CN-121990548-A - Preparation method of controllable porous carbon based on super-crosslinked resin, porous carbon and application

CN121990548ACN 121990548 ACN121990548 ACN 121990548ACN-121990548-A

Abstract

The invention relates to a preparation method of adjustable porous carbon based on super-crosslinked resin, porous carbon and application thereof. The preparation method comprises the steps of taking low-crosslinked polystyrene resin with the crosslinking degree of 1-2% as a raw material, carrying out polymerization reaction in a chlorinated alkane solvent system under the action of a Lewis acid catalyst to obtain a super-crosslinked resin precursor, washing the super-crosslinked resin precursor, drying the super-crosslinked resin precursor to constant weight to obtain the super-crosslinked resin precursor after impurity removal, placing the super-crosslinked resin precursor after impurity removal in inert atmosphere for carbonization treatment, and cooling the super-crosslinked resin precursor to room temperature after the carbonization treatment is finished to obtain a porous carbon material, wherein the pore structure of the porous carbon material is regulated and controlled by regulating and controlling the crosslinking degree of the super-crosslinked resin precursor and the carbonization treatment temperature and time, and the crosslinking degree of the super-crosslinked resin precursor is regulated and controlled by the specific type of the Lewis acid catalyst, the polymerization reaction temperature and the dosage of the chlorinated alkane solvent corresponding to the low-crosslinked polystyrene resin per unit mass.

Inventors

ZHANG CHENYUAN
LI ZHI
LIU CHAO
YANG WEI
LIU BAINAN
LUO FEI

Assignees

溧阳天目先导电池材料科技有限公司

Dates

Publication Date: 20260508
Application Date: 20241104

Claims (10)

1. The preparation method of the controllable porous carbon based on the super-crosslinked resin is characterized by comprising the following steps of: Taking low-crosslinking polystyrene resin with the crosslinking degree of 1-2% as a raw material, and carrying out polymerization reaction in a chlorinated alkane solvent system under the action of a Lewis acid catalyst to prepare a precursor of the super-crosslinking resin; Washing the super-crosslinked resin precursor, and drying to constant weight to obtain the ultra-crosslinked resin precursor after impurity removal; placing the ultra-crosslinked resin precursor subjected to impurity removal in inert atmosphere for carbonization treatment, and cooling to room temperature after the carbonization treatment is finished to obtain a porous carbon material; The porous carbon material comprises a porous carbon material, a super-crosslinked resin precursor, a Lewis acid catalyst, a polymerization reaction temperature and a chlorinated alkane solvent, wherein the pore structure of the porous carbon material is regulated and controlled by regulating and controlling the crosslinking degree of the super-crosslinked resin precursor and the carbonization treatment temperature and time, and the crosslinking degree of the super-crosslinked resin precursor is regulated and controlled by the specific type of the Lewis acid catalyst, the polymerization reaction temperature and the consumption of the chlorinated alkane solvent corresponding to the low-crosslinked polystyrene resin in unit mass.
2. The preparation method according to claim 1, wherein the low crosslinked polystyrene resin with the crosslinking degree of 1-2% is specifically that divinylbenzene as a crosslinking agent is added in the process of preparing the polystyrene resin to account for 1-2% of the mass of the monomer.
3. The method of claim 1, wherein the lewis acid catalyst comprises one or more of ZnCl 2 、FeCl 3 、AlCl 3 ; the temperature of the polymerization reaction is 25-80 ℃, and the duration of the polymerization reaction is 6-48 h; The chlorinated alkane solvent comprises one or more of dichloromethane, dichloroethane, dichloropropane or 1, 2-dichloroethane.
4. The preparation method according to claim 1, wherein the addition amount of the chlorinated alkane solvent per gram of the low crosslinked polystyrene resin is 5-15 ml; The mass ratio of the low crosslinked polystyrene resin to the Lewis acid catalyst is 2:0.5-2:1.5.
5. The method according to claim 1, wherein the solvent used for washing comprises ethanol; The temperature of the drying is 100-120 ℃ and the time is 2-6 hours.
6. The method of claim 1, wherein the inert atmosphere comprises a nitrogen atmosphere or an argon atmosphere; the carbonization treatment specifically comprises the steps of heating to 600-1000 ℃ at a heating rate of 2-10 ℃ per minute, and preserving heat for 1-5 hours.
7. A porous carbon material prepared by the method for preparing a regulatable porous carbon based on a super cross-linked resin according to any one of claims 1 to 6.
8. A negative electrode material, characterized in that the negative electrode material comprises the porous carbon material according to claim 7.
9. A conductive additive, characterized in that, the conductive additive comprising the porous carbon material of claim 7.
10. A secondary battery comprising the porous carbon material according to claim 7.

Description

Preparation method of controllable porous carbon based on super-crosslinked resin, porous carbon and application Technical Field The invention relates to the technical field of porous carbon preparation, in particular to a preparation method of adjustable porous carbon based on super-crosslinked resin, porous carbon and application. Background Porous carbon is a type of carbon material with a highly developed pore structure, covering the types of activated carbon, carbon molecular sieves, carbon fibers, carbon aerogels, and the like. Porous carbon can be classified into micropores (< 2 nm), mesopores (2-50 nm) and macropores (> 50 nm) according to pore size. Because of excellent conductivity, high specific surface area, low density and chemical stability, the porous carbon has wide application prospect in the fields of energy storage and conversion (such as super capacitor and lithium ion battery), environmental management, petrochemical industry, biological medicine and the like. Currently, the preparation of porous carbon relies mainly on template and activation methods. Wherein the activation method comprises chemical activation and physical activation. The chemical activation method uses activating agents such as KOH, H 3PO4, znC l 2 and the like, so that a porous structure with developed pores can be obtained, but the preparation process has higher requirements on equipment and pollutant emission control. Physical activation is activated by CO 2 or water vapor, but requires high equipment and precursor quality. The template method is classified into a hard template method and a soft template method. The hard template method can realize a uniform pore structure, but the template removing process is complex and has high cost, and the soft template method regulates and controls the material structure through intermolecular force, and has the advantages of relatively simplified process, high reagent cost and difficult industrial popularization. Therefore, it is imperative to develop a method for preparing a porous carbon material in one step. In recent years, a top-down synthesis strategy is gradually rising, and the precise regulation and control of the pore structure are realized through the structural design of the precursor. For example, metal organic framework Materials (MOFs) can directly form porous carbon materials through high-temperature pyrolysis due to ordered pore structures. However, the complex synthesis process and high cost of MOFs limit their large-scale application. Another direction of investigation is through the co-carbonization of precursor composites, such as phenolic resins with arylboronic acids, using arylboronic acids as porogens. However, this method still requires acid or alkali washing to remove residual templates or inorganic salts on the process, adding to the complexity and cost of the process. Disclosure of Invention The invention aims at overcoming the defects in the prior art, and provides a preparation method of adjustable porous carbon based on super-crosslinked resin, the porous carbon and application. The method is based on the regulation and control of the crosslinking degree of the super-crosslinked resin precursor and the temperature time of the carbonization reaction, and the controllable design of the pore structure of the porous carbon can be realized through single-step carbonization reaction. To achieve the above object, in a first aspect, the present invention provides a method for preparing a regulatable porous carbon based on a super-crosslinked resin, comprising: Taking low-crosslinking polystyrene resin with the crosslinking degree of 1-2% as a raw material, and carrying out polymerization reaction in a chlorinated alkane solvent system under the action of a Lewis acid catalyst to prepare a precursor of the super-crosslinking resin; Washing the super-crosslinked resin precursor, and drying to constant weight to obtain the ultra-crosslinked resin precursor after impurity removal; placing the ultra-crosslinked resin precursor subjected to impurity removal in inert atmosphere for carbonization treatment, and cooling to room temperature after the carbonization treatment is finished to obtain a porous carbon material; The porous carbon material comprises a porous carbon material, a super-crosslinked resin precursor, a Lewis acid catalyst, a polymerization reaction temperature and a chlorinated alkane solvent, wherein the pore structure of the porous carbon material is regulated and controlled by regulating and controlling the crosslinking degree of the super-crosslinked resin precursor and the carbonization treatment temperature and time, and the crosslinking degree of the super-crosslinked resin precursor is regulated and controlled by the specific type of the Lewis acid catalyst, the polymerization reaction temperature and the consumption of the chlorinated alkane solvent corresponding to the low-crosslinked polystyrene resin in unit mass. Preferably, the