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Nanometer carbon nitride/copper oxide composite material, and nanometer carbon nitride/copper oxide composite solid-phase micro-extractor, preparation method and applications thereof

A technology of composite materials and carbon nitride, applied in chemical instruments and methods, material separation, analysis of materials, etc., can solve the problem of few reports on sample pretreatment

Inactive Publication Date: 2019-12-06
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In recent years, its application scope has become more and more extensive, but there are few reports on sample pretreatment

Method used

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  • Nanometer carbon nitride/copper oxide composite material, and nanometer carbon nitride/copper oxide composite solid-phase micro-extractor, preparation method and applications thereof
  • Nanometer carbon nitride/copper oxide composite material, and nanometer carbon nitride/copper oxide composite solid-phase micro-extractor, preparation method and applications thereof
  • Nanometer carbon nitride/copper oxide composite material, and nanometer carbon nitride/copper oxide composite solid-phase micro-extractor, preparation method and applications thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The preparation process of nanometer carbon nitride / copper oxide composite material is as follows:

[0040] 1) Commercially available carbon nitride is usually bulk carbon nitride (b-g-C 3 N 4 ), which is prepared by thermal polymerization of organic molecules, and there is obvious agglomeration phenomenon, which seriously affects its performance. For this reason, the present invention first ultrasonically disperses the purchased bulk carbon nitride in an 8 M NaOH solution to obtain a suspension, and then stirs the suspension at 70°C for 3 h, during which the suspension becomes It is more viscous. After the reaction, the viscous suspension obtained is centrifuged and the precipitate is collected. The obtained precipitate is washed several times with absolute ethanol until the washing solution is neutral, and the nanometer carbon nitride powder is obtained after drying.

[0041] 2) Weigh 47.4 mg of nano-carbon nitride obtained in step 1) and ultrasonically disperse it ...

Embodiment 2

[0049] The preparation process of the solid-phase microextractor of the nanometer carbon nitride / copper oxide composite material is as follows:

[0050] 1) Thoroughly mix tetraethyl silicate and ethanol evenly, add pH about 2-3 HCl aqueous solution drop by drop under strong stirring with a magnetic stirrer, continue stirring to mix evenly, and obtain clarification after ultrasonic treatment of the reaction mixture Transparent solution, sealed and placed at room temperature, that is, SiO 2 Sol.

[0051] 2) Cut off a quartz fiber with a length of 10-12 cm, and immerse one end of the quartz fiber with a protective layer in acetone for 20-30 min to remove the polyimide on the surface of the fiber to obtain a bare fiber, and dip the bare fiber into Ultrasonic immersion in 1-2 mol / L NaOH solution for 1-2 h to activate the surface of the fiber, ultrasonic vibration with 0.05-0.2 mol / L HCl solution for 30 minutes to neutralize excess NaOH on the fiber, and finally use ultrapure water...

Embodiment 3

[0059] The application of the solid-phase microextractor of nano carbon nitride / copper oxide composite material in the determination of polycyclic aromatic hydrocarbons in water samples comprises the following steps:

[0060] The first step is to determine the content of polycyclic aromatic hydrocarbons in water samples

[0061] The water samples were filtered with a 0.45 μm water-based filter membrane and then directly subjected to subsequent enrichment and adsorption. The solid-phase microextraction process is as follows: Before performing the SPME process, insert the obtained nano-carbon nitride / copper oxide solid-phase microextractor into a 5 μL microinjector, and then place the extraction fiber under the GC condition where the inlet temperature is 280 °C Aging for 1-2 hours to remove impurities on the extraction head; put the water sample and magnets to be tested in the sample bottle, immerse half of the bottle body in the water bath, and push the extraction fiber out of ...

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Abstract

A purpose of the invention is to provide a nanometer carbon nitride / copper oxide composite material, and a nanometer carbon nitride / copper oxide composite solid-phase micro-extractor, a preparation method and applications thereof. The preparation method of the nanometer carbon nitride / copper oxide composite solid-phase micro-extractor comprises: dispersing nanometer carbon nitride in deionized water, adding a copper nitrate solution while stirring, adding a hexamethylenetetramine solution in a dropwise manner, continuously stirring until the materials are uniformly mixed, stopping the stirring, carrying out a constant temperature reaction for 3-5 h at a temperature of 80-100 DEG C, collecting the precipitate after the reaction is completed, washing, drying to obtain a nanometer carbon nitride / copper oxide composite material, and wrapping the surface of quartz fibers with the nanometer carbon nitride / copper oxide composite material through a silica colloid to prepare the solid-phase micro-extractor. According to the present invention, the nanometer carbon nitride / copper oxide composite material has good adsorption performance on polycyclic aromatic hydrocarbons, and the solid-phasemicro-extractor prepared from the composite material has high extraction efficiency on polycyclic aromatic hydrocarbons, and can meet the detection requirements of polycyclic aromatic hydrocarbons.

Description

technical field [0001] The invention belongs to the technical field of detection of polycyclic aromatic hydrocarbons, and in particular relates to a nanometer carbon nitride / copper oxide composite material, a nanometer carbon nitride / copper oxide composite solid phase microextractor and a preparation method and application thereof. Background technique [0002] Polycyclic aromatic hydrocarbons (PAHs) are volatile hydrocarbons produced when coal, petroleum, wood, tobacco, organic polymers and other substances are incompletely burned, and widely exist in the human living environment such as the atmosphere, water, soil and crops. As important environmental and food pollutants, more than 200 PAHs have been discovered so far. Recent studies have shown that polycyclic aromatic hydrocarbons are non-degradable and potentially carcinogenic. Therefore, for complex samples such as soil, it is of great significance to develop a simple, rapid and sensitive detection method. [0003] As ...

Claims

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Application Information

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IPC IPC(8): B01D15/08B01J20/02B01J20/30G01N30/02G01N30/06G01N30/16G01N30/68
CPCB01D15/08B01J20/0237G01N30/02G01N30/06G01N30/16G01N30/68G01N2030/027G01N2030/062
Inventor 卢明华杨艺欣王友梅朱金花周倩
Owner HENAN UNIVERSITY
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