Graphitized carbon-based adsorption material as well as preparation method and application thereof

An adsorption material and graphitization technology, applied in chemical instruments and methods, separation methods, other chemical processes, etc., can solve the problems of affecting the selectivity and adsorption recovery rate of target compounds, increasing the content of metal elements, and complex preparation processes. The effect of low energy cost, low preparation temperature and simple preparation process

Pending Publication Date: 2022-04-05
光大理工环境技术研究院(青岛)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this type of method can be carried out at a relatively low temperature, the preparation process is complicated and the efficiency is low, and the use of a catalyst will increase the content of metal elements in the material, which will seriously affect the selectivity and adsorption recovery of the target when used as an adsorbent. Rate

Method used

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  • Graphitized carbon-based adsorption material as well as preparation method and application thereof
  • Graphitized carbon-based adsorption material as well as preparation method and application thereof
  • Graphitized carbon-based adsorption material as well as preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0026] Weigh 10g of thermoplastic phenol-formaldehyde resin in a vacuum tube furnace, heat continuously at a rate of 10°C / min to 1200°C under nitrogen, keep the temperature for 3 hours, and continuously lower it to room temperature at a rate of 10°C / min to obtain 5g of crude product , Grinding and sieving to obtain 50-60 mesh black granular products.

[0027] The prepared carbon material has a specific surface area of ​​100m 2 / g, using X-ray diffraction to observe the structure of materials, see figure 1 ,Depend on figure 1 It can be seen that after the carbon material is heat-treated, the diffraction peaks at 2θ=25.5° and 43.2° are the diffraction peaks of the C(002) and C(100) crystal planes, indicating that the interplanar distance d(002) of the (002) crystal plane decreases Small, the degree of ordering and graphitization of carbon materials increases.

Embodiment 2

[0029] Weigh 20g of thermoplastic phenol-formaldehyde resin in a vacuum tube furnace, heat continuously at a rate of 5°C / min to 1400°C under argon gas, keep the temperature for 2 hours, and then cool down to room temperature at a rate of 20°C / min to obtain the crude product 9.0g, grinded and sieved to obtain 60-80 mesh black granular products.

[0030] The prepared carbon material has a specific surface area of ​​20m 2 / g, using scanning electron microscopy to observe the structure of the material, see figure 2 ,Depend on figure 2 It can be seen that an obvious graphitized sheet structure appears on the surface of the carbon material, indicating that high-temperature heat treatment improves the degree of ordering of the carbon material, and the appearance of concentric rings indicates that the material has a high degree of graphitization after high-temperature treatment.

Embodiment 3

[0032] Weigh 5g of thermoplastic phenol-formaldehyde resin in a vacuum tube furnace, heat it up to 1600°C at a rate of 20°C / min under nitrogen, and then cool it down to room temperature at a rate of 30°C / min for 1 hour. The obtained crude product is 2.0 g, after grinding and sieving to obtain 80-100 mesh black granular products.

[0033] The prepared carbon material has a specific surface area of ​​10m 2 / g, nitrogen adsorption / desorption isotherm diagram see image 3 . According to the calculation of the isotherm, the specific surface area of ​​the carbon material reaches 10m after high-temperature heat treatment. 2 / g.

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Abstract

The invention discloses a graphitized carbon-based adsorption material and a preparation method thereof. The preparation method comprises the following steps: placing phenolic resin under the protection of inert gas, continuously heating to 1200-1600 DEG C at a certain rate, continuously heating at constant temperature, carrying out high-temperature anaerobic carbonization, cooling to room temperature, crushing, and sieving to obtain a black granular product. The method adopts the thermoplastic phenol-formaldehyde resin as the unique raw material, does not need any additive, is lower in preparation temperature, avoids the defects of high preparation temperature, serious energy consumption, high metal content and the like in the traditional method, is simple in preparation process, and is suitable for industrial large-scale preparation; the prepared graphitized carbon-based adsorption material can replace a commercially available graphitized carbon black material recommended in the determination isotope dilution high-resolution gas chromatography-high-resolution mass spectrometry (HJ 77.2-2008) of ambient air and waste gas-dioxins, the recovery rate range of PCDD/Fs extraction internal standard is 80%-107%, and the requirements are met.

Description

technical field [0001] The invention belongs to the technical field of carbon materials, and in particular relates to a graphitized carbon-based adsorption material and its preparation method and application. Background technique [0002] Dioxins refer to a group of polychlorinated substituted planar aromatic hydrocarbons with similar structures and physical and chemical properties, belonging to chlorinated oxygen-containing tricyclic aromatic hydrocarbons, including 75 polychlorinated dibenzo-p-dioxins (polychlorodibenzo -p-dioxins, PCDDs) and 135 polychlorinated dibenzofurans (polychloro-dibenzofurans, PCDFs), abbreviated as PCDD / Fs or dioxin. The most well-studied toxic dioxins are 17 homologue isomer monomers (congenor) substituted by chlorine atoms at the 2-, 3-, 7-, and 8-positions, among which 2,3,7,8-tetrachloro Dibenzo-p-dioxin (2,3,7,8-TCDD) is currently the most toxic dioxin monomer among all known compounds (oral LD50 is only 0.6 μg / kg), and also It has a varie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/30B01D53/02
Inventor 李义华关亚风谭伟强石磊陶俊杰赵彬周乾李宁张建军
Owner 光大理工环境技术研究院(青岛)有限公司
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