Metallocene titanium compound and its preparing process
A titanium compound and metallocene technology, applied in the field of metallocene titanium compound and its preparation, can solve the problem of low catalytic effect and achieve the effect of easy separation and purification, simple process and low cost
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Example Embodiment
[0031] Calculation, C: 37.10% H: 4.68% [Example 2]
[0032] (Preparation of compound B): Under the protection of argon, the alkoxy alcohol (R 1 =CH(CH 3 )CH 2 , R 2 = Methyl) and the ether solution of lower fatty amine (triethylamine), slowly added to CpTiCl with a molar ratio of 1:1.5 to alcohol 3 In the ether solution, at 25° C., the reaction was stirred for 8 hours, filtered, and the clear liquid was drained. The obtained oil was recrystallized with toluene and n-hexane to obtain a clear yellow oil. The analysis and test results are as follows:
[0033] Molecular formula: C 9 H 14 Cl 2 O 2 Ti; mass spectrum shows molecular ion peak 272 (4, M + ).
[0034] Infrared spectrum data (cm -1 ): 3107m, 2932m, 2890m, 1441m, 1373w, 1147m, 1110s, 1093s, 1014s, 822s, 790s.
[0035] NMR data ( 1H NMR, ppm): 6.94 to 6.72 (m, 5H), 4.99 (m, 1H), 3.49 to 3.45 (m, 2H), 3.45 (s, 3H), 1.35 (d, 3H, J=6.6 Hz).
[0036] Elemental analysis data: actual measurement, C: 38.41% H: 4.64%
Example Embodiment
[0037] Calculation, C: 39.59% H: 5.18% [Example 3]
[0038] (Preparation of compound C): Under the protection of argon, the aryloxy alcohol ( R 2 = Methyl) and the benzene solution of the lower aliphatic amine (triethylamine), slowly added to CpTiCl with a molar ratio of 1:1.2 to the alcohol 3 In the benzene solution, stirred and reacted at 10°C for 24 hours, filtered, and the clear liquid was drained. The obtained oil was recrystallized with toluene and n-hexane to obtain a clear black-red oil. The analysis and test results are as follows:
[0039] Molecular formula: C 12 H 12 Cl 2 O 2 Ti; mass spectrum shows molecular ion peak 306 (7, M + ).
[0040] Infrared spectrum data (cm -1 ): 3108m, 1612w, 1596m, 1501s, 1484m, 1361w, 1263s, 1225s, 1100s, 1022m, 824s, 794s, 750s.
[0041] NMR data ( 1 H NMR, ppm): 6.93-6.85 (m, 4H), 6.62-6.45 (m, 5H), 3.88 (s, 3H).
[0042] Elemental analysis data: actual measurement, C: 47.08% H: 4.07%
Example Embodiment
[0043] Calculation, C: 46.94% H: 3.95% [Example 4]
[0044] (Preparation of compound D): Under the protection of argon, the alkoxy alcohol (tetrahydrofurfuryl alcohol) and the lower aliphatic amine (triethylamine) in an ether solution with a molar ratio of 1:1.2 are slowly added To CpTiCl equimolar with alcohol 3 In the ether solution, at 25° C., the reaction was stirred for 8 hours, filtered, and the clear liquid was drained. The obtained oil was recrystallized with toluene and n-hexane to obtain a clear yellow oil. The analysis and test results are as follows:
[0045] Molecular formula: C 10 H 14 Cl 2 O 2 Ti; mass spectrum shows molecular ion peak 284 (0.2, M + ).
[0046] Infrared spectrum data (cm -1 ): 3107w, 2950m, 2870m, 1440m, 1367w, 1118s, 1077s, 1025m, 826s, 793m.
[0047] NMR data ( 1 H NMR, ppm): 6.82 ~ 6.59 (m, 5H), 4.73 ~ 4.52 (m, 2H), 4.03 ~ 3.98 (m, 1H,), 3.88 ~ 3.84 (t, 1H, J = 6.8H), 3.83 ~ 3.78 (t, 1H, J=6.8H), 2.01 to 1.72 (m, 4H).
[0048] Elemental
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