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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

Active Publication Date: 2006-10-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There have been reports on the compounding of traditional Ziegler / Natta catalysts and single-site catalysts, such as Mobil's WO 99 / 03899. This type of catalyst is much better than the Ziegler / Natta catalyst copolymerization performance due to metallocene catalysts, and Ziegler The molecular weight of the polymer obtained by / Natta catalyst is relatively large. In the obtained resin, the branching degree of the high molecular weight part is low, or even unbranched, while the branching degree of the low molecular weight part is high. This material cannot achieve processing performance and strength. Balanced compatibility

Method used

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  • Composite catalytic system for preparing wide/dual-peak distributed high density polyethylene
  • Composite catalytic system for preparing wide/dual-peak distributed high density polyethylene
  • Composite catalytic system for preparing wide/dual-peak distributed high density polyethylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Synthesis of compound (A):

[0051] Bis(3-tert-butylsalicylidenecyclohexyl)-(cyclopentadienyl)zirconium chloride.

[0052] (1) Preparation of ligand compound 3-tert-butyl salicylidene cyclohexylamine:

[0053] Take 17.8g (0.1mol) of 3-tert-butylsalicylaldehyde and 0.2mol of cyclohexylamine and add it to 100ml of ethanol medium, heat to reflux under stirring, react for 2 hours, cool to room temperature, and a large number of crystals are produced. Filtration and recrystallization of the solid with 30 ml of ethanol solvent finally gave 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, aroma), 1.47(s, 9H, C(CH 3 ) 3 )

[0055] (2) Preparation of the lithium salt of 3-tert-butyl salicylidene cyclohexylamine:

[0056] Add 2.910g (11.5mmol) 3-tert-butylsalicylidenecyclohexylamine and 30ml tetrahydrofuran into a 100ml Schlenk bottle, cool the solution to...

Embodiment 2

[0063] The synthesis of metallocene compound B: (Me 4 Cp) 2 ZrCl 2 Preparation of adducts:

[0064] Under a nitrogen atmosphere, add 20 g (0.164 mol) of newly distilled tetramethylcyclopentadiene to the three-necked flask, add 200 ml of tetrahydrofuran to dissolve, then lower the temperature to below -70°C, and slowly add 65.6 ml (0.164 mol) of n-butyl Lithium-based 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 add it dropwise to the dissolved 19.1g (0.082mol)ZrCl 4 100ml of tetrahydrofuran solution, after dripping, it was gradually raised to room temperature, and then reacted for about 18 hours; after vacuum distillation, evaporated to dryness, dispersed with hexane, filtered, and washed twice with hexane to obtain 39g of purple metallocene Compound B powder, Zr% = 18 (ICP), based on Zr, the yield was 94.1%.

Embodiment 3

[0066] Synthesis of metallocene compound C: (n-BuMeCp) 2 ZrCl 2 Preparation of adducts:

[0067] Under a nitrogen atmosphere, add 20 g (0.147 mol) of newly distilled methyl butyl cyclopentadiene to the three-necked flask, add 200 ml of tetrahydrofuran to dissolve, then lower the temperature to below -70°C, and slowly add 58.9 ml (0.147 mol) of n-butyl 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 add it dropwise to dissolve 16.43g ( 0.074mol) ZrCl 4 100ml of tetrahydrofuran solution, after dripping, gradually rise to room temperature, and then react for about 18 hours; vacuum distillation, evaporate to dryness, disperse with hexane, filter, wash 2 times with hexane to obtain 35g yellow metallocene Compound C powder, Zr%=17.5 (ICP), based on Zr, the yield was 91%.

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Abstract

The invention supplies a compounding catalyst system used to make wide / bimodal distribution high density polyethylene. It could take catalysis olefinic polymerization or copolymerizing to make bimodal distribution high density polyethylene.

Description

Technical field: [0001] The invention relates to a composite catalytic system for preparing wide / bimodal distribution high-density polyethylene, a preparation method and application. Background technique: [0002] Methods for preparing polymers with bimodal / broad molecular weight distribution include melt blending, staged reaction, and single reactor methods. The melt blending method is to blend two resins with different molecular weights by melting. This method has the problems of poor uniformity and high operating costs. The segmented reaction method mostly uses reactors connected in series, and different processes are used in different reaction stages. It also has the problem of high operating cost and complicated operation. The single-reactor mixed catalyst method is to use the performance difference of the different active centers of the two catalysts and the different chain termination speeds to broaden the molecular weight distribution of the resin. [0003] The cur...

Claims

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Application Information

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IPC IPC(8): C08F110/02C08F4/642
Inventor 陈伟郑刚邓晓音刘东兵王洪涛邱波胡建军何雪侠周歆刘长城胡青
Owner CHINA PETROLEUM & CHEM CORP
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