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Method for co-producing hydroxycitronellal and hydroxycitronellol

A technology of hydroxycitronellol and hydroxycitronellal, which is applied in chemical instruments and methods, preparation of hydroxy compounds, production of bulk chemicals, etc., can solve unsatisfactory technical methods, harsh reaction conditions, low conversion rate, etc. question

Active Publication Date: 2020-12-25
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The technical method of hydrating citronellol is not quite satisfactory, and the main problems involved are: (1) conversion rate is low (yield of about 40%); (2) by-product ether pollution is arranged
[0008] Therefore, the preparation routes of hydroxycitronellal and hydroxycitronellol in the comprehensive prior art all have obvious technical defects: (1) the reaction conditions are harsh, the catalyst is easily deactivated, and the reaction conversion rate and yield are relatively low; (2) ) There are many by-products, which adversely affect the aroma of the target product, and separation is difficult; (3) The requirements for equipment are high and there are many three wastes, and the post-processing is difficult

Method used

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  • Method for co-producing hydroxycitronellal and hydroxycitronellol
  • Method for co-producing hydroxycitronellal and hydroxycitronellol
  • Method for co-producing hydroxycitronellal and hydroxycitronellol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Cobalt oxide preparation:

[0073] a) Mix cobalt acetate, isopentyl glycol and triethylamine in a molar ratio of 1:1:2, place in an autoclave, heat up to 150°C in an airtight manner, separate solid and liquid after 8 hours of heat preservation, and obtain nano-cobalt oxide after drying. The diameter is 57nm, and the average surface roughness (Ra) is 1.43nm.

[0074] Preparation of hydrogenation catalyst CAT1:

[0075] a) 0.30g FeCl 3 , 10.47g RuCl 3 Dissolve in 20g of water, stir well until completely dissolved, and make impregnating solution;

[0076] b) adding the impregnation solution prepared in a) dropwise to 100 g of nano-cobalt oxide until the end of the dropwise addition, and completing the equal-volume impregnation of the metal salt solution;

[0077] c) roasting the mixture obtained in step b) at 500° C. under a nitrogen atmosphere for 5 hours, and then lowering to room temperature after the roasting is completed, to obtain a cobalt oxide-supported catalys...

Embodiment 2

[0093] Cobalt oxide preparation:

[0094] a) Mix cobalt acetate, isopentyl glycol and triethylamine at a molar ratio of 1:1.7:2.7, place in an autoclave, heat up to 170°C in a closed manner, separate solid and liquid after keeping warm for 2 hours, and obtain nano-cobalt oxide after drying. The diameter is 83nm, and the average surface roughness (Ra) is 2.8nm. ;

[0095] Preparation of hydrogenation catalyst CAT1:

[0096] a) 0.89g FeCl 3 , 8.37g RuCl 3 Dissolve in 20g of water, stir well until completely dissolved, and make impregnating solution;

[0097] b) adding the impregnation solution prepared in a) dropwise to 100 g of nano-cobalt oxide until the end of the dropwise addition, and completing the equal-volume impregnation of the metal salt solution;

[0098] c) Calcining the mixture obtained in step b) at 560° C. under a nitrogen atmosphere for 12 hours, and then lowering to room temperature after the roasting is completed, to obtain a cobalt oxide-supported catalys...

Embodiment 3

[0113] Cobalt oxide preparation:

[0114] a) Mix cobalt acetate, isopentyl glycol and triethylamine at a molar ratio of 1:2.6:3.6, place in an autoclave, heat up to 220°C in a sealed manner, separate solid and liquid after heat preservation for 14 hours, and obtain nano-cobalt oxide after drying. The diameter is 61nm, and the average surface roughness (Ra) is 2.3nm;

[0115] Preparation of hydrogenation catalyst CAT1:

[0116] a) 1.77g FeCl 3 , 6.28g RuCl 3 Dissolve in 20g of water, stir well until completely dissolved, and make impregnating solution;

[0117] b) adding the impregnation solution prepared in a) dropwise to 100 g of nano-cobalt oxide until the end of the dropwise addition, and completing the equal-volume impregnation of the metal salt solution;

[0118] c) roasting the mixture obtained in step b) at 620° C. under a nitrogen atmosphere for 16 hours, and then lowering to room temperature after the roasting is completed, to obtain a cobalt oxide-supported catal...

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Abstract

The invention discloses a method for co-producing hydroxycitronellal and hydroxycitronellol. The method comprises the following steps of: arranging a reactive rectification zone I, a common rectification zone and a reactive rectification zone II which are connected from top to bottom as a reactive rectification system, carrying out hydration reaction on citronellal and water in the reactive rectification zone II to prepare hydroxycitronellal, and carrying out hydrogenation reaction on citronellal and hydrogen in the reactive rectification zone I to generate citronellol, and bringing the citronellol into the reactive rectification zone II to be subjected to a hydration reaction to obtain hydroxycitronellol. Citronellal is fed from a tower kettle of the reactive rectification zone II; wateris fed from a tower kettle of the reactive rectification zone II; and hydrogen is fed from the common rectification zone. According to the method, citronellal is used as the raw material, and hydrogenation reaction, hydration reaction and rectification separation are combined to co-produce hydroxycitronellal and hydroxycitronellol. The technological process is greatly simplified, and the method has the advantages of high yield, few three wastes, high selectivity and the like.

Description

technical field [0001] The invention relates to a method for co-producing hydroxycitronellal and hydroxycitronellol by using citronellal as raw material by combining hydrogenation reaction, hydration reaction and rectification separation. Background technique [0002] Hydroxycitronellal has a lily-of-the-valley and lily-like floral aroma. It is one of the important bulk spices. It has a delicate and pleasant lily-of-the-valley and lily-like floral aroma. It is sweet and powerful, and is widely used in daily chemical flavors and fragrances. [0003] At present, the synthetic method of hydroxycitronellal mainly contains following two kinds: [0004] Route 1 uses citronellal as a raw material, uses sodium bisulfite (or secondary amines such as dimethylamine) to protect the aldehyde group, then undergoes a hydration reaction at the terminal double bond under acidic conditions, and finally obtains hydroxycitronellal by deprotection. This method is currently the mainstream produc...

Claims

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Application Information

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IPC IPC(8): C07C47/19C07C45/64C07C33/025C07C29/141C07C29/80B01J27/24
CPCC07C45/64C07C29/141C07C29/80B01J27/24C07C47/19C07C33/025Y02P20/10
Inventor 王联防董菁蔺海政于斌成
Owner WANHUA CHEM GRP CO LTD
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