Composite catalytic system for preparing wide/dual-peak distributed high density polyethylene
A high-density polyethylene and bimodal distribution technology is applied in the field of composite catalytic systems for preparing broad/bimodal high-density polyethylene, which can solve the problems of low branching degree, inability to achieve balanced compatibility of processability and strength, and the like. To achieve the effect of improving processing performance
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[0049] Example 1
[0050] Synthesis of compound (A):
[0051] Bis(3-tert-butylsalicylidenecyclohexyl)-(cyclopentadienyl) zirconium chloride.
[0052] (1) Preparation of the ligand compound 3-tert-butyl salicylidene cyclohexylamine:
[0053] Take 17.8 g (0.1 mol) of 3-tert-butyl salicylaldehyde and 0.2 mol of cyclohexylamine into 100 ml of ethanol medium, heat to reflux with stirring, react for 2 hours, and cool to room temperature, that is, a large amount of crystals are produced. After filtration, the solid was recrystallized with 30 ml of ethanol solvent to finally obtain the ligand 3-tert-butyl salicylidene aniline with a yield of 92%.
[0054] 1 H NMR(CDCl 3 , 500MHz) δ: 13.93 (br, 1H, D 2 O, OH), 8.64(s, 1H, CH=N), 7.46~6.96(m, 8H, arom), 1.47(s, 9H, C(CH 3 ) 3 )
[0055] (2) Preparation of lithium salt of 3-tert-butyl salicylidene cyclohexylamine:
[0056] Add 2.910g (11.5mmol) 3-tert-butyl salicylidene cyclohexylamine and 30ml tetrahydrofuran into a 100ml Schlenk bottle, co...
Example Embodiment
[0062] Example 2
[0063] Synthesis of metallocene compound B: (Me 4 Cp) 2 ZrCl 2 Preparation of adduct:
[0064] Under a nitrogen atmosphere, add 20g (0.164mol) of tetramethylcyclopentadiene that was newly steamed in a three-necked flask, add 200ml of tetrahydrofuran to dissolve it, then lower the temperature to below -70℃, and slowly add 65.6ml (0.164mol) of n-butyl. Base lithium solution (2.5M), react at this temperature for 1 hour, slowly warm up to room temperature, and react for 4 hours; transfer this solution to a constant pressure dropper, and slowly drop it until 19.1g is dissolved below -70°C (0.082mol)ZrCl 4 In 100ml tetrahydrofuran solution, after dripping, gradually warm to room temperature, and then react for about 18 hours; after vacuum distillation, evaporation to dryness, disperse with hexane, filter and wash with hexane twice to obtain 39g of purple metallocene plus Compound B powder, Zr% = 18 (ICP), the yield based on Zr was 94.1%.
Example Embodiment
[0065] Example 3
[0066] Synthesis of metallocene compound C: (n-BuMeCp) 2 ZrCl 2 Preparation of adduct:
[0067] Under a nitrogen atmosphere, add 20g (0.147mol) of methylbutylcyclopentadiene that was newly steamed in a three-necked flask, add 200ml of tetrahydrofuran to dissolve it, then lower the temperature to below -70℃, and slowly add 58.9ml (0.147mol) of n-butyl Lithium solution (2.5M), react at this temperature for 1 hour, slowly warm to room temperature, and react for 4 hours; transfer this solution to a constant pressure dropper, and slowly drop it until 16.43g ( 0.074mol)ZrCl 4 In 100ml of tetrahydrofuran solution, after dripping, gradually warm to room temperature, and then react for about 18 hours; after vacuum distillation, evaporation to dryness, disperse with hexane, filter, and wash with hexane twice to obtain 35g of yellow metallocene plus Compound C powder, Zr% = 17.5 (ICP), the yield was 91% based on Zr.
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