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Magnetic self-flocculation material with Raman-enhanced properties and its preparation method and application

A self-flocculation and magnetic technology, applied in the analysis of materials, Raman scattering, material excitation analysis, etc., can solve the problems of low recovery efficiency and easy residual water, and achieve the effect of simple preparation method

Active Publication Date: 2022-02-11
ANHUI UNIVERSITY OF ARCHITECTURE
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Problems solved by technology

[0004] The purpose of the present invention is to solve the above problems, providing a magnetic self-flocculation material with Raman enhancement properties and its preparation method, to solve the problem that the existing magnetic SERS substrates are relatively dispersed in water bodies, easily residual water bodies, and low recovery efficiency and other technical issues

Method used

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  • Magnetic self-flocculation material with Raman-enhanced properties and its preparation method and application
  • Magnetic self-flocculation material with Raman-enhanced properties and its preparation method and application
  • Magnetic self-flocculation material with Raman-enhanced properties and its preparation method and application

Examples

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preparation example Construction

[0024] A method for preparing a magnetic self-flocculation material with Raman enhanced properties, comprising the following steps:

[0025] (1) Preparation of magnetic Fe 3 o 4 Granules: Take 0.5-1.0g of ferrous sulfate heptahydrate and 0.2-0.5g of citric acid, add 5-10mL of deionized water, stir evenly, pour into the lined polytetrafluoroethylene, then add 8-12mL of 40-50% wt hydrazine hydrate, then put it into the reaction kettle at 140-160 ℃ for 6-8 h in a constant temperature drying oven, collect the black precipitate with a magnet after cooling, and wash it repeatedly for 3-5 times to obtain the magnetic Fe 3 o 4 particles.

[0026] (2) Preparation of highly efficient SERS materials with magnetic self-flocculation: take the magnetic Fe from step (1) 3 o 4 Particles, after dispersing with deionized water, add 0.02-0.05 g polyethyleneimine (PEI), and ultrasonically disperse evenly; mix 5-10 mL of 50-70 mM silver nitrate solution and 2-4 mL of 0.04-0.06 g / mL polyviny...

Embodiment 1

[0031] This example provides a method for preparing materials with magnetic self-flocculation efficient extraction and recovery and SERS enhancement properties, such as figure 1 shown, including the following steps:

[0032] (1) Preparation of magnetic Fe 3 o 4 Particles: Dissolve 0.8 g of ferrous sulfate heptahydrate and 0.3 g of citric acid in 10 mL of deionized water, stir evenly, pour into the lined polytetrafluoroethylene, then add 10 mL of 45%wt hydrazine hydrate, and then put it into the reaction kettle Put it in a constant temperature drying oven at 150 °C for 8 h, collect the black precipitate with a magnet after cooling, and wash it repeatedly for 3-5 times to obtain the magnetic Fe 3 o 4 particles.

[0033] (2) Preparation of highly efficient SERS materials with magnetic self-flocculation: take the above magnetic Fe 3 o 4Add deionized water to the particles, then add 0.03g polyethyleneimine to mix, ultrasonically disperse evenly, then add 10mL of 70 mM silver ...

Embodiment 2

[0042] This embodiment provides another material with magnetic self-flocculation efficient extraction and recovery and SERS enhancement properties and its preparation method, including the following steps:

[0043] (1) Preparation of magnetic Fe 3 o 4 Particles: Dissolve 1.0g of ferrous sulfate heptahydrate and 0.3g of citric acid in 10mL of deionized water, stir evenly and pour into the lined polytetrafluoroethylene, then add 10mL of 45% hydrazine hydrate, then put into the reaction kettle Put it in a constant temperature drying oven at 160 °C for 7 h, collect the black precipitate with a magnet after cooling, and wash it repeatedly for 3-5 times to obtain the magnetic Fe 3 o 4 particles.

[0044] (2) Preparation of highly efficient SERS materials with magnetic self-flocculation: take the above magnetic Fe 3 o 4 Add deionized water to the particles, then add 0.02 g polyethyleneimine to mix, ultrasonically disperse evenly, then add 10 mL of 65 mM silver nitrate solution a...

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Abstract

The present invention relates to a kind of magnetic self-flocculation material with Raman enhanced characteristic and its preparation method and application, the steps include: 3 O 4 The surface of the particles is coated with polyethyleneimine, and then the silver nitrate solution dispersed and supported by polyvinylpyrrolidone is added, so that the amino group in the PEI molecular structure unit combines with the carbonyl group on the PVP molecular structure unit to undergo a carbonyl ammonia reaction, and finally a small amount of NaOH solution and A certain hydrazine hydrate solution, silver ions in the hydrazine hydrate reduction solution form silver nanoparticles to wrap around the outside, and a highly efficient SERS material with self-flocculation function is obtained. Compared with the prior art, the magnetic self-flocculation material prepared by the present invention not only has the dual functions of solid phase extraction easy separation and SERS enhanced detection, but also has a self-flocculation function, which can be applied to the enrichment and recovery of pollutants in water bodies to achieve high-efficiency extraction and easy separation effect.

Description

technical field [0001] The invention belongs to the technical field of solid-phase extraction Raman analysis, and in particular relates to a magnetic self-flocculation material with Raman enhancement characteristics, a preparation method and application thereof. Background technique [0002] Surface enhancement of Raman scattering (SERS) technology can provide information at the molecular level that is not easily obtained by other detection techniques. It has short detection time, low water interference, and does not require complicated sample processing. It is widely used in Chemical, biological detection, environmental pollutant detection and many other fields. [0003] Currently, Au / Ag-coated magnetic particles as magnetic SERS substrates have attracted widespread interest due to their simultaneous combination of the advantages of both materials. However, although these magnetic SERS substrates can enrich target molecules from water samples and perform SERS detection, th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/65
CPCC02F1/488G01N21/658
Inventor 唐建设唐曦璞项丽吴焕乐崔兆行严政王一
Owner ANHUI UNIVERSITY OF ARCHITECTURE
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