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Method for preparing 2, 3, 4-trichloronitrobenzene through micro-channel nitration reaction

A technology of trichloronitrobenzene and nitration reaction, which is applied in the field of preparation of pesticide chemical intermediates, can solve the problems of large impurity ratio, difficult separation, poor selectivity, low production efficiency, etc., and achieves reduction of post-processing process and product purity High and low production cost

Active Publication Date: 2022-07-29
上海农帆生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem solved by the present invention is: the method for preparing 2,3,4-trichloronitrobenzene by using a kettle-type batch reactor currently has many processing steps, low production efficiency, low yield, and poor selectivity. The proportion of impurities is large, it is difficult to separate, the production capacity is low, the production cost is high, and the reaction is exothermic, the safety is poor, and the amount of three wastes is large.

Method used

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  • Method for preparing 2, 3, 4-trichloronitrobenzene through micro-channel nitration reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Mixed acid preparation: Mix 98% sulfuric acid and 95% nitric acid to obtain mixed acid, wherein the molar ratio of nitric acid and sulfuric acid is 1:4.0.

[0028] Preparation of raw materials: preheat and dissolve 1,2,3-trichlorobenzene without adding solvent 1,2-dichloroethane, in which the moles of 1,2,3-trichlorobenzene and 1,2-dichloroethane are The ratio was 1:0; no catalyst was added.

[0029] The temperature of the external heat exchanger was set to 70°C, that is, the preheating temperature was set to 70°C, so that the system circulation temperature reached equilibrium.

[0030] The 1,2,3-trichlorobenzene and mixed acid are respectively passed into the preheating module through a tetrafluoro advective pump for preheating, and then enter the reaction module of the microchannel continuous flow reactor. Adjust the flow rate of 1,2,3-trichlorobenzene to 4.2mL / min, adjust the flow rate of mixed acid to be 12.1mL / min, make the molar ratio of 1,2,3-trichlorobenzene an...

Embodiment 2

[0034] Mixed acid preparation: Mix 98% sulfuric acid and 95% nitric acid to obtain mixed acid, wherein the molar ratio of nitric acid and sulfuric acid is 1:1.08.

[0035] Preparation of catalyst caprolactam-m-hydroxybenzenesulfonate ionic liquid: add 0.2 moles of caprolactam and 40 mL of water to a round-bottomed flask to fully dissolve, and add 40 mL of m-hydroxybenzenesulfonic acid aqueous solution with a concentration of 5 mol / L dropwise in an ice-water bath with stirring, The reaction was carried out at room temperature for 18h. Rotary evaporation, washing with benzene, and vacuum drying at 65 °C to obtain caprolactam-m-hydroxybenzenesulfonate ionic liquid.

[0036] Preparation of raw materials: 1,2,3-trichlorobenzene and 1,2-dichloroethane, a solvent of equal quality, are prepared into a mixture, wherein the mixture of 1,2,3-trichlorobenzene and 1,2-dichloroethane is The molar ratio is 1:1.83; and the caprolactam-m-hydroxybenzenesulfonate ionic liquid is added therein, wh...

Embodiment 3

[0042] Mixed acid preparation: Mix 98% sulfuric acid and 95% nitric acid to obtain mixed acid, wherein the molar ratio of nitric acid and sulfuric acid is 1:1.08.

[0043] Preparation of catalyst caprolactam p-hydroxybenzenesulfonate ionic liquid: add 0.2 moles of caprolactam and 40 mL of water to a round-bottomed flask to fully dissolve, and add 40 mL of an aqueous solution of p-hydroxybenzenesulfonic acid with a concentration of 5 mol / L dropwise in an ice-water bath with stirring, The reaction was carried out at room temperature for 18h. Rotary evaporation, washing with benzene, and vacuum drying at 65 °C to obtain caprolactam p-hydroxybenzenesulfonate ionic liquid.

[0044] Preparation of raw materials: 1,2,3-trichlorobenzene and 1,2-dichloroethane, a solvent of equal quality, are prepared into a mixture, wherein the mixture of 1,2,3-trichlorobenzene and 1,2-dichloroethane is The molar ratio was 1:1.83; and the caprolactam-p-hydroxybenzenesulfonate ionic liquid was added t...

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Abstract

The invention discloses a method for preparing 2, 3, 4-trichloronitrobenzene through a micro-channel nitration reaction. The preparation method comprises the following steps: respectively inputting a mixture of 1, 2, 3-trichlorobenzene, a solvent (optional solvent) and a catalyst (optional catalyst), and mixed acid prepared from concentrated nitric acid and concentrated sulfuric acid into a preheating module in a microchannel continuous flow reactor through a constant-flux pump for preheating, and then entering a reaction module for reacting, and cooling the reactant flowing into the collecting tank, uniformly stirring, standing for layering, respectively conveying to an organic storage tank and an inorganic storage tank, and dehydrating the mixed acid in the inorganic storage tank for recycling. The preparation method is high in total yield and high in product purity, the raw material conversion rate and selectivity are further improved when the catalyst is adopted for preparation, the impurity proportion is small, the productivity is large, the production cost is relatively low, safety is good, the amount of three wastes is small, stability and repeatability are good, amplification can be achieved, and good application prospects are achieved.

Description

technical field [0001] The invention relates to a method for preparing 2,3,4-trichloronitrobenzene by microchannel nitration reaction, and belongs to the technical field of preparation of pesticide chemical intermediates. Background technique [0002] Acloxyfen is a diphenyl ether herbicide belonging to acloxyfen and is an inhibitor of protoporphyrin oxidase. Pre-emergence application to control broadleaf weeds and grass weeds such as sunflower, potato and winter wheat fields. And because of its relatively high efficiency, low toxicity, and low residues, it occupies an important position in the pesticide industry and is more and more widely used. 2,3,4-Trichloronitrobenzene is a key intermediate in the production of acifluorfen technical materials. The current production process is mainly by the amination of 2,3,4-trichloronitrobenzene through the 2-chlorine amination. Afterwards, etherification reaction with phenol is carried out to obtain acifluorfen. However, in the pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/08C07C205/12B01J19/00
CPCC07C201/08B01J19/0093C07C205/12Y02P20/54
Inventor 吴克崇吴海琴王攀登贾俊超
Owner 上海农帆生物科技有限公司
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