A kind of dodecaphosphomolybdate H 3 PMo 12 O 40 ·21H 2 Preparation method of O crystal material
A technology of h3pmo12o40·21h2o, dodecaphosphomolybdic acid, applied in the direction of polycrystalline material growth, crystal growth, chemical instruments and methods, etc., can solve the problem of low molybdenum conversion rate, long reaction time, and no literature report on the preparation method of single crystal material. and other problems, to achieve the effects of high reaction yield, simple and easy-to-operate synthesis method, and high yield
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Embodiment 1
[0016] ①. Weigh 2.0g of ammonium molybdate and 1.2g of aluminum nitrate in a 50mL flask, add 15mL of distilled water, and dropwise add 0.08mL of phosphoric acid, place the flask on a magnetic stirrer and stir for 10 minutes to obtain a mixed solution.
[0017] ②. Transfer the uniformly mixed solution to a 25mL autoclave.
[0018] ③. Put the autoclave into an oven, heat it from room temperature to 190 °C at a rate of 1 °C / min, keep it at this temperature for 12 hours, and then lower it to room temperature at a rate of 0.2 °C / min to obtain the following: figure 1 photo, figure 2 and 3 The shape shown in the curve grows polyhedral crystal material well, and the yield is 73%.
[0019] pass figure 1 It can be seen that the product is a polyhedral single crystal with regular shape and good growth.
[0020] pass figure 2 It can be seen that: the XRD diffraction peak of the product is strong, indicating that the crystallinity is high; there are no other diffraction peaks, indic...
Embodiment 2
[0023] ①. Weigh 2.0g of ammonium molybdate and 1.2g of aluminum nitrate in a 50mL flask, add 15mL of distilled water, and dropwise add 0.08mL of phosphoric acid, place the flask on a magnetic stirrer and stir for 10 minutes to obtain a mixed solution.
[0024] ②. Transfer the uniformly mixed solution to a 25mL autoclave.
[0025] ③. Put the autoclave into an oven, heat it from room temperature to 190 °C at a rate of 1 °C / min, keep it at this temperature for 10 hours, and then lower it to room temperature at a rate of 0.25 °C / min to obtain the following: figure 1 photo, figure 2 and 3 The shape shown in the curve grows polyhedral crystal material well, and the yield is 71%.
Embodiment 3
[0027] ①. Weigh 2.0g of ammonium molybdate and 1.2g of aluminum nitrate in a 50mL flask, add 15mL of distilled water, and dropwise add 0.08mL of phosphoric acid, place the flask on a magnetic stirrer and stir for 10 minutes to obtain a mixed solution.
[0028] ②. Transfer the uniformly mixed solution to a 25mL autoclave.
[0029] ③ Put the autoclave into an oven, heat it from room temperature to 190 °C at a rate of 1 °C / min, keep it at this temperature for 12 hours, and then lower it to room temperature at a rate of 0.3 °C / min to obtain the following figure 1 photo, figure 2 and 3 The shape shown in the curve grows well polyhedral crystal material with a yield of 75%.
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