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CN-122010084-A - Compact porous carbon material and preparation method and application thereof

CN122010084ACN 122010084 ACN122010084 ACN 122010084ACN-122010084-A

Abstract

The invention relates to a compact porous carbon material, a preparation method and application thereof. The preparation method comprises the steps of adding a surfactant, a carbon source material and a template raw material into a solvent, uniformly mixing, performing spray drying treatment to obtain a mixed precursor, performing low-temperature pre-carbonization treatment on the mixed precursor in an inert atmosphere at 300-600 ℃ to obtain a pre-carbonized material, crushing and grading the pre-carbonized material, performing etching treatment on the crushed and graded material by using an etching agent, cleaning and drying to obtain a porous carbon precursor, performing secondary carbonization treatment on the porous carbon precursor at 700-1100 ℃, and cooling and discharging to obtain the compact porous carbon material. According to the preparation method, the surfactant is introduced into the precursor to optimize the distribution of the carbon source in the template material, and the densification of the carbon layer and the regulation and control of the pore structure are gradually realized through the three steps of low-temperature pre-carbonization, etching and high-temperature carbonization and the control of technological parameters, so that cracks in particles are avoided, and the mechanical strength and the structural stability of the material are improved.

Inventors

  • 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
20260512
Application Date
20241112

Claims (10)

  1. 1. A method for preparing a dense porous carbon material, the method comprising: adding a surfactant, a carbon source material and a template raw material into a solvent, uniformly mixing, and then performing spray drying treatment to obtain a mixed precursor; Carrying out low-temperature pre-carbonization treatment on the mixed precursor in an inert atmosphere at 300-600 ℃ to obtain a pre-carbonized material; Crushing and grading the pre-carbonized material; etching the crushed and graded material by using an etchant, and cleaning and drying to obtain a porous carbon precursor; and (3) carrying out secondary carbonization treatment on the porous carbon precursor at 700-1100 ℃ in inert atmosphere, and cooling and discharging to obtain the compact porous carbon material.
  2. 2. The preparation method according to claim 1, wherein the surfactant comprises one or more of polyoxyethylene polyoxypropylene ether Pluronic F127, cetyltrimethylammonium bromide CTAB, sodium dodecyl sulfate SDS, and polyethylene glycol PEG; The carbon source material comprises one or more of glucose, corn starch, glycerol, fructose, maltose, sucrose, phenolic resin, polyvinyl alcohol PVA, polyethylene terephthalate PET and asphalt; the template raw materials comprise one or more of magnesium citrate, magnesium gluconate, magnesium acetate, magnesium glycinate, polymethylphenylsiloxane PMPS and polyphenyl silsesquioxane PPSSO; the solvent comprises water or ethanol.
  3. 3. The preparation method according to claim 1, wherein the mass ratio of the surfactant, the carbon source material and the template raw material is 1:2-5:1-10; the mixing specifically comprises stirring and mixing, wherein the stirring speed is 400-1000rpm, the stirring temperature is 25-80 ℃, and the stirring time is 12-24 hours; in the spray drying treatment, the temperature of an air inlet is 150-180 ℃, the temperature of an air outlet is 70-90 ℃, and the frequency of an atomizer is 220Hz.
  4. 4. The method according to claim 1, wherein the low-temperature pre-carbonization treatment equipment comprises one or more of a tube furnace, an atmosphere furnace, a rotary furnace and a box furnace; the low-temperature pre-carbonization treatment time is 1-4 hours, and the temperature rising rate is 1-5 ℃ per minute; the inert atmosphere is argon atmosphere or nitrogen atmosphere.
  5. 5. The preparation method according to claim 1, wherein after the crushing and classification treatment, the particle size parameters of the obtained material are D00 is more than or equal to 1 μm, D10 is more than or equal to 3 μm, D50 is more than or equal to 7 μm-15 μm, D90 is less than or equal to 50 μm, and D99 is less than or equal to 90 μm.
  6. 6. The method according to claim 1, wherein the etchant comprises one or more of HCl, H 2 SO 4 、HNO 3 , HF, KOH and NaOH having a solution concentration of 0.1-5 mol/L; the etching treatment time is 2-8h, and the etching treatment temperature is 25-80 ℃; the cleaning is water washing; The drying equipment comprises one or more of a blast oven, a vacuum oven, a tunnel oven and a rotary drum dryer; The drying temperature is 70-110 ℃ and the drying time is 8-20h.
  7. 7. The method according to claim 1, wherein the secondary carbonization treatment is carried out for 1 to 3 hours at a temperature rising rate of 1 to 5 ℃.
  8. 8. A dense porous carbon material prepared by the method of any one of claims 1-7.
  9. 9. The dense porous carbon material of claim 8, wherein the dense porous carbon material has a mesoporosity of not less than 40% and a compressive strength of not less than 5MPa.
  10. 10. Use of the dense porous carbon material of claim 8, wherein the dense porous carbon material is used for an electrode material of a lithium ion battery, an electrode material of a supercapacitor or a fuel cell catalyst support.

Description

Compact porous carbon material and preparation method and application thereof Technical Field The invention relates to the technical field of new energy materials, in particular to a compact porous carbon material, a preparation method and application thereof. Background In modern material science, the porous carbon material is widely applied to the fields of catalysis, adsorption, energy storage, sensors and the like, in particular to the fields of lithium ion battery electrode materials, super capacitors, electrocatalyst support materials and the like due to excellent electrochemical performance, good conductivity, high specific surface area and porous structure. Conventional porous carbon material preparation methods generally include a pyrolysis process, which easily causes cracks to occur inside the material, thereby affecting mechanical strength and structural stability thereof. Therefore, how to effectively prevent the generation of cracks becomes an important challenge in the current porous carbon material preparation field. In the prior art, various methods have been proposed to solve this problem. For example, chinese patent document CN114933294a discloses a "high bulk density multi-layer dense porous carbon nanoplatelet and a preparation method", which prepares a dense porous carbon nanoplatelet having a high specific surface area and excellent electrochemical properties by dispersing two-dimensional Layered Double Hydroxide (LDH), mixing with a carbon precursor and an activator, calcining, and post-treating. However, the method is still easy to crack in the high-temperature treatment process, and the preparation process is relatively complex and has high cost. In the preparation method of the porous carbon material, the hard template method is one of effective methods for preparing the dense porous carbon material because the pore diameter and the pore structure can be accurately controlled. The hard template method generally employs an inorganic material (e.g., silica, alumina, etc.) as a template, and forms a carbon material in the surface or pores thereof. However, the conventional hard template method has some drawbacks in practical applications, such as difficulty in removing the template material, insufficient uniformity or densification of the pore structure of the carbon material, etc., resulting in poor stability and reproducibility of material properties, and the problem of internal cracks of the material due to the pyrolysis process is not substantially solved. Disclosure of Invention Aiming at the defects existing in the prior art, the invention provides a compact porous carbon material, a preparation method and application thereof, and the surfactant, the carbon source and the hard template are added, and the optimized low-temperature pre-carbonization, etching process and secondary carbonization treatment are combined, so that the generation of cracks in the material in the pyrolysis process can be obviously reduced, and the mesoporous rate and the pressure resistance of the material are improved. In order to achieve the above object, the present invention provides a method for preparing a dense porous carbon material, comprising: adding a surfactant, a carbon source material and a template raw material into a solvent, uniformly mixing, and then performing spray drying treatment to obtain a mixed precursor; Carrying out low-temperature pre-carbonization treatment on the mixed precursor in an inert atmosphere at 300-600 ℃ to obtain a pre-carbonized material; Crushing and grading the pre-carbonized material; etching the crushed and graded material by using an etchant, and cleaning and drying to obtain a porous carbon precursor; and (3) carrying out secondary carbonization treatment on the porous carbon precursor at 700-1100 ℃ in inert atmosphere, and cooling and discharging to obtain the compact porous carbon material. Preferably, the surfactant comprises one or more of polyoxyethylene polyoxypropylene ether (Pluronic F127), cetyltrimethylammonium bromide (CTAB), sodium Dodecyl Sulfate (SDS), polyethylene glycol (PEG); The carbon source material comprises one or more of glucose, corn starch, glycerol, fructose, maltose, sucrose, phenolic resin, polyvinyl alcohol (PVA), polyethylene terephthalate (PET) and asphalt; the template raw materials comprise one or more of magnesium citrate, magnesium gluconate, magnesium acetate, magnesium glycinate, polymethylphenylsiloxane (PMPS, polymethylphenylsiloxane) and polyphenyl silsesquioxane (PPSSO, polyphenylsilsesquioxane); the solvent comprises water or ethanol. Preferably, the mass ratio of the surfactant to the carbon source material to the template raw material is 1:2-5:1-10; the mixing specifically comprises stirring and mixing, wherein the stirring speed is 400-1000rpm, the stirring temperature is 25-80 ℃, and the stirring time is 12-24 hours; in the spray drying treatment, the temperature of an air inlet is 150-180 ℃, the temperature of