Catalyst compositions comprising small silica support materials and methods of use in polymerization reactions
a technology of catalyst composition and support material, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, chemical/physical process, etc., can solve the problems of reduced polymer product bulk density, limited production rate of certain gas phase reactors,
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example 1
[0100] For laboratory-prepared precursors, silicas first were dehydrated under nitrogen flow in a laboratory Carbolite Vertical Furnace, Model No. VST 12 / 32 / 400 / 2408 CP-FM supplied by Carbolite, Inc., provided with a quartz glass tube of 3.0 cm outer diameter and 70 cm in total length, and two thermocouples. One thermocouple was placed in a thermowell within the quartz glass tube, while the other was affixed to the skin of the quartz glass tube by placing it between the two folding halves of the furnace, then clamping the folding halves shut. The thermocouples were hooked up to a Nomad OM-SP1700 data logger supplied by Omega Engineering. A collection flask for excess blowout silica was attached at the top of the tube, which in turn was attached to a bubbler via a glass elbow.
[0101] About 25-30 grams of silica was poured via a funnel into the quartz glass tube to fill the tube about ⅔ full within the heating zone. A preset program was started to begin the dehydration, using a Euroth...
example 2
[0125] Scaled-up catalyst compositions were prepared in a pilot plant laboratory using a jacketed vessel (that may be referred to as a mix tank) according to the procedure set forth below. The capacity of the mix tank is on the order of about 2 pounds of catalyst material.
[0126] Silica dehydrated at 600° C. has a hydroxyl nominal concentration of 0.7 mmole OH / gram. The TEAL-on-Silica (“TOS”) prepared for these scaled-up batches has a target aluminum loading of 0.5 mmole / gram. As TEAL reacts with hydroxyl according to a 1-to-1 molar ratio, then about 0.2 mmole OH / gram will remain unreacted on the TOS.
[0127] First, about 850 grams of silica were charged to the mix tank, for ES 757 silica and Davison 955-600 silica. About 3.5 liters of isopentane then were added, after which about 0.59 grams of 10% TEAL in isopentane (0.93 ml) were added for every gram of silica charged. The TEAL reacts exothermically with the silica to form ethane. Accordingly, the TEAL charge was metered so as to k...
example 3
[0140] Sample catalyst compositions prepared in the manner described above were reacted in a polymerization process in a pilot plant reactor.
[0141] Polymerization was conducted in a 24 inch diameter gas-phase fluidized bed reactor operating at approximately 300 psig total pressure. The reactor bed weight was approximately 500-600 pounds. Fluidizing gas was passed through the bed at a velocity of approximately 2.0 feet per second. The fluidizing gas exiting the bed entered a resin-disengaging zone located at the upper portion of the reactor. The fluidizing gas then entered a recycle loop and passed through a water-cooled heat exchanger and cycle gas compressor. The shell side water temperature was adjusted to maintain the reaction temperature to the specified value. Ethylene, hydrogen, 1-hexene and nitrogen were fed to the cycle gas loop just upstream of the compressor at quantities sufficient to maintain the desired gas concentrations. Triethylaluminum cocatalyst was fed to the rea...
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