A kind of vanadium phosphorus oxide and preparation method thereof
A vanadium phosphorus oxide, oxide technology, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problems of introducing impurities, environmental pollution, etc. The effect of slowing down the deactivation rate of carbon deposits
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[0039] (1) Preparation of ionic liquid
[0040] Will M 1 and M 2 Add to water, M 1 with M 2 The molar ratio is 1:1~1:2, heated to the reaction temperature under stirring conditions, the reaction temperature is 60~150°C, and the constant temperature reaction is 1~4h. After the reaction is completed, cool to room temperature, centrifuge, and filter to obtain the ionic liquid I .
[0041] Will M 3 and M 4 Mixed, M 3 with M 4 The molar ratio is 1:1~1:2, and the constant temperature reaction is 20~30h at the reaction temperature of 70~100°C to obtain a colorless viscous liquid, which is cooled to room temperature, washed 2~6 times with ether, and heated at 60~100°C Drying at low temperature for 24~50h, the intermediate product was obtained, which was added to acetone, and then M 1 , stirring at room temperature, suction filtration, washing, washing liquid and filtrate combined, with anhydrous MgSO 4 After drying overnight, acetone and water were evaporated by rotary evapo...
Embodiment 1
[0047] Dimethylammonium chloride 300g, ammonium tetrafluoroborate 190g, pure water 450g, mixed, heated to 80°C under stirring, kept at constant temperature for 1 hour, clarified, naturally cooled to about 30°C, centrifuged to filter out the solid to obtain 300g of ionic liquid I , the water content is about 3.5wt%, and the yield is 73wt%.
[0048] Take 1.92 mol of chloroethanol and 1.28 mol of methylimidazole and reflux at 80°C for 24 hours under the condition of microwave heating. After the reaction, a viscous colorless transparent liquid is obtained. Cool to room temperature and wash four times with ether to obtain colorless crystal 1-hydroxyethyl Base-3-methylimidazolium chloride ionic liquid, dried in a vacuum oven at 80°C for 48h. Take 100g (0.6mol) of dried 1-hydroxyethyl-3-methylimidazolium chloride ionic liquid and add it to 600ml acetone, then add 72g (0.68mol) sodium tetrafluoroborate, stir at room temperature for 24h, filter with suction, the filter residue is wax ...
Embodiment 2
[0051] Diethylammonium chloride 250g, ammonium tetrafluoroborate 180g, pure water 400g, mixed, heated to 90°C under stirring, kept at constant temperature for 1.5h, clarified, naturally cooled to about 30°C, centrifuged to filter out the solid to obtain ionic liquid I 260g, water content about 3.5wt%, yield 73wt%.
[0052] The preparation steps of 1-(4′-hydroxy)butyl-3-methylimidazolium fluoroborate ionic liquid are the same as in Example 1.
[0053] 250g ionic liquid I is joined in the four-neck flask with stirrer, add vanadium pentoxide 30.0g, auxiliary agent ferric nitrate hexahydrate 0.3g, auxiliary agent zirconium nitrate 0.5g, this reaction system is heated to the reaction temperature of 96°C, reflux reaction time 2.5h; dropwise add 35.5g of concentrated phosphoric acid with a concentration of 100% to the reaction system, the phosphorus / vanadium molar ratio is 1.1, and continue to reflux for 5h; then add 150g of 1-(4′-hydroxy)butyl Base-3-methylimidazolium fluoroborate ...
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