Spherical mesoporous material for supported metallocene catalyst and manufacturing method thereof
A technology of metallocene catalysts and mesoporous materials, applied in the field of metallocene-loaded spherical mesoporous materials, can solve the problems of low ethylene polymerization activity, affecting loading effect, and pore wall collapse
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Embodiment 1
[0030] Preparation of Spherical Mesoporous Materials Supporting Cocatalyst Methylaluminoxane (MAO) and Metallocene Catalyst Precursor Bis(1-Methyl-3-butyl-cyclopentadienyl)Zirconium Dichloride
[0031] In step 1, 2.0 grams of F108 (Fuka's trade name is Synperonic □ Substance F108) with 5.24 g K 2 SO 4 Add to 60 grams of 2N (2N) hydrochloric acid solution, stir at 38°C until F108 is completely dissolved;
[0032] In the second step, add 4.2 grams of ethyl orthosilicate to the above solution, stir at 38°C for 15 minutes, and stand at 38°C for 24 hours;
[0033] In the third step, the obtained solution was transferred to a polytetrafluoroethylene-lined reactor and crystallized at 100°C for 24 hours;
[0034] Step 4, obtain the original powder mesoporous material after adding 100 grams of deionized water to dilute, filter, wash and dry;
[0035] Step 5, wash the original powder mesoporous material with ethanol under reflux conditions for 24 hours, remove the template agent, an...
Embodiment 2
[0040] The application method of the spherical mesoporous material supporting cocatalyst methylaluminoxane (MAO) and main catalyst bis(1-methyl-3-butyl-cyclopentadienyl) zirconium dichloride in polyolefin.
[0041] Homopolymerization of ethylene
[0042] In a 2-liter stainless steel autoclave, replace three times with nitrogen and ethylene respectively, then add 200 milliliters of hexane solvent, raise the temperature of the kettle to 80 ° C, then add the remaining 800 milliliters of hexane solvent, with the addition of hexane, Add 2 ml of 1 mol / L triethylaluminum (TEA) hexane solution, then add 139 mg of FDU-MB, raise and maintain the pressure to 1.0 MPa, and react at 80°C for 1 hour. After the polymerization reaction finishes, collect polyethylene particle powder, weigh 139 grams, the efficient of catalyst is 876g PE / gcat h (26000000g PE / (mol Zr h)), bulk density (BD) is 0.255g / ml, Melt index: MI 2.16 = 0.016 g / 10 min.
Embodiment 3
[0044] Ethylene copolymerization
[0045] In a 2-liter stainless steel autoclave, replace three times with nitrogen and ethylene respectively, then add 200 milliliters of hexane solvent, raise the temperature of the kettle to 80 ° C, then add the remaining 800 milliliters of hexane solvent, with the addition of hexane, Add 2 ml of 1 mol / L triethylaluminum (TEA) hexane solution and 10 ml of hexene, then add 121 mg of FDU-MB, raise and maintain the pressure to 1.0 MPa, and react at 80°C for 1 hour. After the polymerization reaction was finished, the polyethylene particle powder was collected and weighed to obtain 139 grams. The efficiency of the catalyst was 952gPE / gcat h (28000000gPE / (mol Zr h)), and the bulk density (BD) was 0.176g / ml. Index: MI 2.16 = 0.176 g / 10 min.
[0046] figure 1 It is the XRD structure comparison chart of spherical mesoporous materials FDU and FDU-MB. Figure (1)a is the XRD spectrum of the spherical mesoporous material FDU, and Figure (1)b is the XR...
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