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Preparation method of 2,4-dinitroaniline

A technology of dinitroaniline and dinitrochlorobenzene is applied in the field of preparation of 2,4-dinitroaniline, can solve the problems of high reaction temperature, high reaction pressure, production safety risks and high cost, and achieves stable reaction The effect of sufficient, low cost and significant quality benefits

Active Publication Date: 2021-08-06
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has high production efficiency and fully utilizes the waste heat of the ammonification reaction process, but the reaction temperature is still high, the reaction pressure is high, and the production safety risk and cost are high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 101g of 2,4-dinitrochlorobenzene, 45g of urea and 150g of 30% ethanol aqueous solution into the reaction kettle, raise the temperature of the reaction kettle to 110°C, control the pressure at 0.2MPa, keep the reaction for 3 hours, and detect the reaction by liquid chromatography At the end point, after the reaction is finished, the reaction product is centrifugally filtered and washed to obtain 2,4-dinitroaniline product in the form of yellow powder. In order to make full use of the mother liquor obtained by filtration and achieve the purpose of increasing production and reducing consumption, this batch of mother liquor is applied mechanically to the next batch as a solvent for recycling. After testing, the product prepared in this embodiment has a purity of 99.03% and a yield of 98.1%.

Embodiment 2

[0027] Add 101g of 2,4-dinitrochlorobenzene, 50g of urea and 170g of 50% ethanol aqueous solution to the reaction kettle, raise the temperature of the reaction kettle to 120°C, control the pressure at 0.25MPa, keep the reaction for 3 hours, and detect the reaction by liquid chromatography At the end point, after the reaction is finished, the reaction product is centrifugally filtered and washed to obtain 2,4-dinitroaniline product in the form of yellow powder. In order to make full use of the mother liquor obtained by filtration and achieve the purpose of increasing production and reducing consumption, this batch of mother liquor is applied mechanically to the next batch as a solvent for recycling. After testing, the product prepared in this example has a purity of 99.20% and a yield of 98.3%.

Embodiment 3

[0029] Add 101g of 2,4-dinitrochlorobenzene, 60g of urea and 220g of 65% ethanol aqueous solution to the reaction kettle, raise the temperature of the reaction kettle to 125°C, control the pressure at 0.3MPa, keep the reaction for 4 hours, and detect the reaction by liquid chromatography At the end point, after the reaction is finished, the reaction product is centrifugally filtered and washed to obtain 2,4-dinitroaniline product in the form of yellow powder. In order to make full use of the mother liquor obtained by filtration and achieve the purpose of increasing production and reducing consumption, this batch of mother liquor is applied mechanically to the next batch as a solvent for recycling. After testing, the product prepared in this embodiment has a purity of 99.35% and a yield of 98.5%.

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PUM

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Abstract

The invention relates to the field of pharmaceutical chemicals, and discloses a preparation method of 2,4-dinitroaniline. The preparation method comprises the following four steps: (1) adding 2,4-dinitrochlorobenzene and urea in a molar ratio of 1: (1.5-2.5) into a reaction kettle; (2) adding an ethanol water solvent into the reaction kettle, wherein the ethanol concentration of the ethanol water solvent is 30%-100%, and the adding amount of the ethanol water solvent is 1.5-3 times of the mass of the 2,4-dinitrochlorobenzene; (3) heating the reaction kettle to 110-135 DEG C, controlling a pressure to be 0.2-0.3 MPa, and carrying out a heat preservation reaction for 3-5 hours; and (4) after the reaction is finished, centrifugally filtering and washing a reaction product to obtain the 2,4-dinitroaniline. According to the invention, the urea is used for replacing ammonia water and ammonia gas, and relatively low reaction temperature and pressure are adopted, so the explosion risk of ammonia gas volatilization is avoided, production cost is reduced, product purity and yield are improved, and the method has remarkable safety benefit, economic benefit and quality benefit.

Description

technical field [0001] The invention relates to the field of medicine and chemical industry, in particular to a preparation method of 2,4-dinitroaniline. Background technique [0002] 2,4-Dinitroaniline is a chemical substance with the molecular formula C 6 h 5 N 3 o 4 , yellow needle-like crystal; insoluble in water, slightly soluble in ethanol, soluble in hot hydrochloric acid; stable in nature; used in the production of dyes such as sulfur dark blue 3R, disperse red B, and disperse violet 2R; also used in the production of pesticide dinitrate powder, etc. As well as toner for printing ink and preparation of preservatives. [0003] At present, 2,4-dinitroaniline is usually prepared with 2,4-dinitrochlorobenzene and ammonia water as raw materials. The reaction principle is: 2,4-dinitrochlorobenzene and ammonia water undergo amination reaction to generate 2,4 -Dinitroaniline, this amination reaction belongs to the bimolecular nucleophilic substitution reaction; firstly,...

Claims

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Application Information

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IPC IPC(8): C07C209/10C07C211/52
CPCC07C209/10C07C211/52Y02A50/30
Inventor 刘志威王乐强王亮亮张世凤李保铃王金亭
Owner SHANDONG HUIHAI PHARMA & CHEM