Alkane-soluble non-metallocene precatalysts
A technology of alkyl and compounds, applied in the field of alkane-soluble non-metallocene precatalysts, can solve problems such as inappropriateness and temperature rise
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[0109] Isoalkane fluid: ISOPAR-C from ExxonMobil.
[0110] Mineral oil: HYDROBRITE 380PO white mineral oil from Sonneborn.
[0111] Preparation 1A: An activator formulation comprising spray-dried methylalumoxane / treated fumed silica (sdMAO) in hexane / mineral oil was prepared. 1.6 kg of treated fumed silica (CABOSIL TS-610) was slurried in 16.8 kg of toluene, then a 10 wt% solution (11.6 kg) of MAO in toluene was added to obtain a mixture. Using a spray dryer set at 160°C and an outlet temperature at 70°C to 80°C, the mixture is introduced into the atomization device of the spray dryer to produce droplets of the mixture, which are then contacted with a stream of hot nitrogen gas to remove the The liquid was evaporated to give a powder. The powder is separated from the gas mixture in a cyclone and the separated powder is discharged into a vessel to obtain sdMAO as a fine powder.
[0112] Preparation 1B: A slurry of the activator formulation of Preparation 1A was prepared. Th...
example 2
[0134] Inventive Example 2 (IE2): Synthesis of Compound (2a) from Compound (3a) (Compound (2) wherein M is Zr and each X is Cl)
[0135] An oven-dried 400 mL glass bottle was charged with a PTFE-coated magnetic stirrer, compound (3a) (12.62 g, 22.0 mmol) and 250 mL of dry degassed diethyl ether in a glove box under nitrogen atmosphere. Chlorotrimethylsilane (6.2 mL, 48.5 mmol) was added, and the mixture was stirred at 25°C for 24 hours. The mixture was cooled in a glove box refrigerator for 1 hour. Precipitated (2a) was filtered off, and the filter cake was washed with cold n-pentane. The washed (2a) was dried under reduced pressure to obtain 10.77 g (88.0% yield) of compound (2a), bis(2-(pentamethylphenylamido)ethyl)-amine, as a white powder Zirconium(IV) dichloride. 1 H NMR (400 MHz, benzene-d 6 )δ3.40(dt,1H),2.95(dt,1H),2.59(dp,2H),2.49(s,3H),2.46(s,3H),2.43-2.34(m,1H),2.13(s ,3H), 2.06(s,3H), 2.04(s,3H). 13 C NMR (101 MHz, benzene-d 6 )δ 145.64, 133.37, 133.20, 13...
example 3
[0136] Inventive Example 3 (IE3): Synthesis of Compound (1A) from Compound (2a) (Compound (1), wherein M is Zr and each R is CH 2 -(1,4-phenylene)-C(CH 3 ) 3 )
[0137] An oven-dried bottle was loaded with a PTFE-coated magnetic stir bar, compound (2a) (1.5 g, 2.69 mmol), and 100 mL of dry degassed toluene to prepare a solution of compound (2a) in toluene. The bottle and a separate bottle containing the solution of 4-tert-butylbenzylmagnesium chloride of Preparation 4 were placed in a glove box refrigerator for 15 minutes to cool to -30°C. The solution of 4-tert-butylbenzylmagnesium chloride was then added to the addition funnel, and the contents of the addition funnel were added dropwise to the solution of compound (2a). The mixture was stirred and allowed to reach room temperature (r.t.) within 1 hour. Then 0.5 mL of 1,4-dioxane was added, and the resulting mixture was filtered through celite. The filtrate was concentrated under reduced pressure, and the resulting res...
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