Supported olefin polymerization catalyst
A catalyst and carrier technology, applied in the field of catalysts and their preparation, can solve problems such as loss of activity and failure
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Embodiment 1
[0040] Example 1: Catalysts supported on silica treated with trimethyl borate extend the shelf life
[0041] Catalyst preparation
[0042] Catalyst 1A: Silica (Davison 948, 10-20 grams) was placed in a quartz tube with a sinter used as a gas distributor plate. Nitrogen is used to fluidize the silica in the tube. The quartz tube was placed in a heating furnace, and the silica was heated at 150°C for 4 hours. The tube was then heated to 250°C in 1 hour and then cooled to 150°C. A syringe was used to add trimethyl borate (1.6 mmol / g silica after correction for 5% volatilization in silica) into the fluidized bed. The silica in the fluidized bed was fluidized for 2 hours, and then cooled and discharged into a storage container under a nitrogen atmosphere.
[0043] The cyclopentadienyl (1-methyl borate benzene) · zirconium dichloride (0.046 g, 0.12 mmol / g SiO 2 ) And trityl tetrakis (pentafluorophenyl) borate (0.13 g, 0.14 mmol / g SiO 2 ) Was dissolved in toluene (5 ml) under a nitrogen ...
Embodiment 2
[0048] Example 2: Catalyst supported on HMDS treated silica
[0049] Catalyst preparation
[0050] Catalyst 2A:
[0051] Pure hexamethyldisilylamine (HMDS) in an amount equivalent to 12.5 (weight)% of the silica was slowly added to the stirring silica. After treatment, silica generally contains 4.0-4.2% carbon. The HMDS treated silica is dried in a fluidized bed dryer at 600°C under a stream of dry nitrogen for 6 hours before storage.
[0052] In a dry box with an inert atmosphere (nitrogen), the HMDS-treated silica (2.0 g) was transferred to a three-necked flask equipped with a gas inlet tube, overhead stirrer and rubber septum. In another vial, mix bis(1-methyl borate benzene) zirconium dichloride (0.034 g, 0.10 mmol) and trityl tetrakis(pentafluorophenyl) borate (0.111 g, 0.12 mmol) Mol) was dissolved in dry toluene (2 mL). The vial is sealed with a rubber septum. The catalyst / co-catalyst solution was then added dropwise to the treated silica via a syringe with rapid stirring, ...
Embodiment 3
[0058] Example 3: The catalyst supported on silica treated with HMDS extends the shelf life
[0059] Catalyst preparation
[0060] Catalyst 3: Except that cyclopentadienyl (1-borate benzene) · zirconium dichloride (0.032 g, 0.010 mmol) is used instead of bis (1-borate benzene) · zirconium dichloride, the rest The step of preparing catalyst 2A is carried out.
[0061] Aggregation test
[0062] The polymerization reaction was carried out in a 1-liter stainless steel high-pressure reactor. Hydrogen (0.7 mmol) was introduced into the reactor from a 50 ml vessel, and the amount of hydrogen added was determined by measuring the pressure difference of the vessel. Triethylaluminum (0.38 mmol; 2.3 mL of 0.1 molar heptane solution) was added to a reactor filled with isobutane (approximately 500 mL), the temperature had reached 75°C and was equilibrated. Ethylene was added to the reactor (to a pressure of 400 psig), followed by a mixture of supported catalyst and 1.5 milliliters of triethyl ...
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