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Adsorbent as well as preparation method and application thereof

An adsorbent and reaction technology, applied in the field of analysis and detection, can solve the problems affecting the accuracy, sensitivity and cost of analysis methods, difficult quantification, and complex environmental sample components.

Active Publication Date: 2022-06-03
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the concentration of BPs in the water environment is only at trace levels (ng / L or μg / L), and the composition of environmental samples is complex, it is difficult to directly and accurately quantify, so it is necessary to use effective pretreatment methods to detect the target substances in environmental samples. Enrichment and purification to meet the detection requirements of the instrument
Sample pretreatment directly affects the accuracy, sensitivity and cost of the analytical method, and becomes the bottleneck of detection technology

Method used

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  • Adsorbent as well as preparation method and application thereof
  • Adsorbent as well as preparation method and application thereof
  • Adsorbent as well as preparation method and application thereof

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preparation example Construction

[0055] According to a typical embodiment of the present invention, a method for preparing an adsorbent is provided, the method comprising:

[0056] S1. Get MCN;

[0057] S1.1. Disperse the molecular sieve in the second solvent, then centrifuge and evaporate to obtain a white solid;

[0058] In some embodiments, the molecular sieve can be SBA-15, which is a kind of mesoporous molecular sieve. SBA-15 has a two-dimensional hexagonal through-hole structure and a P6mm space group. In the XRD diffraction pattern, the main peak is around 1°, which is the (10) crystal plane peak. The second strongest peaks are (11) peak and (20) peak in turn. Other peaks are weak and difficult to observe. In addition, the silica on the SBA-15 framework is generally amorphous, and no obvious diffraction peaks can be observed in wide-angle XRD diffraction. Generally speaking, the typical synthesis process of SBA-15 is: under the condition of 35-40°C, dissolve the tri-block surfactant P123 (Aldrich, ...

Embodiment 1

[0081] A preparation method of adsorbent, said method comprising:

[0082] The preparation method of MCN is as follows: Disperse 1.0 g of SBA-15 in 10.0 mL of an aqueous solution containing 8.0 g of hexamethylenetetramine, stir at room temperature for 5 h, collect the solid by high-speed centrifugation, heat and evaporate at 50 ° C, and transfer the obtained white solid to In a closed crucible, heat up to 600°C at a rate of 2°C / min, keep heating for 2h, and cool down to room temperature naturally. Soak the obtained dark powder in 4mol / L ammonium bifluoride aqueous solution for 48h to remove the silica skeleton. Finally, the dark sample was collected by high-speed centrifugation, washed repeatedly with ultrapure water and absolute ethanol, and vacuum-dried at 60°C for 4 hours to obtain MCN.

[0083] Preparation of MCN / CoFe by Hydrothermal Synthesis 2 o 4, the specific method is as follows: add 75mg MCN to 70mL ethylene glycol, after ultrasonic dispersion is uniform, add 154....

experiment example

[0095] Utilize Scanning Electron Microscope (SEM), Field Emission Transmission Electron Microscope (TEM), Fourier Transform Infrared Spectrometer (FT-IR), X-ray Diffraction Instrument (XRD) and Vibrating Sample Magnetometer (VSM) to respectively analyze embodiment 1 The SBA-15 and its constructed MCN and MCN / CoFe 2 o 4 The surface morphology, crystal structure and composition, specific surface area, pore distribution, and magnetic strength of the composites were characterized.

[0096] Through the SBA-15, MCN and MCN / CoFe 2 o 4 The SEM morphology characterization found that, as Figure 3-5 As shown, the prepared MCN and MCN / CoFe 2 o 4 The morphology all presents a uniform and regular short rod-like structure, which is consistent with the morphology of the template SBA-15, and the MCN / CoFe 2 o 4 The uniform distribution of nanoparticles can be observed on the surface ( Figure 5 ).

[0097] In order to further observe the internal microstructure of the material, the ex...

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Abstract

The invention particularly relates to an adsorbent and a preparation method and application thereof, and belongs to the technical field of analysis and detection.The method comprises the steps that mesoporous carbon nitride (MCN) is obtained; dissolving the MCN in a first solvent to obtain a magnetic mesoporous carbon nitride (MCN) solution; mixing the MCN solution with CoCl2. 6H2O and FeCl3. 6H2O, and then carrying out pH (Potential of Hydrogen) regulation, so as to obtain a mixed solution; and reacting the mixed solution to obtain the adsorbent. The MCN / CoFe2O4 magnetic solid-phase extraction adsorbent is prepared through a hydrothermal synthesis method, MCN / CoFe2O4 serves as an MSPE adsorbent, high performance liquid chromatography-variable wavelength detection is combined, a new method for analyzing bisphenol estrogens (BPs) in the water environment is established, BPs in the water environment can be simply, efficiently and economically analyzed, a new thought is provided for enrichment and purification of organic pollutants in the water environment, and the method has a wide application prospect. And the bottleneck of BPs sample pretreatment is broken through.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to an adsorbent and its preparation method and application. Background technique [0002] Bisphenol estrogens (Bisphenols, BPs) are the most widely used type of artificial chemical substances in environmental estrogens, which have the effect of simulating estrogen. They are named for the two hydroxyl groups in the phenol structure. In industry, BPs are mainly used to synthesize compounds and monomers such as polycarbonate plastics, epoxy resins and polyester resins, and are often used as additives in the production of chemical products such as plasticizers, flame retardants, stabilizers and coatings. BPs in the water environment mainly come from industrial wastewater and domestic sewage discharged from factories. After entering aquatic organisms and the human body through the food chain, they bind to estrogen receptors in the body, affect the binding of en...

Claims

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Application Information

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IPC IPC(8): B01J20/06B01J20/28B01J20/30G01N30/06G01N30/02G01N30/74
CPCB01J20/06B01J20/02B01J20/28009B01J20/28083G01N30/06G01N30/02G01N30/74G01N2030/062G01N2030/027
Inventor 王曼曼李子凌
Owner NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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