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Green method of synthessing benzaldehyde from near critical water

A green synthesis, near-critical water technology, used in hydrolysis to prepare carbonyl compounds, bulk chemical production, organic chemistry, etc., can solve the problems of waste lye need to be neutralized, low conversion rate, etc., achieve simple reaction process, achieve green The effect of chemical and high yield

Inactive Publication Date: 2005-03-23
ZHEJIANG UNIV
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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 method for the green synthesis of benzaldehyde in near-critical water, which solves the problems of strengthening the contact between the two phases, low conversion rate and neutralization of waste lye in the existing cinnamon oil alkaline hydrolysis method question
[0008] The advantage of the present invention is that no catalyst needs to be added in the reaction process, and the cinnamon oil is hydrolyzed in the near-critical water to generate benzaldehyde by utilizing the self-acid-base catalytic characteristics of the near-critical water and the characteristics of being able to dissolve organic matter, which solves the need for alkaline hydrolysis of the cinnamon oil. Strengthen the contact between the two phases and the problem of environmental pollution, the reaction process is simple, the yield is high, and the green production process is realized, laying the foundation for environmentally friendly industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Into a 500ml autoclave, inject 300ml of deionized water, blow nitrogen for 2 hours for deoxidation treatment, fill with nitrogen and pressurize, heat up to a temperature of 200°C and a pressure of 3MPa, and then inject 15ml of cinnamon oil (85% by mass of cinnamaldehyde %, the same below) reacts with 15ml ethanol (analytically pure, the same below), after reacting for 4hr, the product is emitted, and the cinnamaldehyde conversion rate is 26% through gas chromatography analysis, and the benzaldehyde yield is 18% (wt%, below same).

Embodiment 2

[0013] Into a 500ml autoclave, inject 300ml of deionized water, blow it with nitrogen for 5 hours for deoxidation treatment, fill it with nitrogen and pressurize, raise the temperature to 200°C and pressure 3MPa, and then inject 15ml of cinnamon oil and 30ml of ethanol to react. After 8 hours, the conversion rate of cinnamaldehyde was 40%, and the yield of benzaldehyde was 28%.

Embodiment 3

[0015] In a 500ml autoclave, inject 300ml of deionized water, blow with nitrogen for 0.5 hour for deoxidation treatment, fill with nitrogen and pressurize, heat up to a temperature of 240°C and a pressure of 5MPa, then inject 15ml of cinnamon oil and 30ml of methanol (analytical pure, The same below) reacted, the reaction time was 4hr, the conversion rate of cinnamaldehyde was 42%, and the yield of benzaldehyde was 28%.

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PUM

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Abstract

A process for synthesizing benzaldehyde in near-supercritical water without environmental pollution nicludes such steps as adding deionized water to high-pressure agitated reactor, deoxidizing, heating, adding laurel oil and solubilizer, reaction and vacuum distilling.

Description

technical field [0001] The invention relates to a green synthesis method of benzaldehyde in near-critical water. Background technique [0002] The aroma quality of natural benzaldehyde is better than that of chemical synthesis, and it is a widely used food flavor. The production methods that have been reported so far mainly contain the following three kinds. [0003] The traditional production method of natural benzaldehyde is to use nuts containing amygdalin as raw materials, and it is prepared through fermentation, hydrolysis, alkali washing and other processes. However, due to the highly toxic hydrocyanic acid produced in the hydrolysis process, it can only be obtained by completely removing it. Qualified product, so the production cost is higher. [0004] Cinnamon oil is a special product of my country, and has relatively large output in areas such as Guangxi, Guangdong, and Yunnan. The method of commercialization is to use cinnamon bark (or cinnamon branches and leave...

Claims

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Application Information

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IPC IPC(8): C07C45/42C07C47/54
CPCY02P20/54
Inventor 吕秀阳高飞
Owner ZHEJIANG UNIV
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