Binuclear beta-diketone catalyst for synthesizing syndiotactic polystyrene and its preparation method
A polystyrene and catalyst technology, applied in the field of dual-nuclear catalysts and their preparation, can solve the problems of low polymerization activity and the like, and achieve the effects of low production cost, improved activity and life, and high olefin polymerization activity
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Embodiment 1
[0031] In a 100ml two-necked flask equipped with a stirrer, add 20ml of ethanol and 2.3g of alkali metal sodium, under the reflux temperature of ethanol, add 1.5g of acetylacetone and 2g of dichlorohexane respectively, react for 2 hours, filter and dry to obtain the ligand ( CH 3 CO) 2 CH-(CH 2 ) 6 -CH(COCH 3 ) 2 0.85g. N at 0°C 2 Dissolve 0.5g of the ligand in ether solution and add to the solution containing 1.5ml of Ti(OPh) 4 Carry out complex coordination in the diethyl ether solution, when the temperature reaches room temperature, then raise the temperature to the solvent reflux temperature, reflux for 6 hours, filter and wash the precipitate, and vacuum dry to obtain the main catalyst A 2 Ti(OPh) 2 (A=(CH 3 CO) 2 CH-(CH 2 ) 6 -CH(COCH 3 ) 2 ) 0.46g. In a 100ml two-necked flask replaced by nitrogen and equipped with a stirrer, add 15ml of toluene distilled by reflux of metal sodium, stir and raise the temperature to 20°C, add the main catalyst A 2 Ti(OPh) ...
Embodiment 2
[0033] In a 100ml two-necked flask equipped with a stirrer, add 20ml of ethanol and 2.3g of alkali metal sodium, and at the reflux temperature of ethanol, add 1.5g of acetylacetone and 2g of potassium iodide respectively, react for 2 hours, filter and dry to obtain the ligand (CH 3 CO) 2 CH-CH (COCH 3 ) 2 0.63g. N at 0°C 2 Dissolve 0.4g of the ligand in ether and add to the solution containing 1.5ml of TiCl 4 Carry out complexation and coordination in the diethyl ether solution, when the temperature reaches room temperature, then raise the temperature to the solvent reflux temperature, reflux for 6 hours, filter and wash the precipitate, and vacuum dry to obtain the main catalyst ATiCl 3 (A=(CH 3 CO) 2 CH-CH (COCH 3 ) 2 ) 0.26g. In a 100ml two-necked flask replaced by nitrogen and equipped with a stirrer, add 15ml of toluene distilled by reflux of metal sodium, heat up to 80°C under stirring, add the main catalyst ATiCl 3 19.69mg (the concentration is 1×10 -3 mol / L...
Embodiment 3
[0035] In a 100ml two-necked flask equipped with a stirrer, add 20ml of ethanol and 2.3g of alkali metal sodium, and add (CH 3 CO)(CF 3 CO)CH 2 1.5g and p-dichlorobenzene 1.3g, reacted for 2 hours, filtered and dried to obtain ligand (CH 3 CO)(CF 3 CO)CH-C 6 h 4 -CH(CH 3 CO)(CF 3 CO) 1.1 g. N at 0°C 2 Dissolve 0.3g of the ligand in ether solution and add to the solution containing 1.5ml NiCl 2 Carry out complexation and coordination in the ether solution, then heat up to the solvent reflux temperature, reflux for 6 hours, filter and wash the precipitate, and vacuum dry to obtain the main catalyst ANiCl 2 (A=(CH 3 CO)(CF 3 CO)CH-C 6 h 4 -CH(CH 3 CO)(CF 3 CO)) 0.26g. In a 100ml two-necked flask replaced by nitrogen and equipped with a stirrer, add 15ml of toluene distilled by metal sodium reflux, heat up to 80°C under stirring, add the main catalyst ANiCl 23.68mg (the concentration is 1.619×10 -4 mol / L), according to the mol ratio of co-catalyst and main catal...
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