from 200°C to 70-...

Embodiment 2

[0044] A kind of preparation method of hydroxycitronellal of embodiment 2

[0045] Step 1, preparation of solid dehydrogenation catalyst:

[0046] Using zeolite as the carrier, the supported dehydrogenation catalyst was prepared by impregnation method, in which the CuO loading rate in the zeolite was 5%, the ZnO loading rate was 4%, the NiO loading rate was 1%, and the K 2 O load rate 0.01%.

[0047] The above-mentioned zeolite loaded with dehydrogenation catalyst was filled in a fixed bed with a pipe diameter of 10 cm, and the filling height was 8 m.

[0048] Step 2. Reaction

[0049] Configure 300g of hydroxycitronellol in the reaction kettle, enter the fixed bed after heating and vaporization, heat the fixed bed with heat transfer oil, control the reaction temperature at 220°C, the vacuum degree of the reaction system is 20kpa, and set the mass space velocity to 8h -1 ;

[0050] The fixed bed top extraction fluid produced by the above reaction system is cooled from 200°...

Embodiment 3

[0054] Embodiment 3 A kind of preparation method of hydroxycitronellal

[0055] Step 1, preparation of solid dehydrogenation catalyst:

[0056] Using zeolite as the carrier, the supported dehydrogenation catalyst was prepared by impregnation method, in which the CuO loading rate in the zeolite was 8%, the ZnO loading rate was 1%, the NiO loading rate was 1%, and the K 2 O load rate 1%.

[0057] The above-mentioned zeolite loaded with dehydrogenation catalyst was filled in a fixed bed with a pipe diameter of 2 cm, and the filling height was 8 m.

[0058] Step 2. Reaction

[0059] Configure 300g of hydroxycitronellol in the reaction kettle, and enter the fixed bed after heating and vaporization, heat the fixed bed with heat conduction oil, control the reaction temperature at 150°C, the vacuum degree of the reaction system is 5kpa, and the mass space velocity is set at 2h -1 ;

[0060] The fixed bed top extraction fluid produced by the above reaction system is cooled from 200...

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Abstract

The invention provides a method for preparing hydroxycitronellal, which comprises the steps of preparing a solid dehydrogenation catalyst; the preparation of the solid dehydrogenation catalyst: adopts zeolite as a carrier to support the dehydrogenation catalyst. The zeolite supports an alkali metal oxide, and the alkali metal oxide can be K 2 O, Rb 2 O, Cs 2 Any one of O, preferably K 2 O, Cs 2 O, the mass ratio of the loading amount of the alkali metal oxide to the zeolite is: 0.001˜0.01:1, preferably 0.006˜0.008:1. The invention has simple process and high efficiency; the loaded solid dehydrogenation catalyst has easy-to-obtain raw materials, high catalytic activity and low reaction temperature.

Description

technical field [0001] The invention belongs to the fields of spice chemistry and fine chemicals, in particular to a preparation method of hydroxycitronellal. Background technique [0002] Hydroxycitronellal is one of the important bulk spices. The pure product is a viscous colorless liquid with a delicate and pleasant lily-of-the-valley and lily-like floral aroma. It is sweet and powerful. It is widely used in many daily chemical flavors In the formula, the dosage can reach 20%. It is mainly used to prepare citrus, watermelon, cherry and other melon and fruit flavors, thickening and thickening, making the fragrance round and harmonious. [0003] At present, the main catalysts for preparing hydroxycitronellal by catalytic dehydrogenation of hydroxycitronellol are metals and their oxides, such as copper, nickel, copper oxide, zinc oxide, etc. The catalyst is easily deactivated under high temperature conditions, and the reaction conversion rate is not high. Hydroxycitronellal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/19C07C45/00B01J23/80
CPCB01J23/002B01J23/80B01J2523/00C07C45/002C07C47/19B01J2523/13B01J2523/17B01J2523/27B01J2523/847
Inventor 马啸方万军黄冬樊国涛许鹏宋江刘正良殷治国谢坤于明
Owner SHANDONG NHU PHARMA
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