Catalyst systems and their use in polymerization process
A catalyst, metallocene catalyst technology, applied in chemical instruments and methods, compounds of elements of Group 4/14 of the periodic table, organic chemistry, etc.
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Embodiment 1
[0162] Example 1: Catalyst system comprising a hafnium catalyst containing a Group 15 element
[0163] Preparation (2,4,6-Me 3 C 6 h 2 )NHCH 2 CH 2 ] 2 NH (ligand)
[0164] In a 2-liter single-necked Schlenk flask equipped with a magnetic stir bar, diethylenetriamine (23.450 g, 0.227 mol), tricresyl bromide (90.51 g, 0.455 mol), tris(dibenzyl Dipalladium (1.041g, 1.14mol), rac-2.2'-bis(diphenylphosphino)-1.1'-binaphthyl (2.123g, 3.41mol), sodium tert-butoxide (65.535g , 0.682mol), and toluene (800ml). The reaction mixture was heated to 95°C and stirred. After 4 days, the reaction was judged to be complete by proton nuclear magnetic resonance (NMR) spectroscopy. All solvent was removed under vacuum and the residue was dissolved in diethyl ether (1 L). The ether was washed three times with water (1 L) and saturated aqueous NaCl (500 mL), and dried over magnesium sulfate. The red oil obtained by removing the ether in vacuo was dried under vacuum at 70° C. for 12 hours ...
Embodiment 2
[0181] Example 2: Mixed Catalyst System Comprising a Group 15 Element-Containing Hafnium Metal Catalyst and a Bulk Ligand Metallocene Catalyst
[0182] In the following examples the bulky ligand metallocene catalyst compound (n-propyl-cyclopentadienyl) was used 2 ZrCl2 , which was obtained from Boulder Scientific, Meade, Colorado. [(2,4,6-Me 3 C 6 h 2 )NHCH 2 CH 2 ] 2 NH (ligand), and {[(2,4,6-Me 3 C 6 h 2 ) NCH 2 CH 2 ] 2 NH}Hf(CH 2 Ph) 2 (Hf-HN3).
[0183] Preparation of Mixed Catalyst 2A
[0184] Into a 100 mL round-bottomed flask containing 1.85 g of MAO (6.18 g of a 30% solution in toluene, Albemarle Corporation, Baton Rouge, Louisiana) and 6.63 g of toluene, 0.139 g of the Hf-HN prepared above and 0.025 g (normal Propyl-cyclopentadienyl) 2 ZrCl 2 . The solution was stirred for 10 minutes. Then, 4.98 g of silica (Crosfield ES-70, calcined at 600°C, commercially available from Crosfield Limited, Warrington, England) were added by mixing. The mixture wa...
Embodiment 2A
[0187] Example 2A: Slurry Phase Ethylene Polymerization
[0188] Polymerization was carried out in the slurry phase in a 1 liter autoclave reactor equipped with mechanical stirrer, external water jacket for temperature control, septum inlet and vent tube with regulated feed of dry nitrogen and ethylene . The reactor was dried and degassed at 160°C. Isobutane (400 mL) was added as a diluent and 0.7 mL of a 25% by weight solution of trioctylaluminum in hexane as a scavenger using a gas-tight syringe. The reactor was heated to 90°C. 0.100 g of mixed Catalyst 2A was charged with ethylene pressure and the reactor was pressurized with 136 psi (938 kPa) of ethylene. Polymerization was continued for 30 minutes while maintaining the reactor at 90°C and 136 psi (938 kPa) by a constant flow of ethylene. The reaction was terminated by rapid cooling and venting. Obtain 83.0g ethylene homopolymer (I 21 =3.5, the activity is 4770 g PE / mmol catalyst·atmospheric pressure·hour).
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