Method for supplying solid catalyst to a solution polymerization reactor
A technology for polymerization reactors and catalysts, applied in the field of supplying solid catalysts to solution polymerization reactors, can solve problems such as increasing production costs
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Embodiment 1-5
[0092] Embodiment 1-5-aliphatic hydrocarbon solvent
[0093] A set of ethylene and propylene copolymers was prepared in a batch reactor using catalyst suspensions to demonstrate the concept. The catalyst dimethyl·bis(p-triethylsilylphenyl)methylene(cyclopentadienyl)(3,8-di-tert-butylfluorenyl)hafnium (alkylated homogeneous single site catalyst) and dimethylanilinium tetrakis(heptafluoro-2-naphthyl)borate activator were mixed with 2 ml of isohexane to form a catalyst suspension. The molar ratio of activator to catalyst is 1:1. Reactions in a 2-liter autoclave equipped with agitator, external water / steam jacket for temperature control, regulated supplies of dry nitrogen, ethylene, propylene, and septum inlets for introduction of other solvent, catalyst, and scavenger solutions Polymerization in the container. The catalyst concentration in the solvent (as a suspension) before injection into the reactor was 1.2 mmol / liter in each of Examples 1, 2, 4 and 5, and 0.53 mmol / liter i...
Embodiment 6-11
[0096] Examples 6-11 - dry feed
[0097] Examples 6-11 were prepared in a 2-liter autoclave reactor following the same procedure used for Examples 1-5, except that the catalyst and activator were delivered to the reactor as dry powders. Dimethyl rac-dimethyl silylbis(indenyl)hafnium (homogeneous single-site catalyst for alkylation) and tetrakis(heptafluoro-2-naphthyl)boronic acid dimethylbenzene A dry powder of ammonium (activator) was added to the catalyst delivery tube and then flushed into the reactor with propylene. The molar ratio of activator to catalyst is 1:1. 5 ml of tri-n-octylaluminum (TNOA) solution (25 wt% in hexane, Sigma Aldrich), followed by 600 ml of isohexane (solvent) were added to the reactor. The mixture is then stirred and heated to the desired temperature. Then, the catalyst / activator powder was flushed into the reactor with 400ml of propylene. Ethylene was fed as needed to maintain a constant reactor pressure during the polymerization. Ethylene con...
Embodiment 12
[0100] Example 12 - Mineral Oil Suspension
[0101] Example 12 was prepared in a 2-liter autoclave reactor following the same procedure used for Examples 6-11 except that the catalyst and activator were suspended in mineral oil. Mix 2.4 mg of dimethyl rac-dimethyl silylbis(indenyl) hafnium and 5.8 mg of dimethylanilinium tetrakis(heptafluoronaphthyl)borate in 20 ml of white mineral oil (available from Obtained by Sonneborn, Parsippany, New Jersey). To ensure uniform mixing, the mixture was kept in an oven at 120°C for 20 minutes, then hand shaken and cooled down to room temperature for polymerization. The catalyst concentration in mineral oil was 0.24 mmol / liter before injection into the reactor. Polymerization was carried out at 70° C. and 2 ml of tri-n-octylaluminum (TNOA) solution (25 wt % in hexane, Sigma Aldrich) and other conditions were kept the same as those listed in Table 2. The polymerization reaction lasted 30 minutes and the yield was 106.7 grams. The examples...
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