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Preparation method of energetic metal coordination compound of 5-methyltetrazole

A technology of methyl tetrazole and metal coordination, applied in 1/11 groups of organic compounds without C-metal bonds, organic chemistry methods, organic chemistry and other directions, can solve the problems of high reaction temperature and low yield, and achieve High Purity, High Yield, High Yield Effect

Active Publication Date: 2019-10-15
NINGXIA UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the solvent required for the synthesis of such complexes is an organic solvent, the reaction temperature is high, and the yield is generally low

Method used

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  • Preparation method of energetic metal coordination compound of 5-methyltetrazole
  • Preparation method of energetic metal coordination compound of 5-methyltetrazole
  • Preparation method of energetic metal coordination compound of 5-methyltetrazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Dissolve 8.4 mg (0.1 mmol) of 5-methyltetrazole (Mtta) in 6 mL of distilled water, add 25.5 mg (0.15 mmol) of AgNO 3 , after stirring for 30 minutes, put it into a 15mL reaction kettle with a polytetrafluoroethylene liner, react at a constant temperature of 120°C for 72h, then lower it to 80°C and keep it for 12h, and then lower it to room temperature at a rate of 3°C / h to obtain the target The product 5-methyltetrazole energetic metal coordination compound has a yield of 92% and a purity of 99.9%.

[0028] The powder diffraction pattern of the 5-methyltetrazole energetic metal coordination compound prepared in this example is shown in figure 1 , see the infrared spectrum figure 2 ,Depend on figure 1 and figure 2 The compound can be obtained as [Ag(Mtta)] n . The crystallographic data of the 5-methyltetrazole energetic metal coordination compound prepared in this example are shown in Table 1. Use the oxygen bomb calorimeter to measure the heat of combustion of t...

Embodiment 2

[0033] Dissolve 8.4 mg (0.1 mmol) of methyl tetrazole (Mtta) in 6 mL of distilled water, add 17.0 mg (0.1 mmol) of AgNO 3 , that is, Mtta and AgNO 3 The molar ratio is 1:1. After stirring for 30 minutes, put it into a 15mL reaction kettle with a polytetrafluoroethylene liner, react at a constant temperature of 119°C for 71h, then lower it to 80°C and keep it for 12h, and then at a rate of 3°C / h The rate was lowered to room temperature, and the target product 5-methyltetrazole energetic metal coordination compound was obtained with a yield of 90% and a purity of 99.9%.

Embodiment 3

[0035] Dissolve 8.4 mg (0.1 mmol) of methyl tetrazole (Mtta) in 6 mL of distilled water, add 34.0 mg (0.2 mmol) of AgNO 3 , that is, Mtta and AgNO 3 The molar ratio is 1:2. After stirring for 30 minutes, put it into a 15mL reaction kettle with a polytetrafluoroethylene liner, react at a constant temperature of 121°C for 70h, then lower it to 82°C and keep it for 12h, and then at a rate of 3°C / h The rate was reduced to room temperature, and the target product 5-methyltetrazole energetic metal coordination compound was obtained with a yield of 91% and a purity of 99.9%.

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Abstract

The invention discloses a preparation method of an energetic metal coordination compound of 5-methyltetrazole, and belongs to the technical field of preparation of energetic metal coordination compounds. The preparation method comprises the following steps: dissolving methyltetrazole in distilled water, adding a nitrate, performing stirring for 30 min, adding the obtained solution into a reactor with a polytetrafluoroethylene liner, carrying out a constant-temperature reaction at 120 + / - 1 DEG C for 72 h, then lowering the temperature to 80 DEG C, keeping the temperature for 12 h, and then lowering the temperature to room temperature at a rate of 3 DEG C / h to obtain the target coordination compound. The coordination compound has good explosion heat, good heat stability and low mechanical sensitivity, and the product with a high purity and a high yield can be prepared by the green environmentally-friendly method.

Description

technical field [0001] The invention relates to the technical field of preparation of energetic metal coordination compounds, in particular to a preparation method of 5-methyltetrazole energetic metal coordination compounds. Background technique [0002] Energetic materials include explosives, propellants and pyrotechnics, etc., which are widely used in various fields, such as: aerospace propellants, mining engineering, pyrotechnics manufacturing, etc. With the increasingly widespread application of energetic materials, the requirements for them are also constantly changing, and have gradually evolved from the pursuit of high energy to the pursuit of "safety, green, high energy, and high density". Due to the advantages of high density, good thermal stability, excellent mechanical strength and hardness, energetic metal complexes can better meet the requirements of high energy and insensitivity, and will become a new generation of energetic materials. According to comprehensi...

Claims

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Application Information

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IPC IPC(8): C07D257/04
CPCC07D257/04C07B2200/13C07F1/005
Inventor 刘翔宇周惠良杨金会马晓慧曹森妮
Owner NINGXIA UNIVERSITY
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