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Preparation method and application method of atrazine surface molecularly imprinted magnetic mesoporous material

A technology of surface molecular imprinting and atrazine, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve the problem of low adsorption rate of atrazine molecular imprinting polymers Solve problems such as elution and long equilibration time, achieve fast solid-liquid phase separation, short equilibration time and large adsorption capacity

Inactive Publication Date: 2018-07-06
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The adsorption rate of atrazine molecularly imprinted polymers prepared by traditional imprinting techniques such as bulk polymerization is generally not high, and the equilibration time is long, making it difficult to elute

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Dissolve 3.33g of polyethylene glycol solution in 30mL of ultrapure water. 2.86g FeSO 4 ·7H 2 O and 8.10g Fe(NO 3 ) 3 9H 2 O was dissolved in 75mL of ultrapure water, mixed evenly to obtain a brown solution, and then polyethylene glycol solution was mixed with it, ammonia water was slowly added under the protection of nitrogen, and the pH was adjusted to 11-12, while ultrasonic stirring. After separating the obtained particles with a magnet, they were washed twice with pure water and ethanol, and finally the volume was adjusted to 100 mL with ethanol.

[0026] (2) Take 50 mL of the magnetic fluid obtained in (1), disperse it in a mixed solution of 70 mL of ethanol and 20 mL of pure water, and after ultrasonic treatment for 15 min, add 7 mL of NH 3 ·H 2 O and 8 mL tetraethyl orthosilicate (TEOS), stirred at room temperature for 12 h, then washed several times with ethanol, and dilute to 100 mL.

[0027] (3) get the Fe obtained in (2) 3 o 4 @SiO 2 Add 20 mL ...

Embodiment 2

[0032] Carry out various index experiments to the material obtained in Example 1.

[0033] 50 mg of the material obtained in Example 1 was added to 100 mL of 500 μg / L solutions with different pH values ​​to investigate the effect of pH values ​​on the adsorption effect. The results showed that the adsorption capacity was the largest when the pH was around 6.

[0034] 50 mg of the material obtained in Example 1 was added to 100 mL of a pH=6 solution containing 500 μg / L, and the influence of adsorption time on the adsorption effect was investigated. The results showed that after 60 min, the adsorption reached equilibrium, and the adsorption process obeyed the second-order kinetics.

[0035] 50 mg of the material obtained in Example 1 was added to solutions with different initial concentrations, and adsorbed in a constant temperature oscillator at 25°C for 3 hours to study the variation of the adsorption amount of the material with the initial concentration, and through the fitt...

Embodiment 3

[0039] The material obtained in Example 1 was used for the solid phase extraction separation and enrichment of trace amounts of atrazine in the solution.

[0040] Add 50 mg of the material to 100 mL of a sample solution containing a certain concentration of atrazine, adjust the pH to 6, and shake at 200 rpm for 20 min. The adsorbed material was separated with a magnet, then 1 mL of acetonitrile was added, and ultrasonically eluted for 10 min. The concentration of atrazine in the eluate was measured by gas chromatography-mass spectrometer, and the recovery rate was calculated by the standard addition method.

[0041] The material can be reused 5 times.

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Abstract

The invention relates to a preparation method and an application method of an atrazine surface molecularly imprinted magnetic mesoporous material, and belongs to the technical field of composite material. The preparation method comprises following steps: sol-gel method is adopted to coat the surface of ferriferrous oxide with a layer of mesoporous silica, modification with vinyl tri-methoxysilaneis carried out, mixing with an acetonitrile solution of functional monomer itaconic acid is carried out, initiator azodiisobutyronitrile is added for a certain time of reaction, atrazine is added, nitrogen is introduced into a reaction system to remove oxygen for prepolymerization, azodiisobutyronitrile and cross-linking agent ethylene dimethacrylate are added for polymerization; an applied magnetic field is adopted for magnetic separation of obtained products; a mixed solution of acetic acid and methanol is adopted for elution of template molecules, and then magnetic separation and vacuum drying are carried out so as to obtain the atrazine surface molecularly imprinted magnetic mesoporous material. In the application method, the atrazine surface molecularly imprinted magnetic mesoporous material is added into sample solutions such as environment water sample or food containing atrazine, so that high efficiency adsorption separation on atrazine can be realized, treatment speed is high,anti-interference capability is excellent, the atrazine surface molecularly imprinted magnetic mesoporous material can be recycled for a plurality of times, and the application value of the atrazinesurface molecularly imprinted magnetic mesoporous material in selective adsorption removing of atrazine and detection pretreatment of trace atrazine is high.

Description

technical field [0001] The invention relates to the preparation and application of a highly selective adsorption material, in particular to a method for preparing a molecularly imprinted magnetic mesoporous material on the surface of atrazine, and the preparation of the material in solution samples (such as environmental water samples, food samples, etc.) The application in the adsorption removal and separation and enrichment of middle atrazine belongs to the technical field of composite materials. Background technique [0002] Atrazine (2-chloro-4-ethylamino-6-isopropylamino-1,3,5-triazine) is a triazine herbicide and is one of the most commonly used herbicides in the world. Widely used for weed control in the production of crops such as soybean, corn and sorghum. Therefore, atrazine may contaminate soil, surface water, groundwater and agricultural products, posing a threat to drinking water and food safety. The European Union and the United States list atrazine as a pote...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J20/30C02F1/28C02F101/30
CPCB01J20/268B01J20/28009C02F1/285C02F2101/306
Inventor 马晓国李歆黄仁峰谢晓纹郭丽慧张梦圆
Owner GUANGDONG UNIV OF TECH
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