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[Chemical Knowledge]：Production and manufacturing method and process flow of o-nitrochlorobenzene

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The manufacturing method
of o-nitrobenzene chloride
1. Introduction

o-nitrobenzene chloride is an important organic chemical raw material, widely used in dyes, medicine, pesticides and other fields. Therefore, it is of great practical significance to study the manufacturing method of o-nitrochlorobenzene. This paper will introduce the preparation of o-nitrochlorobenzene by nitration and chlorination with benzene, chlorine and nitric acid as raw materials.

2. experimental principle

The preparation reaction of o-nitrochlorobenzene mainly includes two steps of nitration reaction and chlorination reaction. First, benzene and mixed acid (nitric acid and sulfuric acid) nitration reaction to generate nitrobenzene, and then nitrobenzene and chlorine gas chlorination reaction to generate o-nitrochlorobenzene.

3. Experimental Steps

1. Nitration Reaction

In a 250mL three-necked flask equipped with a stirrer, a thermometer and a dropping funnel, 60mL of benzene and 60mL of mixed acid (the volume ratio of nitric acid to sulfuric acid is 1:1) were added, heated to 60 ° C., and the mixed acid was added dropwise. After completion of the dropwise addition, the reaction was continued with heating for 2 hours. After completion of the reaction, the reaction solution was poured into ice water to precipitate a yellow solid, which was filtered under suction and washed with cold water until neutral to obtain nitrobenzene.

2. Chlorination

In a 250mL three-necked flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, the nitrobenzene prepared above and 60mL of chloroform were placed and heated to 40°C. Then, 30mL chlorine gas was slowly added dropwise through a constant pressure dropping funnel, and the reaction temperature was controlled between 40-50°C. After the dropwise addition was completed, the reaction was stirred for 1 hour. After completion of the reaction, the reaction solution was poured into ice water to precipitate a yellow-green solid, which was filtered by suction and washed with cold water until it was neutral to obtain a crude product of o-nitrochlorobenzene.

4. Experimental results and discussion

1. Experimental results

Through the above experimental steps, we successfully prepared o-nitrochlorobenzene with high yield and purity of more than 90%.

2. Experimental discussion

In the nitrification reaction, the selection and dosage of the nitrating agent have a great influence on the experimental results. In this experiment, mixed acid was used as nitrating agent, and the ratio of nitric acid and sulfuric acid was 1:1. Under these conditions, the nitration reaction was relatively complete and the purity of the obtained nitrobenzene was relatively high. In the chlorination reaction, controlling the reaction temperature is the key. Too high temperature will increase the side reaction and affect the purity of the product. In this experiment, controlling the reaction temperature between 40-50 ℃ can effectively reduce the occurrence of side reactions and improve the purity of the product.

5. conclusion

In this paper, o-nitrochlorobenzene was prepared from benzene, chlorine and nitric acid by nitration and chlorination reaction. The experimental results show that the method is simple, the yield is high, and the purity is more than 90%. By controlling the reaction conditions and optimizing the experimental operation, the purity and yield of the product can be further improved.

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