Palladium catalyst, preparation method thereof and dimethyl oxalate synthesis method
A technology of dimethyl oxalate and palladium catalyst is applied in catalyst activation/preparation, chemical instrument and method, physical/chemical process catalyst, etc., can solve the problem of high cost, achieve high activity and selectivity, stable structure, and preparation method simple effect
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Embodiment 1
[0047] A kind of palladium catalyst, concrete preparation method is as follows:
[0048] 1) Measure 25 μL of concentrated hydrochloric acid (commercially available product, the mass concentration of concentrated hydrochloric acid is 36%-38%) and dissolve in 30 mL of water to obtain a dilute hydrochloric acid solution, and weigh 0.17 g of PdCl 2 , 0.54g of CuCl 2 Add to the dilute hydrochloric acid solution to dissolve, add 20 μg tetradecyltrimethylammonium bromide, add water to make up to 100 mL, and then mix evenly in an oil bath at 80°C to obtain the first mixed solution;
[0049] 2) Take sodium borohydride and dissolve it in sodium hydroxide solution (the temperature of the sodium hydroxide solution is lower than room temperature) to prepare the second mixed solution whose sodium borohydride concentration is 0.5mmol / L, and add a small amount of surfactant to mix Evenly, take 7mL of the second mixed solution and slowly add it to the first mixed solution, ultrasonically reac...
Embodiment 2
[0053] A kind of palladium catalyst, concrete preparation method is as follows:
[0054] 1) Measure 25 μL of concentrated hydrochloric acid (commercially available product, the mass concentration of concentrated hydrochloric acid is 36%-38%) and dissolve in 30 mL of water to obtain a dilute hydrochloric acid solution, and weigh 0.42 g of PdCl 2 , 1.01g of CuCl 2 Add to the dilute hydrochloric acid solution to dissolve, add 40 μg of tetradecyltrimethylammonium bromide, add water to make up to 100 mL, and then mix evenly in an oil bath at 80°C to obtain the first mixed solution;
[0055] 2) Take sodium borohydride and dissolve it in sodium hydroxide solution (the temperature of the sodium hydroxide solution is lower than room temperature) to prepare the second mixed solution whose sodium borohydride concentration is 0.5mmol / L, and add a small amount of surfactant to mix Evenly, take 13mL of the second mixed solution and slowly add it to the first mixed solution, ultrasonically ...
Embodiment 3
[0059] A kind of palladium catalyst, concrete preparation method is as follows:
[0060] 1) Measure 25 μL of concentrated hydrochloric acid (commercially available product, the mass concentration of concentrated hydrochloric acid is 36%-38%) and dissolve in 30 mL of water to obtain a dilute hydrochloric acid solution, and weigh 0.84 g of PdCl 2 , 0.67g of CuCl 2 Add to the dilute hydrochloric acid solution to dissolve, add 40 μg of tetradecyltrimethylammonium bromide, add water to make up to 100 mL, and then mix evenly in an oil bath at 80°C to obtain the first mixed solution;
[0061] 2) Take sodium borohydride and dissolve it in sodium hydroxide solution (the temperature of the sodium hydroxide solution is lower than room temperature) to prepare the second mixed solution whose sodium borohydride concentration is 0.5mmol / L, and add a small amount of surfactant to mix Evenly, take 15mL of the second mixed solution and slowly add it to the first mixed solution, ultrasonically ...
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