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CN-121975351-A - Preparation method of high-specific-surface conductive carbon black

CN121975351ACN 121975351 ACN121975351 ACN 121975351ACN-121975351-A

Abstract

The invention relates to the technical field of carbon material preparation and modification, in particular to a preparation method of high-specific surface conductive carbon black. The preparation method comprises the steps of heating raw material carbon black to 350-550 ℃ for first heat treatment under a protective atmosphere, heating to 800-950 ℃ for second heat treatment, continuously heating to 1300-1600 ℃ for third heat treatment to obtain intermediate carbon black, and sequentially performing steam activation and carbon dioxide activation on the intermediate carbon black to obtain the high-specific-surface conductive carbon black, wherein the steam activation temperature is 850-950 ℃, and the carbon dioxide activation temperature is 900-1000 ℃. According to the invention, impurities are removed and a carbon skeleton is rearranged through gradient heat treatment, and then the micropore and mesoporous structure is cooperatively regulated and controlled by utilizing physical activation of water vapor and CO 2 , so that the high specific surface and high conductivity are realized.

Inventors

  • YANG BINGJUN
  • LIU JINPENG
  • ZHANG XU
  • YANG JUAN
  • MA PENGJUN

Assignees

  • 中国科学院兰州化学物理研究所

Dates

Publication Date
20260505
Application Date
20260129

Claims (10)

  1. 1. The preparation method of the high-specific-surface conductive carbon black is characterized by comprising the following steps of: Under a protective atmosphere, heating the raw material carbon black to 350-550 ℃ for first heat treatment, heating the raw material carbon black to 800-950 ℃ for second heat treatment, and continuing heating the raw material carbon black to 1300-1600 ℃ for third heat treatment to obtain intermediate carbon black; And sequentially carrying out steam activation and carbon dioxide activation on the intermediate carbon black to obtain the high-specific-surface conductive carbon black, wherein the steam activation temperature is 850-950 ℃, and the carbon dioxide activation temperature is 900-1000 ℃.
  2. 2. The preparation method according to claim 1, wherein the heat preservation time of the first heat treatment is 0.5-1.5 h.
  3. 3. The method according to claim 1, wherein the second heat treatment is performed for a holding time of 1 to 2 hours.
  4. 4. The preparation method according to claim 1, wherein the third heat treatment is performed for a heat preservation time of 1 to 3 hours.
  5. 5. The method according to claim 1, wherein the water vapor activation is performed for a period of 0.5 to 2 hours.
  6. 6. The preparation method according to claim 1, wherein the flow rate of the water vapor is 0.5-5.0L/min when the water vapor is activated.
  7. 7. The method according to claim 1, 5 or 6, wherein the water vapor is introduced by a carrier gas during the activation of the water vapor.
  8. 8. The method according to claim 1, wherein the flow rate of carbon dioxide is 0.2-0.6L/min when the carbon dioxide is activated.
  9. 9. The method according to claim 1 or 8, wherein the carbon dioxide activation is performed for a period of 2 to 4 hours.
  10. 10. The method of claim 1, wherein the high specific surface area of the conductive carbon black is >500 m 2 /g and the average resistivity is <0.2 Ω -cm.

Description

Preparation method of high-specific-surface conductive carbon black Technical Field The invention relates to the technical field of carbon material preparation and modification, in particular to a preparation method of high-specific surface conductive carbon black. Background The conductive carbon black is a carbonaceous filler commonly used for improving the conductive performance of materials, and has the advantages of low cost, good stability, strong processability and the like. However, the traditional conductive carbon black is mostly prepared by adopting an oil furnace method, a groove method or an acetylene cracking method, the microstructure of the conductive carbon black mainly comprises amorphous carbon and a small amount of disordered layer graphite, the specific surface area is limited (about 30-80 m 2/g), the micropore development is insufficient, and the carbon skeleton structure is disordered, so that the electron conduction path is discontinuous, thereby limiting the application of the conductive carbon black in high-energy-density energy storage devices. Disclosure of Invention In view of the above, the invention aims to provide a preparation method of high-specific-surface conductive carbon black, which has high specific surface area and excellent conductive performance and can meet the requirements of the field of new energy materials for high-performance conductive fillers. In order to achieve the above object, the present invention provides the following technical solutions: the invention provides a preparation method of high-specific-surface conductive carbon black, which comprises the following steps: Under a protective atmosphere, heating the raw material carbon black to 350-550 ℃ for first heat treatment, heating the raw material carbon black to 800-950 ℃ for second heat treatment, and continuing heating the raw material carbon black to 1300-1600 ℃ for third heat treatment to obtain intermediate carbon black; And sequentially carrying out steam activation and carbon dioxide activation on the intermediate carbon black to obtain the high-specific-surface conductive carbon black, wherein the steam activation temperature is 850-950 ℃, and the carbon dioxide activation temperature is 900-1000 ℃. Preferably, the heat preservation time of the first heat treatment is 0.5-1.5 h. Preferably, the heat preservation time of the second heat treatment is 1-2 h. Preferably, the heat preservation time of the third heat treatment is 1-3 h. Preferably, the heat preservation time of the water vapor activation is 0.5-2 h. Preferably, the flow rate of the water vapor is 0.5-5.0L/min during the water vapor activation. Preferably, the water vapor is introduced by a carrier gas during the activation of the water vapor. Preferably, when the carbon dioxide is activated, the flow rate of the carbon dioxide is 0.2-0.6L/min. Preferably, the carbon dioxide activation heat preservation time is 2-4 hours. Preferably, the specific surface area of the high-specific surface conductive carbon black is more than 500 m 2/g, and the average resistivity is less than 0.2 ohm cm. The invention provides a preparation method of high-specific-surface-area conductive carbon black, which comprises the following steps of heating raw material carbon black to 350-550 ℃ for first heat treatment under a protective atmosphere, heating to 800-950 ℃ for second heat treatment, continuously heating to 1300-1600 ℃ for third heat treatment to obtain intermediate carbon black, and sequentially performing steam activation and carbon dioxide activation on the intermediate carbon black to obtain the high-specific-surface-area conductive carbon black, wherein the steam activation temperature is 850-950 ℃, and the carbon dioxide activation temperature is 900-1000 ℃. According to the method, oxygen-containing functional groups on the surface of raw material carbon black are removed through first heat treatment, carbon skeleton rearrangement and structure densification are promoted through second heat treatment, high-temperature graphitization is completed through third heat treatment, conductive continuity of a carbon layer is improved, the surface layer of the carbon black is slightly gasified through steam activation, a uniform micropore structure is generated, the specific surface area is improved, micropores are further widened through carbon dioxide activation to form mesopores, pore size distribution is optimized (electron-ion cooperative transmission is facilitated), the specific surface area is improved, and finally the combination of high specific surface area and high conductivity is achieved. The results of the examples show that the specific surface area of the high-specific surface conductive carbon black prepared by the invention is more than 500m 2/g, and the average resistivity is less than 0.2 omega cm. In addition, the invention adopts double physical activation of water vapor and carbon dioxide, compared with the traditional meth