Magnetic molecularly imprinted polymer for separating atrazine, and preparation method for magnetic molecularly imprinted polymer

A technology of imprinted polymers and magnetic molecules, which is applied in the field of magnetic molecular imprinted polymers for separating atrazine and its preparation, can solve the problems of easy shedding and leakage of magnetic fluid, and achieve good stability, cheap and easy-to-obtain raw materials, and simple operation Effect

Inactive Publication Date: 2012-04-18
JIAXING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Fe used in this method 3 o 4 Modification of ferrofluid with oleic acid only changes Fe 3 o 4 The solubility of magnetic fluid in organic solvents without functional modification on its surface, s

Method used

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  • Magnetic molecularly imprinted polymer for separating atrazine, and preparation method for magnetic molecularly imprinted polymer
  • Magnetic molecularly imprinted polymer for separating atrazine, and preparation method for magnetic molecularly imprinted polymer
  • Magnetic molecularly imprinted polymer for separating atrazine, and preparation method for magnetic molecularly imprinted polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Preparation of Fe 3 o 4 : by chemical co-precipitation method

[0033] (1) Weigh FeSO at a molar ratio of 1:1.75 4 ·7H 2 O and FeCl 3 ·6H 2 O was added to a 100mL reaction bottle, and 20mL of N-filled 2 Deoxygenated water, N-filled 2 React for 30min, add 10mLNH dropwise to the constant pressure funnel 3 ·H 2 O, react in an oil bath at 65°C for 2h;

[0034] (2) Add 1.0 g of citric acid, react for 1.5 h, add cellulose acetate particles to the above mixed solution, and magnetically stir for 2 h, the mass concentration of cellulose acetate in the mixed solution is 10%;

[0035] (3) After the reaction is completed, wash with ethanol and water to neutrality respectively, and dry under vacuum at 60° C. overnight;

[0036] Fe 3 o 4 The infrared spectrum of figure 1 As shown in a, 580cm -1 The nearby stretching vibration absorption peak is the characteristic absorption peak of Fe-O bond; Fe 3 o 4 X-ray diffraction such as figure 2 As shown, Fe appeared at 2θ=30.3...

Embodiment 2

[0038] Fe 3 o 4 SiO 2 Preparation and activation:

[0039] (1) Fe prepared in 0.1g embodiment 1 3 o 4 Disperse in 120mL ethanol and 10mL water, add 1mL NH 3 ·H 2 O. 2mL TEOS (tetraethyl orthosilicate), stirred at 25°C for 24h;

[0040] (2) Magnetic separation, washing with ethanol and water respectively, vacuum drying at 60°C, 0.1g Fe 3 o 4 SiO 2 , add 10mL of HCl with a concentration of 10%, reflux in an oil bath at 50°C for 6h, wash, and dry under vacuum at 60°C to obtain activated Fe 3 o 4 SiO 2 .

[0041] Fe 3 o 4 SiO 2 The infrared spectrum of figure 1 As shown in b, 1096cm -1 The antisymmetric stretching vibration absorption peak of nearby Si-O-Si, 954cm -1 The characteristic vibration peak of Si-O in the nearby Si-OH bond and the 799cm -1 The bending vibration absorption peaks of nearby Si-O-Si are all SiO 2 The main characteristic absorption peaks of the structure, indicating that the Fe 3 o 4 The surface of magnetic microspheres was successfully ...

Embodiment 3

[0043] Fe 3 O4SiO 2 Modifiers:

[0044] (1) get the Fe activated in 0.3g embodiment 2 3 o 4 SiO 2 Nanoparticles dispersed in 100mL toluene;

[0045] (2) Add 2mL MPS (KH570γ-methacryloxypropyltrimethoxysilane), 2 Under ambient conditions, reflux at 65°C for 12 hours;

[0046] (3) Wash three times with dimethyl sulfoxide and ethanol respectively, and dry to obtain composite magnetic nanoparticles Fe 3 o 4 SiO 2 -MPS.

[0047] in Fe 3 o 4 SiO 2 Surface modified with MPS from Figure 5 Composite magnetic nanoparticles Fe can be seen in 3 o 4 SiO 2 - MPS saturation susceptibility compared to Fe 3 o 4 SiO 2 Microspheres increased, possibly due to the binding of MPS to Fe 3 o 4 SiO 2 surface; from Figure 5 Fe can be seen in 3 o 4 SiO 2 -The thermal stability of MPS is different from that of Fe 3 o 4 SiO 2 Quite, both than Fe 3 o 4 Good thermal stability; Figure 8 The TEM image also shows that the experiment successfully synthesized Fe 3 o 4 The mag...

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Abstract

The invention discloses a method for preparing a magnetic molecularly imprinted polymer for separating atrazine. The method comprises the following steps of: 1) activating Fe3O4atSiO2 particles, and performing surface modification by using a silane coupling agent to obtain composite magnetic nano-particles; and 2) adding the atrazine and methacrylic acid into an organic solvent and preassembling,adding the composite magnetic nano-particles, a crosslinking agent and an initiator, performing polymerization reaction at the temperature of between 60 and 70 DEG for 20 to 24h in an anaerobic environment, and removing the atrazine to obtain the magnetic molecularly imprinted polymer. The method is easy to operate and is suitable for large-scale production; the time consumption is low; raw materials are cheap and readily available; and membrane materials with micron-scale and nano-scale diameters can be obtained. The invention also provides the magnetic molecularly imprinted polymer preparedby the method. Magnetic molecules are firmly combined, and the magnetic molecularly imprinted polymer is high in stability and has stronger adsorption capacity when separating the atrazine.

Description

technical field [0001] The invention relates to the field of magnetic separation and solid phase extraction, in particular to a magnetic molecular imprint polymer for separating atrazine and a preparation method thereof. Background technique [0002] Molecular imprinting technology uses the target molecule as a template, combines with functional monomers through non-covalent bonds or covalent bonds, adds a cross-linking agent for polymerization, and elutes the template molecules after the reaction, so as to obtain molecules with fixed pore size and shape and Imprinted polymers with defined arrays of functional groups. Molecularly imprinted polymers have the advantages of acid and alkali resistance, organic solvent resistance, good thermal stability, long service life, etc., and have good specific recognition performance, so they are used in pretreatments such as selective enrichment and material separation. [0003] Fe 3 o 4 Magnetic nanoparticles have the characteristics...

Claims

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Application Information

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IPC IPC(8): C08F220/06C08F222/14C08F2/44C08J9/26C08K9/06C08K3/36C08K3/22
Inventor 李蕾门海芬张祖磊
Owner JIAXING UNIV
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