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In-situ polymerization preparation method of spinning-level high-heat-conductivity graphene/nylon composite material

A technology of nylon composite materials and high thermal conductivity graphite, which is applied in the direction of graphene, chemical instruments and methods, carbon compounds, etc., can solve the problems of poor dispersion and easy agglomeration of graphene, and achieve good thermal conductivity and good spinning performance Effect

Active Publication Date: 2016-09-21
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a spinning grade high thermal conductivity graphene / nylon composite material in-situ polymerization preparation method, which solves the problem of poor graphene dispersion and easy agglomeration, and prepares a spinning grade high thermal conductivity graphene / nylon composite

Method used

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  • In-situ polymerization preparation method of spinning-level high-heat-conductivity graphene/nylon composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Synthesis of Graphene Oxide:

[0028] (1) The expanded graphite sheet is pre-oxidized by electrochemical method, the expanded part is intercepted, rinsed with deionized water, dried for 8 hours at 80°C, pulverized, sieved with 60 mesh, and the obtained large sheet is reserved for later use;

[0029] (2) Under ice bath, in a 1000mL three-neck flask, add 140mL concentrated H 2 SO 4 Then under magnetic stirring, 3g of pre-oxidized flake graphite powder, then add 2g NaNO 3 , slowly add 15g KMnO 4 , ensure that the reaction temperature is within 0-10°C, and the reaction is carried out for 0.5 hours;

[0030] (3) Stir for 0.5 hours in a water bath at 40°C; raise the temperature to 97°C, and while stirring, quickly add 500mL of deionized water and react for 0.5 hours;

[0031] (4) Take a 2000mL beaker, pour the reactant from the three-necked flask into the beaker, add deionized water to 2000mL under magnetic stirring, then slowly add 15mL H 2 o 2 (30%H 2 o 2 );

[003...

Embodiment 2

[0040] Graphene oxide was synthesized according to the steps in Example 1.

[0041] Preparation of graphene / PA11 composites:

[0042] (1) Weigh 0.5 parts of graphene oxide concentrate and add 30 parts of water to dilute and disperse, and ultrasonically vibrate for 2 hours to obtain graphene oxide dispersion;

[0043] (2) Put the graphene oxide dispersion and 99.5 parts of PA11 monomer into the reaction kettle, heat and mix evenly, pass in nitrogen gas for 3 times, stir for 30 minutes, and the temperature is 90°C;

[0044] (3) Adjust the polymerization pressure by releasing water vapor, raise the temperature to about 190°C for 1-2 hours, keep the polymerization pressure at 1.6-2.5MPa, then raise the temperature to about 260°C for 6-7 hours, keep the polymerization pressure at 1.6-2. 2.8 MPa;

[0045] (4) After the reaction is finished, cool at a rate of 0.5 to 0.7°C / min, and when the temperature drops to 90 to 110°C, cool at a rate of 3 to 5°C / min until cooled to room tempera...

Embodiment 3

[0048] Graphene oxide was synthesized according to the steps in Example 1.

[0049] Preparation of graphene / PA12 composite:

[0050] (1) Weigh 0.5 part of graphene oxide concentrated solution and add 30 parts of water, and ultrasonically vibrate for 2 hours to obtain graphene oxide dispersion;

[0051] (2) Put the graphene oxide dispersion and 99.5 parts of PA12 monomer into the reaction kettle, heat and mix evenly, pass in nitrogen for 3 times, stir for 30 minutes, and the temperature is 90°C;

[0052] (3) Adjust the polymerization pressure by releasing water vapor, raise the temperature to about 190°C for 1-2 hours, keep the polymerization pressure at 1.6-2.5MPa, then raise the temperature to about 260°C for 6-7 hours, keep the polymerization pressure at 1.6-2. 2.8 MPa;

[0053] (4) After the reaction is finished, cool at a rate of 0.5 to 0.7°C / min, and when the temperature drops to 90 to 110°C, cool at a rate of 3 to 5°C / min until cooled to room temperature; release the pre...

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Abstract

The invention relates to an in-situ polymerization preparation method of a spinning-level high-heat-conductivity graphene / nylon composite material, belonging to the field of high-polymer composite materials. The in-situ polymerization preparation method comprises the following steps: diluting and dispersing a graphene oxide concentrated solution and water, and carrying out ultrasonic oscillation to obtain a graphene oxide dispersion solution; adding the graphene oxide dispersion solution into a nylon monomer, heating and uniformly mixing, and carrying out stepwise heating polymerization; and carrying out after-treatment to obtain the graphene / nylon composite material. The in-situ polymerization method is adopted to solve the problems of poor dispersity and high aggregation tendency of the graphene in the nylon monomer, and the nylon monomer and the oxygen-containing functional group of the graphene oxide can form a firm chemical bond. The synthesized graphene / nylon composite material has favorable heat conductivity, and the heat conductivity coefficient is 0.23-6.12 W / (m.K). Besides, the graphene / nylon composite material has favorable spinning properties, and can be used for spinning by melt spinning, electrostatic spinning or any other spinning process.

Description

technical field [0001] The invention belongs to the field of polymer composite materials, and relates to a preparation method for in-situ polymerization of a spinning grade high thermal conductivity graphene / nylon composite material. The synthesized graphene / nylon composite material has good thermal conductivity and spinning performance. Background technique [0002] Nylon material has good comprehensive properties, such as mechanical properties, heat resistance, wear resistance, chemical resistance and self-lubrication, low friction coefficient, certain flame retardancy, easy processing, widely used in spinning, chemical industry , instruments, automobiles and other fields. [0003] Due to its unique planar two-dimensional structure, graphene has excellent mechanical properties and structural rigidity. Due to its high conductivity, high strength, ultra-thin and other characteristics, it is widely used in catalysts, electrode materials, water treatment, sensors, biological m...

Claims

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Application Information

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IPC IPC(8): C08L77/02C08K3/04C08L77/06C01B31/04
CPCC01B2204/04C01B2204/24C08K3/04C08L2203/12C08L77/02C08L77/06
Inventor 潘凯邱远游罗婷
Owner BEIJING UNIV OF CHEM TECH
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