A kind of olefin polymerization catalyst and olefin polymerization method and polyolefin
An olefin polymerization and catalyst technology, applied in the field of polyolefins, can solve the problems of ineffective regulation of the comonomer ratio, high price, and increased cost of polymerization products, etc.
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preparation example 1
[0035] This preparation example is used to illustrate the salicylaldimine catalyst precursor represented by formula (II) provided by the present invention and its preparation method.
[0036] Dissolve 3-methyl-(E)-salicylaldehyde pentafluoroaniline (1mol) in ether and cool to -78°C, then add a hexane solution of n-butyllithium (1.05mol), and react at this temperature 2h, then raise the temperature to 30°C for another 15min, then transfer it to -78°C TiCl 4 (0.5mol) of tetrahydrofuran solution and react for half an hour, return to room temperature at 30°C and react for 16 hours, filter and remove the solvent, and then use a mixed solvent of petroleum ether and dichloromethane (the volume of petroleum ether and dichloromethane The ratio is 4:1, the same below) to obtain a reddish-brown product by recrystallization with a yield of 90%.
[0037] Anal.Calc.for C 28 h 14 Cl 2 f 10 N 2 o 2 Ti (%): C, 46.76; H, 1.96; N, 3.90. Found (%): C, 46.70; H, 1.94; N, 3.87. FD-MS: m / z 7...
preparation example 2
[0039] This preparation example is used to illustrate the salicylaldimine catalyst precursor represented by formula (III) provided by the present invention and its preparation method.
[0040] 3,5-Dimethyl-(E)-salicylaldehyde aniline (1mol) was dissolved in ether and cooled to -78°C, then a hexane solution of n-butyllithium (1.05mol) was added, at this temperature React for 2h, then raise the temperature to 30°C for another 15min, then transfer it to -78°C TiCl 4 (0.5mol) THF solution and reacted for half an hour, returned to room temperature at 30°C and reacted for 16 hours, filtered and removed the solvent, and then recrystallized with a mixed solvent of petroleum ether and dichloromethane to obtain a reddish-brown product. The yield 90%.
[0041] Anal.Calc.for C 42 h 52 Cl 2 N 2 o 2 Ti (%): C, 68.57; H, 7.12; N, 3.81. Found (%): C, 68.55; H, 7.09; N, 3.80. FD-MS: m / z 734.2 (calcd 734.3).
Embodiment 1
[0043] This example is used to illustrate the olefin polymerization catalyst and olefin polymerization method provided by the present invention.
[0044] Preparation of polyethylene: evacuate the heated and dried 500mL polymerization kettle with nitrogen for two times, and then introduce ethylene gas after vacuuming, then add 10mL (8.6mmol) of trimethylaluminum toluene solution in sequence, and pass through anhydrous and anhydrous Oxygen-treated toluene 336mL and water (4.3mmol), under stirring, feed ethylene with a pressure of 1atm. After the solution reaches saturation, add 4mL (21.3μmol) of toluene solution of the salicylaldimine catalyst precursor shown in formula (II) ), and reacted at 20°C for 5min under this pressure, then added an acidified solution of ethanol to terminate the reaction, and obtained 5.66g of polyethylene. According to calculation, the polymerization activity was 3.2×10 6 g·mol -1 (Ti)·h -1 .
[0045] The melting point of the polyethylene as measured...
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