A kind of palladium catalyst complexed with sulfide ionic liquid and its preparation method and application
A technology of ionic liquid and palladium catalyst, which is applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, catalytic reaction, etc., can solve the problem that is not suitable for improving the deactivation and large-scale The limitations of the industrial application of production equipment, the unsatisfactory catalyst stability and other problems, to achieve good economy and industrial application value, high stability and low loading effect
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Embodiment 1
[0066] Select columnar activated carbon as the carrier, its particle size is 40 mesh, the ash content is 3.0wt%, and the specific surface area is 950m 2 / g, a pore volume of 0.45 mL / g, and treated with 300 ml of 10 wt% hydrochloric acid at 25° C. for 3 h. The treated carrier was washed with deionized water until neutral, dried at 110 °C for 12 h, and used for later use.
[0067] Synthesis of Sulfide Ionic Liquid A:
[0068] The ionic liquid 1-butyl-3-methylimidazolium chloride and sulfur powder were mixed in a mass ratio of 1:0.5, stirred in a water bath at 40 °C for 10 min, and then added with acetonitrile solution, dissolved, and stirred at 40 °C for 12 hours. The above mixed solution was stirred evenly, then filtered to remove unreacted sulfur powder, and the obtained filtrate was dried at 110 ° C. Subsequently, the sample obtained after drying was dissolved in dichloromethane, and an appropriate amount of desulfurization was added. Ionized water and sodium bicarbonate so...
Embodiment 2
[0072] The main difference between this example and Example 1 is that the type of ionic liquid is different, and its influence on the catalytic performance of the catalyst is studied.
[0073] Synthesis of Sulfide Ionic Liquid B:
[0074] Mix the ionic liquid 1-propyl-3-methylimidazolium tetrafluoroborate with sulfur powder in a mass ratio of 1:0.5, stir in a water bath at 40 °C for 10 min, add acetonitrile solution, dissolve, and stir at 40 °C After 12 hours, the above mixture was stirred evenly, then filtered to remove the unreacted sulfur powder, and the obtained filtrate was dried at 110°C. Appropriate amount of deionized water and sodium bicarbonate solution were used to further remove impurities in the solution. Finally, after drying the above mixture at 110 °C for 16 hours, recrystallized at room temperature to obtain the required sulfide ionic liquid. B.
[0075] Select columnar activated carbon as the carrier, its particle size is 40 mesh, the ash content is 3.0wt%,...
Embodiment 3
[0079] Select columnar activated carbon as the carrier, its particle size is 40 mesh, the ash content is 3.0wt%, and the specific surface area is 950m 2 / g, pore volume 0.6 mL / g, and treated with 300 ml of 10 wt% hydrochloric acid at 25° C. for 3 h. The treated carrier was washed with deionized water until neutral, dried at 110 °C for 12 h, and used for later use.
[0080] Synthesis of Sulfide Ionic Liquid A:
[0081] The ionic liquid 1-butyl-3-methylimidazolium chloride and sulfur powder were mixed in a mass ratio of 1:0.5, stirred in a water bath at 40 °C for 10 min, and then added with acetonitrile solution, dissolved, and stirred at 40 °C for 12 hours. The above mixed solution was stirred evenly, then filtered to remove unreacted sulfur powder, and the obtained filtrate was dried at 110 ° C. Subsequently, the sample obtained after drying was dissolved in dichloromethane, and an appropriate amount of desulfurization was added. Ionized water and sodium bicarbonate solution...
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