Continuous flow method for preparing benzaldehyde from benzyl dichloride through hydrolysis

A technology of benzyl dichloride and benzaldehyde, which is applied in the field of chemical production, can solve the problems of high equipment requirements, unstable operation, and large amount of wastewater, and achieve the effects of improving efficiency, reducing equipment investment, and reducing wastewater discharge

Active Publication Date: 2013-01-16
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The acidic or alkaline hydrolysis of benzyl dichloride is produced by hydrolysis in a traditional batch reactor, which has some problems such as large amount of waste water, high equipment requirements, unstable operation and unsafety.
In recent years, there have also been some continuous reports on the production of benzaldehyde by hydrolysis of benzyl dichloride, but there are characteristics such as high equipment requirements and complicated processes.
[0004] So far, there has been no technological research on the preparation of benzaldehyde by hydrolysis of benzyl dichloride in the Corning microchannel continuous flow mode. Process route of benzaldehyde

Method used

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  • Continuous flow method for preparing benzaldehyde from benzyl dichloride through hydrolysis
  • Continuous flow method for preparing benzaldehyde from benzyl dichloride through hydrolysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) The device used: select figure 1 Corning micro-channel reaction module (Corning straight channel module + Corning heart-shaped channel module), refer to figure 2 Determine the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.

[0023] (2) Set the volume flow rate of each metering pump as F dichlorobenzyl = 10ml / min, F industrial hydrochloric acid = 15ml / min, put the materials into the straight channel glass module for preheating, and set the temperature of the heat exchanger At 120°C, the molar ratio of water to benzyl dichloride is 10:1. The residence time of the reaction was 115s. The reaction product flows out of the reactor in the state of continuous flow of oil-water mixed phase after being cooled by a coiled ice-water bath.

[0024] (3) The product can be detected by gas chromatography after oil-water sepa...

Embodiment 2

[0026] (1) The device used: select figure 1 Corning micro-channel reaction module (Corning straight channel module + Corning heart-shaped channel module), refer to figure 2 Determine the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.

[0027] (2) Set the volume flow rate of each metering pump as F dichlorobenzyl = 10ml / min, F industrial hydrochloric acid = 15ml / min, put the materials into the straight channel glass module for preheating, and set the temperature of the heat exchanger At 130°C, the molar ratio of water to benzyl dichloride is 10:1. The residence time of the reaction was 115s. The reaction product flows out of the reactor in the state of continuous flow of oil-water mixed phase after being cooled by a coiled ice-water bath.

[0028] (3) The product can be detected by gas chromatography after oil-water sepa...

Embodiment 3

[0030] (1) The device used: select figure 1 Corning micro-channel reaction module (Corning straight channel module + Corning heart-shaped channel module), refer to figure 2 Determine the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.

[0031] (2) Set the volume flow rate of each metering pump as F dichlorobenzyl = 10ml / min, F industrial hydrochloric acid = 15ml / min, put the materials into the straight channel glass module for preheating, and set the temperature of the heat exchanger At 140°C, the molar ratio of water to benzyl dichloride is 10:1. The residence time of the reaction was 115s. The reaction product flows out of the reactor in the state of continuous flow of oil-water mixed phase after being cooled by a coiled ice-water bath.

[0032] (3) The product can be detected by gas chromatography after oil-water sepa...

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Abstract

The invention discloses a continuous flow method for preparing benzaldehyde from benzyl dichloride through hydrolysis, belonging to the technical field of chemical production. The continuous flow method is a method for preparing the benzaldehyde from the benzyl dichloride serving as raw material through catalytic hydrolysis of hydrochloric acid in a micro-channel reactor, and relates to the field of organic synthesis application. The raw material benzyl dichloride and industrial hydrochloric acid are pumped into the micro-channel reactor through a metering pump, and are preheated, mixed and reacted to obtain a benzaldehyde rough product. According to the method, the conventional benzaldehyde production time is shortened from several hours to several minutes; and the method has the advantages of easiness in operation, low equipment loss, small environment pollution and the like. The conversion rate of the benzyl dichloride reaches 69.2 percent, and the selectivity of the benzaldehyde is 100 percent.

Description

technical field [0001] The present invention relates to a continuous flow method for preparing benzaldehyde by hydrolysis of benzyl dichloride, more specifically a continuous flow production process for preparation of benzaldehyde by hydrolysis of benzyl dichloride in a Corning high-flux-microchannel reactor, It belongs to the technical field of chemical production. Background technique [0002] Benzaldehyde is an important chemical raw material and pharmaceutical intermediate, widely used in the synthesis of fine chemicals such as fragrances, dyes and drugs. [0003] At present, the existing production process of benzaldehyde is toluene side chain chlorination hydrolysis method and toluene oxidation method, and domestic manufacturers mostly adopt toluene side chain chlorination hydrolysis method. This method chlorinates the side chain of toluene to produce a mixture of benzyl chloride, benzyl dichloride and a small amount of benzyl trichloride, then rectifies to produce be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/54C07C45/43
Inventor 张跃陈代祥严生虎刘建武沈介发
Owner CHANGZHOU UNIV
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