A kind of vanadium complex, its preparation method and its application in isoprene polymerization
A technology of isoprene and vanadium complexes, applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic compounds of group 5/15 without C-metal bonds, etc., can solve selectivity low molecular weight polyisoprene and other problems, to achieve the effect of simple preparation method and increased molecular weight
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preparation example 1
[0023] V[ONS] complex shown in the preparation formula II:
[0024] Under nitrogen atmosphere, add sodium hydride (31.6mg, 1.3mmol) and 5mL tetrahydrofuran into a dry reaction tube, cool to -30°C, and add ligands in equimolar ratios. The structural formula of the ligands is shown in formula (1). React at room temperature for 4 hours to obtain a salt solution of the ligand. Add VCl to another dry reaction tube 3 (THF) 3 (447mg, 1.2mmol) and 5mL tetrahydrofuran to obtain a vanadium solution, the ligand salt solution was added to the vanadium solution at room temperature, and stirred overnight at room temperature. Concentrate the reaction solution, filter out sodium chloride and unreacted sodium hydride, continue to concentrate to 5 mL, add 20 mL of n-hexane to precipitate a solid, filter and dry in vacuum to constant weight, and obtain a dark brown solid which is the target product of this example. rate 35%.
[0025] Mass Spectrometry: C 18 h 20 ClNO 2 SV[M-Cl] + Theoret...
preparation example 2
[0028] According to the method of Preparation Example 1, the V[ONS] complex shown in formula III was prepared: the structural formula of the ligand is shown in formula (2).
[0029] After filtration and vacuum drying to constant weight, a dark brown solid was obtained, which was the target product of this example, with a yield of 39%.
[0030] Mass Spectrometry: C 19 h 22 ClNO 2 SV[M-Cl] + Theoretical value: 414.0499; measured value: 414.0455.
[0031] Elemental Analysis: Theoretical Value: C 19 h 22 Cl 2 NO 2 SV: C, 50.68%; H, 4.92%; N, 3.11%; Found: C, 50.73%; H, 4.77%; N, 3.15%.
preparation example 3
[0033] The V[ONS] complex shown in Formula IV was prepared according to the method of Preparation Example 1: the ligand structural formula is shown in Formula (3).
[0034] After filtration and vacuum drying to constant weight, a black solid was obtained, which was the target product of this example, with a yield of 48%.
[0035] Mass Spectrometry: C 23 h 22 Cl 2 NO 2 SV[M-Cl] +Theoretical value: 462.0499; measured value: 462.0473.
[0036] Elemental Analysis: Theoretical Value: C 23 h 22 Cl 2 NO 2 SV: C, 55.43%; H, 4.45%; N, 2.81%; Found: C, 53.97%; H, 4.51%; N, 2.75%.
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