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A kind of nano-iron compound/mesophase carbon microsphere composite material and preparation method thereof

A technology of mesocarbon microspheres and composite materials, which is applied in the direction of electrochemical generators, structural parts, electrical components, etc., can solve the problems of easy agglomeration of nucleating agent particles and difficulty in uniform dispersion, and achieve simple and easy-to-operate synthesis steps, The process is simple and feasible, and the effect of reversible capacity improvement

Active Publication Date: 2020-10-30
郑州中科新兴产业技术研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of method can improve the electrochemical properties of mesocarbon microspheres and regulate the yield and particle size, but there are technical problems that the nucleating agent particles are easy to agglomerate and difficult to disperse uniformly

Method used

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  • A kind of nano-iron compound/mesophase carbon microsphere composite material and preparation method thereof
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  • A kind of nano-iron compound/mesophase carbon microsphere composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation of nano iron compound / mesophase carbon microsphere composite material, the steps are as follows:

[0027] Select high-temperature coal tar to distill to obtain coal tar pitch, and the coal tar pitch is pretreated to remove quinoline insoluble matter. Take 500 g of dequinoline-insoluble coal tar pitch, iron oleate and sublimed sulfur, and mix them uniformly into the reactor at a mass ratio of 100: 3: 0.2. At a reaction temperature of 380 ° C, a reaction pressure of 2 MPa, a stirring speed of 100 rpm, and a heating Under the condition of a rate of 5 °C / min, the reaction was carried out in a nitrogen atmosphere for 4 h, and the nitrogen flow rate was 1 L / min. The product was separated from washing oil and then vacuum-dried to obtain the precursor of nano-iron compound / mesophase carbon microspheres. The mass ratio of washing oil to product was 3:1, and the dissolution temperature was 180°C. The composite material precursor was carbonized under argon protect...

Embodiment 2

[0033] The preparation of nano iron compound / mesophase carbon microsphere composite material, the steps are as follows:

[0034] Another kind of coal tar pitch is selected, and the coal tar pitch is pretreated to remove quinoline insoluble matter. Take 500 g of dequinoline-insoluble coal tar pitch, ferrocene and sublimed sulfur, and mix them uniformly into the reactor at a mass ratio of 100: 1: 0.1. At a reaction temperature of 400 ° C, a reaction pressure of 1 MPa, a stirring speed of 150 rpm, and a heating Under the condition of a rate of 5 °C / min, the reaction was carried out in a nitrogen atmosphere for 2 h, and the nitrogen flow rate was 0.5 L / min. The product was separated from toluene and then vacuum-dried to obtain the precursor of nano-iron compound / mesophase carbon microspheres. The mass ratio of toluene to product was 1:1, and the dissolution temperature was 80°C. The composite material precursor was further carbonized at 900 °C for 2 h under argon protection, with...

Embodiment 3

[0037] The preparation of nano iron compound / mesophase carbon microsphere composite material, the steps are as follows:

[0038] Select 500g of petroleum asphalt, ferric oleate and mercaptan according to the mass ratio of 100: 7: 0.6 and evenly blend them into the reactor. Under the condition of , react in nitrogen atmosphere for 6 h, nitrogen flow rate 1.5L / min. The product was separated from the washing oil and then vacuum-dried to obtain the precursor of nano-iron compound / mesophase carbon microspheres. The mass ratio of washing oil to product was 4:1, and the dissolution temperature was 150°C. The composite material precursor was further carbonized under nitrogen protection at 1000 °C for 1 h, with a heating rate of 5 °C / min and a nitrogen flow rate of 100 mL / min, to obtain nano-iron compound / mesophase carbon microsphere composites.

[0039] Compared with the reaction without the addition of oil-soluble iron, the yield of carbon microspheres increased by 8 % and the D50 p...

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Abstract

The invention discloses a nano-iron compound / intermediate-phase carbon microsphere composite material and a preparation method thereof, in the composite material, a nano-iron compound is uniformly dispersed, coated or embedded in intermediate-phase carbon microspheres, and the mass fraction of the nano-iron compound is 0.1%-10%. The preparation method comprises the following steps: uniformly dispersing an oil-soluble iron precursor and a sulfur additive in asphalt, carrying out a thermal polymerization reaction under the conditions of proper temperature, pressure and inert atmosphere protection, separating a product to obtain a composite material precursor, and further carbonizing to prepare the nano iron compound / mesophase carbon microsphere composite material. The preparation method hasthe advantages that the oil-soluble iron precursor forms uniformly dispersed nanoparticles in situ, so that the formation of a high-quality mesophase carbon microsphere composite material is promoted,and the product yield and particle size can be regulated and controlled. The lithium ion battery negative electrode material prepared from the composite material has good electrochemical characteristics.

Description

technical field [0001] The invention relates to the technical field of preparation of micro-nano composite materials and negative electrode materials of lithium-ion batteries, in particular to a nano-iron compound / mesophase carbon microsphere composite material and a preparation method thereof. Background technique [0002] Mesocarbon microspheres are micron-sized spherical carbon materials with a nematic liquid crystal structure and a layered stacking structure. Magnification performance and other characteristics. However, the low specific capacity (300-350mAh / g) of mesocarbon microspheres is the key factor restricting its development. Iron oxides and iron sulfides in iron compounds have excellent lithium storage properties in the application of lithium-ion battery electrode materials, but the poor conductivity of iron compounds makes it difficult to fully utilize the active materials, and is prone to volume expansion during charge and discharge, causing structural damage....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/587H01M4/62H01M10/0525
CPCY02E60/10
Inventor 聂毅杜俊涛吕家贺郏慧娜郑双双
Owner 郑州中科新兴产业技术研究院
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