Highly active supported catalyst compositions
A composition and supported technology, applied in the field of supported metallocene catalysts and their preparation, can solve the problems such as the inability to achieve dehydroxylation of the heat-treated carrier, the expensive chemical treatment of the carrier material, and the pollution of the carrier.
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Embodiment 1
[0078] 48.5 grams of Sylopol by Grace Davison, a division of W.R. Grace Co.-Conn. _ Silica supplied by 952 ("952 silica gel") was dry blended with 1.5 grams of ammonium hexafluorosilicate supplied by Aldrich Chemical Company (Milwaukee, Wisconsin), the former's N 2 The pore volume is 1.63 ml / g and the surface area is 312 m 2 / gram. The ammonium hexafluorosilicate added corresponds to 1.05 mmoles of fluorine per gram of silica gel. The mixture was transferred to a pyrex borosilicate glass tube with an inner diameter of 5 cm and a length of 50 cm, with a middle frit stopper 3.8 cm from one end. Insert the tube into a tube furnace, N 2 Flow (220 ml / min) was passed through the frit to fluidize the silica gel bed. The furnace was heated according to the following scheme.
[0079] Temperature rises from 25°C to 150°C within 5 hours
[0080] 4 hours at 150°C
[0081] Temperature rises from 150°C to 500°C within 2 hours
[0082] 4 hours at 500°C
[0083] Stop heating and at N...
Embodiment 2-14
[0087] In a similar manner, 952 silica gel was treated as described in Example 1, except that different weights and fluorochemicals were used. The details are listed in Table 1. Column 3 indicates the weight percent fluorine-containing compound present in the entire silica / fluorine compound sample prior to heating. "Added" noted in column 4 indicates the weight percent fluorine present in the sample prior to heating. "Derived" noted in column 5 indicates the weight percent fluorine in the sample after heating. The weight percent in column 5 is higher than the value in column 4, reflecting in part the loss of water during heating.
[0088] Example
[0089] 1. Not determined
Embodiment 15
[0092] In a manner similar to Example 1, 48.15 grams of 952 silica gel was dry blended with 1.85 grams of ammonium fluoride obtained from Aldrich Chemical Company (Milwaukee, Wisconsin). The ammonium fluoride added corresponds to 1.05 mmol fluorine / g silica gel. Use the following heating protocol.
[0093] Increase temperature from 25°C to 150°C in 5 hours
[0094] 4 hours at 150°C
[0095] Increase temperature from 150°C to 600°C in 2 hours
[0096] 4 hours at 600°C
[0097] Stop heating and at N 2 under cooling
[0098] When cooled store the fluorinated silica in N 2 Down. Neutron activation analysis indicated 2.00 ± 0.09% by weight fluorine.
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Abstract
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