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Method for synthesizing 1-amino-3-nitroguanidine

A synthesis method and technology of nitroguanidine, which is applied in the field of synthesis of 1-amino-3-nitroguanidine, can solve the problems of complex processing and long reaction steps, and achieve the effect of simple operation process

Inactive Publication Date: 2016-04-20
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method mainly has the following disadvantages: the reaction steps are long, and the post-reaction treatment is complicated

Method used

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  • Method for synthesizing 1-amino-3-nitroguanidine
  • Method for synthesizing 1-amino-3-nitroguanidine
  • Method for synthesizing 1-amino-3-nitroguanidine

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Experimental program
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Effect test

Embodiment 1

[0018] At room temperature, add 2g (19.4mmol) 2-methyl-3-nitroisothiourea into 40mL of water, add 80% 1.21g (19.4mmol) hydrazine hydrate dropwise, raise the temperature to 50°C after adding, keep it warm for 5h, and cool , filtered, and the filter cake was rinsed with ethanol and dried to obtain 1.28 g of a white solid, with a yield of 50%.

[0019] Structure Identification

[0020] Infrared Spectrum IR(KBr,cm -1 )ν: 3390, 3323, 3295, 3216, 1668, 1618, 1578, 1281, 1179, 1010, 708, 639

[0021] NMR spectrum: 13 CNMR (DMSO-d6, 125MHz), δ: 161.549;

[0022] 1 HNMR (DMSO-d 6 ,500MHz) δ:9.324,8.267,7.549,4.678

[0023] Elemental Analysis: Structural Formula C 1 h 5 N 5 o 2

[0024] Theoretical value: C10.08, H4.20, N58.82;

[0025] Measured value: C9.83, H4.35, N58.73;

[0026] The above structure identification data confirm that the substance obtained in this step is indeed 1-amino-3-nitroguanidine.

Embodiment 2

[0028] At room temperature, add 4g (38.8mmol) 2-methyl-3-nitroisothiourea into 40mL of water, add 80% 1.21g (19.4mmol) hydrazine hydrate dropwise, raise the temperature to 50°C after adding, keep it warm for 5h, and cool , filtered, and the filter cake was rinsed with ethanol and dried to obtain 1.15 g of a white solid, with a yield of 45%.

Embodiment 3

[0030] At room temperature, add 2g (19.4mmol) 2-methyl-3-nitroisothiourea into 40mL of water, add 80% 1.21g (19.4mmol) hydrazine hydrate dropwise, raise the temperature to 70°C after adding, keep it warm for 6h, and cool , filtered, and the filter cake was rinsed with ethanol and dried to obtain 1.2 g of a white solid, with a yield of 47%.

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Abstract

The invention discloses a method for synthesizing 1-amino-3-nitroguanidine. The method comprises the following steps of adding 2-methyl-3-nitryl isothiourea to water, dropwise adding hydrazine hydrate with the concentration being 80%, after adding of the hydrazine hydrate is ended, raising the temperature to 40-70 DEG C, preserving the temperature for 3-6 hours, conducting cooling and filtration, and conducting elution and drying with water and ethyl alcohol, so that amino nitroguanidine is obtained, wherein the mole ratio of the hydrazine hydrate to the 2-methyl-3-nitryl isothiourea is 1: (1-2). The method is mainly applied to 1-amino-3-nitroguanidine synthesis.

Description

technical field [0001] The invention relates to a synthesis method for synthesizing 1-amino-3-nitroguanidine, which belongs to the field of energetic materials. Background technique [0002] High-nitrogen energetic compounds are a new class of energetic materials developed in recent years with good application prospects. They have high positive enthalpy of formation and good thermal stability. Oxygen balance is easily achieved, and the N in the combustion product 2 High content, H 2 O and CO 2 The low content reduces the characteristic signal of the outlet gas product. The electrostatic sensitivity, shock wave sensitivity and friction sensitivity of some compounds are relatively low. Due to the superiority of high-nitrogen energetic compounds, they have potential application prospects in the field of energetic materials such as low characteristic signal propellants and new high-energy insensitive explosives. 1-amino-3-nitroguanidine (ANG) has a density of 1.722g / cm 3 ,...

Claims

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Application Information

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IPC IPC(8): C07C281/16
CPCC07C281/16
Inventor 贾思媛毕福强王伯周李祥志霍欢
Owner XIAN MODERN CHEM RES INST
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