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Preparation method of nitrogen-enriched porous carbon desulfurizer with superhigh specific surface area

A technology of ultra-high specific surface area, porous carbon, applied in separation methods, chemical instruments and methods, catalysts for physical/chemical processes, etc., can solve the problems of cumbersome preparation process, low carbon yield, high energy consumption, and achieve broad application prospects , The effect of simple process and easy availability of raw materials

Inactive Publication Date: 2017-03-01
DALIAN UNIV OF TECH
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0006] Chinese patent, publication number: CN105107459A, introduces a method for preparing a desulfurizer by activating walnut shells with KOH. This process has problems such as corrosion of equipment and low carbon yield.
[0007] Chinese patent, publication number: CN104826581A, introduces a method for treating porous carbon materials with ammonia gas. Due to the use of toxic ammonia gas at high temperature, the process has high energy consumption and serious pollution, and the amount of nitrogen doping in the material is relatively high. Low, nitrogen-containing functional groups are unstable, and the pore structure is destroyed
[0008] Chinese patent, publication number: CN102773075A, introduces the preparation of porous carbon for hydrogen sulfide adsorption using SBA-15 as a template. The preparation process of this method is cumbersome, long cycle, high cost, and toxic hydrofluoric acid

Method used

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  • Preparation method of nitrogen-enriched porous carbon desulfurizer with superhigh specific surface area
  • Preparation method of nitrogen-enriched porous carbon desulfurizer with superhigh specific surface area
  • Preparation method of nitrogen-enriched porous carbon desulfurizer with superhigh specific surface area

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preparation example Construction

[0040] figure 1 It is a schematic diagram of the preparation process of nitrogen-doped porous carbon in the present invention, and the specific preparation process is as follows:

[0041] (1) Combine small molecule precursors (adenine or glycine or glucose and melamine) with molten salt (KCl-ZnCl 2 or NaCl-ZnCl 2 ) for mechanical mixing, the mechanical mixing methods used include grinding, ball milling or a combination of grinding and ball milling;

[0042] (2) Place the precursor and molten salt mixture in an inert atmosphere for carbonization treatment, and the inert protective gas used is selected from one or more mixtures of nitrogen, argon, helium and other gases;

[0043] (3) The carbonized product is washed with acid and deionized water, and the acid used is selected from one or more mixtures of inorganic acids such as hydrochloric acid, sulfuric acid, nitric acid, and phosphoric acid.

Embodiment 1

[0046] 1.0g adenine, 1.90g KCl and 8.10g ZnCl 2 (KCl in KCl-ZnCl 2 The mole fraction in is 0.3) mixing and grinding evenly. The mixture was placed in a quartz tube, heated to 800 °C in a nitrogen atmosphere and kept at a constant temperature for 1 h for carbonization. Cool to room temperature. Product in 1mol L -1 Stir in hydrochloric acid solution for 12 hours, filter with suction, wash with deionized water, and dry to obtain a nitrogen-doped porous carbon material (denoted as NPC-A-K / Zn0.3-800). The elemental analysis results show that the nitrogen content in the nitrogen-doped porous carbon is 20.79wt.%. figure 2 Shown is a scanning electron microscope picture of the NPC-A-K / Zn 0.3-800 sample, from which it can be seen that the sample is composed of very small nanoparticles. image 3 It is the nitrogen adsorption-desorption curve and pore size distribution curve of the sample. The nitrogen adsorption test results show that the sample presents micropore-mesopore charac...

Embodiment 2

[0048] 1.0g adenine, 3.54g KCl and 6.46g ZnCl 2 (KCl in KCl-ZnCl 2 The mole fraction in is 0.5) mix and grind evenly. The mixture was placed in a quartz tube, heated to 800 °C in a nitrogen atmosphere and kept at a constant temperature for 1 h for carbonization. Cool to room temperature, the product is in 1mol L -1 Stir in hydrochloric acid solution for 12 hours, filter with suction, wash with deionized water, and dry to obtain a nitrogen-doped porous carbon material (denoted as NPC-A-K / Zn 0.5-800). Elemental analysis results showed that the nitrogen content was 21.94wt.%. Figure 5 Shown is a scanning electron microscope picture of the NPC-A-K / Zn 0.5-800 sample, from which it can be seen that the sample is composed of aggregated carbon spheres. Image 6 It is the nitrogen adsorption-desorption curve and pore size distribution curve of the sample. The nitrogen adsorption test results show that the sample presents micropore-mesopore characteristics, and the specific surface...

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Abstract

The invention belongs to a preparation method of a nanometer functional material and especially relates to the field of application of a nitrogen-doped porous carbon material to environment protection. A preparation method of a nitrogen-enriched porous carbon desulfurizer with superhigh specific surface area comprises the following steps: firstly, mechanically mixing a micromolecular biomass precursor and inorganic molten salt, placing the mixture into a quartz tube, and carbonizing in an inert atmosphere. By the utilization of polymerization among the precursor in the heating process and phase separation of carbon generated by carbonization and fuse salt, ion pair or cluster formed by fuse salt is used as a pore forming agent; and washing is followed to remove the molten salt so as to obtain the nitrogen-doped porous carbon desulfurizer. The nitrogen-doped porous carbon has a well-developed pore structure and rich nitrogen-containing function group, can be used as a non-metal catalyst for catalytic oxidation of hydrogen sulfide at room temperature to convert to elemental sulfur, and has a wide application prospect in the field of environment protection. In addition, the method has characteristics of simple operation, low cost, environment-friendly preparation and easy industrial production, and is an important carbon nanomaterial preparation method.

Description

technical field [0001] The invention belongs to a preparation method of nanometer functional materials, in particular relates to the application of nitrogen-doped porous carbon materials in the field of environmental protection, in particular to a preparation method of a nitrogen-rich porous carbon desulfurizer with an ultra-high specific surface area. Background technique [0002] Hydrogen sulfide (H 2 S) Widely present in natural gas, synthesis gas and industrial waste gas, containing H 2 S gas will corrode production equipment and poison industrial catalysts during transportation and reaction; direct discharge will seriously pollute the environment and cause waste of sulfur resources. Therefore, the development of H 2 The high-efficiency removal technology of S is always the core problem faced by the petrochemical industry, and the key is the development of high-performance desulfurizers. Porous carbon materials have been widely used as adsorbents to remove H2 due to t...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/10B01J20/20B01J20/30B01D53/02B01D53/86B01D53/52
CPCB01D53/02B01D53/8612B01J20/20B01J20/3085B01J27/24B01J35/618B01J35/638
Inventor 王旭珍余正发侯亚男邱介山
Owner DALIAN UNIV OF TECH
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