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Gaseous-phase in-situ polymerization method for preparing ultra-high molecular weight polyethylene graphene composite material

An ultra-high molecular weight, gas-phase in-situ technology, which is applied in the field of gas-phase in-situ polymerization to prepare ultra-high molecular weight polyethylene graphene composite materials, can solve the problems of material brittle fracture, material impact resistance reduction, failure, etc., and achieve brittleness Fracture, excellent performance, and strong impact resistance

Inactive Publication Date: 2013-05-08
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, most of the current preparation methods of polymer-based graphene composite materials adopt the method of blending, such as CN102618955A discloses a kind of ultra-high molecular weight polyethylene / graphene composite fiber, as nano-scale graphene with higher surface energy It is said that if only a simple blending method is used, it is difficult to uniformly disperse it, and there are many aggregates in the obtained composite material, which usually leads to a decrease in the impact resistance of the material, and may cause brittleness of the material during long-term use. Serious consequences such as fracture and failure

Method used

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  • Gaseous-phase in-situ polymerization method for preparing ultra-high molecular weight polyethylene graphene composite material

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Experimental program
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Effect test

Embodiment 1

[0042] Take 0.12 g of graphene and treat it at 110°C for 1.0 hour, make a suspension of the treated graphene and 100 ml of heptane, add 0.5 ml , heated to reflux temperature, and reacted at this temperature for 0.5 hours, and filtered. Gained solid was washed 3 times at 30~60 DEG C with 30 milliliters of hexanes, then in 60 DEG C The solid catalyst was obtained by drying in a stream for 1 hour. Its graphene content is 63wt%. Use a 500 ml three-necked flask equipped with a stirrer and a constant temperature system Replace by pumping three times, and replace once with ethylene. Add 200 ml of hexane, 0.15 ml of 1.5M triisobutylaluminum and 0.004 g of solid catalyst (molar ratio 30:1) in sequence, start stirring, and after 5 min, remove the solvent and feed ethylene gas, at 40°C and normal pressure The reaction was stopped after 2 hours, and the obtained polymer was dried in an oven to obtain 50 grams of off-white powdery composite material.

[0043] The graphene content i...

Embodiment 2

[0045] Take 0.25 grams of graphene and treat it at 150°C for 6 hours, make a suspension of the treated graphene and 100 milliliters of heptane, add 0.5 milliliters , heated to reflux temperature, and reacted at this temperature for 2 hours, and filtered. Gained solid was washed 3 times at 30~60 DEG C with 30 milliliters of hexanes, then in 60 DEG C The solid catalyst was obtained by drying in stream for 0.5-1 hour. Its graphene content is 81wt%. Use a 500 ml three-necked flask equipped with a stirrer and a constant temperature system Replace by pumping three times, and replace once with ethylene. Add 200 ml of hexane, 0.8 ml of 1.5M triisobutylaluminum and 0.012 g of solid catalyst (molar ratio 100:1) in sequence, start stirring, and after 10 min, remove the solvent and feed ethylene gas, at 50 ° C, 0.01 MPa The reaction was stopped after 5 hours, and the obtained polymer was dried in an oven to obtain 50 grams of off-white powdery composite material.

[0046] The graph...

Embodiment 3

[0048] Take 0.5 grams of graphene and treat it at 200°C for 6 hours, make a suspension of the treated graphene and 100 milliliters of heptane, add 0.5 milliliters , heated to reflux temperature, and reacted at this temperature for 2 hours, and filtered. Gained solid was washed 3 times at 30~60 DEG C with 30 milliliters of hexanes, then in 60 DEG C The solid catalyst was obtained by drying in stream for 0.5-1 hour. Its graphene content is 90wt%. Use a 500 ml three-necked flask equipped with a stirrer and a constant temperature system Replace by pumping three times, and replace once with ethylene. Add 200 ml of hexane, 0.42 ml of 1.5M triisobutylaluminum and 0.027 g of solid catalyst (molar ratio 45:1) in sequence. After 15 minutes, remove the solvent, start stirring, and feed ethylene gas. The reaction was stopped after 10 hours, and the obtained polymer was dried in an oven to obtain 50 grams of off-white powdery composite material.

[0049] The graphene content in the...

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Abstract

The invention discloses a gaseous-phase in-situ polymerization method for preparing an ultra-high molecular weight polyethylene graphene composite material. The method comprises the following steps of: reacting graphene which serves as a catalyst carrier with a transition metal compound to prepare a solid catalyst under a certain conditions, and reacting to prepare the ultra-high molecular weight polyethylene graphene composite material under the gaseous-phase conditions without a diluent. Graphene serves as the catalyst carrier and a reinforcing filler and is reacted under the gaseous-phase conditions, so that the polymerization activity can be improved through catalyst loading; and graphene in the composite material is uniformly dispersed, so that the composite material has excellent performance and particularly high impact resistance, and the problems that the traditional composite material is subjected to brittle rupture and is ineffective in long-term use process are solved.

Description

technical field [0001] The invention relates to the technical field of preparation of nanocomposite materials, in particular to the preparation of ultrahigh molecular weight polyethylene graphene composite materials by a gas phase in-situ polymerization method. Background technique [0002] The molecular weight of Ultra High Molecular Weight Polyethylene (UHMWPE) is generally 10 6 The above is 2 orders of magnitude higher than ordinary polyethylene (PE), so it has some excellent properties that ordinary PE does not have, such as wear resistance is 8~9 times that of steel, impact resistance is 2 times that of polycarbonate PC , Acrylonitrile-butadiene-styrene copolymer ABS 5 times, polyoxymethylene POM 15 times, chemical resistance and excellent noise reduction and low friction coefficient, etc. It has been more and more widely used in high-tech fields such as biomedicine, microelectronics, chemical machinery, as well as in grain processing, textile machinery and other indus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F110/02C08F2/44C08F2/34C08F4/02C08F4/64C08K3/04
Inventor 潘炳力李宁张军凯成玉梅杜锦屏杜三明刘继纯张永振
Owner HENAN UNIV OF SCI & TECH
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