Wells-dawson type phosphotungstic acid and preparation method thereof
A technology of phosphotungstic acid and phosphoric acid, which is applied in the preparation of tungsten compounds, chemical instruments and methods, tungsten compounds, etc., can solve the problems of high content and lower purity of final products, and achieve high purity, less impurities, increased yield and The effect of purity
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[0026] The preparation method of the Wells-Dawson type phosphotungstic acid provided in this embodiment comprises the following steps:
[0027] Divide the tungsten trioxide powder into 9-12 parts, and add them in batches into phosphoric acid at 60-80°C within 6-10 hours and mix evenly, then heat in a water bath or microwave to 120-180°C for 12-24 hours to obtain phosphorus Tungstic acid solution, the molar ratio of phosphoric acid to tungsten trioxide is 12-18:1; preferably, the particle size of tungsten trioxide powder is 30-60 μm, and the tungsten trioxide powder is heated to 60-80°C and added to phosphoric acid, Mix tungsten trioxide powder and phosphoric acid evenly and react at 160-170°C for 12-16 hours to obtain phosphotungstic acid solution.
[0028] Mix phosphotungstic acid solution with inorganic acid and place it for 3-5 hours to acidify, then use ether to extract 5-8 times, and dry the collected lower layer liquid at 100-120°C for 6-12 hours to obtain phosphotungsti...
Embodiment 1
[0033] This embodiment provides a kind of preparation method of Wells-Dawson type phosphotungstic acid, comprising the following steps:
[0034] Add 40mL of phosphoric acid into a 100mL four-necked flask with a cooling reflux device, stir and heat to 60°C; divide 11.6g of tungsten trioxide powder into 10 equal parts, add them in batches to the four-necked flask within 6 hours and mix Obtain the reaction solution evenly, then put the four-neck flask into the hydrothermal synthesis kettle and heat it to 120°C for 12 hours, cool to room temperature to obtain the phosphotungstic acid solution, add 10mL hydrochloric acid to the phosphotungstic acid solution and leave it for 3 hours for acidification , and then pour the acidified phosphotungstic acid solution into the separatory funnel, add 50mL ether to the separatory funnel for 5 extraction operations, collect the lower layer liquid after each extraction to obtain the phosphotungstic acid ether mixture, and finally use rotary evapo...
Embodiment 2
[0036] This embodiment provides a kind of preparation method of Wells-Dawson type phosphotungstic acid, comprising the following steps:
[0037] Add 60mL of phosphoric acid into a 100mL four-neck flask with a cooling reflux device, stir and heat to 80°C; heat 11.6g of tungsten trioxide powder to 80°C, divide it into 10 equal parts, and add it to the flask in batches within 8 hours Mix well in the four-necked flask to obtain a reaction solution, then put the four-necked flask into a synthesis kettle and heat it with microwave to 160°C for 18 hours, then cool to room temperature to obtain a phosphotungstic acid solution, add 20mL of hydrochloric acid to the phosphotungstic acid solution and place it Acidify for 5 hours, then pour the acidified phosphotungstic acid solution into the separatory funnel, add 80mL ether to the separatory funnel for 8 extraction operations, collect the lower layer after each extraction to obtain the phosphotungstic acid ether mixture, and finally use ...
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