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Preparation method of magnetic nanometer molecular imprinting composite material related to estrogen

A magnetic molecular imprinting and magnetic nanotechnology, which is applied in the field of preparation of amino-functional nano-ferric oxide magnetic molecular imprinting composite materials, can solve the problems of limited active sites, weak adsorption, cumbersome operation, etc., and achieve a functional group ratio. control, shorter reaction cycle, and simple preparation process

Inactive Publication Date: 2012-07-18
NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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Problems solved by technology

However, due to the use of functional monomers with low nitrogen content in the reaction, such as: 2-vinyl-pyridine, etc., the active sites (-N<) contained in this functional group are limited, and the reaction cycle is long and the operation is cumbersome. The magnetic content and the proportion of functional groups are not easy to control, therefore, its application is greatly limited

Method used

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  • Preparation method of magnetic nanometer molecular imprinting composite material related to estrogen
  • Preparation method of magnetic nanometer molecular imprinting composite material related to estrogen
  • Preparation method of magnetic nanometer molecular imprinting composite material related to estrogen

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preparation example Construction

[0022] The preparation method of the magnetic nano molecular imprinted composite material of estrogen in the present invention comprises the following steps:

[0023] 1. Preparation of monodisperse Fe3O4 / polymer composite microspheres with high magnetic content: Nano-Fe3O4 particles were prepared by chemical co-precipitation method, and the surface was modified with oleic acid, and then prepared by suspension polymerization method. Ferric oxide / polymer composite microspheres with monodisperse magnetic content; specifically include the following sub-steps:

[0024] 1.1. Preparation of nanometer iron ferric oxide particles: dissolving divalent iron salt and ferric salt in water, the concentration of ferrous salt is 0.1-0.4mol / L, and the concentration of ferric salt is 0.2-0.8mol / L; After ultrasonic dispersion for 1-10 minutes, add excess ammonia water at 60-90°C until the pH of the solution is 10.0-12.0, stir at 300-600 rpm, mechanically stir at constant temperature and speed, ...

Embodiment 1

[0036] (1) Weigh 5.56g FeSO 4 ?7H 2 O and 10.58 g FeCl 3 ?6H 2 O, dissolved in 200.0mL ultrapure water, ultrasonically dispersed for 5.0 minutes, heated to 60°C, stirring at 300 rpm, adding excess ammonia water until the pH was -11.0, reacting at constant temperature and speed for 1.0 hours, magnetic separation, successively Washing with ultra-pure water and ethanol for several times until the pH is 6-8, and drying in vacuum at 60°C for 12 hours to prepare nanometer ferric oxide particles.

[0037] (2) Weigh 2.0 g of the nano-iron ferric oxide particles prepared in step (1), and add it to 200.0 mL of ethanol solution, ultrasonically disperse for 5.0 minutes, and stir the reaction at a constant temperature of 60 ° C at a stirring speed of 300 rpm Minutes, 20.0mL oleic acid was added dropwise at a constant speed within 10 minutes, and after 1.0 hours of reaction, magnetically separated, washed with ethanol several times until the pH was 6-8, and vacuum-dried at 60°C for 12 ho...

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Abstract

The invention discloses a preparation method of a magnetic nanometer molecular imprinting composite material related to estrogen, comprising the following steps: dissolving bivalent iron salt and trivalent iron salt into water, performing ultrasonic dispersion, heating and regulating the system till being alkali, stirring the system, performing magnetic separation, washing the system till that pH is 6-8, and drying the system; adding ethanol solution, performing heating, stirring and dropping oleic acid, performing magnetic separation, washing the system till that pH is 7.0, and drying the system; adding a dispersant, a polymerization monomer, a functional monomer and a cross linker, and performing ultrasonic dispersion; adding an initiator, performing heating, stirring and magnetic separation, washing the system till that pH is 6-8, and drying the system; adding a composite reaction liquid of a template molecule and amino functional reagent, performing heating, stirring and magnetic separation, washing the system till that pH is 6-8, and drying the system to obtain a target product. The preparation method has the advantages of simple preparation process, controllable magnetic content, controllable functional group proportion and so on, and can arrive at a high enrichment factor when being applied in residual trace phenol environmental estrogens in enrichment drinking water.

Description

technical field [0001] The invention relates to a preparation method of an amino-functional nano-ferric iron tetroxide magnetic molecular imprinting composite material with a core-shell structure, in particular to a preparation method of an aminated nano-ferric iron tetroxide magnetic molecular imprinting composite material. Background technique [0002] With the rapid development of modern industry and agriculture, the pollution and harm of phenolic environmental estrogens have become the focus of attention of all countries in the world. The latest research shows that 0.1μg / L or even lower levels of phenolic environmental estrogen can cause biological effects in experimental animals and interfere with the secretion of endogenous hormones in organisms. an important direction of research. Among them, some phenolic environmental estrogens are used as additives for the preparation of epoxy resins and polycarbonate plastics. When they enter the organism, they can cause endocrin...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08F220/14C08F220/32C08F8/32C08J9/26B01J20/26B01J20/28B01J20/30C02F1/28C02F1/58
Inventor 赵永纲金米聪陈晓红
Owner NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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