Ethylene slurry ring tube polymerization or copolymerization method
A technology of copolymerization and ethylene, which is applied in the field of slurry loop copolymerization of ethylene and α-olefin, which can solve the problems of unsatisfactory polymer density and achieve the effect of good particle shape, reduced usage, and firm and broken
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Embodiment 1
[0033] (1) Synthesis of catalyst
[0034] In the reactor fully replaced by high-purity nitrogen, 2.4g of magnesium dichloride, 40ml of toluene treated with molecular sieves, 3.9ml of epichlorohydrin, and 4.1ml of tributyl phosphate were added in sequence, and the temperature was raised to 80°C under stirring. After 2 hours, the solid had completely dissolved to form a homogeneous solution. Add 0.3ml of ethanol and 0.8ml of isooctyl alcohol, and react at 80°C for 1 hour. Add 30ml of dehydrated hexane and 2.3g of silica gel, cool the system to 0°C, slowly add 8ml of titanium tetrachloride dropwise, then slowly raise the temperature to 80°C, react for 2 hours, add 5ml of tetrahydrofuran, at 80°C The reaction was continued for 1 hour. Stop stirring, let it stand, the suspension will be separated quickly, remove the upper clear night, wash with hexane four times, add 1.8ml of 2.2mol / l diethylaluminum chloride, react at 50°C for 30min, add 1.5mol / l l 1.2ml of tri-n-hexylaluminum ...
Embodiment 2
[0038] (1) The synthesis of catalyst is the same as in Example 1.
[0039] (2) Ethylene copolymerization
[0040] Use N for the φ150×3000 loop reactor 2 After full replacement, add 6.0 L of hexene, 2.0 mmol / l of triethylaluminum, use isobutane as diluent, 0.6 g of the above solid catalyst, raise the temperature to 75°C, and feed ethylene / hydrogen mixed gas with a hydrogen concentration of 38 %. The reaction pressure is 2.5MPa, the reaction temperature is 85°C, and the residence time is 1 hour. The molar contents of hydrogen: ethylene: 1-hexene in the system are 13.5%: 21.6%: 64.9%, respectively. The aggregation results are shown in Table 1.
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