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Three-dimensional macroporous carbon anchored monatomic iron catalyst as well as preparation method and application thereof

A technology of three-dimensional macropores and iron catalysts, applied in chemical instruments and methods, physical/chemical process catalysts, applications, etc., can solve the problems of large energy consumption, low removal efficiency, long removal time, etc., to improve utilization rate, remove High efficiency and high activity effect

Pending Publication Date: 2022-08-05
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the research on the method of removing chloramphenicol from soil has also become a research hotspot. Common removal methods include biological removal, adsorption, and Fenton oxidation, but there are defects such as long removal time, low removal efficiency, and large energy consumption.

Method used

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  • Three-dimensional macroporous carbon anchored monatomic iron catalyst as well as preparation method and application thereof
  • Three-dimensional macroporous carbon anchored monatomic iron catalyst as well as preparation method and application thereof
  • Three-dimensional macroporous carbon anchored monatomic iron catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 Synthesis of catalytic material 3D Fe-NC

[0029] Dopamine (0.5g), Sodium Chloride (1g), FeCl 3 ·6H 2 O (20mg) was added to 100ml of water, and after 2 hours of conventional sonication, freeze-dried at -54°C for 5 days, and the obtained white powder was calcined in an argon atmosphere at a calcination temperature of 800°C and a heating rate of 3°C / min. The time was 2 h; the calcined black powder was washed with water and 0.5M sulfuric acid solution to remove the template sodium chloride, and then dried in an oven at 70 °C for one night, which was 3D Fe-NC, and the iron loading was 17.wt% , called 1.7% 3DFe-NC.

[0030] 3D Fe-NC SEM microstructure such as figure 1 The high-angle annular dark field-scanning transmission electron microscope image shown in figure 2 shown; by figure 1 It can be seen that the 3D Fe-NC is a three-dimensional macroporous shape with a pore diameter of about 1 μm; figure 2 A uniform distribution of iron atoms can be seen.

[00...

Embodiment 2

[0036] Example 2 Catalyst material 3D Fe-NC for the removal of chloramphenicol in soil

[0037] (a) Take 1 g of soil with an initial pollutant concentration of 100 mg / kg of chloramphenicol and put it into a quartz tube. At this time, pH=7.60 and water content is 15%;

[0038] (b) Add 30 mg of catalyst material (Example 1) or a comparative catalyst material, and then microwave catalysis for 5 minutes at a power of 1200 W;

[0039] (c) Add 5 ml of methanol to the microwave-catalyzed soil for ultrasonic leaching for 30 min and then centrifuge. The resulting clear night was put into a liquid phase vial, and the concentration of chloramphenicol was determined by HPLC.

[0040] The removal results of different catalysts for the initial pollution concentration of 100 mg / kg soil are as follows: Figure 4 , AC is commercially available activated carbon, and MW is microwave; it can be seen that the catalyst of the present invention achieves the best removal rate of 1.7% 3D Fe-NC, and r...

Embodiment 3

[0042] Example 3 Removal of different pollutants

[0043] (a) Take 10 g of soil with an initial contaminant concentration of 100 mg / kg and put it into a quartz tube and stir it on a mixer; the initial contaminants are 2,4-dichlorophenol, di-n-propyl phthalate ester, phenanthrene or benzaldehyde;

[0044] (b) 300 mg of the above catalyst material 1.7% 3D Fe-NC was added, and microwave catalyzed at 1200 W for 5 min;

[0045] (c) Add 50 ml of methanol to the soil after microwave catalysis for ultrasonic leaching for 30 min and then centrifuge. The obtained clear night was put into a liquid phase vial, and the concentration of each pollutant was determined by HPLC; the removal results of different pollutants are shown in Figure 5 , it can be seen that the catalyst of the present invention 1.7% 3D Fe-NC to benzaldehyde also reaches 99.9% removal rate within 5min.

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Abstract

The invention discloses a three-dimensional macroporous carbon anchored monatomic iron catalyst as well as a preparation method and application thereof. Monatomic iron is anchored on three-dimensional macroporous carbon to serve as a microwave catalyst to be used for removing organic pollutants such as chloramphenicol in soil. Specifically, dopamine is used as a carbon source, sodium chloride is used as a template, and a ferric chloride aqueous solution is used as an ion source to prepare 3D Fe-NC; the preparation method comprises the following steps: firstly, carrying out freeze drying, then carrying out high-temperature calcination, and then washing off a sodium chloride template by using water and 0.5 M sulfuric acid, thereby obtaining the 3D Fe-NC. Natural soil is selected as experimental soil, pollutants are added, then a catalyst is added, and a reaction is initiated under microwave radiation; the removal efficiency is high (the removal rate reaches 99.9% in 5 min), the repaired soil is low in toxicity, the applicable pH range is wide, and energy is saved.

Description

technical field [0001] The invention belongs to the technical field of microwave catalyst materials, and in particular relates to a 3D Fe-NC as a microwave adsorbent and catalyst, a preparation method thereof, and the use of 3D Fe-NC for removing chloramphenicol in soil. Background technique [0002] In daily life, chloramphenicol (2,4-DCP) is a synthetic antibiotic that inhibits protein synthesis by binding to bacterial ribosomes to achieve bacteriostatic purposes. Due to its low cost and excellent antibacterial effect, chloramphenicol is also widely used in animal husbandry and aquatic product breeding. It has been detected in soil, surface water and groundwater. Once it enters the food chain, it will bring risks to people's health. . Due to its high toxicity, persistence, and bioaccumulation, there is an urgent need to develop eco-friendly and efficient methods for removing chloramphenicol from contaminated soils. At present, the research on the removal of chloramphenic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/745B01J27/24B01J35/10B01J20/28B01J20/30B01J20/20B09C1/00B09C1/08C09K17/04
CPCB01J23/745B01J27/24B01J20/20B01J20/28064B01J20/28085B01J20/0203B09C1/08B09C1/00C09K17/04B01J35/617B01J35/653Y02A50/20
Inventor 路建美贺竞辉
Owner SUZHOU UNIV