Green gas generating agent hydrated pentazole metal salt and preparation method thereof
A technology of hydrated pentazole and green gas, which is applied in the field of green gas generating agent hydrated pentazole metal salt and its preparation, can solve problems such as burning out of control, achieve good thermal stability, and the effect of simple and efficient preparation method
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Embodiment 1
[0045] Preparation of pentazole anion solution
[0046] see Figure 5As shown, add 5mL of methanol / acetonitrile into a 25mL three-necked flask, place it in a low-temperature reactor and cool it down to -45°C, and then add 0.191g of 3,5-dimethyl-4-hydroxyarylpentazole (1mmol) , Dissolve 0.966g of tetrabutylammonium bromide (3mmol) in a mixed solution of 1mL of deionized water + 1mL of methanol, cool to -45°C and add to a three-necked flask. Subsequently, 1.645g of cerium ammonium nitrate (3mmol) and 0.1g of ferrous chloride tetrahydrate (0.5mmol) were dissolved in a mixed solution of 3mL of deionized water and 3mL of methanol, cooled to -45°C and added dropwise to a three-necked flask , after stirring and reacting for 30 min, the temperature was raised to 0° C., and the reaction was continued for 2 hours. The reaction solution was detected by mass spectrometry, and it was confirmed that pentazole negative ions were generated. Then filter, spin evaporate, soak with 10ml of met...
Embodiment 2
[0048] Taking sodium chloride as an example to prepare the crystal of pentazole sodium
[0049] Configure the ethanol / water (volume ratio 1:1) mixed solution of sodium chloride NaC, and the concentration is 1 mol / L; Configure the ethanol / water (volume ratio 1:1) mixed solution of pentazole, and the concentration is 1mol / L; Mix the above two solutions in equal volumes. If a small amount of precipitate precipitates or becomes turbid immediately after mixing, add ethanol or deionized water until clarification; ultrasonic for 30 minutes, filter with an ultrafiltration membrane; place in a constant temperature and humidity box, 70 ℃, humidity 10%, until 1 / 2 of the solvent evaporates; lower the temperature to 10 ℃, humidity 100%, the solvent slowly evaporates, and crystals form.
Embodiment 3
[0051] The volume ratio of the two ethanol / water solutions in Example 2 was adjusted to 60%:40%, and the temperature of the constant temperature and humidity box was set at 40°C to stand still. The obtained crystals were characterized as in Example 2.
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