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Halloysite nanotube / epoxy nanocomposite

A technology of halloysite nanotubes and nanocomposites, which is applied in the field of halloysite nanotubes/epoxy resin nanocomposites to achieve good practical value, enhance interface interaction, and improve mechanical properties

Active Publication Date: 2016-08-17
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the use of branched polyethyleneimine to graft modified halloysite nanotubes for toughening and reinforcing epoxy resin has not been introduced, but the surface modification of other nanoparticles by polyethyleneimine has been reported

Method used

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  • Halloysite nanotube / epoxy nanocomposite
  • Halloysite nanotube / epoxy nanocomposite
  • Halloysite nanotube / epoxy nanocomposite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] (1) Acidification of halloysite nanotubes: mix halloysite nanotube particles with 1mol / L hydrochloric acid solution at a mass ratio of 1:20, ultrasonically disperse for 60 minutes, stir for 4 hours, centrifuge, filter, and wash with water until medium properties, acidified halloysite nanotubes were obtained after drying at 110°C for 2 hours;

[0052] (2) Surface modification of halloysite nanotubes by silane coupling agent: prepare a homogeneous suspension with acidified halloysite nanotubes and toluene at a mass ratio of 1:50, and continue ultrasonic treatment for 30 minutes. Add dropwise γ-glycidyl etheroxypropyltrimethoxysilane (KH560) with 20% mass of acidified halloysite nanotubes, and stir and react at 120°C for 4 hours; after the reaction, filter, wash, and dry to obtain surface-modified Halloysite nanotubes with epoxy groups (KH560-HNTs);

[0053] (3) Branched polyethyleneimine grafted halloysite nanotubes: the epoxy group-modified halloysite nanotubes obtained i...

Embodiment 2

[0066] (1) Acidification of halloysite nanotubes: Mix halloysite nanotube particles with 2mol / L sulfuric acid solution at a mass ratio of 1:30, ultrasonically disperse for 30 minutes, stir for 12 hours, centrifuge, filter, and wash with water until neutral ; Import the washed product into a clean container, and dry at 100°C for 3 hours to obtain acidified halloysite nanotubes;

[0067] (2) Surface modification of halloysite nanotubes by silane coupling agent: take halloysite nanotubes by weighing, add 20 times the mass of acetone solution, ultrasonic treatment for 30 minutes; -(3,4-epoxycyclohexyl)ethyltrimethoxysilane (A-186), continue ultrasonic stirring for 30 minutes, add sodium hydroxide solution to make the pH of the mixture neutral, and react at 70°C for 5 hour; after the reaction finishes, filter, wash, dry, obtain the halloysite nanotube that the surface is modified with epoxy group;

[0068] (3) Branched polyethyleneimine grafted halloysite nanotubes: ultrasonically...

Embodiment 3

[0076] (1) Acidification of halloysite nanotubes: halloysite nanotube particles are mixed with 30% hydrogen peroxide at a mass ratio of 1:10, ultrasonically dispersed for 45 minutes to obtain a uniformly dispersed system; transferred to 80°C and stirred for 48 hours, Centrifuge, filter, wash with water until neutral, and dry at 110°C for 2.5 hours to obtain acidified halloysite nanotubes;

[0077] (2) Surface modification of halloysite nanotubes by silane coupling agent: Weigh acidified halloysite nanotubes, add 10 times the mass of ethanol solution (volume ratio of ethanol to water is 95 / 5), and continue ultrasonic treatment for 45 minutes ; The pH value of the solution is adjusted to 4 to 5 with dilute hydrochloric acid, and γ-glycidyl etheroxypropylmethyldimethoxysilane (AC-661) of acidified halloysite nanotube quality 50% is added dropwise, at 80°C The reaction was stirred for 24 hours. After the reaction is finished, filter, wash, and dry to obtain halloysite nanotubes w...

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Abstract

The present invention relates to the field of nano-composite materials, and specifically relates to a halloysite nanotube / epoxy nanocomposite. The halloysite nanotube is a branched polymine grafted halloysite nanotube; the branched polymine grafted weight halloysite nanotube and epoxy resin are in the weight ratio of 0.2-20:100, preferably 0.5-5:100. The hyperbranched polymine is grafted onto epoxidized HNTs, so that the branched structure has rich amino groups to generate stronger chemical bonds or hydrogen bonds between the halloysite nanotube and an epoxy matrix and to enhance the interface effect. The prepared modified halloysite nanotube can effectively improve the impact resistance of epoxy resin and reduce brittle fracture of epoxy resin, and has broad application prospects in the fields of automotive, electronics, functional materials and aerospace.

Description

technical field [0001] The invention relates to the field of nanocomposite materials, in particular to a halloysite nanotube / epoxy resin nanocomposite material. Background technique [0002] Halloysite nanotubes are inexpensive natural nanotubes formed from sheets of kaolinite that curl under certain climatic conditions. Generally, the outer diameter of the tube is 40-100 nm, and the length is about 0.2-2 μm. HNTs are double-layer 1:1 aluminosilicates with the molecular formula Al 2 SiO 5 (OH) 4 ·nH 2 O (n=0 or 2), is formed by dislocation and coiling of aluminum-oxygen octahedra in the inner layer and silicon-oxygen tetrahedron in the outer layer, and crystal water exists between the layers. The outer surface of HNTs is mainly composed of Si-O-Si bonds, and the inner wall is mainly composed of aluminum hydroxyl groups. There are silicon / aluminum hydroxyl groups on the crystalline edges of HNTs or the end faces of the tubes, while a small amount of embedded hydroxyl gr...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08K9/04C08K9/06C08K7/00C08K3/34
Inventor 孙攀刘国明吕冬刘学新赵莹董侠周勇苏允兰吴景深王笃金
Owner INST OF CHEM CHINESE ACAD OF SCI
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