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Synthesis process of p-nitroaniline

A p-nitroaniline and synthesis process technology, applied in the field of p-nitroaniline synthesis process, can solve the problems of unstable product quality, long reaction cycle, high production energy consumption, etc., achieve improved filler classification effect, reduce activation capacity, increase selective effect

Inactive Publication Date: 2019-04-02
黄山利臻新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The intermittent ammonolysis production process commonly used by domestic manufacturers has the disadvantages of unstable product quality, long reaction cycle, high production energy consumption, and a large amount of saline wastewater. As domestic environmental protection requirements become more and more stringent, there is an urgent need for Only by developing a new p-nitroaniline synthesis process that is environmentally friendly, low energy consumption, and stable product quality can meet the common requirements of enterprise production and environmental ecological protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of p-nitroaniline synthetic technique, comprises the following steps:

[0025] (1) Preheating: Dissolve p-nitrochlorobenzene in an appropriate amount of solvent, adjust the pH value to 6.5, put it into a mixer with a temperature of 95°C and a rotation speed of 180r / min and stir for 40min to obtain a mixture A;

[0026] (2) Mixed reaction: Put the heated mixture A, ammonia and phase transfer catalyst into the reactor, wherein the ratio of the mass of mixture A to ammonia is 1:5-, react at high temperature, and the pressure of the reaction is It is 3.5MPa, and mixture B is obtained after cooling to room temperature;

[0027] (3) Azeotropic hydrolysis: add sodium carbonate solution to the mixture B, adjust the pH value to 9.5, and perform azeotropic hydrolysis at 50° C. to obtain the mixture C;

[0028] (4) Separation and purification: the mixture C is passed through cooling water to lower the temperature, and after cooling, it is filtered under reduced pressure to...

Embodiment 2

[0037] A kind of p-nitroaniline synthetic technique, comprises the following steps:

[0038] (1) Preheating: Dissolve p-nitrochlorobenzene in an appropriate amount of solvent, adjust the pH value to 6.5-8.5, put it into a mixer with a temperature of 88°C and a rotation speed of 160r / min and stir for 60min to obtain a mixture A;

[0039] (2) Mixed reaction: put the heated mixture A, ammonia and phase transfer catalyst into the reactor, wherein the ratio of the mass of mixture A to ammonia is 1:7, react at high temperature, and the pressure of the reaction is 2.5MPa, mixture B was obtained after cooling to room temperature;

[0040] (3) Azeotropic hydrolysis: add sodium carbonate solution to the mixture B, adjust the pH value to 10, and perform azeotropic hydrolysis at 55°C to obtain the mixture C;

[0041] (4) Separation and purification: the mixture C is passed through cooling water to lower the temperature, and after cooling, it is filtered under reduced pressure to separate...

Embodiment 3

[0050] A kind of p-nitroaniline synthetic technique, comprises the following steps:

[0051] (1) Preheating: Dissolve p-nitrochlorobenzene in an appropriate amount of solvent, adjust the pH value to 8.5, put it into a mixer with a temperature of 95°C and a rotation speed of 200r / min and stir for 45min to obtain a mixture A;

[0052] (2) Mixed reaction: put the heated mixture A, ammonia and phase transfer catalyst into the reactor, wherein the ratio of the mass of mixture A to ammonia is 1:10, react at high temperature, and the pressure of the reaction is 5.0MPa, mixture B was obtained after cooling to room temperature;

[0053] (3) Azeotropic hydrolysis: add sodium carbonate solution to the mixture B, adjust the pH value to 10, and perform azeotropic hydrolysis at 50°C to obtain the mixture C;

[0054] (4) Separation and purification: the mixture C is passed through cooling water to lower the temperature, and after cooling, it is filtered under reduced pressure to separate p-...

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PUM

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Abstract

The invention relates to the technical field of synthesis processes, and particularly relates to a synthesis process of p-nitroaniline. The preparation steps comprise the four steps of pre-heating, mixing reaction, co-boiling hydrolysis, and separation and purification. The invention provides the synthesis process of p-nitroaniline, co-boiling hydrolysis is carried out by reducing the temperature,the mutual relation between similar substances generated in nitration reactions and temperatures for carrying out the reactions is utilized to reduce activation capacity of electrophilic reaction substitution, and selectivity of generation of para-compounds on benzene rings is improved, so that ortho-position side reaction substances generated in the reaction are removed through hydrolysis and filtration, and purity of a final product obtained through reduced pressure filtration in a final step is ensured. Compared with a conventional process, the synthesis process provided by the invention has the following advantages that expensive special solvents are not needed to be used, anhydrous operation is not required, condition requirements of the process are simplified, the purity of the prepared final product p-nitroaniline is high, and thus efficient utilization of reaction materials is realized.

Description

technical field [0001] The invention relates to the technical field of product synthesis technology, in particular to a synthesis technology of p-nitroaniline. Background technique [0002] p-Nitroaniline, yellow needle-like crystal, highly toxic, easy to sublime. Slightly soluble in cold water, soluble in boiling water, ethanol, ether, benzene and acid solution. It is widely used in artificially synthesized chemicals in the dye industry. It is an intermediate of various printing and dyeing and pharmaceutical chemicals, and can also be used as an analytical reagent. [0003] Nitroaniline is also an extremely important intermediate in the dye industry, which can be directly used in the synthesis of the following varieties: direct sunfast black G, direct green B, BE, 2B-2N, black green NB, direct gray D, acid black 10B, ATT , Disperse Red P-4G, Cationic Deep Yellow 2RL, Fur Black D, p-phenylenediamine, o-chloro-p-nitroaniline, 2.6-dichloro-4-nitroaniline, 5-nitro-2-chlorophe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/10C07C209/86C07C211/52
CPCC07C209/10C07C209/86C07C211/52
Inventor 孔令洪潘水木方文斌
Owner 黄山利臻新材料科技有限公司