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Preparation method for p-anisidine

A technology of p-aminoanisole and p-nitroanisole, which is applied in the field of preparation of p-aminoanisole, can solve the problems of unpredictability and unstable scale, and achieve high selectivity, high selectivity and conversion rate , the effect of mild reaction conditions

Active Publication Date: 2016-01-27
NINGXIA ZHONGSHENG NEW TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At least, judging from the disclosure of this patent, this method is also unstable on a laboratory scale, and it cannot be predicted how to simultaneously obtain p-aminoanisole with high selectivity and high yield
[0012] In summary, the prior art has so far failed to realize the method for preparing p-aminoanisole with high selectivity and high yield on the scale of industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 6000kg p-nitroanisole, 120kg catalyst Ni-Mo-B (wherein the weight percentages of Ni, Mo and B are respectively 95.0wt%, 3.0wt% and 2.0wt%) and 7500L methanol into a 16000L reactor to form Mixture.

[0040] Introduce nitrogen to the reactor to 0.5MPa and then evacuate, repeat 5 times to remove the air in the reactor; then, feed hydrogen to 0.5MPa and then evacuate, repeat 5 times to remove the nitrogen in the reactor.

[0041] After replacement, feed hydrogen into the reactor to 1.2MPa, open the steam valve to raise the temperature of the reactor, and close the steam valve when the temperature rises to 80°C. Turn on the reactor stirrer (slowly increase the speed through the frequency converter) to stir the mixed solution at a stirring speed of 80rpm to carry out the hydrogenation reaction; 1.2MPa.

[0042] During the reaction, the mixed solution was detected once per hour; when the content of p-nitroanisole in the mixed solution (removing methanol content) dropped ...

Embodiment 2

[0046] 3000kg p-Nitroanisole, 6kg catalyst Ni-Mo-B (wherein Ni, Mo, the weight percent of B are respectively 95.0wt%, 3.0wt% and 2.0wt%) and 3030L methyl alcohol are added embodiment 1 and leave catalyst In the 16000L reactor, a mixed solution is formed.

[0047] Introduce nitrogen to the reactor to 0.5MPa and then evacuate, repeat 3 times to remove the air in the reactor; then, feed hydrogen to 0.5MPa and then evacuate, repeat 3 times to remove the nitrogen in the reactor.

[0048] After the replacement is completed, feed hydrogen into the reactor to 1.0MPa, open the steam valve to raise the temperature of the reactor, and close the steam valve when the temperature rises to 90°C. Turn on the reactor stirrer (slowly increase the speed through the frequency converter) to stir the mixed solution at a stirring speed of 120rpm, and carry out the hydrogenation reaction; 1.0 MPa.

[0049] During the reaction, the mixed solution was detected once per hour; when the content of p-nit...

Embodiment 3

[0053] Add 6000kg p-nitroanisole, 12kg catalyst Ni-Mo-B (wherein Ni, Mo, the weight percent of B are respectively 95.0wt%, 3.0wt% and 2.0wt%) and 7000L methyl alcohol to add embodiment 2 and leave catalyst In the 16000L reactor, a mixed solution is formed.

[0054] Feed nitrogen into the reactor to 0.5MPa and then evacuate, repeat 4 times to remove the air in the reactor; then, feed hydrogen to 0.5MPa and then evacuate, repeat 4 times to remove the nitrogen in the reactor.

[0055] After the replacement is completed, feed hydrogen into the reactor to 1.6MPa, open the steam valve to raise the temperature of the reactor, and close the steam valve when the temperature rises to 100°C. Turn on the reactor stirrer (slowly increase the speed through the frequency converter) to stir the mixed solution at a stirring speed of 160rpm to carry out the hydrogenation reaction; 1.6MPa.

[0056] During the reaction, the mixed solution was detected once per hour; when the content of p-nitroa...

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PUM

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Abstract

The invention relates to a preparation method for p-anisidine. In the presence of a ternary amorphous alloy catalyst being Ni-Mo-B or Ni-Co-P, liquid-phase p-nitroanisole is subjected to hydrogenation through intermittent hydrogenation, and therefore p-anisidine with a selectivity of more than 99.7% can be obtained. In the preparation method, reaction conditions are mild, the solvent and the catalyst can be recycled, and the preparation method is liable to industrial production.

Description

technical field [0001] The invention relates to a preparation method of p-aminoanisole. Background technique [0002] P-aminoanisole, also known as p-methoxyaniline, is an important intermediate for dyes, medicines and fragrances. Compared with anthranil, p-aminoanisole is more widely used in the dye industry. For example, in the dye industry, p-aminoanisole is used to synthesize blue salt VB, bay red base GP, naphthol AS-SG, AS-RL, and reddish red. In addition, 2-amino-4-acetylaminoanisole can be synthesized by using p-aminoanisole, which is an important raw material for disperse dyes and can be used to further synthesize a series of disperse dyes, such as C.I. Disperse Blue 79, 139, 226 , 265, 301, disperse purple 58, disperse navy blue S-2GL, etc. In the pharmaceutical industry, p-aminoanisole is mainly used to synthesize adipine, primaquine, indomethacin, etc., among which indomethacin is a species with relatively large consumption of p-aminoanisole. [0003] Since t...

Claims

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Application Information

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IPC IPC(8): C07C217/84C07C213/02
CPCY02P20/584
Inventor 王明和王春敏
Owner NINGXIA ZHONGSHENG NEW TECH CO LTD
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