Method for preparing small-size Pd<KBr>@HSC by in-situ bromine addition
A small-sized, in-situ addition technology, applied in chemical instruments and methods, catalyst activation/preparation, chemical/physical processes, etc., can solve the problems of low catalyst recycling rate, low selectivity, active component shedding, etc., to achieve Effects of improving reuse efficiency, improving catalyst activity, and improving selectivity
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Embodiment 1
[0041] (1) Preparation of Pd KBr @SiO 2 : Take cyclohexane (40mL), n-octanol (10mL) as the oil phase, polyethylene glycol monohexadecyl ether (Brij56) (6.521g) as the surfactant, mix and dissolve at 35°C; 0.03gKBr as the functional The molecule was added to 1 mL of chloropalladium acid solution with a concentration of 0.075M, dissolved and added dropwise to the above oil phase solution as the water phase to form reverse micelles. Because the water phase is incompatible with the oil phase, a rigid film with strong rigidity will be formed at the interface of the two phases, so the water phase will form an independent nanoscale microreactor ( figure 1 -I). After the above solution was stirred for 2 h, 300 μL of NaBH was added 4 (10wt%) solution, palladium ion (Pd 2+ ) by NaBH 4 rapidly reduced to palladium nanoparticles ( figure 1 -II). After reacting for 10min, add 3ml NH dropwise 3 ·H 2 O, provide an alkaline environment for the hydrolysis of TEOS, and then add TEOS dr...
Embodiment 2
[0045] (1) Take a mixture of 35ml of n-heptane and 5ml of propanol as the oil phase, and 6g of nonylphenol polyoxyethylene ether as the surfactant, mix them and dissolve them at 30°C to obtain product A;
[0046] (2) Add 0.02gNH 3 Add Br as a functional molecule to 1ml of chloropalladium acid solution with a concentration of 0.07M, dissolve it and add it to product A as the water phase to form reverse micelles to obtain product B;
[0047] (3) After stirring product B for 1 h, add 250 μL of 10 wt% NaBH 4 solution, continue to add 2ml NH after reacting for 5min 3 ·H 2 O, to be NH 3 ·H 2 After O was fully dispersed around the palladium nanoparticles, TEOS was added dropwise to react for 5 hours, then 40ml of ethanol was added, and finally washed by centrifugation with ethanol to obtain Pd KBr @SiO 2 catalyst;
[0048] (4) Pd obtained with step (3) KBr @SiO 2 The catalyst is used as a template agent, dispersed into a mixture of 60ml of deionized water and 30ml of ethanol...
Embodiment 3
[0052] (1) Take the mixture of 45ml of isooctane and 15ml of n-heptanol as the oil phase, and 7g of sodium lauryl sulfate as the surfactant, mix it and dissolve it at 40°C to obtain product A;
[0053] (2) Adding 0.04g NaBr as a functional molecule into 1ml of chloropalladium acid solution with a concentration of 0.08M, after dissolving, add it to product A as the water phase to form reverse micelles to obtain product B;
[0054] (3) After stirring product B for 3 hours, add 350 μL of NaBH with a concentration of 10 wt%. 4 solution, continue to add 4ml NH after reacting for 15min 3 ·H 2 O, to be NH 3 ·H 2 After O was fully dispersed around the palladium nanoparticles, TEOS was added dropwise to react for 7 hours, then 60ml of ethanol was added, and finally washed by ethanol centrifugation to obtain PdKBr@SiO 2 catalyst;
[0055] (4) Pd obtained with step (3) KBr @SiO 2 The catalyst is used as a template agent, dispersed into a mixture of 80ml deionized water and 40ml et...
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