Nitrogen-containing heterocyclic palladium phosphinesulfonate catalyst and ligand and application thereof
A palladium phosphine sulfonate and catalyst technology, which is applied in the field of olefin polymerization, can solve the problems of low activity and low molecular weight of polyethylene, and achieve the effect of improving reaction activity and increasing molecular weight
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[0051] The specific preparation steps include: (1) 8 mL of n-hexane solution containing 20 mmol of n-butyllithium was slowly added dropwise and dissolved in 25 mL of tetrahydrofuran solution containing 10 mmol of benzenesulfonic acid at 0°C, reacted for 1 h, and cooled to - After 78 °C, 25 mL of a tetrahydrofuran solution containing 10 mmol of phenylphosphine dichloride was added thereto, and reacted at -78 °C for 1 h to obtain a mixed solution A; (2) Under nitrogen protection, 20 mL of 2-(N-tetrahydrofuran containing 10 mmol of pyrrolyl) bromobenzene in tetrahydrofuran was cooled to -78°C, 4 mL of n-hexane solution containing 10 mmol n-butyllithium was slowly added to it, and the reaction was performed at -78°C for 1 h to obtain a lithium salt solution; (3) at -78°C , the lithium salt solution was added to the mixed solution A, then it was naturally raised to room temperature from -78°C, and continued to stir for 24h; (4) the solvent was spin-dried, the residue was dissolved i...
example 1
[0080] In Example 1, a method for catalyzing polymerization of ethylene with a catalyst shown in the above formula (I) is provided, comprising the steps of: (1) in a glove box in a nitrogen atmosphere, adding 20 mL of toluene and 10 μmol of nickel acetate into into a 350 mL autoclave with a magnetic stirring device, an oil bath heating device and a thermometer, connect the container to the high-pressure pipeline and evacuate the pipeline, heat the container to 80°C with an oil bath, and keep it warm for 10 minutes; (2 ) 2mL of dichloromethane dissolved with 10 μmol N-morpholinyl-substituted phosphine sulfonate palladium catalyst is injected into the polymerization system of the reaction mixture through a syringe, the valve is closed, and the ethylene pressure is adjusted to be 8 atmospheres, and the reaction is 60min; (3) The reaction was stopped, the reactor was opened, ethanol was added to precipitate the solid, filtered under reduced pressure, and dried in a vacuum drying ov...
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