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Preparation method of p-aminoacetanilide

A technology of aminoacetanilide and nitroacetanilide, which is applied in the field of preparation of p-aminoacetanilide, can solve the problems of heavy environmental pollution, achieve high reduction yield, avoid post-processing, and broad development prospects

Pending Publication Date: 2020-01-31
新乡市锦源化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Above method produces a large amount of acid waste water equally, and environmental pollution is heavier, for these deficiencies, it is necessary to develop a kind of preparation method of p-aminoacetanilide that preparation method is simple, pollution is little and easy to make; Therefore, develop a kind of preparation method The preparation method of p-aminoacetanilide which is simple, less polluting and convenient to make has very important significance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method of p-aminoacetanilide, the preparation steps are as follows:

[0019] ①Put p-nitroacetanilide, zinc powder, ammonium chloride and water into the reaction kettle, mix well, heat and keep warm;

[0020] 2. cooling and crystallizing the solution of step 1., and filtering;

[0021] 3. After completely dissolving and cooling in the solution of step 2., recrystallize with ethanol, and filter to obtain p-aminoacetanilide solution;

[0022] ④ filter the p-aminoacetanilide solution in step ③ at 65° C., distill, cool down, and then filter to obtain the crude p-aminoacetanilide;

[0023] ⑤ After heating and dissolving the crude p-aminoacetanilide, cool down, filter, and dry in vacuum to obtain the p-aminoacetanilide product.

[0024] The temperature at which p-nitroacetanilide, zinc powder, ammonium chloride and water are added to the reaction kettle is 95°C.

[0025] The heating and holding time in step ① is 0.5h.

[0026] The yield in step ① is 95%.

[...

Embodiment 2

[0030] A preparation method of p-aminoacetanilide, the preparation steps are as follows:

[0031] ①Put p-nitroacetanilide, zinc powder, ammonium chloride and water into the reaction kettle, mix well, heat and keep warm;

[0032] 2. cooling and crystallizing the solution of step 1., and filtering;

[0033] 3. After completely dissolving and cooling in the solution of step 2., recrystallize with ethanol, and filter to obtain p-aminoacetanilide solution;

[0034] ④ filter the p-aminoacetanilide solution in step ③ at 70°C, distill, cool down, and then filter to obtain the crude p-aminoacetanilide;

[0035] ⑤ After heating and dissolving the crude p-aminoacetanilide, cool down, filter, and dry in vacuum to obtain the p-aminoacetanilide product.

[0036] The temperature at which p-nitroacetanilide, zinc powder, ammonium chloride and water are added to the reaction kettle is 98°C.

[0037] The heating and holding time in step ① is 1h.

[0038] The yield in step ① is 95%.

[0039...

Embodiment 3

[0042] A preparation method of p-aminoacetanilide, the preparation steps are as follows:

[0043] ①Put p-nitroacetanilide, zinc powder, ammonium chloride and water into the reaction kettle, mix well, heat and keep warm;

[0044] 2. cooling and crystallizing the solution of step 1., and filtering;

[0045] 3. After completely dissolving and cooling in the solution of step 2., recrystallize with ethanol, and filter to obtain p-aminoacetanilide solution;

[0046] ④ filter the p-aminoacetanilide solution in step ③ at 75°C, distill, cool down, and then filter to obtain the crude p-aminoacetanilide;

[0047] ⑤ After heating and dissolving the crude p-aminoacetanilide, cool down, filter, and dry in vacuum to obtain the p-aminoacetanilide product.

[0048] The temperature at which p-nitroacetanilide, zinc powder, ammonium chloride and water are added to the reaction kettle is 99°C.

[0049] The heating and holding time in step ① is 1.5h.

[0050] The yield in step ① is 95%.

[00...

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Abstract

The invention relates to a preparation method of p-aminoacetanilide, and the method comprises the following steps: (1) adding p-nitroacetanilide, zinc powder, ammonium chloride and water into a reaction kettle, uniformly mixing, heating, and keeping the temperature; (2), cooling, crystallizing and filtering the solution obtained in the step 1; (3) completely dissolving in the solution obtained inthe step (2), cooling, recrystallizing with ethanol, and filtering to obtain a p-aminoacetanilide solution; (4) filtering the p-aminoacetanilide solution obtained in the step (3) at 65-75 DEG C, distilling, cooling, and then filtering to obtain a p-aminoacetanilide crude product; (6) heating and dissolving the p-aminoacetanilide crude product; cooling, filtering and drying in vacuum to obtain a p-aminoacetanilide product, wherein the temperature of the p-nitroacetanilide, the zinc powder, the ammonium chloride and the water added into the reaction kettle is 95-100 DEG C, the heating and heat preservation time in the step (1) is 0.5-1.5 hours, the yield in the step (1) is 95%, the zinc powder and the ammonium chloride are used as reducing agents, the water is used as a solvent to reduce thep-nitroacetanilide, and the p-aminoacetanilide is synthesized.

Description

technical field [0001] The invention belongs to the technical field of industrial dyes, and in particular relates to a preparation method of p-aminoacetanilide. Background technique [0002] p-aminoacetanilide, also known as N-acetyl p-phenylenediamine, is an important dye intermediate, mainly used in the preparation of disperse dyes, direct dyes, acid dyes and reactive dyes, such as disperse yellow G, direct acid-resistant scarlet 4BS, acid-resistant products Red 6B, active blue AG, etc. There are currently two methods for industrial production of p-aminoacetanilide. Method 1: Acetanilide is nitrated with mixed acid and then reduced with iron powder. Method 2: p-nitroaniline reacts with acetic anhydride under the action of a catalyst to prepare p-nitroacetanilide, and then reduces it with iron powder. Above method produces a large amount of acid waste water equally, and environmental pollution is heavier, for these deficiencies, it is necessary to develop a kind of prepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/43C07C231/12
CPCC07C231/12C07C233/43
Inventor 蔡红新闫玲玲樊明伟王书擘刘媛媛
Owner 新乡市锦源化工有限公司
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