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A kind of nanocomposite material and its preparation method and method for detecting mercury ions

A nano-composite material and magnetic separation technology, applied in the field of nano-materials, can solve the problems of packing column enrichment flow rate limitation, complicated operation, etc., and achieve the effects of accurate detection, simple operation and rapid separation

Inactive Publication Date: 2018-09-28
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the functionalization based on nanomaterials has strong enrichment performance, the enrichment flow rate of column packing is limited and the operation is cumbersome

Method used

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  • A kind of nanocomposite material and its preparation method and method for detecting mercury ions
  • A kind of nanocomposite material and its preparation method and method for detecting mercury ions
  • A kind of nanocomposite material and its preparation method and method for detecting mercury ions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] This embodiment provides a nanocomposite Fe@SiO 2 -SH, which is prepared by the following method:

[0055] Step 1, respectively weigh 0.87g of ferric chloride and 50mg of polyvinylpyrrolidone (PVP) and dissolve them in 60mL of ethanol solution with a volume fraction of 70%, add 0.2mL of tetraethyl orthosilicate (TEOS), and ultrasonically disperse for 20min Obtain solution A; Add 20mL concentration of 1mol / L sodium borohydride (NaBH 4 ) solution was reacted for 2 hours, and the experimental temperature was kept at 15°C during the reaction, followed by magnetic separation (in this embodiment, an external magnet was used to carry out magnetic separation of the reaction product), and then deionized water and absolute ethanol were used to wash 5 times successively, and the magnetic separation The non-magnetic by-products were removed, and finally vacuum-dried at 45 °C for 8 h to obtain Fe@SiO 2 .

[0056] Step 2, take the Fe@SiO obtained in step 1 2 Dissolve 0.4g in 40mL...

Embodiment 2

[0070] This example provides the Fe@SiO prepared in the example 2 -SH method for detecting mercury ions:

[0071] Step 1, take the nanocomposite material Fe@SiO prepared in the example 2 -SH ultrasonically disperses into the solution to be tested, adjust the pH value of the solution to be tested with hydrochloric acid and sodium hydroxide, and oscillate at a constant temperature at a temperature of 25°C with an oscillation speed of 270rpm for adsorption; then magnetically separate the adsorbed solution, Remove the solution and collect the adsorbed nanocomposites;

[0072] Step 2, adding hydrochloric acid solution to elute the adsorbed nanocomposite material with constant temperature oscillation, the oscillation temperature is 25°C, and the oscillation speed is 270rpm; then perform magnetic separation, take the supernatant and add hydrochloric acid to adjust to the amount added to the fluorescence carrier After coincidence, carry out fluorescence photometer detection, and cal...

Embodiment 3

[0085] Embodiment 3 Coexistence ion influence experiment

[0086] Weigh 8mg of the nanocomposite material Fe@SiO prepared in Example 1 2 -SH ultrasonic dispersion to 200mL mercury ion concentration is 0.0125ppb coexisting ions are Na + 、K + , Ca 2+ , Mg 2+ , Cl - The concentration is 100ppm, NO 3 - , SO 4 2- , CO 3 2- Concentration is 50ppm, Fe 3+ 、Cr 3+ , Mn 2+ Concentration of 100ppb, Cu 2+ , Pb 2+ 、Ni 2+ In different solutions with a concentration of 50ppb, 30ppb, and 30ppb, use hydrochloric acid and sodium hydroxide solution to adjust the pH to be neutral, add a film to seal, cover and tighten, and then place it in a water bath constant temperature oscillator with a temperature of 25°C and a speed of 270rpm Leave on for thirty minutes. After the shaking is completed, the reaction system is physically separated by an external magnetic field, and the solution part is discarded. After adding 2.5mL of 0.5% hydrochloric acid, place it in a water bath constant t...

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Abstract

The invention provides a nano composite material and a preparation method thereof, and a mercury ion detection method. The preparation method of the nano composite material comprises the steps that ferric chloride and polyvinylpyrrolidone react with ethyl orthosilicate to obtain Fe@SiO2; then, the Fe@SiO2 reacts with 3-aminopropyl triethoxy silane to obtain Fe@SiO2-NH2; then the Fe@SiO2-NH2 reacts with 4-mercaptobenzoic acid, N-hydroxyl succinimide and 1-(3-dimethylamino propyl)-3-ethylcarbodiimide hydrochloride to obtain the nanocomposite material Fe@SiO2-SH. The prepared nanocomposite material is used for detecting mercury ion content. Firstly, mercury ion enrichment is performed, then an applied magnetic field is adopted to perform separation and elution, and the mercury ion content is calculated through detection of an atomic fluorescence photometer. The prepared nanocomposite material can perform rapid enrichment of mercury ions and is simple in operation, rapid in separation and capable of accurately detecting a trace amount of mercury ions by magnetic separation and elution, and the detection accuracy can reach the order of magnitude PPT.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and relates to a nanocomposite material, a preparation method thereof and a method for detecting mercury ions. Background technique [0002] With the development of industry and economy, the problem of water pollution is becoming more and more severe, and various pollutants have an indirect or direct impact on the ecosystem. Environmental pollution can be seen as a small-scale impact in the short term, but as time goes on, it will inevitably cause global problems. The total amount of water resources on the earth is relatively large, but the reserves of fresh water resources available to humans are relatively low. Compared with other regions such as the Middle East and Africa, the per capita fresh water resources are very small, and the problem of water shortage is very serious. The current situation of water resources in my country is also not optimistic. , and this crisis tends to de...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/30B01J20/22B01J20/286B82Y40/00B82Y30/00B01D15/08G01N21/64
CPCB01D15/08B01J20/02B01J20/22B01J20/286B82Y30/00B82Y40/00G01N21/6404G01N2015/0096
Inventor 周庆祥贾国骁肖军平范慧俐
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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