Method for synthesizing pinacol through photocatalysis
A technology of photocatalysis and catalyst, applied in chemical instruments and methods, preparation of organic compounds, preparation of hydroxyl compounds, etc., can solve the problems of low conversion rate, no pinacol, poor selectivity, etc., and achieve high activity and simple separation , stable effect
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Embodiment 1
[0020] Preparation of pure rutile TiO by using P25 as raw material and calcination at 900 °C for 10 hours 2 nanoparticles. Take 1g of pure rutile TiO 2 Disperse in 200ml of isopropanol-water reaction liquid with a volume fraction of 70% isopropanol, add 1.5ml of chloroplatinic acid (1g / 10ml) according to the loading capacity of 3%, stir magnetically and blow in nitrogen. After removing the air in the system, stop feeding nitrogen, turn on the 500W ultraviolet light source, and reduce chloroplatinic acid to platinum particles by in-situ photocatalysis and load them on nano-TiO 2 On the surface, photocatalytic isopropanol was oxidized to synthesize pinacol, the reaction temperature was 10°C, and the reaction time was 24h. After the reaction solution was centrifuged and precipitated, gas chromatography analysis showed that the pinacol selectivity in the liquid phase product was 80%, and the isopropanolization rate was 2.3%.
Embodiment 2
[0022] In Zn(AC) 2 2H 2 O ethanol solution, according to Zn 2+ Diethanolamine was added at a molar ratio of 5:6 to the surfactant, stirred at 70°C for 40 minutes, and aged for 24 hours to obtain a transparent sol. After centrifugal separation, drying at 80°C and heat treatment at 400°C, white wurtzite ZnO nanoparticles were obtained. Take 1g of wurtzite ZnO nanoparticles and disperse them into 300mL of isopropanol-water reaction liquid with a volume fraction of 20% isopropanol, add 0.3ml of chloroauric acid (1g / 10ml) according to the loading capacity of 3%, magnetically stir and pass into Nitrogen, after removing the air in the system, stop feeding nitrogen, turn on the 800W ultraviolet light source, reduce chloroauric acid to gold particles by in-situ photocatalysis and load them on the surface of nano-ZnO, and perform photocatalytic isopropanol oxidation to synthesize pinacol. The temperature is 70°C, and the reaction time is 360h. After the reaction solution was centrif...
Embodiment 3
[0024] 2mmolZn(CH 3 COO) 2 2H 2 O was dissolved in distilled water, and while stirring with a magnetic stirrer, ammonia water (1 mL / min) was added dropwise into the solution until the pH of the solution was 9-10. The above solution was moved into a 50 mL self-made reaction kettle with a polytetrafluoroethylene liner (filling ratio was 60%), and then 4.5 mmol of Na was added to the reaction kettle. 2 S·9H 2 O and 21mmol of CO(NH 2 ) 2 . Put the sealed reaction kettle into a drying oven and keep it warm at 120°C for 24h. After the reaction, it was naturally cooled to room temperature, and the product was washed several times with distilled water, then dried at 80°C for 4h, and heat-treated at 400°C to zinc blende ZnS nanoparticles. Take 1g of sphalerite ZnS nanoparticles and disperse them in 200mL of isopropanol-water reaction liquid with a volume fraction of 10% isopropanol, add silver nitrate according to the loading capacity of 5%, magnetically stir and vacuumize, and ...
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