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Temperature-sensitive graphene oxide and preparation method thereof

A graphene and temperature-sensitive technology, which is applied in the field of temperature-sensitive graphene oxide and its preparation, can solve the problems of temperature-sensitive materials use and weak bonding, and achieve high phase change enthalpy, good heat setting and thermal stability , the effect of good application prospects

Active Publication Date: 2017-06-13
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the three invention applications, there is only van der Waals force between the phase change material and graphene, but no chemical bond, the combination is not strong, and it cannot be used as a temperature-sensitive material

Method used

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  • Temperature-sensitive graphene oxide and preparation method thereof
  • Temperature-sensitive graphene oxide and preparation method thereof
  • Temperature-sensitive graphene oxide and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] The preparation method of graphene oxide grafted n-hexadecyl acrylate thermosensitive graphene material comprises the steps:

[0044] 1) Prepare GO using the following modified Hummers method:

[0045] a) Graphite powder pre-oxidation treatment: measure 40mL of concentrated sulfuric acid in a measuring cylinder and put it into a dry three-necked flask (250mL) equipped with mechanical stirring, and heat up to 80°C; add 8.4g of potassium persulfate and 8.4g of phosphorus pentoxide, and start stirring; Weigh 10g of graphite powder into a three-necked flask, and react at 80°C for 4.5h; after the reaction, wash and filter the sample repeatedly, put it in a petri dish to dry naturally, and set aside;

[0046] b) Preparation of graphene oxide: Measure 115mL of concentrated sulfuric acid in a measuring cylinder and put it into a three-necked flask (2L) equipped with mechanical stirring, place the three-necked flask in an ice-water bath, keep the temperature of the reaction syst...

Embodiment 2

[0052] The preparation method of graphene oxide grafted n-hexadecyl methacrylate thermosensitive graphene oxide material comprises the following steps:

[0053] 1) Using commercially available few-layer graphene powder as raw material, after treating with nitric acid and hydrochloric acid (mass ratio 3:1) at 25°C for 5 hours, washing with water to prepare graphene oxide;

[0054] 2) Weigh 50 mg of the graphene oxide prepared in step 1), and ultrasonically disperse it in 100 mL of toluene. The above dispersion was added into a 250mL three-necked flask, and 100mmol of hexadecyl methacrylate (inhibitor removal agent) was added at the same time, and nitrogen gas was passed for 1h to remove oxygen in the reaction system. Then, the toluene solution of the initiator BPO was added dropwise into the three-necked flask, wherein the amount of BPO was 0.08% of the amount of monomer cetyl methacrylate. Afterwards, the temperature of the reaction system was raised to 65° C., and the reacti...

Embodiment 3

[0059] The preparation method of graphene oxide grafted n-pentacyl acrylate thermosensitive graphene oxide material comprises the following steps:

[0060] 1) Utilize above-mentioned improved Hummers method to prepare graphene oxide;

[0061] 2) Weigh 150 mg of the graphene oxide prepared in step 1), and ultrasonically disperse it in 100 mL of DMF. The above dispersion liquid was added into a 250 mL three-necked flask, and 100 mmol n-pentacyl acrylate monomer (inhibitor removal agent) (0.19%) was added at the same time, and nitrogen gas was passed for 1 hour to remove oxygen in the reaction system. Then, the DMF solution of the initiator AIBN was added dropwise into the three-necked flask, and the amount of the initiator AIBN was 0.05% of the amount of the n-pentadecyl acrylate monomer. Afterwards, the temperature of the reaction system was raised to 70° C., and the reaction was carried out for 48 hours under stirring conditions to obtain a reaction mixture.

[0062] 3) Prec...

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Abstract

The invention discloses temperature-sensitive graphene oxide and a preparation method thereof. The preparation method comprises the following steps: 1) uniformly dispersing graphene oxide in a dispersing agent; 2) adding graphene oxide dispersion liquid and a reactive monomer into a reaction container, stirring, introducing inert gas, dropwise adding an initiator, then heating to the temperature of 60-70 DEG C, and stirring until reaction is completed, so that reaction mixed liquor is obtained, wherein the reactive monomer is at least one of n-alkyl methacrylate and n-alkyl acrylate or mixture of the two; 3) precipitating by utilizing an alcohol solvent, then dissolving precipitates into the dispersing agent, centrifuging for removing graphene oxide which is not involved in the reaction, and collecting precipitates II; and 4) dissolving the precipitates II into acetone or ethyl acetate, repeatedly centrifuging, collecting precipitates, and carrying out vacuum drying, so that the temperature-sensitive graphene oxide is obtained. The preparation method disclosed by the invention has the advantages that a phase change material is grafted to the surface of graphene oxide, the temperature-sensitive graphene oxide with stable performance is obtained, and the temperature-sensitive graphene oxide has high phase change enthalpy value and good thermal stability.

Description

technical field [0001] The invention relates to the field of preparation of phase change materials, in particular to a temperature-sensitive graphene oxide and a preparation method thereof. Background technique [0002] Graphene is a sp 2 Monoatomic sheets of carbon materials composed of hybridized carbon atoms with a two-dimensional (2D) structure are the basic units of other carbon nanomaterials. Graphene is an ideal composite modification and support material due to its light weight, high mechanical strength and hardness, and good thermal conductivity. In particular, the thermal conductivity of graphene is as high as 5000W / m·K, which is the material with the highest thermal conductivity so far. However, due to the natural hydrophobicity of graphene, it is almost insoluble by most organic solvents, which limits its application in the field of composite materials. The properties of graphene oxide (GO) are basically similar to those of graphene, and it can be regarded as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08F220/18C09K5/06
CPCC08F292/00C09K5/063C08F220/1818
Inventor 张兴祥曹瑞瑞陈赛刘海辉王学晨
Owner TIANJIN POLYTECHNIC UNIV
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