Method for preparing catalyst for slurry-process ethylene polymerization process
A technology for ethylene polymerization and catalysts, which is applied in the field of preparation of supported titanium-based polyethylene catalysts. It can solve the problems of narrow polymer molecular weight adjustment range, restrictions on the development of high value-added special materials, and low catalyst efficiency. It achieves small wax content and particle size. Good morphology and high catalyst activity
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[0053] Example 1:
[0054] Add the raw material Mg(OC 2 H 5 ) 2 10g, 200ml n-heptane, stir and warm up. At 55°C, add 6 ml of diisobutyl phthalate and 3.3 ml of tetramethoxysilane, and keep the temperature constant for 30 minutes. When the temperature reaches 75℃, add TiCl 4 9.6ml. After the addition, the reaction was continued for 1 hour. Stop heating and cool down naturally to 50°C. Settling for 15 minutes, withdraw the upper clear liquid. Add 100ml of hexane, stir and raise the temperature to 60°C, stop stirring after 30 minutes, stop heating, settle for 1 hour, and extract the upper clear liquid. Repeat the above washing step 5 times. The catalyst suspension is dried to obtain a solid catalyst.
[0055] After fully replacing the 2L stainless steel reactor with nitrogen, add 1L of hexane, 3ml of triethylaluminum, 5mg of the catalyst obtained above, and 0.2MPa hydrogen. The temperature is raised to 50°C, ethylene is introduced, and the reaction temperature is maintained at 8...
Example Embodiment
[0056] Example 2:
[0057] Add the raw material Mg(OC 2 H 5 ) 2 10g, 200ml n-heptane, stir and warm up. At 60°C, add 8.5ml of di-n-butyl phthalate and 1.6ml of methoxytrimethylsilane and keep the temperature constant for half an hour. When the temperature reaches 95℃, add TiCl 4 24.1ml. After the addition, the reaction was continued for 1 hour. Stop heating and cool down naturally to 50°C. Settling for 15 minutes, withdraw the upper clear liquid. Add 100ml of hexane, stir and raise the temperature to 65°C, stop stirring after 30 minutes, stop heating, settle for 1 hour, and extract the upper clear liquid. Repeat the above steps 6 times. The catalyst suspension is dried to obtain a solid catalyst.
[0058] After fully replacing the 2L stainless steel reactor with nitrogen, add 1L of hexane, 3ml of triethylaluminum, 5mg of the catalyst obtained above, and 0.2MPa hydrogen. The temperature is raised to 50°C, ethylene is introduced, and the reaction temperature is maintained at 80...
Example Embodiment
[0059] Example 3:
[0060] Add the raw material Mg(OC 2 H 5 ) 2 10g, 200ml n-heptane, stir and warm up. At 55°C, add 8.5ml of di-n-butyl phthalate and 1.6ml of methoxytrimethylsilane and keep the temperature constant for half an hour. When the temperature reached 83°C, 178.8 ml of ethyl titanate was dropped. After the addition, the reaction was continued for 1 hour. Stop heating and cool down naturally to 50°C. Settling for 15 minutes, withdraw the upper clear liquid. Add 100ml of hexane, stir and raise the temperature to 60°C, stop stirring after 30 minutes, stop heating, settle for 1 hour, and extract the upper clear liquid. Repeat the above steps 6 times. The catalyst suspension is dried to obtain a solid catalyst.
[0061] After fully replacing the 2L stainless steel reactor with nitrogen, add 1L of hexane, 3ml of triethylaluminum, 5mg of the catalyst obtained above, and 0.2MPa hydrogen. The temperature is raised to 50°C, ethylene is introduced, and the reaction temperatu...
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