Preparation method for N-acetyl acetanilide

A technology for acetoacetanilide and aniline, applied in the field of preparing N-acetoacetanilide, can solve the problems of low utilization rate of equipment, a large amount of waste water, easy agglomeration, etc., and achieve the effects of reducing water volume, increasing saturation, and preventing agglomeration

Active Publication Date: 2013-07-31
NANTONG ACETIC ACID CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The N-acetylacetanilide product produced by the conventional process is in the form of powder, and it is easy to agglomerate when pl

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 354.4Kg of deionized water into a 1000L reactor, cool down to 5°C, add 6.94Kg of seed crystals, 0.02Kg of emulsifier D 3 , dropwise add a mixture of 84.07Kg (1Kmol) of diketene and 93.12Kg (1Kmol) of aniline, the stirring speed is 50 rpm, the dropping temperature is 15°C, and the dropping time is 1.5 hours; the temperature is naturally raised to 38°C, and the heat preservation reaction is 3.5 After hours, cool to 0°C, filter, and dry to obtain 182.56Kg of N-acetoacetanilide finished product, the product yield is 98.52%, the product content is 99.6%, and the particle size is 89.6% above 50 mesh.

Embodiment 2

[0018] Add 548.1Kg of deionized water into a 1000L reactor, cool down to 5°C, add 13.66Kg of seed crystals, 0.11Kg of emulsifier D 4 , add dropwise a mixture of 126.11Kg (1.5Kmol) of diketene and 93.12Kg (1Kmol) of aniline, the stirring speed is 65 rpm, the dropping temperature is 18°C, and the dropping time is 1.7 hours; the temperature is naturally raised to 42°C, and the heat preservation reaction After 4 hours, cool to 0°C, filter, and dry to obtain 191.14Kg of N-acetoacetanilide, the product yield is 99.35%, the product content is 99.7%, and the particle size is 91.2% above 50 mesh.

Embodiment 3

[0020] Add 642.54Kg of deionized water into a 1000L reactor, cool down to 2°C, add 15.21Kg of seed crystals, 0.22Kg of emulsifier Vi-D 4 , add dropwise a mixture of 121.06Kg (1.3Kmol) of diketene and 93.12Kg (1Kmol) of aniline, the stirring speed is 75 rpm, the dropping temperature is 20°C, and the dropping time is 1 hour; the temperature is naturally raised to 46°C, and the heat preservation reaction After 4 hours, cool to 0° C., filter, and dry to obtain 193.39 Kg of N-acetoacetanilide, the product yield is 99.3%, the product content is 99.6%, and the particle size is 92.3% above 50 mesh.

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PUM

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Abstract

The invention relates to a preparation method for N-acetyl acetanilide. The method comprises the following steps of adding N-acetyl acetanilide crystal seeds and an emulsifying agent to deionized water at a temperature of 0-10 DEG C to carry out a reaction; then dropwise adding diketene and aniline simultaneously under the control of a certain temperature; keeping the reaction at the temperature; cooling to a temperature of 0 DEG C; filtering and drying to obtain the N-acetyl acetanilide. The method has the advantages of effectively preventing product caking, improving product appearance and performance, increasing product yield and greatly reducing wastewater quantity.

Description

technical field [0001] The invention relates to a method for preparing chemical dyes, organic pigments or pesticide intermediates, in particular to a method for preparing N-acetylacetanilide. Background technique [0002] N-Acetoacetanilide is a white crystalline powder, slightly soluble in water and easily soluble in organic solvents such as ethanol, ether, chloroform and hot benzene. It is an intermediate of dyes, organic pigments and pesticides, and is mainly used in the synthesis of neutral yellow dyes, Organic yellow pigments and pesticides, such as rustling. [0003] At present, the conventional production method of N-acetoacetanilide in industry is as follows: at 0-10°C, equimolar diketene and aniline are added dropwise to a large amount of water to react at the same time, and after the reaction of the materials is completed, they are directly cooled and filtered. The N-acetoacetanilide product produced by the conventional process is in the form of powder, and it is ...

Claims

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Application Information

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IPC IPC(8): C07C231/04C07C235/80C07C231/24
Inventor 丁彩峰朱小刚刘芳姚俊生
Owner NANTONG ACETIC ACID CHEM
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