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Phenol formaldehyde resin carbon micro-sphere preparation method and application of phenol formaldehyde resin carbon micro-sphere in lithium ion battery electrode

A technology of phenolic resin and carbon microspheres, applied in battery electrodes, circuits, electrical components, etc., can solve the problems of difficult control of particle size, harsh synthesis conditions, complex synthesis equipment, etc., and achieve controllable particle size, good shape, The effect of simplifying the synthesis process

Inactive Publication Date: 2014-01-29
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the phenolic resin microspheres prepared by the synthesis system of phenol and formaldehyde through suspension polymerization, emulsion polymerization and other synthesis methods have large particle size (above 10um), The particle size distribution is wide and the particle size is difficult to control. For example, Arjun Singh et al. used phenol, formaldehyde, triethylamine, PVA, and HMTA synthesis systems to obtain phenolic resin glass balls with a particle size of 0.1 to 2.0 mm through suspension polymerization [Singh Arjun , Yadav Rakesh Kumar, Srivastava Anurag. Synthesis of Resole-Type Phenolic Beads from Phenol and Formaldehyde by Suspension Polymerization Technique [J]. Polym. Adv. Technol., DOI 10.1002 / app.29480:1005-1011.]
Zhong Hong et al. used phenol, formaldehyde and sodium hydroxide system to obtain hollow / porous phenolic resin microspheres with a particle size of 10-60um through O / W / O multiphase emulsion polymerization [Zhou Hong, Huang Guangsu, Gao Pin, Long Chengqun . Preparation of porous / hollow particles of phenolic resin [J]. Polym. Adv. Technol., 2007, 18: 582–585.], in addition, the above synthesis method also has the disadvantages of complex synthesis equipment, harsh synthesis conditions and high cost

Method used

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  • Phenol formaldehyde resin carbon micro-sphere preparation method and application of phenol formaldehyde resin carbon micro-sphere in lithium ion battery electrode
  • Phenol formaldehyde resin carbon micro-sphere preparation method and application of phenol formaldehyde resin carbon micro-sphere in lithium ion battery electrode
  • Phenol formaldehyde resin carbon micro-sphere preparation method and application of phenol formaldehyde resin carbon micro-sphere in lithium ion battery electrode

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 Mix 5g of phenol, 8.62ml of formaldehyde solution, and 0.106g of sodium hydroxide in a molar ratio of 1:2:0.05 and add them into a 100ml three-necked flask, and react at 60°C for 12h to obtain the first mixed solution. Mix 2ml of the first mixed solution (adjusted to pH 4) and 30ml of vegetable oil at a volume ratio of 1:15, then add a nonionic surfactant with a volume fraction of 0.06 and mix evenly to obtain the second mixed solution, and stir the second mixed solution at room temperature After the emulsification treatment, put it into a blast oven at 100° C. to react for 12 hours to obtain a reaction product, which was centrifuged and washed with acetone to obtain phenolic resin microspheres.

[0029] Under an inert atmosphere, heat the phenolic resin balls at 700°C for 4 hours to obtain phenolic resin carbon microspheres.

[0030] Utilize scanning electron microscope to analyze the phenolic resin microsphere that obtains in embodiment 1 namely carbon micro...

Embodiment 2

[0035] Example 2 Mix 5 g of phenol, 4.31 ml of formaldehyde solution, and 1.704 g of sodium hydroxide in a molar ratio of 1:1:0.8 and add them into a 100 ml three-necked flask, and react at 30°C for 24 hours to obtain the first mixed solution. Mix 2ml of the first mixed solution (adjusted to pH 7) and 30ml of vegetable oil at a volume ratio of 1:15, then add a nonionic surfactant with a volume fraction of 0.06 and mix evenly to obtain the second mixed solution, and stir the second mixed solution at room temperature After the emulsification treatment, put it into a blast oven at 150° C. to react for 12 hours to obtain a reaction product, which was centrifuged and washed with acetone to obtain phenolic resin microspheres.

[0036] Under an inert atmosphere, heat the phenolic resin balls at 700°C for 4 hours to obtain phenolic resin carbon microspheres.

Embodiment 3

[0037] Example 3 Mix 5 g of phenol, 17.25 ml of formaldehyde solution, and 0.0022 g of sodium hydroxide in a molar ratio of 1:4:0.001 and add them into a 100 ml three-necked flask, and react at 200° C. for 1 hour to obtain the first mixed solution. Mix 2ml of the first mixed solution (adjusted to pH 7) and 30ml of vegetable oil at a volume ratio of 1:15, then add a nonionic surfactant with a volume fraction of 0.06 and mix evenly to obtain the second mixed solution, and stir the second mixed solution at room temperature After the emulsification treatment, put it into a blast oven at 90° C. to react for 12 hours to obtain a reaction product, which was centrifuged and washed with acetone to obtain phenolic resin microspheres.

[0038] Under an inert atmosphere, heat the phenolic resin balls at 700°C for 5 hours to obtain phenolic resin carbon microspheres.

[0039] The particle size test of the phenolic resin microsphere obtained in embodiment 3, its average diameter is 3um, and t...

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Abstract

The invention provides a phenol formaldehyde resin carbon micro-sphere preparation method. The phenol formaldehyde resin carbon micro-sphere preparation method comprises the following steps: firstly preparing phenol formaldehyde resin micro-spheres under an emulsion polymerization condition, then carrying out carbonization treatment to obtain the phenol formaldehyde resin carbon micro-spheres with the average particle size diameter being 1-6 micrometers, which have good morphology and small particle sizes and are uniform in particle size distribution. When serving as lithium ion battery negative electrode materials, the phenol formaldehyde resin carbon micro-spheres with the small particle sizes, which are synthesized by using the method, show high reversible capacity and rate capability; the specific discharge capacity of the phenol formaldehyde resin carbon micro-spheres is 350mAh / g-190mAh / g at 50mA / g-1A / g.

Description

technical field [0001] The invention relates to the application field of lithium-ion battery electrode materials, in particular to a phenolic resin carbon microsphere, a preparation method and an application in lithium-ion battery negative electrode materials. Background technique [0002] Polymer-based carbon microspheres have the same electrical and thermal conductivity as metals, have the same corrosion resistance and heat resistance as ceramics, have the same molecular structure as organic polymers, light weight, and have low density and good chemical stability. , Good biocompatibility and so on. The isotropy of the spherical sheet of polymer-based carbon microspheres is conducive to the intercalation and extraction of lithium ions from all directions, which solves the problems of volume expansion and collapse caused by the intercalation and extraction of lithium ions in anisotropic electrode materials, and its smooth surface is conducive to Improve the first Coulombic ...

Claims

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Application Information

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IPC IPC(8): H01M4/583H01M4/62
CPCH01M4/604Y02E60/10
Inventor 宋怀河吴清霞陈晓红
Owner BEIJING UNIV OF CHEM TECH
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