Polyolefin and preparation method thereof
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[0125]As the organic reagent and the solvent that are required to prepare the catalyst and to perform the polymerization, products manufactured by Aldrich, Co., Ltd. were purified according to the standard method and used, and highly pure products manufactured by Applied Gas Technology, Co., Ltd. were passed through the water and oxygen filtering device and then used as ethylene. In all steps of the catalyst synthesis, the supporting, and the olefin polymerization, air and water contacts were blocked, thus increasing the reproducibility of the experiment.
[0126]To confirm the structure of the catalyst, the spectrum was obtained by using the 300 MHz NMR (Bruker). The apparent density was measured by using the apparent density tester (Apparent Density Tester 1132 manufactured by APT Institute fr Prftechnik, Co., Ltd.) according to the method of DIN 53466 and ISO R 60.
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Preparation Example 1
Preparation of the First Metallocene Catalyst—Synthesis of [tBu—O—(CH2)6—C5H4]2ZrCl2
[0127]6-chlorohexanol was used to prepare t-Butyl-O—(CH2)6—Cl according to the method that was described in the document (Tetrahedron Lett. 2951 (1988)), and NaCp was reacted in respects to this to obtain t-BUtYl-O—(CH2)B—C5H5 (yield 60%, b.p. 80° C. / 0.1 mmHg). In addition, t-Butyl-O—(CH2)6—C5H5 was dissolved in THF at −78 normal butyl lithium (n-BuLi) was slowly added thereto, the temperature was increased to room temperature, and the reaction was performed for 8 hours. The solution was additionally reacted at room temperature for 6 hours while the synthesized lithium salt solution was slowly added to the suspension solution of ZrCl4(THF)2 (1.70 g, 4.50 mmoD / THF (30 ml) at −78° C. All the volatile substances were dried under vacuum, and the hexane solvent was added to the obtained oily liquid substance and then filtered. After the filtered solution was dried under vacuum, hexan...
Example
Preparation Example 2
Preparation of the First Metallocene Catalyst—Synthesis of [tBu—O—(CH2)6—C5H4]2HfCl2
[0130]6-chlorohexanol was used to prepare t-Butyl-O—(CH2)6—Cl according to the method that was described in the document (Tetrahedron Lett. 2951 (1988)), and NaCp was reacted in respects to this to obtain t-Butyl-O—(CH2)6—C5H5 (yield 60%, b.p. 80° C. / 0.1 mmHg). In addition, t-Butyl-O—(CH2)6—C5H5 was dissolved in THF at −78° C., normal butyl lithium (n-BuLi) was slowly added thereto, the temperature was increased to room temperature, and the reaction was performed for 8 hours. The solution was additionally reacted at room temperature for 6 hours while the synthesized lithium salt solution was slowly added to the suspension solution of HfCl4 (1.44 g, 4.50 mmoD / THF (30 mH) at −78° C. All the volatile substances were dried under vacuum, and the hexane solvent was added to the obtained oily liquid substance and then filtered. After the filtered solution was dried under vacuum, hexane...
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