Process of preparation of catalytic support and supported metallocene catalysts for production of homopolymers and copolymers of ethylene with alfa - olefins, of high and ultra high molecular weight and with broad molecular weight distribution in slurry, bulk and gas phase processes and products thereof
a technology of supported metallocene and catalyst, which is applied in the field of catalytic support and supported metallocene catalyst, can solve the problems of poor morphology of the polymer material obtained, the use of toluene, which is commonly used in the formulation of aluminoxanes solution, and the general anti-economic effect of poliolefin production in industrial scale based on these catalytic systems
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example 1
a) Preparation of the Catalytic Support
[0136]In a 5 L reactor equipped with mechanical stirring and previously purged with nitrogen, was added 44.5 g (0.462 mol) of MgCl2 and 2.5 L of dried THF. This mixture was heated until 60° C. and stirred at 100 rpm for 5 h for complete solubilization of the MgCl2. The obtained solution was, after this period, cooled down to 35° C. In this solution, 300 g of silica XPO-2402 were added, previously dehydrated at 600° C. and treated with 22.3 ml (0.163 mol) of diluted TEAL in n-hexane for 50 minutes at temperature of 25° C. Once finished the addition of silica, the mixture was heated up to 60° C. and stirred at 100 rpm for 1 h. After this period, we stop the stirring and start the THF evaporation through vacuum until the THF content to be incorporated in the support to reach a range between 8 and 12% wt.
[0137]The catalytic support obtained was characterized, presenting the following characteristics:[0138]THF content: 11.2% wt[0139]Mg content: 2.3%...
example 2
b) Preparation of Supported Metallocene Catalyst
[0152]In a 200-mL reactor equipped with mechanical stirring and previously purged with nitrogen, 6.1 g of the catalytic support prepared in the step a) of the EXAMPLE 1 and 50 mL of n-hexane were added. In this suspension, stirred at 200 rpm and under temperature of 25° C., it was slowly added 0.4 mL (4.1 mmol) of diluted TMAL in n-hexane (Al / THF=0.45). The suspension was stirred for 2 h and, after this period, the solvent was removed by siphonation. The catalytic support obtained, after this treatment, was characterized presenting the following characteristics:[0153]THF content: 3.3% wt
[0154]In a schlenk, equipped with magnetic stirrer and dipped in a heat oil bath, 0.61 g (2.8 mmol) of the CpTiCl3 and 70 mL of n-hexane were transferred. In this suspension heated up to 50° C. and under stirring, 1.4 mL (5.5 mmol) of diluted TIBAL in n-hexane (Al / Ti=2) was slowly added. The dark solution obtained was stirred for 2.5 h at 50° C.
[0155]In...
example 3
b) Preparation of Supported Metallocene Catalyst
[0163]In a 200-mL reactor equipped with mechanical stirring and previously purged with nitrogen, 6.1 g of the catalytic support prepared in the step a) of the EXAMPLE 1 and 50 mL of n-hexane were added. In this suspension, stirred at 200 rpm and the temperature of 25° C., it was slowly added 1.44 mL (4.2 mmol) of diluted TNHAL in n-hexane (Al / THF=0.45). The suspension was stirred for 2 h and after this period, the solvent was removed by siphonation. The catalytic support obtained, after this treatment, was characterized presenting the following characteristics:[0164]THF content: 3.4% wt
[0165]In a schlenk, equipped with magnetic stirrer and dipped in a heat oil bath, 0.61 g (2.8 mmol) of the CpTiCl3 and 70 mL of n-hexane were transferred. In this suspension heated up to 50° C. and under stirring, 1.4 mL (5.5 mmol) of diluted TIBAL in n-hexane (Al / Ti=2) was slowly added. The dark solution obtained was stirred for 2.5 h at 50° C.
[0166]In ...
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