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Preparation method of core-shell type mesocarbon microbeads

A technology of mesocarbon microspheres and core-shell type, which is used in the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc., can solve the problem of inability to control the thickness of the carbon layer, the difference in coating uniformity, and the difference between the two-phase surface and interface. And other issues

Active Publication Date: 2021-12-28
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the coating method or modification method is an effective means to construct the core-shell structure, the performance of the mesophase carbon microspheres can be regulated by the type of coating material, the thickness of the coating layer, and the modification material, but these methods are limited to a certain extent. It will increase the complexity and difficulty of the process, and there are large differences in the uniformity of the coating and the surface and interface differences that are easy to form two phases
In fact, the mesophase carbon microspheres prepared by the traditional emulsification method and suspension method often have a thin layer of carbon layer derived from isotropic pitch, which shows that the core-shell mesophase carbon microspheres can be obtained directly. advantages and potentials, but these two methods do not control the thickness of the carbon layer

Method used

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  • Preparation method of core-shell type mesocarbon microbeads

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] First, the isotropic pitch with a softening point of 210°C and the mesophase pitch with a softening point of 275°C were melted at 260°C and 310°C respectively, and then the isotropic pitch with a viscosity of Phase asphalt was melt blended at a mass ratio of 10:100, and the ratio of asphalt would affect the viscosity of the blended asphalt. The mixing speed was 500 rpm, the blending temperature was 340 ° C, and the blending time was 5 hours. Then under the conditions of extrusion temperature 340°C and extrusion pressure 0.5MPa under the spinning device, the viscosity of the blended asphalt piece is adjusted to 100Pa·s for capillary extrusion to obtain "beaded" asphalt liquid beads, and drop to The density gradient composed of tetrahydrofuran and carbon tetrachloride ranges from 0.888 to 1.595 cm 3 / g, in the uniform gradient density receiving phase with a height of 100cm, the span of the density gradient affects the dissolution of asphalt components and the subsequent c...

Embodiment 2

[0020] First, the isotropic pitch with a softening point of 210°C and the mesophase pitch with a softening point of 275°C were melted at 280°C and 350°C, and then the isotropic pitch with a viscosity of 5000Pa·s and the mesophase pitch with a viscosity of 10000Pa·s Melt blending is carried out at a mass ratio of 20:100. The asphalt ratio will affect the viscosity of the blended asphalt. The mixing speed is 200rpm, the blending temperature is 340°C, and the blending time is 1h. Then under the conditions of extrusion temperature 360°C and extrusion pressure 1.0MPa under the spinning device, the viscosity of the blended asphalt piece is adjusted to 300Pa·s for capillary extrusion to obtain "beaded" asphalt liquid beads, and drop to The density gradient composed of ethanol and carbon tetrachloride ranges from 0.789 to 1.595 cm 3 / g, in the receiving phase with a height of 100cm, the span of the density gradient has an impact on the dissolution of the asphalt component and the subse...

Embodiment 3

[0023] First, the isotropic pitch with a softening point of 210°C and the mesophase pitch with a softening point of 275°C are melted at 270°C and 370°C, and then the isotropic pitch with a viscosity of 1000Pa·s and the mesophase pitch with a viscosity of 10000Pa·s Melt blending is carried out at a mass ratio of 20:100. The asphalt ratio will affect the viscosity of the blended asphalt. The mixing speed is 600rpm, the blending temperature is 320°C, and the blending time is 3h. Then under the conditions of extrusion temperature 370°C and extrusion pressure 0.7MPa under the spinning device, the viscosity of the blended asphalt piece is adjusted to 500Pa·s for capillary extrusion to obtain "beaded" asphalt liquid beads, and drop to The density gradient composed of tetrahydrofuran and dibromoethane ranges from 0.888 to 2.137cm3 / g, and in the receiving phase with a height of 100cm, the span of the density gradient affects the dissolution of the asphalt components and the subsequent c...

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Abstract

The invention discloses a preparation method of core-shell type mesocarbon microbeads. The method comprises the steps of firstly, obtaining asphalt fluids with different viscosities from isotropic asphalt and mesophase asphalt at different melting temperatures, then blending the two asphalt fluids with different viscosities according to a mass ratio of (5-30): 100 to prepare mixed asphalt, extruding the mixed asphalt in a capillary tube at the temperature of 340-380 DEG C to form bead-like liquid beads, and directly dripping the bead-like liquid beads into receiving phases with different density gradients, filtering, washing and drying to obtain asphalt microspheres, and finally, pre-oxidizing, carbonizing and graphitizing to obtain the core-shell type mesocarbon microbeads. According to the invention, through melt blending of isotropic asphalt and mesophase asphalt with different viscosity and a capillary extrusion process, the characteristic that the outer layer of the asphalt microsphere is isotropic asphalt and the inner layer of the asphalt microsphere is mesophase asphalt is realized, and then core-shell ratio controllable core-shell type mesocarbon microbeads with disordered carbon on the outer layer and ordered carbon on the inner layer is obtained by derivation.

Description

technical field [0001] The invention belongs to the field of preparation methods of mesophase carbon microspheres. Specifically, the present invention relates to a method capable of preparing core-shell mesophase carbon microspheres. [0002] technical background [0003] In recent years, with the rapid development of electric vehicles, energy storage power supplies, consumer electronics and other fields, energy storage materials with high energy density, high power density, long service life, good safety, low price and environmental friendliness An increasingly urgent need has been raised. Mesophase carbon microspheres are an important negative electrode material for energy storage materials, and the development of mesophase carbon microspheres with specific structures for energy storage materials is the development trend of its electrochemical energy storage research and development. Among them, the core-shell structure carbon material has a double-layer or multi-layer st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/205C01B32/15H01M4/36H01M4/587H01M10/0525B01J13/02
CPCC01B32/205C01B32/15H01M4/366H01M4/587H01M10/0525B01J13/02Y02E60/10
Inventor 杨建校董斯琳祁勇魏文杰
Owner HUNAN UNIV
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