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Process of preparing benzaldehyde through continuous hydrolysis of ammonia spirit catalytic of cinnamaldehyde in near critical water

A technology that catalyzes meat and near-critical water with ammonia water. It is applied in the fields of hydrolysis to prepare carbonyl compounds and organic chemistry. It can solve the problems of slow reaction speed and interstitial reaction, and achieve the effects of good aroma quality, stable quality and easy recycling.

Inactive Publication Date: 2007-12-05
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing benzaldehyde by continuous hydrolysis of cinnamaldehyde catalyzed by ammonia water in near-critical water, which mainly solves the problems of slow reaction speed and gap reaction in the existing method

Method used

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  • Process of preparing benzaldehyde through continuous hydrolysis of ammonia spirit catalytic of cinnamaldehyde in near critical water

Examples

Experimental program
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Effect test

Embodiment 1

[0017] The mixture of deionized water, cinnamon oil and ammonia water is preheated by a heat exchanger and enters a tubular reactor, and is hydrolyzed for 60 minutes under near-critical water conditions at 200°C, wherein the volume ratio of deionized water and cinnamon oil is 5:1, The ammonia concentration in the mixture is 5 mg / L (the hydrolysis time is controlled by the flow rate and the size of the reactor, the same below); the hydrolyzed product is cooled by a heat exchanger, and then decompressed by a back pressure valve to a flash evaporator, where it is removed by flash evaporation The ammonia gas can be recycled after being absorbed by the ammonia absorption tower; after the liquid phase product of the flasher is stratified by the liquid-liquid separator, the lower water phase is recycled, and the upper organic phase is vacuum distilled to obtain the benzaldehyde product. The conversion rate of cinnamaldehyde was 65%, and the yield of benzaldehyde was 57% (mol%, the sam...

Embodiment 2

[0019] The mixture of deionized water, cinnamon oil and ammonia water is preheated by a heat exchanger and enters a tubular reactor, and is hydrolyzed for 50 minutes under near-critical water conditions of 240°C, wherein the volume ratio of deionized water and cinnamon oil is 4:1, The ammonia concentration in the mixture is 20mg / L; the hydrolyzed product is cooled by a heat exchanger, then decompressed by a back pressure valve, and then sent to a flash evaporator, and the ammonia gas is removed by flash evaporation, and the ammonia gas can be recycled after being absorbed by the ammonia absorption tower Use: After the liquid phase product of the flash evaporator is stratified by the liquid-liquid separator, the lower water phase is recycled, and the upper organic phase is vacuum distilled to obtain the benzaldehyde product. The conversion rate of cinnamaldehyde was 84%, and the yield of benzaldehyde was 71%.

Embodiment 3

[0021] The mixture of deionized water, cinnamon oil and ammonia water is preheated by a heat exchanger and enters a tubular reactor, and is hydrolyzed for 40 minutes under near-critical water conditions of 260°C, wherein the volume ratio of deionized water and cinnamon oil is 3:1, The ammonia concentration in the mixture is 60mg / L; the hydrolyzed product is cooled by a heat exchanger, then decompressed by a back pressure valve, and then sent to a flash evaporator, and the ammonia gas is removed by flash evaporation, and the ammonia gas can be recycled after being absorbed by the ammonia absorption tower Use: After the liquid phase product of the flash evaporator is stratified by the liquid-liquid separator, the lower water phase is recycled, and the upper organic phase is vacuum distilled to obtain the benzaldehyde product. The conversion rate of cinnamaldehyde was 92%, and the yield of benzaldehyde was 79%.

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Abstract

This invention discloses a method to prepare benzaldehyde by ammonia-catalyzed continuous cinnamamide hydrolysis in near-critical aqueous media. The method includes following steps: a) the volume ratio of deionized water and cinnamon is 5:1~1:2 and the mixture of deionzed water, cinnamon and 5~200mg / L ammonia enters a tube reactor after preheated in a heat exchanger, the hydrolysis is carried out at 200~350 deg. C in near-critical aqueous conditions for 10~60 minutes; b) hydrolyzed products are cooled in a heat exchanger, decompressed by a unloading valve and go to a transient evaporator where ammonia is transient evaporated and absorbed by ammonia absorption tower for recycling; e) liquid products in the transient evaporator are separated in a liquid-liquid separator, and the lower aqueous layer is recycled and the upper organic layer is vacuum distilled to obtain benzaldehyde products. This invention has the advantages of greatly accelerated cinnamamide hydrolysis rate by only a small amount of ammonia, high yield, continuous operation, simple separation and environmentally friendly production.

Description

technical field [0001] The invention relates to a method for preparing benzaldehyde by continuous hydrolysis of cinnamaldehyde catalyzed by ammonia water in near-critical water. Background technique [0002] Benzaldehyde is a widely used food flavor. Its preparation methods can be divided into two categories: one is obtained by oxidation of toluene as raw material; the other is obtained by hydrolysis or ozonation of natural products as raw materials. The aroma quality of benzaldehyde prepared from natural products is better than that prepared from toluene, so it has higher economic value. There are mainly two methods for preparing benzaldehyde from natural products that have been reported so far: one is to use nuts containing amygdalin as raw materials, and prepare them through processes such as enzymatic hydrolysis and alkali washing. However, due to the highly toxic hydrocyanic acid produced in the hydrolysis process, it can only be qualified if it is completely removed, ...

Claims

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Application Information

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IPC IPC(8): C07C45/42C07C47/54
Inventor 吕秀阳任浩明
Owner ZHEJIANG UNIV