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Method for preparing hydroxycitronellal through hydration reaction of citronellal

A technology for the hydration of hydroxycitronellal and malral, which is applied to the preparation of carbon-based compounds, the preparation of organic compounds, chemical instruments and methods, etc., to achieve the effects of simplified process flow, high selectivity, and reduced costs

Active Publication Date: 2020-10-27
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Comprehensive preparation routes of hydroxycitronellal in the prior art all have obvious technical defects, so there is an urgent need to develop a green synthesis process of hydroxycitronellal

Method used

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  • Method for preparing hydroxycitronellal through hydration reaction of citronellal
  • Method for preparing hydroxycitronellal through hydration reaction of citronellal
  • Method for preparing hydroxycitronellal through hydration reaction of citronellal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Pd / ZSM preparation:

[0065] 1) Preparation of Pd nano-sol

[0066] a) Take 10g polyvinylpyrrolidone, 5g Na 2 PdCl 4 Prepare a solution with 250g of water, and stir thoroughly at 10°C for 10h;

[0067] b) Take 3.86g NaBH 4 Add to the solution of a), fully stir at 10°C for 8h, then let it stand for 15h, and filter to obtain the nano-sol of metal Pd;

[0068] 2) Pd@SiO 2 preparation of

[0069] a1) Add 100g of ethanol and 10g of ammonia water (30wt%) into the metal Pd nano-sol, and fully stir for 5h at 10°C;

[0070] b1) Take 350.47 g of tetraethyl orthosilicate and add it to the mixture of a1), and fully stir at 10°C for 10 h;

[0071] c1) The mixture obtained in b1 was dried at 120°C for 15h to obtain 101.85g of SiO coated with Pd 2 , recorded as Pd@SiO 2 ;

[0072] 3) Preparation of Pd@ZSM

[0073] a2) Take 101.85g Pd@SiO respectively 2 , 1.44g AlOOH and 254.63g tetrapropylammonium hydroxide mixed and fully milled for 4h;

[0074] b2) Transfer the mixture ...

Embodiment 2

[0080] Pd / ZSM preparation:

[0081] 1) Preparation of Pd nano-sol

[0082] a) Take 20g polyvinylpyrrolidone, 5g Na 2 PdCl 4 Prepare a solution with 400g of water, and stir thoroughly for 1 hour at 15°C;

[0083] b) Take 2.58g NaBH 4 Add to the solution of a), fully stir at 25°C for 12h, then let it stand for 10h, and filter to obtain the nano-sol of metal Pd;

[0084] 2) Pd@SiO 2 preparation of

[0085] a1) Add 50g of ethanol and 20g of ammonia water (30wt%) into the metal Pd nano-sol, and fully stir for 1h at 15°C;

[0086] b1) Add 175.24 g of tetraethyl orthosilicate into the mixture of a1), and stir thoroughly at 30° C. for 15 h;

[0087] c1) The mixture obtained in b1 was dried at 110°C for 20 hours to obtain 51.81g of SiO coated with Pd 2 , recorded as Pd@SiO 2 ;

[0088] 3) Preparation of Pd@ZSM

[0089] a2) Take 51.81g Pd@SiO respectively 2 , 0.72g AlOOH and 233.15g tetrapropylammonium hydroxide were mixed and fully ground for 6h;

[0090] b2) transfer the ...

Embodiment 3

[0095] Pd / ZSM preparation:

[0096] 1) Preparation of Pd nano-sol

[0097] a) Take 30g polyvinylpyrrolidone, 5g Na 2 PdCl 4 Prepare a solution with 350g of water, and fully stir for 6 hours at 5°C;

[0098] b) Take 1.29g NaBH 4 Add to the solution of a), fully stir at 5°C for 2h, then let it stand for 20h, and filter to obtain the nano-sol of metal Pd;

[0099] 2) Pd@SiO 2 preparation of

[0100] a1) Add 150g of ethanol and 25g of ammonia water (30wt%) into the metal Pd nano-sol, and fully stir for 3h at 8°C;

[0101] b1) Add 35.05 g of tetraethyl orthosilicate to the mixture of a1), and stir thoroughly at 25°C for 13 hours;

[0102] c1) The mixture obtained in b1 was dried at 100°C for 10 h to obtain 11.78 g of Pd-coated SiO 2 , recorded as Pd@SiO 2 ;

[0103] 3) Preparation of Pd@ZSM

[0104] a2) Take 11.78g Pd@SiO respectively 2 , 0.13g AlOOH and 58.90g tetrapropylammonium hydroxide are mixed and fully ground for 1h;

[0105] b2) transfer the mixture obtained i...

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Abstract

The invention discloses a method for preparing hydroxycitronellal through a hydration reaction of citronellal. The method comprises the following step: under the action of a Pd-coated porous molecularsieve catalyst and an auxiliary agent, citronellal and water are subjected to a hydration reaction to synthesize hydroxyl citronellal in one step. The Pd / Si molar ratio of the Pd-coated porous molecular sieve catalyst is 1: (10-200), and the Si / Al molar ratio of the Pd-coated porous molecular sieve catalyst is (50-100): 1. The auxiliary agent is an ether substance, preferably 3-phenoxy toluene. Under the action of a porous solid catalyst and an auxiliary agent, the raw material citronellal and water are subjected to a catalytic hydration reaction to synthesize hydroxycitronellal in one step,and the method has the advantages of high selectivity, simplified process, less three wastes and the like.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a method for preparing hydroxycitronellal by using citronellal as a raw material through a hydration method. Background technique [0002] Hydroxycitronellal has a delicate and pleasant lily-of-the-valley and lily-like floral aroma, which is sweet and powerful. It is widely used in daily chemical essences. One of the staple spices. [0003] At present, the synthetic method of hydroxycitronellal mainly contains the following two routes: [0004] Route 1 Citronellal Aldehyde Group Protection Method [0005] A typical operation is to use citronellal as a raw material, use sodium bisulfite (or secondary amines such as dimethylamine) to protect the aldehyde group, then undergo a hydration reaction at the terminal double bond under acidic conditions, and finally obtain a hydroxyl group by deprotection Citronellal. This method is currently the mainstream production metho...

Claims

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Application Information

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IPC IPC(8): C07C47/19C07C45/64B01J31/28B01J31/02B01J29/068B01J35/10
CPCC07C45/64B01J31/28B01J31/0204B01J29/068C07C2531/28C07C2531/02C07C2529/068B01J2229/186B01J35/19B01J35/617C07C47/19Y02P20/584
Inventor 王联防董菁张永振黎源于斌成
Owner WANHUA CHEM GRP CO LTD
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