Lignin hard carbon microsphere, hydrothermal preparation method and alkali metal ion battery negative electrode using lignin hard carbon microspheres

A technology of lignin and microspheres, applied in battery electrodes, active material electrodes, negative electrodes, etc., can solve the problems of low initial charge and discharge efficiency, small capacity of negative electrode materials, and low yield of carbon materials, and achieve stable cycle performance. The effect of good sphericity and high preparation efficiency

Inactive Publication Date: 2020-02-14
TIANJIN UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

For example, when lignin is used as a precursor to directly carry out carbonization heat treatment to prepare carbon materials, it mainly occurs in the process of dehydration, thermal cracking and polycondensation aromatization. The prepared carbon materials have low yield, large specific surface area, and developed pores. The prepared negative electrode materials Small capacity, low initial charge and discharge efficiency

Method used

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  • Lignin hard carbon microsphere, hydrothermal preparation method and alkali metal ion battery negative electrode using lignin hard carbon microspheres
  • Lignin hard carbon microsphere, hydrothermal preparation method and alkali metal ion battery negative electrode using lignin hard carbon microspheres
  • Lignin hard carbon microsphere, hydrothermal preparation method and alkali metal ion battery negative electrode using lignin hard carbon microspheres

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Example 1: Add 2 g of sodium lignosulfonate powder into 60 mL of deionized water, and stir until it is completely dissolved to obtain a neutral lignin solution with a solid content of about 3%. Transfer the above prepared lignin solution to a 100mL reaction kettle and seal it. The temperature of the reaction kettle was raised to 250° C., and after 12 hours of holding time, the temperature was naturally lowered to room temperature. After taking out, the hydrothermal reaction product is centrifuged to obtain the bottom sediment; continue to dry in an air blast oven at 80°C to obtain lignin hydrothermal microspheres. The scanning electron micrograph of the figure 1 shown. Depend on figure 1 It can be seen that spherical lignin particles are obtained, the surface of the particle sphere is smooth, and the particle size is 2-3 μm. Put the lignin hydrothermal microspheres in a corundum crucible and put them into a high-temperature tube furnace, raise the temperature to 900...

Embodiment 2

[0042] Example 2: Take 2g of sodium lignosulfonate powder and add it into 60mL of deionized water, and stir until it is completely dissolved to obtain a lignin solution. Add 20mL of 2mol / L sodium hydroxide solution to obtain an alkaline solution with a solid content of 3%. Transfer the alkaline lignin solution prepared above to a hydrothermal reaction kettle with a volume of 100mL, and seal it. The temperature of the reaction kettle was raised to 250° C., and after 12 hours of holding time, the temperature was naturally lowered to room temperature. After taking it out, the solution was centrifuged, and the sediment at the bottom was taken, and dried in a blast oven at 80°C to obtain lignin hydrothermal gel microspheres; its scanning electron micrograph is shown in figure 2 As shown, the particles are spherical, the primary particle size is less than 1 μm, and there is a small amount of fusion and agglomeration. Put the lignin hydrothermal gel microspheres in a corundum cruc...

Embodiment 3

[0043] Example 3: Take 2g of sodium lignosulfonate powder and add it into 60mL of deionized water, and stir until it is completely dissolved to obtain a lignin solution. Then add 20 mL of 1mol / L hydrochloric acid solution to obtain an acidic solution with a solid content of 3%. Transfer the lignin solution prepared above to a hydrothermal reaction kettle with a volume of 100mL, and seal it. The temperature of the reaction kettle was gradually raised to 250°C, and after holding for 60 hours, the temperature was naturally lowered to room temperature. After taking it out, the solution is centrifuged, and the sediment at the bottom is taken, and dried in an air blast oven at 80° C. to obtain lignin hydrothermal microspheres. Put the lignin hydrothermal microspheres in a corundum crucible and put them into a high-temperature tube furnace, raise the temperature to 900°C at a heating rate of 5°C / min, and carbonize at 900°C for 3 hours under the protection of nitrogen to obtain 900°C...

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Abstract

The invention relates to a lignin hard carbon microsphere, a hydrothermal preparation method and an alkali metal ion battery negative electrode using the lignin hard carbon microspheres. Lignin is used as a precursor, and the lignin carbon microspheres are prepared by adopting a hydrothermal method. Lignin is firstly dissolved in water under full stirring to obtain a lignin solution; hydrothermalreaction is directly carried out on the lignin solution or the hydrothermal reaction is carried out after acid and alkali are added to adjust the pH value of the solution to obtain a lignin hydrothermal microsphere precursor; and after drying, the lignin microspheres are put into a tubular furnace, and high-temperature carbonization is carried out under the protection of inert gas to obtain the lignin carbon microspheres. The lignin carbon microsphere is high in sphericity degree, less in adhesion condition, good in structural stability, good in dispersity and capable of keeping a high-dispersion state. Low-cost process synthesis of industrial waste lignin hydrothermal balling is studied, and the industrial waste lignin hydrothermal balling is successfully applied to a negative electrode material of an alkali metal ion battery and high capacity, good rate charge and discharge performance and cycling stability are shown.

Description

technical field [0001] The invention belongs to the technical field of alkali metal (Li / Na / K) ion battery anode materials, and in particular relates to a preparation method of low-cost lignin carbon microspheres with a hard carbon structure and high sphericity and the preparation method thereof in alkali metal (Li / Na / K) ion batteries. / Na / K) ion battery negative electrode applications. Background technique [0002] In the past few decades, social development has been heavily dependent on fossil energy, which has led to serious pollution of the environment, such as the greenhouse effect, smog, etc. Scientists from all over the world continue to develop green energy (solar energy, wind energy, tidal energy, etc.) to replace fossil energy to reduce environmental burdens and meet the energy needs of social development. But the utilization of these new energy sources is limited because of their regionality and intermittency. These reasons have promoted the research and developm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/583H01M10/0525H01M10/054
CPCH01M4/583H01M10/0525H01M10/054H01M2004/027H01M2004/021Y02E60/10
Inventor 樊丽萍于涛谭欣
Owner TIANJIN UNIV
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