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A kind of preparation method and application of graphene masterbatch supported by unsaturated polyolefin

A graphene and polyolefin technology, applied in the field of surface modification and the preparation of polymer-supported graphene masterbatches, can solve the problems of easy self-aggregation of graphene, unsatisfactory graphene dispersion, and difficulty in effective modification of graphene.

Active Publication Date: 2022-01-28
北京航天凯恩新材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the preparation of graphene masterbatches is still mostly carried out by long-term melt blending, so that the shear effect of the polymer transfer equipment is used to promote the dispersion of graphene in the polymer. This method cannot avoid the destruction of the graphene structure.
In addition, graphene is difficult to be effectively modified in the polymer matrix, and graphene's self-aggregation characteristics still exist due to the electronic combination between graphene layers.
When using graphene masterbatches to blend with polymers to prepare conductive composite materials, the graphene in the masterbatches is still dispersed unsatisfactorily after entering the polymer

Method used

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  • A kind of preparation method and application of graphene masterbatch supported by unsaturated polyolefin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Get a 1000ml beaker, configure nitric acid and sulfuric acid in it as 500g of mixed concentrated acid of 1:3, add 10 grams of commercially available graphene (less than 5 layers) to it, place the beaker in an ultrasonic water tank, and adjust the temperature of the water tank At 60°C, after oscillating ultrasonically at a frequency of 20kHz for 3 hours, use a centrifuge to separate the obtained mixed slurry at 4000r / min for 10 minutes to separate the mixed slurry into layers, thereby separating the black graphite at the bottom Alkene suspension. After the suspension was repeatedly washed with water to make the pH value above 6, the suspension was dried in a vacuum oven at 70° C. to a constant weight to obtain 9.8 grams of acidified graphene.

[0044] Take another 500ml beaker, add 45 grams of aliphatic vinyl ether containing (A) characteristic structure and 105 grams of aminopropyltriethoxysilane containing (B) characteristic structure, at 45°C, at a speed of 500rpm St...

Embodiment 2

[0053] Take a 5000ml beaker, configure nitric acid and sulfuric acid in it as 2000g of mixed concentrated acid of 1:3, add 100 grams of commercially available graphene (less than 5 layers) to it, place the beaker in an ultrasonic water tank, and adjust the temperature of the water tank At 70°C, after 8 hours of ultrasonic oscillation at a frequency of 40kHz, the obtained mixed slurry was centrifuged at 4000r / min for 10 minutes to separate the mixed slurry and separate the black graphite at the bottom Alkene suspension. After repeatedly washing the suspension with clean water to make the pH value above 6, the suspension was dried in a vacuum oven at 80° C. to a constant weight to obtain 97.5 grams of acidified graphene.

[0054] Take another 3000ml beaker, add 200 grams of aliphatic vinyl ether containing (A) characteristic structure and 600 grams of aminopropyltrimethoxysilane containing (B) characteristic structure, and stir at 1500rpm at 35°C , the stirring time was 2 hours...

Embodiment 3

[0063] Get a 2000ml beaker, configure nitric acid and sulfuric acid in it as 1000g of mixed concentrated acid of 1:3, add 30 grams of commercially available graphene (less than 5 layers) to it, place the beaker in an ultrasonic water tank, and adjust the temperature of the water tank After oscillating ultrasonically at 50°C for 5 hours at a frequency of 30kHz, use a centrifuge to separate the resulting mixed slurry at 4000r / min for 10 minutes to separate the mixed slurry into layers to separate the black graphite at the bottom Alkene suspension. After repeatedly washing the suspension with water to make the pH value reach 6 or more, the suspension was dried in a vacuum oven at 80° C. to a constant weight to obtain 29.3 grams of acidified graphene.

[0064] Take another 1000ml beaker, add 150 grams of aliphatic vinyl ether (A) and 150 grams of aminopropyltriethoxysilane (B), and stir at 40 ° C at a speed of 1000 rpm for 1 hour. A mixed modifier having an aliphatic vinyl ether ...

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Abstract

A preparation method and application of unsaturated polyolefin-supported graphene masterbatch involves the combination of graphene surface modification technology and unsaturated polyolefin solution convective coagulation technology in the field of preparing graphene-filled masterbatch, in order to achieve short-term Mechanical mixing, the purpose of significantly improving the mechanical properties and electrical conductivity of polymer composites. The method is characterized in that 25-35wt% polyether surfactant and aminosilane coupling agent compound are added to the methanol-water solution, and the acidified graphene content is 0.01 by surface grafting and coating modification method. ‑20wt% liquid phase to modify it, reconfigure it into a methanol suspension with a graphene content of 0.1‑10wt%, and finally convect it with an unsaturated polyolefin cyclohexane solution to complete co-coagulation, to This continuous preparation obtains a master batch with a graphene loading of 0.1-60 wt%. The masterbatch can be blended with a variety of polymers, and the graphene in the prepared composite material is evenly distributed, and the electrical conductivity and mechanical properties are significantly improved.

Description

Technical field: [0001] This application relates to the field of functional polymer composite materials, more specifically to the surface modification of graphene and the preparation method of polymer-loaded graphene master batches. Background technique: [0002] Graphene is a carbon atom with sp 2 The hybrid orbitals form a hexagonal two-dimensional carbon nanomaterial with a honeycomb lattice. The structural characteristics of graphene make it have special surface effects, small size effects, quantum size effects and macroscopic quantum tunneling effects, and the composite materials can also exhibit unique mechanics, heat, magnetism, electricity and optics. and other performance. Using graphene to improve the electrical properties of polymer materials is one of the hotspots in the research of polymer composites in recent years. At present, the addition of graphene has been able to change polymers from insulators to semiconductors and even conductors. In addition, graph...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/12C08K9/02C08K9/10C08K9/06C08K3/04C08L23/12C08L47/00C08L25/06C08J3/22
CPCC08J3/226C08K9/02C08K9/06C08K9/10C08K3/042C08J2447/00C08J2425/06C08K2201/001C08J2323/12
Inventor 郑骏驰孙兆懿郭新利舒帮建陈婧姜昊孟征钱晶肖军敏赵亚风
Owner 北京航天凯恩新材料有限公司