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Preparation method of 4-nitro phthalonitrile

A technology of nitrophthalonitrile and phthalonitrile, which is applied in the field of preparation of 4-nitrophthalonitrile, can solve the problems of many operation steps, serious environmental pollution, long reaction time and the like, and achieves the The effect of shortening the process flow, high yield and reducing operation steps

Active Publication Date: 2014-05-21
HEBEI CHEM & PHARMA COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above two methods have a long reaction time and many operation steps, and the acid mist generated by the thionyl chloride ice-out will seriously pollute the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The first step is to prepare the nitrification reaction solution

[0021] Add 133ml of 120% fuming sulfuric acid dropwise into a four-necked bottle equipped with a thermometer, a reflux condenser for gas guiding, tetrafluoroelectric electric stirring and a constant pressure dropping funnel, and then ice-bath to cool the temperature to 5°C , under PTFE electric stirring, slowly drop 84ml of 196% fuming nitric acid into it with a constant pressure dropping funnel. During the dropping process, control the temperature of the mixed solution below 10°C, and then add Slowly add the catalyst ytterbium perfluorooctane sulfonate into the mixture, then keep the temperature at 10°C, stir for half an hour, then cool down to 5°C.

[0022] The second step is to carry out the nitrification reaction

[0023] Carefully and slowly add 134.4 g of phthalonitrile to the reaction solution prepared in the first step, and carry out nitration reaction to obtain a mixture containing 4-nitrophtha...

Embodiment 2

[0029] The first step is to prepare the nitrification reaction solution

[0030] Add 145ml of 120% fuming sulfuric acid dropwise into a four-necked bottle equipped with a thermometer, a reflux condenser that acts as a gas guide, a tetrafluoroelectric electric stirrer, and a constant pressure dropping funnel, and then use an ice bath to cool the temperature to 5°C , under PTFE electric stirring, slowly drop 86ml of 196% fuming nitric acid into it with a constant pressure dropping funnel. During the dropping process, control the temperature of the mixed solution below 10°C, and then add Slowly add the catalyst ytterbium perfluorooctane sulfonate into the mixture, then keep the temperature at 10°C, stir for half an hour, then cool down to 5°C.

[0031] The second step is to carry out the nitrification reaction

[0032] Add 140.8g of phthalonitrile carefully and slowly to the reaction solution prepared in the first step, and carry out nitration reaction to obtain a mixture contai...

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PUM

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Abstract

The invention discloses a preparation method of 4-nitro phthalonitrile. The method comprises the following steps of: undergoing a nitration reaction on phthalonitrile serving as a raw material and fuming nitric acid serving as a medium under the action of a catalyst to obtain a mixture containing 4-nitro phthalonitrile; separating crude 4-nitro phthalonitrile out of the mixture; and recrystallizing the crude 4-nitro phthalonitrile with methanol to obtain refined 4-nitro phthalonitrile. The method disclosed by the invention has the advantages of short process flow, mild reaction conditions, low cost and high yield.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and in particular relates to a preparation method of 4-nitrophthalonitrile. Background technique [0002] 4-Nitrophthalonitrile is a fine chemical with a wide range of uses. It is generally used as an intermediate in medicine and dyes, and can also be used to produce other raw materials, such as 4-aminophthalonitrile, 4-iodo base phthalonitrile and so on. [0003] Chinese patent application CN1369480A disclosed "a method for synthesizing 3- or 4-nitrophthalonitrile", first 3- or 4-nitrophthalic acid and urea were reacted in a solvent to obtain 4 -Nitrophthalimide, and then 3- or 4-nitrophthalimide is reacted with concentrated ammonia water or ammonia to generate 3- or 4-nitrophthalimide, Finally, 3- or 4-nitrophthaloamide is dehydrated with thionyl chloride to obtain 3- or 4-nitrophthalonitrile. [0004] Chinese patent application CN1508125A discloses "4-Nitrophthalonitrile production...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/51C07C253/30
Inventor 高维娟陈瑞珍程桂花李璟张小华庞秀石琛琛
Owner HEBEI CHEM & PHARMA COLLEGE