Olefin polymerization catalyst composition and application method thereof
A technology of olefin polymerization and composition, which is applied in the field of olefin polymerization catalyst composition, can solve problems such as complex preparation methods, and achieve the effects of simple catalytic system, low environmental hazards, easy preparation and control
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[0027] Example 1
[0028] Synthesis of ligand A, ligand A is a ligand represented by formula I, where R 1 =R 2 =R 3 =R 4 =CH 3 .
[0029] The ligand preparation method is: in a dry reactor, such as adding NaH (1.2g, 30mmol), 30ml anhydrous tetrahydrofuran in a Schlenk tube, slowly adding 3,5-dimethylpyrazole (2.8g, 30mmol) in an ice water bath ), release gas, stir for 30 minutes, add thionyl chloride (1ml, 15mmol), the brown-gray transparent reaction solution turns off-white, remove the ice-water bath, stir for 30 minutes at room temperature, add quinolinal (2.4g, 15mmol), Pyridine (1.2g, 15mmol), refluxed in an oil bath at 80°C for 6 hours, quenched with saturated aqueous sodium bicarbonate solution, extracted with ethyl acetate three times, and purified by column chromatography to obtain a white solid, ligand A (3.5g, yield 71wt%) ).
[0030] 1 H-NMR(δ, ppm, CDCl 3 , TMS): 8.8~7.4 (m, 6H, Quinoline-H), 8.7 (s, 1H, CH), 5.8 (s, 2H, Pyrazole-H), 2.23 (s, 6H, CH) 3 ), 2.18(s, 6H, CH...
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[0031] Example 2
[0032] Synthesis of ligand B, ligand B is a ligand represented by formula I, where R 1 =R 2 =R 3 =R 4 =H.
[0033] The preparation method is the same as that in Example 1 of ligand synthesis, except that 3,5-dimethylpyrazole is replaced with pyrazole, and other conditions remain unchanged. The yield was 74wt%. 1 H-NMR(δ, ppm, CDCl 3 , TMS): 8.8~7.3 (m, 12H, Quinoline-H and Pyrazole-H), 8.7 (s, 1H, CH).
[0034] Polymerization Example
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[0035] Example 3
[0036] Use 300mL stainless steel polymerizer. The autoclave was heated to 100°C, evacuated and replaced with nitrogen several times, and then filled with ethylene until the ethylene pressure was 2MPa, and the temperature was lowered to room temperature. Then add dehydrated toluene at 70°C, and add 10 μmol of the ligand (ligand A), chromium chloride and methylaluminoxane (MAO) in Example 1 at the same time. The total volume of the mixture is 100 mL, in which the ligand, The molar ratio of chromium chloride and methylaluminoxane is 1:1:200, that is, the amount of chromium chloride added is 10μmol, the amount of methylaluminoxane added is 2mmol, the reaction pressure is controlled to 2.0MPa, and ethylene is introduced to carry out ethylene. Oligomerization reaction.
[0037] After the reaction is completed, the system is cooled to room temperature, the gas phase product is collected in a gas metering tank, and the liquid phase product is collected in a conical fla...
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