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Preparation method of high-grafting-ratio epoxied carbon nano tube additive for prepreg resin

An epoxidized carbon and nanotube technology is applied in the field of preparation of epoxidized carbon nanotube additives for prepreg resin, and can solve the problems of polluting the environment and increasing the complexity of the process.

Inactive Publication Date: 2015-04-29
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Canadian patent (CA2529626-A1) first disperses the surface functionalized modified carbon nanotubes in an organic solvent, then adds an epoxy resin matrix to it, removes the solvent after the dispersion is uniform, and then adds a curing agent to prepare a carbon nanotube reinforced ring Oxygen resin composite material, this method achieves the uniform dispersion of carbon nanotubes in the epoxy resin matrix, but the use of a large amount of organic solvents not only pollutes the environment but also increases the complexity of the process

Method used

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  • Preparation method of high-grafting-ratio epoxied carbon nano tube additive for prepreg resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Raw material 1 is multi-walled carbon nanotubes with a purity of >95%, a diameter of 10-20 nm, and a length of 0.5-500 μm, produced by Shenzhen Nanoport Co., Ltd.;

[0035] The ratio of raw material 2 mixed acid is concentrated sulfuric acid / concentrated nitric acid = 4 / 1 (volume ratio), all produced by Beijing Chemical Reagent Company;

[0036] Raw material 3: tetrahydrofuran;

[0037] Raw material 4: Mixture of liquid cycloaliphatic epoxy resin and N,N'-dimethylformamide (DMF), mixture of liquid cycloaliphatic epoxy resin and N,N'-dimethylformamide (DMF) The volume ratio is 1 / 2;

[0038] Raw material 5: Triphenylphosphine (TPP);

[0039] Raw material 6: Liquid cycloaliphatic epoxy resin

[0040]In step I, the mass ratio of raw material 1 to raw material 2 is 1 / 70, the heating and reflux temperature is 100° C., and drying is carried out at 80° C. to constant weight to obtain surface carboxylated carbon nanotubes. In step II, the mass ratio of the surface carboxylat...

Embodiment 2

[0045] Raw material 1: multi-walled carbon nanotubes, purity >95%, diameter 10-20 nm, length 0.5-500 μm, produced by Shenzhen Nanometer Harbor Co., Ltd.;

[0046] Raw material 2: The ratio of mixed acid is concentrated sulfuric acid / concentrated nitric acid = 3 / 1 (volume ratio), all produced by Beijing Chemical Reagent Company;

[0047] Raw material 3: N,N'-dimethylformamide (DMF);

[0048] Raw material 4: a mixture of liquid trifunctional epoxy resin TGAP and N,N'-dimethylformamide (DMF), a liquid trifunctional epoxy resin TGAP and N,N'-dimethylformamide (DMF ) volume ratio is 1 / 2;

[0049] Raw material 5: tetraethylammonium bromide;

[0050] Raw material 6: liquid trifunctional epoxy resin TGAP;

[0051] In step I, the mass ratio of raw material 1 to raw material 2 is 1 / 140, the heating and reflux temperature is 90° C., and drying is carried out at 90° C. to constant weight to obtain surface carboxylated carbon nanotubes. In step II, the mass ratio of the surface carboxy...

Embodiment 3

[0057] Raw material 1: multi-walled carbon nanotubes, purity >95%, diameter 10-20 nm, length 0.5-500 μm, produced by Shenzhen Nanometer Harbor Co., Ltd.;

[0058] Raw material 2: The ratio of mixed acid is concentrated sulfuric acid / concentrated nitric acid = 2 / 1 (volume ratio), all produced by Beijing Chemical Reagent Company;

[0059] Raw material 3: acetone;

[0060] Raw material 4: a mixture of liquid tetrafunctional epoxy resin TGDDM and N,N'-dimethylformamide (DMF), liquid tetrafunctional epoxy resin TGDDM and N,N'-dimethylformamide (DMF ) volume ratio is 1 / 2;

[0061] Raw material 5: triethylamine;

[0062] Raw material 6: liquid tetrafunctional epoxy resin TGDDM;

[0063] In step I, the mass ratio of raw material 1 to raw material 2 is 1 / 350, the heating and reflux temperature is 90° C., and drying is carried out at 90° C. to constant weight to obtain surface carboxylated carbon nanotubes. In step II, the mass ratio of the surface carboxylated carbon nanotubes to t...

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Abstract

The invention belongs to the field of preparation of a carbon fiber composite material and particularly relates to a preparation method of a high-grafting-ratio epoxied carbon nano tube additive for prepreg resin. The preparation method is characterized by utilizing epoxy groups in epoxy resin molecules to react with active functional groups on the surface of a carbon nano tube so as to prepare a high-grafting-ratio epoxied carbon nano tube. The preparation method comprises the following steps: firstly, carrying out acidizing on the carbon nano tube by utilizing mixed acid, introducing the active functional groups into the surface of the carbon nano tube, then grafting low-molecular-weight epoxy monomers to the surface of the carbon nano tube under the action of a catalyst and obtaining the high-grafting-ratio epoxied carbon nano tube by controlling the reaction conditions and selecting epoxy resin with high reaction activity; dispersing the epoxied carbon nano tube into low-viscosity liquid epoxy resin to prepare the carbon nano tube additive in a two-step dispersing manner, i.e. high-speed shearing stirring is firstly carried out and then grinding is carried out by utilizing a three-roller grinder. Addition of the carbon nano tube additive prepared by the preparation method into a prepreg resin system can be helpful for improving the dispersing effect of the carbon nano tube in the resin system and can obtain synchronous improvement on intensity, toughness and heat resistance.

Description

technical field [0001] The invention belongs to the field of preparation of carbon fiber composite materials, in particular to a method for preparing an epoxidized carbon nanotube additive suitable for prepreg resins, which can be used as a reinforcement of a high-viscosity toughened resin matrix, and can obtain strength and toughness Simultaneous improvement with heat resistance. Background technique [0002] As a single reinforced phase composite material system, traditional carbon fiber composites have shown a series of excellent properties and are widely used in aerospace, military industry and sports equipment. However, the traditional composite material system has not been able to give full play to the excellent properties of high-performance fibers and resin materials, making the application of composite materials far from reaching theoretical expectations. At this stage, it is difficult to optimize the modification of CFRP composites to achieve simultaneous improvem...

Claims

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Application Information

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IPC IPC(8): C08J3/22C08L63/02C08L63/04C08L63/00C08K9/04C08K9/02C08K7/00C08K3/04
Inventor 杨小平刘大伟李刚李鹏
Owner BEIJING UNIV OF CHEM TECH
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