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A kind of synthetic method of 2,6-dichlorobenzaldehyde

A technique for the synthesis of dichlorobenzaldehyde and its synthesis method, which is applied in the field of synthesis of 2,6-dichlorobenzaldehyde, which can solve the problems that the catalyst cannot be reused, the process is long and complicated, and the sale of by-products is limited, so as to facilitate industrial production , avoid pollution, high yield effect

Active Publication Date: 2022-07-12
DALIAN QIKAI MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The above methods are all two-step reactions, the process is long and complicated, and chlorine gas participates in the reaction, each step generates a large amount of hydrogen chloride gas, which is highly corrosive to equipment, and the waste water produced by absorbing hydrogen chloride contains a small amount of chlorine gas (hypochlorous acid) as a by-product limited sales
Catalysts cannot be reused, resulting in waste

Method used

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  • A kind of synthetic method of 2,6-dichlorobenzaldehyde

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Experimental program
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Effect test

Embodiment 1

[0028] Preparation method of self-made composite supported catalyst:

[0029] Take 19g of copper nitrate and 29g of cobalt nitrate, add 100ml of deionized water, stir to dissolve, then add 30g of activated alumina, mix well and soak at room temperature for 12-24 hours, then dry at 110°C to constant weight, then at 600-800 calcined at ℃ for 5 to 8 hours to obtain an activated alumina-supported copper-cobalt catalyst. Weigh, and increments are calculated according to the proportion of solute in the solvent.

Embodiment 2

[0031] At room temperature, 80.5g (0.5mol) of 2,6-dichlorotoluene, 270g of methanol, 6.6g of self-made copper-cobalt composite supported catalyst (0.02mol of active ingredient) and 11g of water (0.6mol) were added to a 1000mL stainless steel autoclave. , and then closed the autoclave. Turn on the stirring and test the pressure with nitrogen until no leakage occurs.

[0032] Oxygen replaces the gas in the autoclave three times, heats up to 45°C to stop heating, controls the temperature of the autoclave to 45-60°C through the flow rate of circulating water in the jacket, uses intermittent method to introduce oxygen into the autoclave to 0.5MPa, closes the air inlet valve, when the oxygen pressure When it drops to 0.1MPa, oxygen is injected again, and the oxygen pressure is reduced from 0.5MPa to 0.1MPa for a total of 5-6 times (that is, the amount of oxygen consumed is ~0.5mol). The 2,6-dichlorotoluene ≤ 1% detected by HPLC was regarded as the end of the reaction.

[0033] The...

Embodiment 3

[0035] At room temperature, 80.5g (0.5mol) of 2,6-dichlorotoluene, 400g of methanol, 6.6g of self-made copper-cobalt composite supported catalyst (0.02mol of active ingredient) and 15g of water (0.83mol) were added to a 1000mL stainless steel autoclave. , and then closed the autoclave. Turn on the stirring and test the pressure with nitrogen until no leakage occurs.

[0036] Oxygen replaces the gas in the autoclave three times, heats up to 45°C and stops heating, controls the temperature of the autoclave to 45-55°C through the flow rate of circulating water in the jacket. When it drops to 0.1MPa, oxygen is introduced again, and the oxygen pressure is reduced from 0.5MPa to 0.1MPa for 6-7 times (ie, the amount of oxygen consumed is ~0.5mol). The 2,6-dichlorotoluene ≤ 1% in HPLC was regarded as the end of the reaction.

[0037] The reaction kettle was cooled to room temperature, and the oxygen in the kettle was evacuated. Filter the material in the kettle, rinse the filter ca...

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Abstract

The invention discloses a method for synthesizing 2,6-dichlorobenzaldehyde, and belongs to the field of fine chemicals. Using 2,6-dichlorotoluene as a starting material, in the presence of a composite supported catalyst, 2,6-dichlorobenzaldehyde is obtained by intermittently passing oxygen in an autoclave in one step. The synthesis method uses cheap industrial chemicals as raw materials and reaction reagents, adopts supported catalysts, realizes the recycling of solvents and catalysts, and reduces the generation of waste gas and waste water; intermittent oxygen supply improves the production safety factor and avoids the occurrence of side reactions. Thus, production efficiency and reaction yield are improved, energy saving and environmental protection are realized and production costs are reduced.

Description

technical field [0001] The invention discloses a method for synthesizing 2,6-dichlorobenzaldehyde, which belongs to the field of fine chemical intermediate synthesis. Background technique [0002] 2,6-Dichlorobenzaldehyde is an important fine chemical intermediate with white crystal appearance. It can be used to manufacture fungicides, insecticides, herbicides, dyes and pigments, medicines and other chemical raw materials. The most common synthetic methods are: [0003] 6-Chloro-o-nitrotoluene and chlorine were photochlorinated under the action of phosphorus pentachloride and pyridine to synthesize 2,6-dichlorobenzylidene dichloride, and then hydrolyzed in formic acid under the catalysis of zinc chloride to obtain 2,6-dichlorobenzide Chlorobenzaldehyde, refer to Chinese patent CN1775747A. [0004] 2,6-Dichlorotoluene and chlorine were chlorinated to synthesize 2,6-dichlorobenzylidene dichloride under phosphorus pentachloride and photocatalysis, and then hydrolyzed in acidi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/36C07C47/55B01J23/75
CPCC07C45/36B01J23/75C07C47/55Y02P20/584
Inventor 孙立芹裴雄张洪学姜殿宝
Owner DALIAN QIKAI MEDICAL TECH
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