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Preparation method of polymer/graphene composite material through in situ reduction

A technology of graphene composite and composite materials, which is applied in the direction of conductive materials dispersed in non-conductive inorganic materials, heat exchange materials, chemical instruments and methods, etc., can solve problems such as far apart, and achieve easy control and reaction temperature The effect of low cost and simple preparation process

Active Publication Date: 2010-10-20
成都创威新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, polymer / graphene composites are generally prepared by solution, melt mixing, and in-situ polymerization, but due to the easy aggregation of graphene, so far, the experimental results are still far from theoretical predictions.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 2.5kg of graphite oxide and 1600kg of water into a reaction kettle with an ultrasonic generating device. The ultrasonic power is 200W, the frequency is 200Hz, and the temperature is 40°C. Ultrasonic dispersion is performed for 1 hour to obtain a graphite oxide solution. Add 32.3kg of natural latex and continue After ultrasonic dispersion for 1 hour, 12 kg of hydrazine hydrate was added, and ultrasonic dispersion was continued for 2 hours to obtain a natural latex / graphene composite emulsion. Use 5kg of formic acid demulsifier, demulsify at a temperature of 80°C for 5 minutes, and dry the product to a constant weight at a vacuum degree of 0.09MPa and a temperature of 40°C to obtain a natural rubber / graphene composite masterbatch.

[0034] 20kg natural rubber-coated graphene, 80kg natural rubber, 5kg zinc oxide, 3kg stearic acid, 3kg sulfur, 4kg N-isopropyl-N′-phenyl-p-phenylenediamine, 1.5kg N-cyclohexyl 2-phenylene Benzothiazole sulfenamide and 0.3kg benzothiazole d...

Embodiment 2

[0036] Graphite oxide 100kg and 3000kg ethanol are added in the grinder, and the grinding time is 1.5 hours to obtain graphite oxide solution, add polymethyl methacrylate emulsion 300kg, grind for 1.5 hours, then add sodium borohydride solution 8kg, continue grinding for 2 hours, Obtain polymethyl methacrylate / graphene composite emulsion. Using 30kg of sodium chloride solution, at a temperature of 100°C, the emulsion was broken for 60 minutes, and the product was dried to a constant weight at a vacuum degree of 0.1MPa and a temperature of 230°C to obtain a polymethyl methacrylate / graphene composite masterbatch.

[0037] 34kg of PMMA-coated graphene, 70kg of PMMA, 13kg of bis(tribromophenoxy)ethane and 7kg of PbO3 were prepared by extrusion of PMMA / graphite olefin composite material, extrusion temperature is 200 ℃.

Embodiment 3

[0039] Add 0.01kg of graphite oxide and 100kg of DMF into the ultrasonic irradiation reactor, start the ultrasonic cell pulverizer, the ultrasonic power is 10,000W, the frequency is 20,000Hz, the temperature is 60°C, and the ultrasonic dispersion time is 30 minutes to obtain graphite oxide solution, add 5kg of EVA latex , continue ultrasonication for 30 minutes, then add 4 kg of ethylenediamine, continue ultrasonication for 3 hours, and prepare a stable EVA / graphene composite emulsion. Using 1 kg of sodium sulfate solution, demulsification at a temperature of 10° C. for 1 minute, and drying the product at a vacuum degree of 0.05 MPa and a temperature of 50° C. to constant weight to obtain an EVA / graphene composite masterbatch.

[0040] 21kg of EVA-coated graphene, 80kg of EVA, 20kg of calcium carbonate and 3kg of stearic acid were first extruded and mixed uniformly through a twin-screw extruder, and the extrusion temperature was 180°C. After granulation and drying, the EVA / gra...

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Abstract

The invention relates to a preparation method of a polymer / graphene composite material through in situ reduction, which is characterized by comprising the following steps: adopting ultrasonic wave or grinding to evenly disperse the graphite oxide prepared by a Hummers method into polymer dispersion; introducing reducing agent into the polymer dispersion for in situ reduction, enabling the graphite oxide to be reduced into the grapheme so as to obtain stable polymer / graphene composite emulsion; carrying out demulsification, agglomeration and drying to obtain the composite polymer / grapheme composite master batch; adding the dried polymer / grapheme composite master batch and various assistants into the polymeric matrix according to a certain ratio; and carrying out double-roller mixing, vulcanization, melt extrusion or injection molding to obtain the polymer / graphene composite material with excellent physical and mechanical properties.

Description

technical field [0001] The invention relates to an in-situ reduction preparation method of a polymer / graphene composite material, which belongs to the field of polymer preparation. Background technique [0002] Graphene is a sp 2 A new carbonaceous material with a two-dimensional honeycomb lattice structure formed by close packing of hybridized carbon atoms, with a thickness of one or more atomic layers. According to the number of layers, it can be divided into one or more layers of graphene. Theoretical research on graphene has a history of more than 60 years, and until 2004, two-dimensional graphene sheets that can truly exist independently were obtained by Novoselov at the University of Manchester in the United Kingdom by using tape to peel off highly oriented graphite. So far, graphene has been prepared by the following methods: 1) chemical vapor deposition (Eizenberg M., Blakely J. M. Surf. Sci. 1970, 82, 228-236.); 2) epitaxial growth (Berger C. Song Z., Li X., Wu X...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L7/00C08L33/12C08L23/08C08L31/04C08L9/02C08L9/06C08L55/02C08K13/02C08K3/04C08J3/22H01B1/24B60C1/00C09K5/14
Inventor 夏和生战艳虎费国霞伍金奎闫宁
Owner 成都创威新材料有限公司
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