A kind of preparation method of carbon quantum dot doped decapolytungstate quaternary ammonium salt
A technology of carbon quantum dots and decatungstic acid, which is applied in the field of preparation of carbon quantum dots doped decapolytungstic acid quaternary ammonium salt catalyst, can solve the problem of low quantum efficiency
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Embodiment 1
[0019] Embodiment 1 (1-1~1-4):
[0020] The carbon quantum dot modified tetrabutyl decapoly ammonium tungstate salt provided in this example is prepared according to the following two steps:
[0021] Step (1): According to literature reports (Angew.Chem.Int.Ed.2013,52,3953–3957), citric acid and ethylenediamine were used to prepare nitrogen and oxygen containing 10mg, 20mg, 30mg, and 40mg respectively by the water method. Mix the carbon quantum dot solution with 4g of tetrabutylammonium bromide, add 6ml of deionized water and sonicate until the solution is clear, transfer it to a polytetrafluoroethylene reactor and perform a hydrothermal reaction at 100°C for 24 hours;
[0022] Step (2): In a 100ml round bottom flask equipped with a stirring bar, add 6.4g of sodium tungstate dihydrate and 40mL of deionized water. After heating to boiling, quickly add 3mol / L hydrochloric acid to adjust the pH value to approximately equal to 2.3, Reflux in an oil bath at 100°C for 10 minutes. ...
Embodiment 2
[0029] Embodiment 2 (2-1~2-4):
[0030] Step (1): Prepare the aqueous solution of decapolytungstate tetrabutyl quaternary ammonium salt precipitation by the method described in Comparative Example 1;
[0031] Step (2): Add dropwise 10mg, 20mg, 30mg, 40mg of oxygen-containing, nitrogen-carbon quantum dot aqueous solution prepared by citric acid and ethylenediamine to the precipitation solution prepared in the above (1), control the pH to 2.3, and continue to stir and reflux 30min, and then transferred to a 100ml polytetrafluoroethylene reactor with water heating at 100°C for 24h. After cooling, wash and filter with deionized water and ethanol, and vacuum-dry at 60°C to obtain a carbon quantum dot modified tetrabutylammonium tungstate catalyst.
[0032] According to the method described in [0021], the catalyst prepared by the above-mentioned embodiments 2-1 to 2-4 was evaluated for photocatalytic molecular oxygen selective oxidation of cyclohexane, and the specific results are ...
Embodiment 3
[0036] Embodiment 3 (3-1~3-4):
[0037] Prepare oxygen-containing, nitrogen-carbon quantum dots doped decapolyammonium tungstate catalysts by the method described in Example 1, the difference is that in step (1) carbon quantum dots and tetrabutylammonium bromide mixed solution in polytetrafluoroethylene The temperatures for the hydrothermal reaction in the ethylene reactor were set at 80°C, 110°C, 120°C and 150°C, respectively.
[0038] According to the method described in [0021], the catalyst prepared by the above-mentioned embodiments 3-1 to 3-4 was evaluated for photocatalytic molecular oxygen selective oxidation of cyclohexane, and the specific results are shown in Table 3.
[0039] table 3
[0040]
[0041] As can be seen from Table 3, the nitrogen-containing carbon quantum dot modified decapolytungstate ammonium salt catalyst prepared at different temperatures by the method described in the invention, the conversion rate of photocatalytic oxidation of cyclohexane can r...
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