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Preparation method of superfine nitroguanidine

A technology for ultra-fine nitroguanidine and crude nitroguanidine, which is applied in the chemical industry and can solve problems such as high energy consumption, poor safety performance, and poor fluidity

Pending Publication Date: 2021-05-11
宁夏贝利特生物科技有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the currently prepared nitroguanidine crystals are needle-shaped, and when directly applied to explosives, there will be defects such as poor fluidity and poor mechanical properties.
[0003]At present, the preparation of ultra-fine nitroguanidine at home and abroad is mainly through physical and chemical methods. The chemical method is mainly based on solvent-non-solvent recrystallization refinement technology and microemulsion refinement technology. These two methods have the problems of high energy consumption and poor safety performance

Method used

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  • Preparation method of superfine nitroguanidine
  • Preparation method of superfine nitroguanidine
  • Preparation method of superfine nitroguanidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A kind of preparation method of superfine nitroguanidine is characterized in that, comprises the following steps:

[0032] (1) add vitriol oil in reactor, slowly add guanidine nitrate while stirring, add guanidine nitrate with the speed of 30kg / h, stirring speed is in the 55% ethylene glycol freezing brine control reactor of feeding intake with-15 ℃ The temperature does not exceed 30°C. React after feeding is completed. The reaction temperature is 40°C and the reaction time is 40 minutes. Then the crude nitroguanidine is obtained by cooling to a temperature lower than 15°C for crystallization and centrifugation. The water content of the crude nitroguanidine is 21%. , the centrifugal speed is 1000rpm, the centrifugal time is 5min, the mass fraction of concentrated sulfuric acid is 93%, and the mass ratio of concentrated sulfuric acid and guanidine nitrate is 2:1;

[0033] (2) add polyvinyl alcohol aqueous solution in reactor, then add step (1) gained nitroguanidine crude...

Embodiment 2

[0037] A kind of preparation method of superfine nitroguanidine is characterized in that, comprises the following steps:

[0038] (1) add vitriol oil in reactor, slowly add guanidine nitrate while stirring, add guanidine nitrate with the speed of 30kg / h, the 55% ethylene glycol freezing brine control reactor of -15 ℃ when stirring speed is feeding intake The temperature does not exceed 30°C, react after feeding is completed, the reaction temperature is 42°C, the reaction time is 40min, and then the crude nitroguanidine is obtained by cooling to a temperature lower than 15°C for crystallization and centrifugation, and the water content of the crude nitroguanidine is 22%. , the centrifugal speed is 1000rpm, the centrifugal time is 7min, the mass fraction of concentrated sulfuric acid is 93%, and the mass ratio of concentrated sulfuric acid and guanidine nitrate is 2:1;

[0039] (2) add polyvinyl alcohol aqueous solution in reactor, then add step (1) gained nitroguanidine crude p...

Embodiment 3

[0043] A kind of preparation method of superfine nitroguanidine is characterized in that, comprises the following steps:

[0044] (1) Add concentrated sulfuric acid in the reactor, slowly add guanidine nitrate while stirring, add guanidine nitrate at a rate of 30kg / h, the stirring speed is 750r / min, add 20% calcium chloride freezing of -15 ℃ when feeding The temperature in the reactor is controlled by salt water to not exceed 30°C. After the feeding is completed, the reaction is carried out. The reaction temperature is 45°C and the reaction time is 40 minutes. The water content is 24%, the centrifugal speed is 1000rpm, the centrifugal time is 8min, the mass fraction of concentrated sulfuric acid is 93%, and the mass ratio of concentrated sulfuric acid to guanidine nitrate is 2:1;

[0045] (2) add polyvinyl alcohol aqueous solution in reactor, then add step (1) gained nitroguanidine crude product high-speed stirring, stirring speed is 750r / min, the massfraction of polyvinyl alc...

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Abstract

The invention relates to a preparation method of superfine nitroguanidine, which comprises the following steps of adding concentrated sulfuric acid into a reaction kettle, slowly adding guanidine nitrate while stirring, adding guanidine nitrate at a rate of 30 kg / h, controlling the temperature in the reaction kettle not to exceed 30 DEG C during feeding, reacting after feeding, and carrying out cooling crystallization and centrifugal separation to obtain a nitroguanidine crude product, adding a polyvinyl alcohol aqueous solution into a reaction kettle, then adding a nitroguanidine crude product, stirring at a high speed, heating to 65-70 DEG C, adding ammonia water to adjust the pH value to 7.0, then heating to 85 DEG C, and reacting for 40 minutes, reducing the temperature in the reaction kettle to 10 DEG C from 85 DEG C while stirring, and performing centrifugal separation to obtain the superfine nitroguanidine. The average particle size of the obtained superfine nitroguanidine is 10 microns, the D90 particle size is smaller than 18 microns, the content of the superfine nitroguanidine is higher than 99%, and the yield is higher than 82%.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a preparation method of ultrafine nitroguanidine. Background technique [0002] Nitroguanidine is an important industrial raw material. Based on its low detonation temperature and low sensitivity, it is usually used as a propellant and bullet charge component of rockets, missiles, explosives, etc. The comprehensive performance of nitroguanidine is superior, not only can be used as explosives and other explosive products, but also can be used as an energetic additive of low characteristic signal propellant by utilizing its characteristics of moderate energy and low sensitivity. Most of the currently prepared nitroguanidine crystals are needle-shaped, and when directly applied to explosives, there will be defects such as poor fluidity and poor mechanical properties. [0003] At present, the preparation of ultra-fine nitroguanidine at home and abroad is mainly through physic...

Claims

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Application Information

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IPC IPC(8): C07C277/08C07C279/34
CPCC07C277/08
Inventor 赵黎明王永军王中杰安瑞杰李鹏伟
Owner 宁夏贝利特生物科技有限公司
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