FIELD: chemistry.
SUBSTANCE: invention is intended for production of a polymer-containing Suzuki reaction catalyst based on palladium nanoparticles impregnated in a matrix of super-cross-linked polystyrene by impregnation with respect to moisture capacity (impregnation). The method for preparation of a polymer-containing Suzuki reaction catalyst comprises impregnation of a pre-crushed polymeric support - super-cross-linked polystyrene with a solution of chloromethyl cyanide palladium (CH3CN)2PdCl2 in tetrahydrofuran at a temperature of 20°C to 40°C followed by treatment with aqueous NaOH solution. According to the invention, prior to reduction, the catalyst is dried by evaporation at a temperature of 68 to 72°C under a vacuum⋅ of 0.8 to 1.2⋅10-3 Pa for 4.5 to 5.5 hours. Then, the catalyst is further reduced with hydrogen by sequentially purging the catalyst first with an inert gas, then with hydrogen and again with an inert gas at a gas flow rate of 95 to 105 cm3/min. After that, the catalyst is heated to a temperature of 195 to 205°C and purged with hydrogen at a flow rate of 95 to 105 cm3/min, then heating is stopped and purging with an inert gas is performed at a flow rate of 45 to 55 cm3/min. At that, the polymer carrier - super-cross-linked polystyrene is pre-washed with distilled water and acetone and dried to a constant weight.
EFFECT: increased catalytic properties of the catalyst due to the introduction of additional stages of treatment of the carrier and the active component of the catalyst.
2 cl, ex 6
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Authors
Dates
2017-08-04—Published
2016-10-26—Filed