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A kind of clean production method of 3‑(n, n‑disubstituted) aminoacetanilide compounds

A technology of aminoacetanilide and its production method, which is applied to the preparation of organic compounds, chemical instruments and methods, and the preparation of carboxylic acid amides. It can solve the problems of complex components, high content of organic poisons, and refractory degradation, and achieve the goal of reducing production costs. Effect

Active Publication Date: 2017-08-04
ZHEJIANG LONGSHENG GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the crude product needs to be diluted, alkali analyzed, press-filtered, and washed with water. Although it has been applied mechanically to some of the generated wastewater, it still produces a large amount of high-COD, high-ammonia-nitrogen wastewater
[0009] None of the above patent documents has explained the treatment of mother liquor wastewater in the reaction process. A large amount of mother liquor wastewater generated during the synthesis of the dye intermediate has high content of organic poisons, complex components, and is difficult to degrade. Therefore, it is necessary to find a clean synthetic Technology has become a hot spot of current research

Method used

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  • A kind of clean production method of 3‑(n, n‑disubstituted) aminoacetanilide compounds
  • A kind of clean production method of 3‑(n, n‑disubstituted) aminoacetanilide compounds
  • A kind of clean production method of 3‑(n, n‑disubstituted) aminoacetanilide compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 150 kg of m-acetamido aniline hydrochloride, 370 kg of water, and 85 kg of 17.7% ammonia water into the reaction kettle, stir well, and control the pH of the ammonia water to 6.5-7. Raise the temperature of the material to 90-95°C, add 200kg of 17.7% ammonia water, control the pressure of the reactor below 1.0MPa, pass 133kg of ethyl chloride and 165kg of 17.7% ammonia water from the reaction liquid, control the pH to 5-7, and the temperature to 95 Insulate and react at ~98°C for 18 hours, and use HPLC (high performance liquid chromatography) to measure the end point of sampling, and control the content of monoethyl (ie m-acetamido-N-ethylaniline) within 2%. After the reaction, add 400kg of water to dilute, adjust the pH to 7.0-7.5 with ammonia water, filter and wash with water when the temperature is cooled to below 40°C, and separate the N,N-diethyl-m-acetamidoaniline product (yield about 98% ) and mother liquor containing ammonium chloride.

[0039]

[0040] ...

Embodiment 2

[0042] Add m-acetaminoaniline hydrochloride 185kg, add water 451kg in the reaction kettle, throw 110kg17.7% ammonia water to control pH6.5~7, stir evenly, feed 165kg ethyl chloride and 210kg 17.7% ammonia water under the liquid surface, Raise the temperature to 85°C in about 1.5 hours, keep it warm for 1 hour, then raise the temperature to 95°C, control the pressure of the reactor below 1.0MPa, keep it at about 97°C for 20 hours, use HPLC (high performance liquid chromatography) to measure the end point of the sample, and control the single B base (i.e., m-acetamido-N-ethylaniline) content within 2%, control the monoethyl content within 2.5%, cool down to 70°C, continue stirring, let it cool down naturally, precipitate, after the material precipitates, stir for 2 hours Around 30°C, filter and wash with water to separate the N,N-diethyl-m-acetaniline product (yield about 96%) and the mother liquor containing ammonium chloride.

[0043] The separated ammonium chloride mother liquo...

Embodiment 3

[0045] Add 200kg of 2-amino-4-acetamidoanisole, 330kg of water, and 1.3kg of MF into the reaction kettle, stir well, raise the temperature of the materials to 80-85°C, and keep warm for 1 hour to dissolve. Add 188kg of 96% allyl chloride, add liquid ammonia to control the pH 5-6, and keep the temperature at 80-85°C for 6 hours. The HPLC method (high performance liquid chromatography) is used for sampling to measure the end point, and the control of monopropenyl (ie 3-N -allylamino-4-methoxyacetanilide) content within 4%. After the reaction, add 400kg of water to dilute, stir and crystallize for about 1 hour, until all crystallization is complete, cool down to below 50°C, filter, wash with water, and separate 3-(N,N-diallyl)amino-4-methoxy Acetanilide product (yield about 98%) and mother liquor containing ammonium chloride.

[0046] After the separated ammonium chloride mother liquor is physically filtered, it is passed into an adsorption oxidation reactor filled with DA201-...

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Abstract

The invention relates to a clean production method of 3-(N,N-di-substituted)aminoacetanilide compounds (III). The method comprises the following steps: (1) adding water to a compound of Formula (I), stirring uniformly, adding alkali to regulate the pH value to 6-7 when the substituent group R1 is hydrogen or not regulating the pH value when the substituent group R1 is methoxy group, adding a compound of Formula (II) and an acid-binding agent, and reacting to the end point while controlling the pH value at 4-9 and the temperature at 60-130 DEG C; (2) separating out a compound (III) to obtain a chloride salt-containing mother solution; (3) decolorizing the chloride salt-containing mother solution by using activated carbon or by adsorbing organic matters with a resin, thereby obtaining a colorless chloride salt mother solution; and (4) recovering the chloride salt from the colorless chloride salt mother solution by MVR (mechanical vapor recompression) high-efficiency concentration cooling crystallization or multiple-effect evaporation system concentration crystallization, wherein the concentration condensation water and crystallization mother solution are respectively recycled. The method lowers the production cost, and implements resource recovery and reduction on wastewater.

Description

[0001] (1) Technical field [0002] The invention relates to a clean production process of 3-(N,N-disubstituted)aminoacetanilide compounds, especially the production of 3-(N,N-disubstituted)aminoacetanilide compounds and the treatment of mother liquor wastewater resource utilization process. [0003] (2) Background technology [0004] Among the disperse dyes, C.I. Disperse Violet 93, C.I. Disperse Blue 291, C.I. Disperse Blue 291:1 and other varieties are organic dyes used in large quantities at home and abroad. They can be used alone or in combination with other varieties of dyes, such as The environmentally friendly disperse black dye EXSF compounded with C.I. Disperse Violet 93, C.I. Disperse Blue 291 and / or C.I. Disperse Blue 291:1, C.I. Disperse Orange 288 has excellent dyeing effect, and the domestic production and sales volume is very large. The research on the synthesis process of the body has also been paid more and more attention. [0005] In "Study on the Synthesis...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/43C07C231/12
Inventor 高怀庆余青结祝培明
Owner ZHEJIANG LONGSHENG GROUP