A class of star branched rare earth rubber and its preparation method
A rare-earth rubber and rare-earth technology, applied in the field of functional polymer materials, can solve the problems of star-shaped rubber and low yield of star-shaped polymers, and achieve the effect of simple preparation method, mild reaction conditions, and expanded application fields
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Embodiment 1
[0040] Example 1 Preparation of trialkyl scandium complex Sc(CH 2 C 6 H 4 NMe 2 -ο) 3
[0041] Weigh 13.500g (100mmol) of N,N-dimethyl-o-aniline in a glove box and put it into a 100mL round-bottomed flask with a magnetic stirring bar, add 40mL of ether to dissolve and stir, take 40mL (100mmol) of n-butyllithium Hexane solution (2.5mol / L) was added dropwise to the reaction flask, and the reaction was continuously stirred at room temperature for 3 days. After the reaction was completed, the solvent was removed by vacuuming, and the solid was washed with n-hexane and then drained to obtain a pale yellow powder LiCH 2 C 6 H 4 NMe 2 -o.
[0042] In the glove box, weigh 1.5134g ScCl 3 (10 mmol) was placed in a Schlenk bottle with a magnetic stir bar, and 8 mL of tetrahydrofuran was added. Weigh 4.2341g of LiCH 2 C 6 H 4 NMe-o (30 mmol) was dissolved in 14 mL of tetrahydrofuran and added dropwise to ScCl 3 in THF solution for 30 min. Then, the solvent THF was removed u...
Embodiment 2
[0043] Example 2 Preparation of monolocene dialkyl scandium complex (C 5 Me 4 SiMe 3 )Sc(CH 2 C 6 H 4 NMe 2 -ο) 2
[0044] In the glove box, weigh 1.5370 g of Sc (CH 2 C 6 H 4 NMe-o) 3 (3.45 mmol) was put into a 100 mL Schlenk bottle containing a magnetic stirring bar, and 10 mL of tetrahydrofuran solvent was added to dissolve. Weigh 0.6711g C 5 Me 4 H(SiMe 3 ) (3.45 mmol), dissolved in 5 mL of tetrahydrofuran, and added to a Schlenk bottle at room temperature. The Schlenk bottle was sealed, taken out of the glove box, stirred at 70°C for 12 hours, and then the solvent was removed in vacuo. The residue was washed with ether and dissolved in toluene. After concentrating the toluene solution, it was placed in a -35°C refrigerator overnight. g yellow crystals (C 5 Me4SiMe 3 )Sc(CH 2 C 6 H 4 NMe-o) 2 .
Embodiment 3
[0045] Example 3 Preparation of monolocene dialkyl scandium complex (C 5 H 5 )Sc(CH 2 C 6 H 4 NMe 2 -ο) 2
[0046] In the glove box, weigh 1.790 g (4 mmol) of Sc(CH 2 C 6 H 4 NMe 2 -o) 3 Put it into a Schlenk bottle with a magnetic stir bar, and add 12 mL of tetrahydrofuran solvent to dissolve it. Weigh 0.317g (4.80mmol) of cyclopentadiene (C 5 H 5 ), dissolved in 6 mL of tetrahydrofuran, and added to a Schlenk bottle at room temperature. The Schlenk bottle was sealed and taken out of the glove box, heated to 40 °C and stirred for 1 h, then put into the glove box, and the solvent was removed in vacuo. The residual solid was washed with ether and dissolved in toluene. The toluene solution was concentrated and placed in a -35 °C refrigerator. Overnight, recrystallization gave 1.271 g of yellow crystals (C 5 H 5 )Sc(CH 2 C 6 H 4 NMe 2 -ο) 2 .
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