A kind of supported metallocene catalyst system and preparation method thereof
A technology of metallocene catalysts and metallocene compounds, which is applied in the field of metallocene catalyst systems supported by organic polymer carriers and its preparation, can solve the problems of complex preparation methods and unfavorable release of active centers of metallocene catalysts, and achieve the goal of preparation methods Simple, good shape of catalyst and polymer, high catalyst activity
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Embodiment 1
[0028] Comonomer treatment: use 10% NaOH solution to remove the polymerization inhibitor before use of styrene and divinylbenzene, and then use it after washing with deionized water for 3 times; use neutral alumina chromatography for hydroxyethyl methacrylate The column was used after removing the polymerization inhibitor. The following examples do not specifically illustrate that the comonomers are used after treatment.
[0029] Preparation of organic porous support: In a 250ml glass reactor, add 150ml ethanol and 15ml deionized water, then add 6ml (about 5.6g) styrene, 8ml55% (about 7.5g) divinylbenzene and 5ml methacrylic acid Hydroxyethyl ester (about 5.0g), styrene and divinylbenzene are used to remove the polymerization inhibitor with 10% NaOH solution before use, and then washed with deionized water for 3 times before use, and hydroxyethyl methacrylate is used in neutral The alumina chromatographic column was used after removing the polymerization inhibitor. Stir at r...
Embodiment 2
[0032] Preparation of organic porous support: In a 250ml glass reactor, add 108ml ethanol and 12ml deionized water, then add 3ml (about 2.7g) styrene, 4ml55% (about 3.7g) divinylbenzene and 2ml methacrylic acid Hydroxyethyl ester (about 2.0g), styrene and divinylbenzene use 10% NaOH solution to remove the polymerization inhibitor before use, and then use it after washing 3 times with deionized water. Use neutral hydroxyethyl methacrylate The alumina chromatographic column was used after removing the polymerization inhibitor. Stir at room temperature for 5 minutes, then add 2% polyvinyl alcohol (polymerization degree: 1750) of monomer mass, stir for 1 hour at 45°C, dissolve the polyvinyl alcohol stabilizer, then add 4ml DNBP, and 1.5% monomer mass of AIBN, heated up to 70°C, reacted for 3 hours, then raised the temperature to 80°C, reacted for 5 hours, stirred at 600 rpm, washed 3 times with ethanol, dried to obtain porous organic carrier a-2.
[0033] Loading of the metalloce...
Embodiment 3
[0035] Preparation of organic porous carrier: The preparation of organic porous carrier in Example 3 is different from Example 2 except that the amount of porogen used is different, the preparation steps are the same as the amount of other reagents, and 7mlDNBP is added in Example 3 instead of adding 4mlDNBP to prepare The obtained organic vehicle is designated as a-3.
[0036] Loading of the metallocene catalyst: 4.5 g of the organic porous carrier a-3 prepared by the method of the present invention was vacuum filtered in a vacuum dryer at 120° C. for 24 hours. Add the treated carrier into a 250ml nitrogen-substituted reactor, add 25ml of 10% (mass percent) MAO (produced by CNPC Lanzhou Chemical Research Center) toluene solution, and stir at 20°C for 1 hour. Then add 0.18 g of Cp 2 ZrCl 2 (Dicyclopentadienyl zirconium dichloride) metallocene compound, 10ml of toluene was stirred for 0.5 hours, then reacted at -20°C for 3 hours, the solvent was removed after the reaction, an...
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