P-nitro tribromotoluene synthesis process

A technology of nitrotribromotoluene and p-nitrotoluene, applied in the field of synthesis technology of p-nitrotribromotoluene, can solve the problems of complex production process, low production efficiency, unsuitable for large-scale production, etc. The effect of improving work efficiency, improving single-pass conversion rate and product yield

Inactive Publication Date: 2016-06-08
吕艳
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Problems solved by technology

In the current p-nitrobenzotribromotoluene synthesis process method, the technical process is not easy to implement, the resulting p-nitrobenzobromotoluene product has low purity, low single-pass conversion rate of reactants, complicated production process, low production efficiency and high cost. , not suitable for mass production

Method used

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Experimental program
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Effect test

Embodiment

[0011] The synthetic technique of the p-nitrobenzotribromotoluene of present embodiment, comprises the following steps:

[0012] (1) Add p-nitrotoluene to the reaction kettle, open the tail gas absorption device, and absorb the hydrogen bromide and excess bromine produced by the reaction with water; control the reaction temperature between 150°C, add bromine dropwise, and control the reaction time at 8 Hours; the reaction generates p-nitrodibromotoluene, and the temperature is lowered to 70°C;

[0013] (2) Put carbon tetrachloride, catalyst BTEAB, sodium hydroxide, and water into the above-mentioned reaction kettle in sequence, control the temperature between 50°C, then add bromine dropwise, the reaction time is 5 hours, and filter to obtain the crude product;

[0014] (3) Put the above crude product and ethanol into the reaction kettle, stir, heat up and reflux for 40 minutes, cool to room temperature, filter and dry to obtain the finished product.

[0015] The synthesis pro...

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PUM

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Abstract

The present invention discloses a p-nitro tribromotoluene synthesis process, which is characterized in that in a first-step reaction, p-nitro toluene is added to a reaction kettle, a tail gas absorption device is opened, hydrogen bromide and excess bromine produced from the reaction are absorbed with water, the reaction temperature is controlled at 130-180 DEG C, bromine is added in a dropwise manner, the reaction time is controlled at 3-8 h, p-nitro dibromotoluene is generated through the reaction, and cooling is performed to a temperature of 60-80 DEG C; and in a second-step reaction, carbon tetrachloride, a catalyst BTEAB, sodium hydroxide and water are sequentially poured into the reaction kettle, the temperature is controlled at 40-80 DEG C, bromine is added in a dropwise manner, the reaction time is 2-6 h, filtering is performed to obtain a crude product, the crude product and ethanol are poured into the reaction kettle, stirring and heating reflux are performed for 20-60 min, cooling is performed to achieve a room temperature, and filtering and drying are performed to obtain the finished product. According to the present invention, the whole production process has characteristics of stable operation, easy control, low cost, high yield, and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis process of p-nitrobenzotribromotoluene. Background technique [0002] The synthesis process of p-nitrobenzotribromotoluene at least includes absorption, drying, filtration, cooling and other processes. In the current p-nitrobenzotribromotoluene synthesis process method, the technical process is not easy to implement, the resulting p-nitrobenzobromotoluene product has low purity, low single-pass conversion rate of reactants, complicated production process, low production efficiency and high cost. , not suitable for mass production. Contents of the invention [0003] In order to overcome the above-mentioned technical problems existing in the prior art field, the object of the present invention is to provide a synthesis process of p-nitrobenzotribromolene. The present invention not only has simple production procedures and improves work effi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/11C07C201/12
Inventor 吕艳
Owner 吕艳
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