A method for preparing ester by photocatalytic oxidative esterification of glycerin
A technology of oxidative esterification and photocatalysis, which is applied in the direction of catalyst activation/preparation, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of increasing reaction cost and complicated reaction steps, and achieve high selectivity and mild reaction conditions , active and reusable effect
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Embodiment 1
[0035] 1. Preparation of catalyst-like graphitic carbon nitride
[0036] Add 10 g of urea into the mortar, grind for 10 minutes, transfer the resulting white powder to a 30 mL crucible, compact it, cover the crucible and wrap it tightly with tin foil. The above crucible was put into a muffle furnace for calcination, the heating rate was 10°C per minute, the calcination temperature was 550°C, and the calcination time was 3 hours. After the calcination, it was naturally cooled to room temperature, and the yellow solid obtained in the crucible was taken out and ground to powder. Then the yellow powder obtained above is subjected to secondary roasting: the yellow powder is transferred to a 50mL crucible, and the crucible is placed in a muffle furnace without a cover, the heating rate is 2°C per minute, the roasting temperature is 500°C, and the roasting time is 2 Hour. After the muffle furnace is cooled to room temperature, the yellow powder in the crucible is taken out to obtai...
Embodiment 2
[0044] 1. Preparation of catalyst oxygen-doped graphite-like carbon nitride
[0045] Add 0.5 g of ammonium acetate and 10 g of urea into a mortar, grind for 10 min, transfer the resulting white powder to a 30 mL crucible, compact it, cover the crucible and wrap it tightly with tin foil. The above crucible was put into a muffle furnace for calcination, the heating rate was 10°C per minute, the calcination temperature was 550°C, and the calcination time was 3 hours. After the calcination, it was naturally cooled to room temperature, and the yellow solid obtained in the crucible was taken out and ground to powder. The yellow powder obtained above was then subjected to secondary roasting: the yellow powder was transferred to a 30 mL crucible, and put into a muffle furnace without the lid of the crucible. The heating rate was 2°C per minute, the firing temperature was 500°C, and the firing time was 2 hours. After the muffle furnace is cooled to room temperature, the yellow powder...
Embodiment 3
[0049] 1. Preparation of Catalyst Silver-supported Graphite-like Carbon Nitride
[0050] Take 0.5g of graphite-like carbon nitride prepared in Example 1, disperse it into 50mL of water, then add 10mL of 0.1M silver nitrate aqueous solution, use an ultrasonic machine with an ultrasonic power of 40kHz to ultrasonically disperse for 15min, and then use nitrogen gas bubbling to remove Gas for 30 minutes, then use a 300w xenon lamp to illuminate it, and add a magnetic stirrer at the same time. After irradiating for 15 minutes, centrifuge at 9500r / min for 5 minutes to remove the supernatant, then wash the obtained solid catalyst with deionized water for 5 times, and dry it at 60°C. That is, a silver-loaded graphite-like carbon nitride catalyst is obtained.
[0051] 2. Preparation of ester compounds by photocatalytic oxidative esterification of glycerol
[0052] The silver-supported graphite-like carbon nitride prepared in this example is used as a catalyst to catalyze the photocata...
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