Synthesis process for o-chlorobenzaldehyde

A technology of o-chlorobenzaldehyde and synthesis process, which is applied in the directions of hydrolysis to prepare carbonyl compounds, organic chemistry, halogenated hydrocarbon preparation, etc. The generation of products, the improvement of product quality, the effect of improving quality

Inactive Publication Date: 2017-07-25
NANJING COLLEGE OF INFORMATION TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The problem to be solved by the present invention is that the process of producing o-chlorobenzaldehyde by the existing chlorination oxidation method is complex and difficult to purify, resulting in high production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 900g of o-chlorotoluene in a four-neck flask, stir under light, control the temperature at 100°C, feed chlorine gas, and react for 2 hours to obtain a chlorinated solution. The content of o-chlorobenzyl chloride in the chlorinated solution is 36.13%, and Benzyl chloride is 62.30%, o-chlorotrichlorobenzyl is 1.11%, and the chlorination product on the benzene ring is 0.36%. The above-mentioned chlorinated solution is heated to boiling under reduced pressure, and o-chlorobenzyl chloride is separated. When the content of o-chlorobenzyl chloride is lower than 1%, the heating is stopped, and the remaining mixed solution is reserved for hydrolysis reaction. Add the above residual liquid into the hydrolysis flask, control the temperature to 110°C, add the aqueous solution of catalyst ferric chloride and aluminum chloride under stirring, wherein the amount of catalyst is 0.015% of the mass of the mixed liquid, react for 2.5h, and hydrogen chloride gas is emitted at the begi...

Embodiment 2

[0021] Weigh 900g of o-chlorotoluene in a four-neck flask, stir under light, control the temperature at 110°C, feed chlorine gas, and react for 1.5h to obtain a chlorinated solution. The content of o-chlorobenzyl chloride in the chlorinated solution is 38.3%. Dichlorobenzyl 60.6%, o-chlorotrichlorobenzyl 1.1%. The above-mentioned chlorinated solution is heated to boiling under reduced pressure, and o-chlorobenzyl chloride is separated. When the content of o-chlorobenzyl chloride is lower than 1%, the heating is stopped, and the remaining mixed solution is reserved for hydrolysis reaction. Add the above residual liquid into the hydrolysis flask, control the temperature to 120°C, add the aqueous solution of catalyst ferric chloride and aluminum chloride under stirring, wherein the amount of the catalyst is 0.02% of the mass of the mixed liquid, react for 2 hours, and hydrogen chloride gas is emitted at the beginning of the reaction. Pass into water to obtain hydrochloric acid, t...

Embodiment 3

[0023] Weigh 900g of o-chlorotoluene in a four-neck flask, stir under light, control the temperature at 120°C, feed chlorine gas, and react for 100 minutes to obtain a chlorinated solution. The content of o-chlorobenzyl chloride in the chlorinated solution is 39.2%. Benzyl chloride is 58.7%, and o-chlorotrichlorobenzyl is 2.1%. The above-mentioned chlorinated solution is heated to boiling under reduced pressure, and o-chlorobenzyl chloride is separated. When the content of o-chlorobenzyl chloride is lower than 1%, the heating is stopped, and the remaining mixed solution is reserved for hydrolysis reaction, and o-chlorobenzyl chloride It is reused as a raw material, and the chlorination reaction of the previous step is carried out again to generate o-chlorodichlorobenzyl. Add the above residual liquid into the hydrolysis flask, control the temperature to 100°C, add the aqueous solution of catalyst ferric chloride and aluminum chloride under stirring, wherein the amount of the c...

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PUM

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Abstract

The invention discloses a synthesis process of o-chlorobenzaldehyde. The synthesis process of o-chlorobenzaldehyde comprises the following steps: feeding chlorine in o-chlorotoluene, carrying out catalytic chlorination under the condition of illumination to obtain chlorination liquid, wherein the ratio of the amount of the chlorine to the amount of the o-chlorotoluene is 2-4: 1, the reaction time is 1-2 hours, and the reaction temperature is 100-120 DEG C; distilling the chlorination liquid under reduced pressure, and separating out chlorobenzyl chloride and the o-chlorotoluene to obtain mixed liquid of o-chlorobenzyl dichloride and o-chlorobenzyl trichloride; carrying out hydrolysis reaction on the mixed liquid by using ferric chloride and zinc chloride as catalysts to obtain hydrolysate, wherein the temperature of hydrolysis reaction is 100-120 DEG C, a solvent is water, and the reaction time is 1.5-3 h; and carrying out rectification and purification on the hydrolysate in a vacuum state to obtain o-chlorobenzaldehyde. According to the technical scheme, the cost is further reduced, and the quality of the product is improved. Reasonable catalytic conditions are adopted, the synthesis process is a perfect greening technological synthesis method, generation of by-products is controlled effectively, and the quality of the product is improved further.

Description

technical field [0001] The present invention relates to the synthesis technique of benzaldehyde, in particular to the synthesis technique of o-chlorobenzaldehyde. Background technique [0002] O-chlorobenzaldehyde is an important intermediate in organic synthesis, mainly used in the manufacture of o-chlorobenzaldehyde, o-chlorobenzyl chloride and cloxacillin sodium as the main raw material for pharmaceuticals, and is also widely used in the manufacture of pesticides The raw material of high-efficiency acaricide products has a large market demand. [0003] The synthesis methods of o-chlorobenzaldehyde include chlorination hydrolysis, direct oxidation and indirect oxidation, the most common in industry is the chlorination hydrolysis. The classic chlorination hydrolysis process is to chlorinate o-chlorotoluene into o-chlorobenzyl chloride and then catalyze the hydrolysis to o-chlorobenzaldehyde. However, in addition to 80% o-chlorodichlorobenzyl, there are about 20% o-chlorobe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/43C07C47/55
CPCC07C17/14C07C45/43C07C47/55C07C22/04
Inventor 杨晓辉
Owner NANJING COLLEGE OF INFORMATION TECH
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