Method for preparing p-chloroaniline without adding organic solvent

A technology of p-chloroaniline and organic solvents, which is applied in the field of catalytic hydrogenation production, can solve the problems of increasing product separation and solvent recovery, increasing investment costs, and deteriorating working environment, so as to reduce investment costs, energy consumption, and production costs and equipment investment, the effect of improving production efficiency

Active Publication Date: 2014-01-08
HULUDAO TIANQI SHENGYE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of preparing p-chloroaniline by catalytic hydrogenation of p-nitrochlorobenzene, it is necessary to add a large amount of volatile organic solvents to dissolve the raw materials or products, so as to increase the contact between the reactants, hydrogen and the three phases of the catalyst probability, enhance the mass transfer and heat tr

Method used

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Examples

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Embodiment

[0013] Add 100g of p-nitrochlorobenzene, 3g of catalyst, and 8g of additives into the autoclave, seal the autoclave, open the hydrogen valve, feed hydrogen into the autoclave, stir and heat up the reaction, and the reaction temperature is controlled at 110-120°C. The reaction pressure is controlled at 1.1-1.2Mpa, the reaction speed is set at 700 rpm, and the hydrogen gas valve is closed until no hydrogen is absorbed. After cooling, the autoclave is opened, and the material is discharged. The phase is p-chloroaniline. Sampling, the purity of p-chloroaniline as a result of gas chromatography analysis is 99.85%, and the dechlorination amount is 0.01%. 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 auxiliary agent is ethylenediamine. This method is aimed at the current situation that no solvent is needed in the production process of p-nitrochlorobenzene selective hydrogenatio...

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PUM

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Abstract

The invention discloses a method for preparing p-chloroaniline without adding an organic solvent. The method is characterized by comprising the following steps: adding p-nitrochlorobenzene, a catalyst and an assistant in a high pressure kettle, sealing the high pressure kettle, opening a hydrogen valve to introduce hydrogen into the high pressure kettle, and meanwhile, stirring, heating and boosting, setting the reaction speed at 700 rpm, controlling the reaction temperature within 110-120 DEG C, controlling the reaction pressure within 1.1-1.2 MPa, reacting until no hydrogen is absorbed, closing the hydrogen valve, cooling, opening the high pressure kettle, discharging, filtering, adding the product into a rectifying kettle for distilling, and distilling to obtain the p-chloroaniline. A sample is taken, and a gas chromatography analysis result shows that the purity of the p-chloroaniline is 99.85%. The method disclosed by the invention has the advantages of simple operation, short production period, small environmental pollution, favorable environmental protection and low energy consumption, and is capable of recycling resources, reducing equipment investment and lowering the cost, and suitable for industrial production.

Description

1. Technical field: [0001] The invention belongs to the field of catalytic hydrogenation production, in particular to a method for preparing p-chloroaniline without adding an organic solvent. 2. Background technology: [0002] p-Chloroaniline is an important fine chemical intermediate, which is widely used in the production of fine chemicals such as pesticides, dyes, medicines, spices and rubber additives. In the process of preparing p-chloroaniline by catalytic hydrogenation of p-nitrochlorobenzene, it is necessary to add a large amount of volatile organic solvents to dissolve the raw materials or products, so as to increase the contact between the reactants, hydrogen and the three phases of the catalyst probability, enhance the mass transfer and heat transfer effect, and speed up the reaction rate; however, the use of solvents will increase post-treatment processes such as product separation and solvent recovery, resulting in increased investment costs, reduced system capa...

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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