A kind of preparation method of p-chlorobenzaldehyde

A technology for p-chlorobenzaldehyde and p-chlorotoluene is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, and preparation of carbonyl compounds by hydrolysis. Total amount, high reaction selectivity, and the effect of improving selectivity

Active Publication Date: 2021-11-12
烟台舜康生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] 1. The substitution reaction conditions are harsh and the selectivity is low;
[0021] 2. The yield of hydrolysis reaction is low and the cost is high;
[0022] 3. The amount of hydrolyzed wastewater is large and the treatment is difficult

Method used

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  • A kind of preparation method of p-chlorobenzaldehyde
  • A kind of preparation method of p-chlorobenzaldehyde
  • A kind of preparation method of p-chlorobenzaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Substitution reaction:

[0068] Drop into the p-chlorotoluene of content 99.2% in the dry 500ml four-necked flask that has stirring paddle, chlorine gas pipe, nitrogen gas pipe, reflux condenser (condenser emptying port is connected to tail gas absorption device): 220.0g (1.7252mol ), Bromine: 2.5g. The outer wall of the four-necked flask was heated with heat transfer oil, and the temperature of the heat transfer oil was set at 90°C. Start stirring, turn on nitrogen, and feed 0.5 l / min nitrogen into the four-necked flask for protection. When the temperature of the heat transfer oil reaches 85°C, feed 0.5l / min chlorine gas into the four-necked flask to control the inner temperature of the four-necked flask to 85-90°C (pull out the nitrogen tube, measure the inner temperature with a thermometer, and control the temperature by adjusting the temperature of the heat transfer oil. internal temperature) for a substitution reaction. During the reaction process, the progress ...

Embodiment 2

[0078] Substitution reaction:

[0079] Drop into the p-chlorotoluene of content 99.2% in the dry 500ml four-necked flask that has stirring paddle, chlorine gas pipe, nitrogen gas pipe, reflux condenser (condenser emptying port is connected to tail gas absorption device): 220.2g (1.7268mol ), Bromine: 3.5g. The outer wall of the four-necked flask was heated with heat transfer oil, and the temperature of the heat transfer oil was set at 90°C. Start stirring, turn on nitrogen, and feed 0.5 l / min nitrogen into the four-necked flask for protection. When the temperature of the heat transfer oil reaches 85°C, feed 0.5l / min chlorine gas into the four-necked flask to control the inner temperature of the four-necked flask to 85-90°C (pull out the nitrogen tube, measure the inner temperature with a thermometer, and control the temperature by adjusting the temperature of the heat transfer oil. internal temperature) for a substitution reaction. During the reaction process, the progress ...

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Abstract

The invention discloses a preparation method of p-chlorobenzaldehyde, which uses p-chlorotoluene as a raw material to undergo a substitution reaction with chlorine under the action of a catalyst to obtain a mixture of p-chlorobenzyl chloride and p-chlorobenzylidene dichloride. The mixture of p-chlorobenzyl chloride and p-chlorobenzylidene dichloride undergoes hydrolysis reaction and air catalytic oxidation reaction under the action of a catalyst to obtain p-chlorobenzaldehyde. The present invention reduces the reaction temperature of the substitution reaction through the action of the catalyst, improves the selectivity of the substitution reaction, adopts the combination of the hydrolysis reaction and the air catalytic oxidation reaction to improve the yield of p-chlorobenzaldehyde, and reduces the yield of p-chlorobenzaldehyde through the mechanical application of the catalyst. The amount of waste water from the hydrolysis reaction.

Description

technical field [0001] The invention relates to the field of fine organic chemical synthesis, in particular to a method for preparing a fine chemical intermediate p-chlorobenzaldehyde. Background technique [0002] p-Chlorobenzaldehyde (4-chlorobenzaldehyde), English name: p-Chlorobenzaldehyde (4-Chlorobenzaldehyde). 4-Chlorobenzaldehyde is an important fine chemical intermediate, which is widely used in pesticides, medicines, dyes and other organic synthesis. In terms of pesticides, it is mainly used to synthesize the fungicide tebuconazole and the insecticide chlorfenapyr. In medicine, it is mainly used in the synthesis of sedatives such as Fenalu. In terms of dyes, it is mainly used in the synthesis of acid brilliant blue 6B and so on. [0003] Taking p-chlorotoluene as a raw material through substitution and hydrolysis to prepare p-chlorobenzaldehyde mainly contains the following three methods: 1. P-chlorotoluene is substituted with chlorine under ultraviolet light to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/43C07C47/55C07C17/14C07C25/02
CPCC07C17/14C07C45/43C07C47/55C07C25/02
Inventor 赵乐英
Owner 烟台舜康生物科技有限公司
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