Activating composition of metallocene matches in olefin catalytic copolymerization process
A composition and complex technology, applied in the field of organometallic composition and α-olefin polymerization technology, can solve problems such as not easy to use together, unstable air and moisture, complicated preparation, etc.
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Embodiment 1
[0125] In about 30 minutes, add 2.6g (0.039mol) of cyclopentadiene into 100ml of anhydrous THF containing 1.61g (0.035mol) of sodium metal 50% paraffin dispersion, keep the temperature at 20-25°C, in an inert The mixture was stirred under atmosphere. When no more hydrogen escaped, 3.05 g (0.070 mol) NaH was added in the form of a 55% paraffin dispersion, while 65 g (0.35 mol) C 6 f 6 , and the mixture was heated at reflux for 70 hours. When the heating was completed, the solvent was distilled under vacuum at 30-40° C., and the residue was washed 3 times with 100 ml of petroleum ether and vigorously stirred. The residue was then dissolved in 50 ml of ether, 50 ml of water was added, and 250 ml of petroleum ether was added, the ether phase was separated, filtered through a 5 cm layer of silica gel, and then dried. 50 ml of petroleum ether was added to the semi-solid residue, and the solid product was isolated by filtration. The resulting solid was crystallized from hot hepta...
Embodiment 2
[0126] The crystallized mother liquor of 1,2,4-tris(pentafluorophenyl)cyclopentadiene compound finally obtained in the previous examples was obtained in the form of a white crystalline solid after concentration and separation (eluent petroleum ether) with a silica gel column 0.2 g of 1,2,3-tris(pentafluorophenyl)cyclopentadiene isomer. 1 HNMR: 3.84ppm (d, 2H); 6.98ppm (t, 1H); 19 FNMR: -140.38ppm (m, 4F); -140.8ppm (m, 2F); -151.8ppm (t, 1F); -152.9ppm (t, 1F); -153ppm (t, 1F); -160ppm (m , 6F). Example 3 : Preparation of 1,2,3,4,5,6,7,8-octafluoro-9-hydroxyl-9-(2,4-bis-trifluoromethylphenyl)fluorene (VIII)
Embodiment 3
[0127] Add 7ml (2.5M) of n-butyllithium dropwise to 100ml of anhydrous ether containing 5g (0.017mol) of 2,4-bis(trifluoromethyl)bromobenzene, and cool to -75°C. After 1 hour, 3 g (0.009 mol) of 1,2,3,4,5,6,7,8-octafluorofluorene, which was disclosed in accordance with "Journal of Chemical Society, part C", p2394 (1968), was added in one portion prepared by the method. The mixture was stirred for 1 hour, then hydrolyzed, the ether phase was separated and dried over sodium sulfate. A small amount of cold petroleum ether was added to the solid obtained after filtration and drying to obtain 2.55 g of pure target product (52.64% yield relative to octafluorofluorene). 1 HNMR: 8.8ppm (d, 1H); 8.0ppm (d, 1H); 7.9ppm (s, 1H); 3.0ppm (s, 1H). 19 FNMR: -58.2ppm (s, 3F); -63.2ppm (s, 3F); -133.3ppm (s, 2F); -143.2ppm (d, 2F); -150.2ppm (s, 2F); -152.0ppm (t, 2F). Example 4 : Preparation of 1,2,3,4,5,6,7,8-octafluoro-9-(2,4-bis(trifluoromethyl)phenyl))fluorene (IX)
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