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A kind of preparation method of low entanglement polyethylene

A polyethylene and low-entanglement technology, applied in the field of low-entanglement polyethylene preparation, can solve the problems of inability to continue the polymerization reaction for a long time, poor polymer film strength, affecting product processing performance and mechanical properties, etc. Completeness, good workability, the effect of reducing the probability of overlapping

Active Publication Date: 2018-08-10
宁波链增新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the strength of this physically coated polymer film is poor. During polymerization, the polyethylene grown from the inside of the carrier quickly breaks the polymer film. The control of the knot immediately fails, and the polymerization reaction cannot be continued for a long time, which affects the processing performance and mechanical properties of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Purge the reaction device with high-purity nitrogen to remove air and water in the reaction device. Take 1g porous carrier SiO 2 , The pore volume is 0.7g / ml, add 5ml mixed solution of styrene, 4-chloromethylstyrene, AIBN initiator, the molar ratio of 4-chloromethylstyrene to styrene is 1, AIBN and benzene The molar ratio of ethylene is 0.01, and the porous carrier is immersed in the mixed solution for 24 hours at 30°C. Heat at 60°C for 4 hours, then at 100°C for 2 hours, and finally at 120°C for 2 hours to obtain carrier B. Add 50ml toluene, 0.15g Cp 2 ZrCl 2 Add 1 g of carrier B and stir for 4 hours, wash with 50 ml of toluene three times, and then dry to obtain catalyst B.

[0034] The gas phase polymerization reactor was adjusted to 60° C. and the pressure was 10 bar, and 5 mmol trimethylaluminoxane (MAO), ethylene, and 0.1 g catalyst B were sequentially added to start the polymerization reaction. The reaction was stopped after 2 hours of polymerization, and the obta...

Embodiment 2

[0036] Purge the reaction device with high-purity nitrogen to remove air and water in the reaction device. Take 1g porous carrier SiO 2 , The pore volume is 10g / ml, add 1ml mixed solution of styrene, 4-chloromethylstyrene, AIBN initiator, the molar ratio of 4-chloromethylstyrene to styrene is 0, AIBN and styrene The molar ratio is 0.01, and the porous carrier is immersed in the mixed solution for 4 hours at 10°C. Heat at 60°C for 4 hours, then at 100°C for 2 hours, and finally at 120°C for 2 hours. Obtain carrier C. Add 50ml cyclohexane and 0.15g Ziegler-Natta catalyst. Add 1 g of carrier C and stir for 24 hours, wash with 50 ml of hexane 3 times, and then dry to obtain catalyst C.

[0037] The gas phase polymerization reactor was adjusted to 90° C., the pressure was 1 bar, and 10 mmol trimethylaluminoxane (MAO), ethylene, and 0.1 g of catalyst C were sequentially added to start the polymerization reaction. The reaction was stopped after 8 hours of polymerization, and the obt...

Embodiment 3

[0039] Purge the reaction device with high-purity nitrogen to remove air and water in the reaction device. Take 1g of porous carrier magnesium chloride with a pore volume of 0.01g / ml, add 0.5ml of mixed solution of styrene, 4-bromomethylstyrene, AIBN initiator, and the molar ratio of 4-bromomethylstyrene to styrene It is 10, the molar ratio of AIBN to styrene is 0.1, and the porous carrier is immersed in the mixed solution for 12 hours at 0°C. Heat at 60°C for 4 hours, then at 100°C for 2 hours, and finally at 120°C for 2 hours. Obtain carrier D. Add 10 ml of n-hexane and 0.15 g of late transition metal catalyst (pyridine diimide iron) catalyst. Add 1 g of carrier D and stir for 4 hours, wash with 5 ml of isopentane three times, and then dry to obtain catalyst D.

[0040] The gas phase polymerization reactor was adjusted to -40°C and the pressure was 30 bar, and 8mmol of trimethylaluminoxane (MAO), ethylene and 0.1g of catalyst D were sequentially added to start the polymeriza...

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Abstract

The invention relates to a preparation method of a low entanglement polyethylene. The method employs a styrene in situ free radical polymerization in a porous carrier. The method comprises the steps of: diffusing styrene, a copolymer monomer and an initiator into the carrier, and then initiating polymerization to obtain a modified porous carrier with pores uniformly filled by styrene based copolymer; then using the porous carrier for further support a catalyst; in the process of gas phase polymerization, using the mass transfer resistance of styrene based copolymer on ethylene and the effective separation on an active center to control the growth rate of polyethylene chain, so as to inhibit the probability of chain overlap in polymerization and promote preferential crystallization grown molecular chains in a micro reaction unit; and in finally preparing the low entanglement polyethylene. The method of the invention can produce low entanglement polyethylene with the molecular weight of 10000g / mol-10000000g / mol; and the processing performance and mechanical strength of the product are improved effectively.

Description

Technical field [0001] The invention relates to the technical field of olefin polymerization reactions, in particular to a method for preparing low-entanglement polyethylene. Background technique [0002] The degree of chain entanglement is a very important characteristic in polymer condensed matter physics. It determines to a large extent the polymer’s melt viscoelasticity, segment dynamics, mechanical strength and interfacial adhesion, and also determines The microscopic morphology and physical properties of the polymer processed by the melt are analyzed. Take ultra-high molecular weight polyethylene (UHMWPE) as an example: 1mg of commercial UHMPWE primary particles with a molecular weight of 1 million, the content of entanglement points can reach 10 14 One. A large number of chain entanglements make the material melt viscosity high and processing is extremely difficult. After UHMWPE is fiberized, a large number of chain entanglements will cause uneven fiber thickness and cry...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F110/02C08F4/02C08F212/08C08F212/14C08F220/14C08F216/08
CPCC08F110/02C08F212/14C08F216/08C08F220/14C08F4/025C08F4/022C08F4/02C08F212/08
Inventor 历伟惠磊杨华琴张晶晶
Owner 宁波链增新材料科技有限公司
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