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Synthesis method of triaminoguanidinium nitrate

A technology of guanidine nitrate and synthesis method, applied in the field of synthesis of triaminoguanidine nitrate, can solve problems such as unsatisfactory manufacturing technology, dangerous operation technology, high price, etc., and achieves safe synthesis route, high purity, and synthesis time. short effect

Active Publication Date: 2016-03-02
HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the previous manufacturing technology of TAGN was very unsatisfactory, requiring the reaction of high-purity nitroguanidine and hydrazine in alcohol. This operation technology is very dangerous, and the high-purity hydrazine is expensive, so the output is very limited.

Method used

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  • Synthesis method of triaminoguanidinium nitrate
  • Synthesis method of triaminoguanidinium nitrate
  • Synthesis method of triaminoguanidinium nitrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Synthesis of triaminoguanidine nitrate in 500ml container:

[0031] Adding the concentration of 37ml in the 500ml four-necked flask equipped with a magnetic stirrer, condensing device and tail gas receiving device is 80% hydrazine hydrate and 72ml deionized water, and dripping 42ml concentration under stirring is 65% nitric acid, control The temperature of the system is below 40°C, after the dropwise addition is completed, test the pH value and adjust the pH value to 7;

[0032] Add 73.3g of technical grade guanidine nitrate and 210ml of hydrazine hydrate with a concentration of 80% to the system, and heat up under stirring. When the internal temperature rises to 61°C, the guanidine nitrate is completely dissolved, and then continue to heat up. When the system temperature reaches Reflux starts at 90°C, accompanied by a large amount of gas discharge. When the temperature reaches 95°C, start timing, control the reaction temperature at 95°C~98°C, and control the reaction t...

Embodiment 2

[0037] Synthesis of triaminoguanidine nitrate in 1000ml container:

[0038] Adding the concentration of 75ml in the 1000ml four-necked flask equipped with a magnetic stirrer, condensing device and tail gas receiving device is 80% hydrazine hydrate and 150ml deionized water, and dripping 85ml of concentration under stirring is 65% nitric acid, control The temperature of the system is below 40°C, after the dropwise addition is completed, test the pH value and adjust the pH value to 7;

[0039] Add 146.8g of technical grade guanidine nitrate and 420ml of hydrazine hydrate with a concentration of 80% to the system, heat and heat up under stirring, when the internal temperature rises to 65°C, the guanidine nitrate dissolves completely, then continue to heat up, when the system temperature reaches Reflux starts at 90°C, accompanied by a large amount of gas discharge. When the temperature reaches 95°C, start timing, control the reaction temperature at 95°C~100°C, and control the reac...

Embodiment 3

[0044] Synthesis of triaminoguanidine nitrate in 2000ml container:

[0045] Adding the concentration of 150ml in the 2000ml four-neck flask equipped with a magnetic stirrer, condensing device and tail gas receiving device is 80% hydrazine hydrate and 290ml deionized water, and adding dropwise 210ml concentration is 65% nitric acid under stirring state, control The temperature of the system is below 40°C, after the dropwise addition is completed, test the pH value and adjust the pH value to 7;

[0046] Add 294.0g of technical grade guanidine nitrate and 850ml of hydrazine hydrate with a concentration of 80% to the system, and heat up under stirring. When the internal temperature rises to 62°C, the guanidine nitrate is completely dissolved, and then continue to heat up. When the system temperature reaches The reflux starts at 90°C, and a large amount of gas is discharged. When the temperature reaches 96°C, the timing starts, and the reaction temperature is controlled at 96°C~99°...

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Abstract

The invention relates to a synthesis method of triaminoguanidinium nitrate. The defects of foreign literature report technological approaches are overcome, low-price industrial-grade guanidine nitrate and hydrazine hydrate are used as raw materials, deionized water is used as solvent, nitric acid is used as a catalyst, and triaminoguanidinium nitrate is synthesized through a two-step reaction method. By means of the method, the synthesis time is short, raw materials are low in price, can be easily obtained and are high in utilization rate, the synthesis route is safe, the post-processing method is simple, the synthesized target compound product is high in yield and purity, and byproducts can be recycled. Triaminoguanidinium nitrate synthesized through the method is mainly used for clean type gas generator charging, missiler roll control, start of turbopumps used for servo mechanisms, emergent starters of jet aircrafts, automobile air bags and the like.

Description

technical field [0001] The invention relates to a method for synthesizing triaminoguanidine nitrate (abbreviated TAGN) used in a clean gas generator by adopting a secondary drop method. The triaminoguanidine nitrate synthesized by the method is mainly used for charge of clean gas generators, rolling control of missiles, startup of turbo pumps for servo mechanisms, emergency starters of jet aircraft, automobile airbags and the like. The gas generating agent with TAGN as the oxidant overcomes the shortcomings of ammonium nitrate (abbreviated as AN) type gas generating agent such as low energy and high hygroscopicity, and has the advantages of good ignition and combustion performance and no hydrogen chloride gas in the gas. It is an ideal clean gas generating agent. One of the varieties. Background technique [0002] Gas generating agent is a low-temperature slow-burning propellant, which is mainly used for gas generator charge. Because the gas generator has simple structure,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C281/16
Inventor 王锐孙忠祥李建华信培培张先瑞孙红光肖金武
Owner HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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