Preparation method of phenolic resin-based hard carbon microsphere material

A technology of phenolic resin and microspheres, which is applied in the field of electrochemistry, can solve the problems of high energy consumption, low output and yield, and long production cycle, and achieve the effects of simple operation, high yield, and low energy consumption

Active Publication Date: 2021-08-31
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, whether it is the hydrothermal method or the emulsion method, the preparation process of hard carbon microspheres is cumbersome, the production cycle is long, the output and yield are low, and the energy consumption is high, which is not suitable for large-scale production.

Method used

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  • Preparation method of phenolic resin-based hard carbon microsphere material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Pour 20g of phenol, 58g of water, 8.4g of polyvinyl alcohol with a molecular weight of 77000, and 32wt.% sodium hydroxide solution (NaOH:phenol=1:5, mol ratio) into a three-necked flask, and stir at 92°C for 15min Raise the temperature to 95° C., add 20 g of formaldehyde and stir for 1 h, then add 5 g of formaldehyde and continue stirring for 100 min to obtain a liquid resole resin. The obtained phenolic resole resin was placed in a large beaker, a certain amount of distilled water was added thereto and stirred at room temperature for 2 hours to form a cloudy solution of phenolic resin with a solid content of 3 wt%.

[0030] The cloudy phenolic resin solution was spray-dried under stirring to obtain powdered phenolic resin microspheres. The inlet temperature was set at 120°C and the material flow rate was set at 400mL / h.

[0031] The powdered phenolic resin microspheres were placed in an oven at a constant temperature of 150° C. for 20 h for pre-oxidation to obtain pre-...

Embodiment 2

[0034]Pour 20g of phenol, 58g of water, 8.4g of polyvinyl alcohol with a molecular weight of 77000, and 32wt.% sodium hydroxide solution (NaOH:phenol=1:5, mol ratio) into a three-necked flask, and stir at 92°C for 15min Raise the temperature to 95° C., add 20 g of formaldehyde and stir for 1 h, then add 5 g of formaldehyde and continue stirring for 100 min to obtain a liquid resole resin. The obtained phenolic resole resin was placed in a large beaker, a certain amount of distilled water was added thereto and stirred at room temperature for 2 hours to form a cloudy solution of phenolic resin with a solid content of 3 wt%.

[0035] The cloudy phenolic resin solution was spray-dried under stirring to obtain powdered phenolic resin microspheres. The inlet temperature was set at 180°C and the material flow rate was set at 600mL / h.

[0036] The powdered phenolic resin microspheres were placed in an oven at a constant temperature of 150° C. for 20 h for pre-oxidation to obtain pre-o...

Embodiment 3

[0039] Pour 40g of phenol, 116g of water, 16.8g of polyvinyl alcohol with a molecular weight of 77,000, and 32wt.% sodium hydroxide solution (NaOH:phenol=1:5, mol ratio) into a three-necked flask, and stir at 92°C for 15min Raise the temperature to 95° C., add 40 g of formaldehyde and stir for 1 h, then add 10 g of formaldehyde and continue stirring for 100 min to obtain a liquid resol resin. The obtained phenolic resole resin was placed in a large beaker, a certain amount of distilled water was added thereto and stirred at room temperature for 2 hours to form a cloudy solution of phenolic resin with a solid content of 3 wt%.

[0040] The cloudy phenolic resin solution was spray-dried under stirring to obtain powdered phenolic resin microspheres. The inlet temperature was set at 120°C and the material flow rate was set at 400mL / h.

[0041] The powdered phenolic resin microspheres were placed in an oven at a constant temperature of 150° C. for 20 h for pre-oxidation to obtain p...

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Abstract

The invention discloses a preparation method of a phenolic resin-based hard carbon microsphere material. The preparation method comprises the following steps: (1) subjecting a phenol monomer to reacting with an aldehyde monomer to obtain a liquid phenolic resin oligomer; (2) preparing a phenolic resin emulsion; (3) carrying out spray drying on the phenolic resin emulsion in a stirring state to obtain phenolic resin microspheres; (4) pre-oxidizing the phenolic resin microspheres; and (5) carbonizing the pre-oxidized phenolic resin microspheres to obtain the phenolic resin-based hard carbon microsphere material. According to the preparation method, the phenolic resin emulsion is treated by using a spray drying step and a pre-oxidation method for the first time, and the preparation method has the potential of industrial production. The method provided by the invention provides a new thought for preparation of the carbon microsphere material.

Description

technical field [0001] The invention belongs to the field of electrochemistry, and in particular relates to a preparation method of a phenolic resin-based hard carbon microsphere material. Background technique [0002] At present, coal, oil and natural gas are still the main energy sources that people rely on. However, the large-scale development and use of these non-renewable fossil energy sources will cause environmental pollution and damage, which requires people to develop and use renewable energy such as solar energy, wind energy, and tidal energy. Renewable clean energy sources; these clean energy sources are often intermittent and regional and cannot be used on a large scale. In order to solve this problem, building large-scale energy storage devices and energy transmission systems is a very feasible solution, which promotes the development of energy storage devices. Lithium-ion batteries are favored by consumers due to their high energy density, long cycle life, and...

Claims

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Application Information

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IPC IPC(8): C01B32/05C08L61/10C08L61/12C08L29/04C08L29/14C08L71/02C08G8/10C08G8/22C08G8/20C08J3/12
CPCC01B32/05C08G8/10C08G8/22C08G8/20C08J3/122C08J2361/10C08J2361/12C08J2429/04C08J2429/14C08J2471/02Y02E60/10
Inventor 时志强张丽君任庆娟
Owner TIANJIN POLYTECHNIC UNIV
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