Bis-salicylaldehyde imine vanadium olefin polymerization catalyst as well as preparation method and use thereof
A technology of salicylaldimine vanadium olefin and polymerization catalyst, which is applied in the field of double salicylaldimine vanadium olefin polymerization catalyst and its preparation, and can solve the problems of poor high temperature resistance, low catalytic activity, easy deactivation, etc.
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Embodiment 1
[0024]Add 9.77 g of salicylaldehyde equivalent to 80 mmol, 7.45 g of aniline equivalent to 80 mmol, 50 ml of methanol, and 2 ml of formic acid into a dry reactor, and react at 25° C. for 24 h. The solvent methanol was distilled off with a rotary evaporator, and 1000 ml of a solution of ethyl acetate and petroleum ether with a volume ratio of 1:100 was used as an eluent, and the residue was subjected to column chromatography to obtain 15.0 g of yellow solid Schiff's base. 95%. 1 H NMR (300 MHz, DMSO): δ6.93-7.68 (m, 9H, Ar-H), 8.97 (s, 1H, CH=N), 13.07 (s, 1H, OH). According to mass spectrometry, the molecular ion peak m / e is 197. Elemental analysis measured value: C, 79.30%; H, 5.64%; N, 7.05%; Theoretical value (C 13 h 11 NO): C, 79.16%; H, 5.62%; N, 7.10%.
[0025] Under a nitrogen atmosphere, add 0.78 g of the Schiffer base obtained above, which is equivalent to 4.0 mmol, and 20 ml of anhydrous tetrahydrofuran, to a dry reactor reactor, stir at room temperature for 10 m...
Embodiment 2
[0030] 4.89g of salicylaldehyde is equivalent to 40mmol, and 6.44g of p-trifluoromethylaniline is equivalent to 40mmol to replace the aniline, 60ml of methanol, and 1ml of formic acid in Example 1, and react at 25°C for 12h. The experimental operation is the same as that of Example 1, and a yellow solid is obtained. 9.76 g of the like Schiff's base, the yield is 92%. 1 H NMR (300 MHz, DMSO): δ6.98-7.83 (m, 8H, Ar-H), 9.00 (s, 1H, CH=N), 12.62 (s, 1H, OH). According to mass spectrometry, the molecular ion peak m / e is 265. Elemental analysis measured value: C, 63.25%; H, 3.83%; N, 5.30%; Theoretical value (C 14 h 10 f 3 NO): C, 63.40%; H, 3.80%; N, 5.28%.
[0031] Under a nitrogen atmosphere, add 1.06 g of the above-obtained Schlenk base equivalent to 4.0 mmol and 20 ml of anhydrous tetrahydrofuran into a dry reactor reactor, stir at room temperature for 10 min to dissolve the solid, and add three to another dry Schlenk reactor. Vanadium Chloride Tetrahydrofuran Complex VCl...
Embodiment 3
[0036] 4.89 g of salicylaldehyde is equivalent to 40 mmol, and 4.28 g of p-methylaniline is equivalent to 40 mmol instead of aniline, 30 ml of methanol, and 1 ml of formic acid in Example 1, and reacted at 25 ° C for 12 hours. The experimental operation is the same as that of Example 1, and a yellow solid Buddha alkali 7.85g, yield 93%. 1 H NMR (300MHz, CDCl 3 ): δ2.44(s, 3H, CH 3 ), 6.94-7.65 (m, 8H, Ar-H), 8.96 (s, 1H, CH=N), 13.22 (s, 1H, OH). According to mass spectrometry, the molecular ion peak m / e is 211. Elemental analysis measured value: C, 79.63%; H, 6.25%; N, 6.71%; Theoretical value (C 14 h 13 NO): C, 79.59%; H, 6.20%; N, 6.63%.
[0037] The Schiffer's base g prepared in Example 3 is equivalent to 4 mmol to replace the Schiffer's base obtained in Example 1, and the experimental operation is the same as in Example 1. Under a nitrogen atmosphere, add the above-mentioned Schiffer's base obtained in a dry reactor reactor 0.85g is equivalent to 4.0mmol and 20ml of...
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