Method for producing 2,5-dichloroaniline without anti-dechlorinating agent

A technology of dichloroaniline and dechlorination agent, applied in chemical instruments and methods, preparation of organic compounds, preparation of amino compounds, etc., can solve the problems of increasing product separation operations, worsening labor environment, increasing investment costs, etc. Investment cost and energy consumption, less environmental pollution, the effect of reducing pollution and energy consumption

Active Publication Date: 2013-12-25
HULUDAO TIANQI SHENGYE CHEM
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Problems solved by technology

However, the use of anti-dechlorination agent will increase the product separation operation, which will cause a series of ...

Method used

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Experimental program
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Effect test

Embodiment

[0012] Put 100g of 2,5-dichloronitrobenzene and 3g of catalyst into the autoclave, close the autoclave, open the hydrogen valve, feed hydrogen into the autoclave, stir and raise the temperature to react, the reaction temperature is controlled at 110-120°C, and the reaction The pressure is controlled at 1.1-1.2Mpa, the reaction speed is set at 700 rpm, and the hydrogen gas valve is closed until the hydrogen is not absorbed. After cooling, the autoclave is opened, and the material is discharged. After filtering, add it to the rectification kettle. After the distillation is completed, the oil phase is For 2,5-dichloroaniline. Sampling, the gas chromatography analysis result 2, the purity of 5-dichloroaniline is 99.85%, and the dechlorination amount is 0.006%. The catalyst components and mass ratio are as follows: 5%-10% of platinum (Pt), 1%-3% of copper (Cu), 20%-30% of carbon (C), and the rest is water. The method is to react 2,5-dichloronitrobenzene with hydrogen, and under th...

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Abstract

The invention provides a method for producing 2,5-dichloroaniline without an anti-dechlorinating agent. The method is characterized by comprising the following steps of: adding 2,5-dichloronitrobenzene and a catalyst into a high-pressure kettle, sealing, opening a hydrogen valve, and introducing hydrogen into the high-pressure kettle; stirring, heating and pressurizing, setting the reaction rotating speed to be 700 revolutions/minute, controlling the reaction temperature to be 110-120 DEG C and the reaction pressure to be 1.1-1.2MPa, and reacting until hydrogen cannot be absorbed; closing the hydrogen valve, cooling, opening the high-pressure kettle, and discharging; filtering, adding into a rectifying still for distillation to obtain 2,5-dichloroaniline after the distillation is finished. A sample is collected, and gas chromatography results indicate that the purity of 2,5-dichloroaniline is 99.85 percent, and dechlorination rate is 0.006 percent. The anti-dechlorinating agent is not needed to be extra added, so that the best anti-dechlorination effect can be achieved. The method is easy to operate, short in production cycle and small in environmental pollution, and can reduce generation of side products, so that the product yield can be effectively increased, cost can be reduced, and benefit can be increased. Therefore, the method is suitable for industrial production.

Description

1. Technical field: [0001] The invention relates to a method for producing p-chloroaniline, in particular to a method for producing 2,5-dichloroaniline without using an anti-dechlorination agent. 2. Background technology: [0002] 2,5-Dichloroaniline is an important fine chemical intermediate, which is widely used in the production of fine chemicals such as dyes, medicines, spices and rubber additives. The traditional production methods of 2,5-dichloroaniline mainly include iron powder reduction method, alkali sulfide reduction method, electrochemical reduction method, and catalytic hydrogenation reduction method. The iron powder reduction method produces a large amount of iron sludge, which seriously pollutes the environment, and the product purity is not high; the alkali sulfide reduction method has the disadvantages of complex reduction route, low product yield, and large amount of waste liquid; the electrochemical reduction method consumes too much energy; The hydrogena...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/36
Inventor 杨向党陈晨赵洋洋
Owner HULUDAO TIANQI SHENGYE CHEM
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