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Preparation method for dinitrogen heptyl amide

A technology of bisazeptanamide and aminoheptanenitrile, applied in directions such as organic chemistry, can solve problems such as the large influence of catalyst decomposition rate, and achieve the effects of low production cost, high product purity, and small oxidizing ability

Active Publication Date: 2014-12-10
大庆市华兴化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, some existing catalysts can only maintain activity at high temperatures; the decomposition rate of some catalysts is greatly affected by solvents, resulting in strict requirements for the type of solvent used in production; and some require inducers to play a catalytic role; therefore , it is necessary to provide a catalyst for the production of polyacrylamide with strong activity and little external influence

Method used

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  • Preparation method for dinitrogen heptyl amide
  • Preparation method for dinitrogen heptyl amide

Examples

Experimental program
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Effect test

Embodiment 1

[0013] The preparation method of diazepamamide of the present invention, its steps are as follows:

[0014] A. Raw materials and proportions include: 10 parts of aminoheptanonitrile, 50 parts of 15% sodium hydroxide solution, 2 parts of chlorine gas, 40 parts of ethanol, 10 parts of N,N-dimethylformamide, and 0.5 parts of sodium methoxide and 5 parts of liquefied ammonia, all of which are parts by weight;

[0015] B. Mix 10 parts of aminoheptanitril with 50 parts of 15% sodium hydroxide solution, feed 2 parts of chlorine gas at 0°C within 1 hour, cool down to -5°C, and let it stand at constant temperature for 8 hours. solid sediment;

[0016] C. The solid precipitate obtained in step B is heated and dried at 20°C for 8 hours, and when its water content is ≤3%, add it to 40 parts of ethanol, then add 10 parts of N,N-dimethylformamide and 0.5 Parts of catalyst sodium methoxide, 5 parts of liquid ammonia were added within 5 hours, and after standing at 15°C for 12 hours, the te...

Embodiment 2

[0018] The preparation method of diazepamamide of the present invention, its steps are as follows:

[0019] A. Raw materials and proportions include: 40 parts of aminoheptanitril, 120 parts of 15% sodium hydroxide solution, 8 parts of chlorine gas, 100 parts of ethanol, 40 parts of N,N-dimethylformamide, and 1 part of sodium methoxide And 20 parts of liquefied ammonia, all above are parts by weight;

[0020] B. Mix 40 parts of aminoheptanitril with 120 parts of 15% sodium hydroxide solution, feed 8 parts of chlorine gas at 10°C within 8 hours, cool down to -20°C, let stand at constant temperature for 15 hours, and take whichever solid sediment;

[0021] C. Dry the solid precipitate obtained in step B at 50°C for 15 hours. When its water content is ≤3%, add it to 100 parts of ethanol, then add 40 parts of N,N-dimethylformamide and 1 Parts of catalyst sodium methoxide, add 20 parts of liquid ammonia within 10 hours, stand at 20°C for 36 hours, lower the temperature to -50°C to...

Embodiment 3

[0023] The preparation method of diazepamamide of the present invention, its steps are as follows:

[0024] A. Raw materials and proportions include: 20 parts of aminoheptanonitrile, 80 parts of 15% sodium hydroxide solution, 4 parts of chlorine gas, 50 parts of ethanol, 15 parts of N,N-dimethylformamide, and 0.6 parts of sodium methoxide and 8 parts of liquefied ammonia, all of which are parts by weight;

[0025] B. Mix 20 parts of aminoheptanonitrile with 80 parts of 15% sodium hydroxide solution, feed 4 parts of chlorine gas at 5°C within 5 hours, lower the temperature to -5°C, and let it stand at constant temperature for 10 hours. solid sediment;

[0026] C. The solid precipitate obtained in step B is heated and dried at 30°C for 10 hours, and when its water content is ≤3%, add it to 50 parts of ethanol, then add 15 parts of N,N-dimethylformamide and 0.6 One part of catalyst sodium methoxide, 8 parts of liquid ammonia were added within 5 hours, and after standing at 15°C...

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Abstract

The invention discloses a preparation method for dinitrogen heptyl amide, and relates to a common process as well as aftertreatment for chemical processing ingredients. The preparation method comprises the following steps: mixing 10-40 parts of aminoheptonitrile and 50-120 parts of 15% sodium hydroxide liquor, introducing 2-8 parts of chlorine gas within 1-8 hours at 0-8 DEG C, cooling to (-)5 to (-)20 DEG C, and standing for 8-15 hours at constant temperature, thus getting solid precipitates of the mixture; drying the solid precipitates for 8-15 hours at a constant temperature of 20-50 DEG C, adding the solid precipitates into 40-100 parts of alcohol, then, adding 10-40 parts of N, N-dimethyl formamide and 0.5-1 part of a catalyst sodium methoxide, adding 5-20 parts of liquid ammonia within 5-10 hours, standing for 12-36 hours at 15-20 DEG C, and then cooling to (-) 20 to (-)50 DEG C to separate solids, namely the dinitrogen heptyl amide product. The dinitrogen heptyl amide is especially suitable for producing polyacrylamide, small in oxidative capacity, small in influences on decomposition speed by a solvent, free of induction during decomposition, unlikely to explode during collision, high in product purity and low in production cost.

Description

technical field [0001] The invention relates to a general process and post-treatment of chemical processing ingredients, in particular to a preparation method of diazepamamide. Background technique [0002] There are many kinds of catalysts used in the production of polyacrylamide by polymer polymerization. The function of the catalyst is to ensure the decomposition at an appropriate speed at the polymerization reaction temperature, which is beneficial to the synthesis of polymers. However, some existing catalysts can only maintain activity at high temperatures; the decomposition rate of some catalysts is greatly affected by solvents, resulting in strict requirements for the type of solvent used in production; and some require inducers to play a catalytic role; therefore Therefore, it is very necessary to provide a catalyst for the production of polyacrylamide with strong activity and little external influence. Contents of the invention [0003] For the deficiencies of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C245/04C08F4/04C08F120/56
Inventor 姜中明郭艳宏姜岳岩魏志伟
Owner 大庆市华兴化工有限责任公司
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