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 pol

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

Example Embodiment

[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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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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