Preparation method of benzyl chloride and derivatives of benzyl chloride

A technology of derivatives, benzyl chloride, applied in the field of benzyl halide production technology, can solve the problems of poor selectivity of reaction conditions, irritating unpleasant odor, and difficulty in large-scale promotion, and achieves short reaction time, low cost, and low pollution. Effect

Pending Publication Date: 2020-01-31
江苏环保产业技术研究院股份公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Industrially commonly used benzyl chloride and its derivative preparation technology mainly contain following two kinds at present: one, substituted toluene carries out chlorination reaction by chlorine gas under high temperature condition, and this reaction conditions selectivity is poor, and yield is low, and in the reaction process, be accompanied by Serious exhaust gas pollution; two, adopt catalytic chlorination, utilize substituted toluene and N-chlorosuccinimide (NCS) as reaction raw material, prepare under catalyst condition, but because NCS itself has strong irritation and bad smell It is difficult to control the odor in actual production, and the reaction conditions are relatively complicated, so it is generally difficult to promote on a large scale in industry

Method used

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  • Preparation method of benzyl chloride and derivatives of benzyl chloride
  • Preparation method of benzyl chloride and derivatives of benzyl chloride
  • Preparation method of benzyl chloride and derivatives of benzyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Mix 184.3g of toluene, 233.8g of sodium chloride, 425.8g of sodium chlorate, 1000mL of water and 1000mL of dichloromethane into the body of the liquid-liquid injection intensified reactor through the feed port, open valve 1 and valve 2, and close Valve three, under the action of the circulation pump, the mixed liquid flows back from the discharge port through the circulation pump into the jet pipe and the flow restriction pipe, and is discharged from the through hole of the flow restriction pipe to form a circulation loop, and the circulation flow rate is 200L / h, cyclic reaction at 20 DEG C and natural light conditions for 1 hour, after the reaction was completed, 1M aqueous sodium thiosulfate solution was added to the obtained reaction solution, the mixed solution was filtered, and the filter cake was washed with water to obtain the crude product of chloromethylbenzene, The crude product was recrystallized with 98wt% ethanol, and after drying, 227.3 g of chloromethylbe...

Embodiment 2

[0035]Mix 212.3g of p-xylene, 155.8g of sodium chloride, 141.9g of sodium chlorate, 1000mL of water and 800mL of dichloromethane into the body of the liquid-liquid injection intensified reactor through the feed port, and open valve one and valve two , close the valve three, under the action of the circulating pump, the mixed liquid flows back from the discharge port through the circulating pump into the jet tube and the restrictor tube, and is discharged from the through hole of the restrictor tube to form a circulation loop, and the circulation flow is 300L / h, cyclic reaction at 30°C and natural light for 1 hour, after the reaction, add 1M sodium thiosulfate aqueous solution to the obtained reaction solution, filter the mixed solution, wash the filter cake with water to obtain p-dichlorobenzyl The crude product was recrystallized with 98wt% ethanol, and after drying, 317.3 g of p-dichlorobenzyl was obtained, with a yield of 90.71%.

Embodiment 3

[0037] Mix 212.3g of m-xylene, 350.6g of sodium chloride, 638.8g of sodium chlorate, 1500mL of water and 1000mL of dichloromethane into the body of the liquid-liquid injection intensified reactor through the feed port, and open valve one and valve two , close the valve three, under the action of the circulating pump, the mixed liquid flows back from the discharge port through the circulating pump into the jet tube and the restrictor tube, and is discharged from the through hole of the restrictor tube to form a circulation loop, and the circulation flow is 200L / h, cyclic reaction at 20°C and natural light for 1 hour, after the reaction, add 1M sodium thiosulfate aqueous solution to the obtained reaction solution, filter the mixed solution, wash the filter cake with water to obtain m-dichlorobenzyl The crude product was recrystallized with 98wt% ethanol, and after drying, 302.6 g of m-dichlorobenzyl was obtained with a yield of 86.51%.

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Abstract

The invention discloses a preparation method of benzyl chloride and derivatives of benzyl chloride. A liquid-liquid jet enhanced reactor is adopted. The preparation method comprises the following steps: dissolving substituted toluene shown in formula 1, sodium chloride and sodium chlorate into a mixed solvent; introducing an obtained mixed solution into a main body of the liquid-liquid jet enhanced reactor through a feeding port, opening a circulation system valve, under the action of a circulating pump, conveying the mixed solution to flow back into a jet flow pipe and a flow limiting pipe from a discharge port through the circulating pump, and discharging through a through hole of the flow limiting pipe to form a circulation loop, wherein the mixed solution is reacted for 0.5-2 hours atthe temperature of 20-40 DEG C under the natural illumination condition, and after the reaction is finished, treating the obtained mixed solution through aftertreatment to obtain the benzyl chloride shown in the formula 2 and the derivatives of the benzyl chloride. The method is low in cost, simple to operate, short in reaction time, small in pollution, good in selectivity, high in yield, mild incondition, low in energy consumption, high in safety coefficient and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of benzyl halide production technology, in particular to a preparation method of benzyl chloride and derivatives thereof. Background technique [0002] Benzyl chloride, as a benzylation reagent for heteroatom functional groups, is an important intermediate in organic synthesis and is widely used in various fields such as medicine, pesticides, dyes and chemical auxiliary agents. In recent years, with the expansion of its application scope and the increase of its usage, a chemical product variety with great market potential has been formed. Its series of products such as aldehydes and acids have also become industrial varieties with a certain scale. [0003] Industrially commonly used benzyl chloride and its derivative preparation technology mainly contain following two kinds at present: one, substituted toluene carries out chlorination reaction by chlorine gas under high temperature condition, and this react...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07C17/14C07C22/04B01J19/12B01J4/00
CPCB01J4/00B01J19/12C07C17/14C07C22/04
Inventor吴剑张玲玲陈飞何仁可
Owner江苏环保产业技术研究院股份公司