Low-temperature synthesis method of 2,6-dichloro-4-nitroaniline

A technology for nitroaniline and p-nitroaniline, which is applied in the field of low-temperature synthesis of 2,6-dichloro-4-nitroaniline, can solve the problems of reduced concentration of hydrochloric acid solution, generation of waste water, and high production cost, and achieves the cost of raw materials Low energy consumption, less by-products

Active Publication Date: 2015-05-06
江苏艾科维科技股份有限公司
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Problems solved by technology

However, this process will consume hydrogen chloride to reduce the concentration of hydrochloric acid solution. During the reaction process, a l

Method used

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  • Low-temperature synthesis method of 2,6-dichloro-4-nitroaniline
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  • Low-temperature synthesis method of 2,6-dichloro-4-nitroaniline

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Embodiment 1

[0033] Embodiment 1, a kind of preparation method of 2,6-dichloro-4-nitroaniline, take p-nitroaniline as raw material, carry out the following steps successively:

[0034] 1), after mixing 140mL of 35wt% concentrated hydrochloric acid (1.6mol) and 100mL water as dilute hydrochloric acid, the concentration of this dilute hydrochloric acid is 25.6wt% (marked value).

[0035] Put 13.8g (0.1mol) of p-nitroaniline (0.1mol) and the above dilute hydrochloric acid into a 500mL three-necked flask, cool to -8°C in a low-temperature tank under mechanical stirring, and control at this temperature, pass in about 0.3mol of chlorine gas, stir, and carry out Chlorination reaction; keep stirring for 2h (at this time, TLC detects that the reaction of raw materials is complete).

[0036] After the reaction, the reaction liquid was left naturally at room temperature, and a pale yellow solid was precipitated, which was filtered to obtain a filter cake of 2,6-dichloro-4-nitroaniline and the filtrat...

Embodiment 2

[0040] Embodiment 2, a kind of preparation method of 2,6-dichloro-4-nitroaniline, take p-nitroaniline as raw material, carry out the following steps successively:

[0041] 1), 110mL of 35% concentrated hydrochloric acid (1.27mol) and 130mL of water are mixed as dilute hydrochloric acid, and the concentration of the dilute hydrochloric acid is 20.8%wt% (marked value).

[0042] Put 13.8g (0.1mol) of p-nitroaniline (0.1mol) and the above-mentioned dilute hydrochloric acid into a 500mL three-necked flask, and under mechanical stirring, cool to -10°C in a low-temperature tank. reaction; insulated and stirred for 1 h (at this time, TLC detected that the reaction of the raw materials was complete).

[0043] After the reaction, the reaction liquid was left naturally at room temperature, and a pale yellow solid was precipitated, which was filtered to obtain a filter cake of 2,6-dichloro-4-nitroaniline and the filtrate (which was the mother liquor of hydrochloric acid). After the filte...

Embodiment 3

[0047] Embodiment 3, a kind of preparation method of 2,6-dichloro-4-nitroaniline, take p-nitroaniline as raw material, carry out the following steps successively:

[0048] 1), after mixing 195mL of 35% concentrated hydrochloric acid (2.2mol) and 45mL of water as dilute hydrochloric acid, the concentration of this dilute hydrochloric acid is 31.2wt% (standard value).

[0049] Put 13.8g (0.1mol) of p-nitroaniline (0.1mol) and the above-mentioned dilute hydrochloric acid into a 500mL three-necked flask, and under mechanical stirring, cool to -6°C in a low-temperature tank. reaction; insulated and stirred for 2h (at this time, TLC detected that the reaction of raw materials was complete).

[0050] After the reaction, the reaction liquid was left naturally at room temperature, and a pale yellow solid was precipitated, which was filtered to obtain a filter cake of 2,6-dichloro-4-nitroaniline and the filtrate (which was the mother liquor of hydrochloric acid). After the filter cake ...

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Abstract

The invention discloses a low-temperature synthesis method of 2,6-dichloro-4-nitroaniline. The method comprises the following steps sequentially: (1) by taking 20-35% diluted hydrochloric acid or a filtrate obtained in the following step (2) as a solvent I, firstly adding p-nitroaniline into the solvent I, then, introducing chlorine gas for chlorination reaction, naturally standing a reaction solution at room temperature after the reaction ends, and filtrating so as to obtain 2,6-dichloro-4-nitroaniline and hydrochloric acid mother liquor; (2) by taking the hydrochloric acid mother liquor as a solvent II, adding the solvent II into a three-mouthed flask, then, adding p-nitroaniline, dropwise adding hydrogen peroxide, carrying out stirring reaction while carrying out heat preservation after dropwise adding is completed, naturally standing at room temperature after the reaction ends so as to precipitate solid, and filtrating, thereby obtaining 2,6-dichloro-4-nitroaniline and the filtrate. 2,6-dichloro-4-nitroaniline synthesized by adopting the method disclosed by the invention has advantages of low cost, high atomic economical efficiency, no wastewater discharge, environment friendliness, high efficiency and the like.

Description

technical field [0001] The invention relates to a low-temperature synthesis method of 2,6-dichloro-4-nitroaniline without waste water discharge. Background technique [0002] 2,6-Dichloro-4-nitroaniline, which has the formula C 6 h 4 Cl 2 N 2 o 2 , its structural formula is as follows: [0003] [0004] The pure product of 2,6-dichloro-4-nitroaniline is a yellow needle-like crystal or crystal, which is an important intermediate of azo-type disperse dyes and 3,5-dichloroaniline, and is also a broad-spectrum agricultural bactericide agent. [0005] The method of synthetic 2,6-dichloro-4-nitroaniline mainly contains following several kinds at present: [0006] Method 1. Using p-nitroaniline as the starting material, the temperature ranges from 0 to 80°C, and under the conditions of acidic catalysts such as hydrochloric acid, oxalic acid or sulfuric acid, it is directly chlorinated with chlorine gas, and the yield can reach more than 90%. The raw material of this meth...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/74
Inventor 王玲李于钢时云龙钱超刘建青陈新志
Owner 江苏艾科维科技股份有限公司
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