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

A technology for imprinting polymers and magnetic molecules, which is applied in the field of magnetic molecular imprinting polymers for separation of atrazine and its preparation, can solve the problems of easy detachment and leakage of magnetic fluid, and achieves good stability, less time consumption, and cheap and easy raw materials. the effect

Inactive Publication Date: 2013-09-04
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, so when forming magnetic molecularly imprinted polymers, it is still only embedded in the polymer through physical interaction. When used in bioseparation, Fe 3 o 4 Ferrofluid is easy to fall off and leak

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 :Using chemical co-precipitation method

[0033] (1) The massage ratio is 1:1.75 to weigh FeSO 4 ·7H 2 O and FeCl 3 ·6H 2 Add O to the 100mL reaction flask, add 20mL filled with N 2 Deoxygenated water, charged with N 2 React for 30min, add 10mLNH dropwise to the constant pressure funnel 3 ·H 2 O, react in oil bath at 65℃ for 2h;

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

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

[0036] Fe 3 O 4 The infrared spectrum is as 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 appears at 2θ=30.37°, 35.69°, 43.16°, 53.69°, 57.38°, 62...

Embodiment 2

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

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

[0040] (2) The magnet is separated, washed with ethanol and water, dried in vacuum at 60℃, 0.1g Fe 3 O 4 SiO 2 , Add 10mL HCl with a concentration of 10%, reflux in an oil bath at 50℃ for 6h, wash, and dry under vacuum at 60℃ to obtain activated Fe 3 O 4 SiO 2 .

[0041] Fe 3 O 4 SiO 2 The infrared spectrum is as figure 1 As shown in b, 1096cm -1 The antisymmetric stretching vibration absorption peak of nearby Si-O-Si, 954cm -1 Vibration characteristic peak of Si-O in the nearby Si-OH bond and 799cm -1 The bending vibration absorption peaks of nearby Si-O-Si are all SiO 2 The main characteristic absorption peak of the structure indicates that the Fe 3 O 4 The surface of the magnetic microspheres is successfully coated with a layer of SiO 2 ;Thermogravimetric curve su...

Embodiment 3

[0043] Fe 3 O4SiO 2 The modification:

[0044] (1) Take 0.3g of Fe activated in Example 2 3 O 4 SiO 2 Nano particles are dispersed in 100mL toluene;

[0045] (2) Add 2mL MPS (KH570γ-methacryloxypropyltrimethoxysilane), 2 In the environment, reflux at 65℃ for 12h;

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

[0047] In Fe 3 O 4 SiO 2 The surface is modified with MPS from Figure 5 You can see composite magnetic nanoparticles Fe 3 O 4 SiO 2 -MPS saturation susceptibility compared to Fe 3 O 4 SiO 2 The increase in microspheres may be due to the binding of MPS to Fe 3 O 4 SiO 2 Surface; from Figure 5 It can be seen that Fe 3 O 4 SiO 2 -The thermal stability of MPS is similar to Fe 3 O 4 SiO 2 Quite, better than Fe 3 O 4 Good thermal stability; Figure 8 The TEM image also shows that the experiment successfully synthesized Fe 3 O 4 Magnetic microspheres are microspheres with a core-shell structu...

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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 prepared by 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 molecularly imprinted polymer for separating atrazine and a preparation method thereof. Background technique [0002] Molecular imprinting technology is based on the target molecule as a template, combined with functional monomers through non-covalent bonds or covalent bonds, and cross-linking agent is added for polymerization. After the reaction, the template molecules are eluted to obtain a fixed pore size and shape. There are imprinted polymers with defined 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 can be used in pretreatments such as selective enrichment and separation of substances. [0003] Fe 3 O 4 Magnetic nanoparticles have the characteristics of sm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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