Method for recovering 2,4-dinitrophenol hydrogenation reduction byproduct to prepare 2-amino-4-acetamidoanisole

A technology of acetaminoanisole and dinitrophenol, which is applied in the field of preparation of organic compounds, can solve the problems of farmland and water system pollution, unstable product quality, and large amount of impurities, so as to reduce the content, increase the economic benefits of enterprises, The effect of reducing difficulty

A technology of acetaminoanisole and dinitrophenol, which is applied in the field of preparation of organic compounds, can solve the problems of farmland and water system pollution, unstable product quality, and large amount of impurities, so as to reduce the content, increase the economic benefits of enterprises, The effect of reducing difficulty

CN106866449AActive Publication Date: 2017-06-20彭泽长兴化工有限公司
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  • Method for recovering 2,4-dinitrophenol hydrogenation reduction byproduct to prepare 2-amino-4-acetamidoanisole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 5000Kg 2,4-dinitrophenol hydrogenation reduction product is extracted by solid-liquid separation and the mother liquor after extracting the main product 2-amino-4-nitrophenol is concentrated to obtain 750Kg residue;

[0021] Mix 750Kg residue with sulfuric acid and urea, convert 2-amino-4-nitrophenol in the mixture into 5-nitrobenzoxazolone and remove it to obtain acidic acid containing 2-nitro-4-aminophenol The aqueous solution was further processed to obtain 330Kg of 2-nitro-4-aminophenol crude product with a purity of 97.8%;

[0022] The 2-nitro-4-aminophenol with a purity of 97.8% obtained by the above method is recrystallized by different solvents respectively, and the results are shown in the following table respectively,

[0023]

Embodiment 2

[0025] The 15.4Kg purity obtained through the steps of Example 1 is that 99.8% 2-nitro-4-aminophenol is mixed with 40Kg mass concentration of 10% liquid caustic soda, and 12.6Kg dimethyl sulfate is added to obtain 15.8Kg 2-nitro -4-Aminoanisole.

[0026] 15.8Kg of 2-nitro-4-aminoanisole was mixed with 95Kg of methanol, 10.1Kg of acetic anhydride, and 5.5Kg of sodium carbonate to obtain 19.2Kg of 2-nitro-4-acetamidoanisole.

[0027] 19.2Kg 2-nitro-4-acetamidoanisole and 70Kg methanol, 10Kg water, 1.0Kg FeCl 3 .6H 2 O mixing, adding 6.3Kg hydrazine hydrate and mixing, obtaining 16.8Kg purity is 99.3% 2-amino-4-acetamidoanisole.

Embodiment 3

[0029] 100.5Kg of 2-nitro-4-aminophenol with a purity of 99.8% obtained through the steps of Example 1 was mixed with 66.9Kg of triethylamine and 500Kg of chloroform, and 51Kg of methylene chloride was introduced to obtain 105.8Kg of 2-nitro-4-aminophenol 4-Aminoanisole.

[0030] 105.8Kg 2-nitro-4-aminoanisole is mixed with 50Kg water, 600Kg ethanol, 49.1Kg acetyl chloride, 62.5Kg N-methylpiperidine to obtain 129.6Kg 2-nitro-4-acetamidoanisole .

[0031] 129.6Kg of 2-nitro-4-acetamidoanisole, 80Kg of methanol, 0.4Kg of Raney nickel, and hydrogen gas were introduced to obtain 108.8Kg of 2-amino-4-acetamidoanisole with a purity of 99.5%.

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Abstract

The invention discloses a method for recovering 2,4-dinitrophenol hydrogenation reduction byproduct to prepare 2-amino-4-acetamidoanisole. The method comprises the following steps: separating a 2-amino-4-nitrophenol and 2-nitro-4-aminophenol mixture to obtain a 2-nitro-4-aminophenol single component; mixing the 2-nitro-4-aminophenol with an alkylation reagent, and carrying out a phenolic hydroxyl group alkylation reaction and an amino group acylation reaction to obtain 2-nitro-4-acetamidoanisole; and carrying out nitro group reduction on the 2-nitro-4-acetamidoanisole to obtain the 2-amino-4-acetamidoanisole. The method provides a brand new method for the synthesis of the fine chemical engineering intermediate 2-amino-4-acetamidoanisole with important uses, reduces the content of organic matters in 2-amino-4-nitrophenol production wastewater, reduces the treatment difficulty of enterprises' industrial wastewater, converts wastewater components into the fine chemical engineering intermediate with important production uses, and increases the enterprises' economy income.

Description

technical field [0001] The invention relates to a method for preparing organic compounds, in particular to a method for recovering and preparing 2-amino-4-acetamidoanisole by utilizing 2,4-dinitrophenol hydrogenation reduction by-products. Background technique [0002] 2-Amino-4-acetylaminoanisole, commonly known as "reduced substance", is an important coupling component intermediate of disperse dyes, and is widely used in the synthesis of dyes, such as 291# blue, 79# blue, etc. [0003] The process for synthesizing 2-amino-4-acetamidoanisole mainly includes two routes: Route 1 [CN101880242B, CN106242990A], using p-aminoanisole as the main starting material, and obtaining p-acetamidobenzene through high-temperature acylation with acetic acid Methyl ether; p-acetamidoanisole reacts with mixed acid to obtain 2-nitro-4-acetamidoanisole; because the iron powder reduction process has been listed as a prohibited process by the Ministry of Environmental Protection, at present, seve...

Claims

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Application Information

Patent Timeline
20 Jun 2017
Publication
CN106866449A
IPC
C07C231/10; C07C231/14; C07C233/44
CPC
C07C231/10; C07C231/14; C07C233/44
Inventors
邵玉田; 冯宇