Preparation method of magnetic lead ion surface imprinting polymer

A surface imprinting, lead ion technology, applied in the direction of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., can solve the problems of poor rigidity, thermal instability, limited hydroxyl content, etc. The effect of improving adsorption capacity, improving introduction efficiency, and improving adsorption performance

Inactive Publication Date: 2014-04-09
HEBEI UNIV OF TECH
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Problems solved by technology

[0004] The above methods usually have the following problems: (1) Generally, the magnetic imprints synthesized are based on Fe 3 o 4 As the core, a layer of SiO is coated on the outside 2 , and then using SiO 2 The hydroxyl groups on the surface are directly grafted with functional monomers, or undergo silanization and related subsequent reactions to synthesize imprinted materials
But SiO 2 The hydroxyl content on the surface is limited, which will affect the grafting rate of functional monomers or the effect of silane coupling agent surface modification
(2) Grafting polymerizable double bonds on the outer layer of the carrier, mostly using γ-(methacryloyloxy)propyltrimethoxysilane to introduce double bonds (Zhang Shuanhong, Sun Changmei, Qu Rongjun. Surface molecules (ions) Advances in the preparation and performance of imprinted silica gel / polymer. Polymer Bulletin, 2010(4):17-29.), but it is thermally unstable, under conventional silanization conditions (110°C toluene as solvent for reflux ) will undergo thermal polymerization, but if the temperature is lowered, the efficiency of the introduction of double bonds will be reduced
However, the rigidity of methacrylic acid is not good, and the rigidity of the synthesized imprinted holes is small, which affects the reuse performance
(4) In the reported literature and patents, the adsorbent is often used alone for the adsorption of trace or trace ions, which limits the scope of use of the adsorbent

Method used

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  • Preparation method of magnetic lead ion surface imprinting polymer
  • Preparation method of magnetic lead ion surface imprinting polymer
  • Preparation method of magnetic lead ion surface imprinting polymer

Examples

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Embodiment 1

[0029] (1) Fe 3 o 4 Synthesis of: 2.78g FeSO 4 ·7H 2 O and 4.73gFeCl 3 ·6H 2 O dissolved in 100g ultrapure water (ultrapure water is water that almost completely removes the conductive medium in water, and removes non-dissociated colloidal substances, gases and organic substances in water to a very low level. The resistivity is greater than 18MΩ*cm, Or close to the limit value of 18.3MΩ*cm.) In, through N 2 Under the condition of vigorous stirring (stepless speed regulation booster agitator, the speed regulation gear is set to 2.5 (DW-Ⅱ type, Yuhua Instrument Co., Ltd., Gongyi City), add 10g of 25-28% mass percent Ammonia water, react at 60°C for 1 hour, add 0.5g citric acid to react for 60 minutes, magnetically separate after cooling, collect the black sediment, remove the supernatant, wash with ultrapure water until neutral, then wash with 50mL absolute ethanol for 2 to 3 times, Vacuum dried to obtain Fe 3 o 4 Nanoparticles; (2) Fe 3 o 4 SiO 2 Synthesis of microsp...

Embodiment 2

[0033] (1) Fe 3 o 4 Synthesis of: 5.56g FeSO 4 ·7H 2 O and 9.46 g FeCl 3 ·6H 2 O dissolved in 200g ultrapure water, pass N 2 Under the conditions, add 20g of ammonia water with a mass percentage concentration of 25-28% under vigorous stirring, react at 60°C for 1h, add 1g of citric acid for 90min, and magnetically separate after cooling, collect the black sediment, remove the supernatant, and use ultra-pure Wash with water until neutral, then wash with 50mL absolute ethanol for 2 to 3 times, and dry in vacuum to obtain Fe 3 o 4 Nanoparticles; (2) Fe 3 o 4 SiO 2 Synthesis of microspheres: 2gFe 3 o 4 Ultrasonic dispersion of nanoparticles in a mixed solution consisting of 158g methanol and 40g distilled water, add 6g ammonia water and 12g ethyl orthosilicate, react at room temperature for 24h, magnetically separate the product, collect the sediment, remove the upper solution, successively wash with 50mL distilled water and 50mL Wash with absolute ethanol 2 to 3 times...

Embodiment 3

[0035] (1) Fe 3 o 4 Synthesis of: 2.78g FeSO 4 ·7H 2 O and 4.73gFeCl 3 ·6H 2 Dissolve O in 100g ultrapure water, pass N 2 Under the conditions, add 15g of ammonia water with a mass percentage concentration of 25-28% under vigorous stirring, react at 70°C for 1h, add 0.5g of citric acid for 60min, and magnetically separate after cooling, collect the black sediment, remove the supernatant, and use supernatant Wash with pure water until neutral, then wash with 50mL absolute ethanol for 2 to 3 times, and dry in vacuum to obtain Fe 3 o 4 Nanoparticles; (2) Fe 3 o 4 SiO 2 Synthesis of microspheres: 1 gFe 3 o 4 Ultrasonic dispersion of nanoparticles in a mixed solution consisting of 79g of absolute ethanol and 20g of distilled water, add 4g of ammonia water and 7g of ethyl orthosilicate, react at room temperature for 12h, magnetically separate the product, collect the sediment, remove the upper solution, and successively wash with 50mL of distilled water and 50 mL of abso...

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Abstract

The invention discloses a preparation method of a magnetic lead ion surface imprinting polymer. The method comprises the following steps: firstly, synthesizing magnetic Fe3O4@SiO2 microspheres by using a 'coprecipitation method' and a 'sol-gel method', processing by using an acid, so as to improve the hydroxy content of the surface; then leading polymerizable double bonds to the surfaces of the Fe3O4@SiO2 microspheres by using a 'two-step process', firstly, grafting amino on the surfaces of the microspheres by using an amino silane coupling agent; generating double bonds by using reaction of anhydride and amino; finally taking the Fe3O4@SiO2 microspheres as a carrier, the Pb(II) as a template, ethylene glycol dimethacrylate as a crosslinking agent and methacrylic acid and salicylaldoxime as monomers to carry out polymerization reaction; and washing off the template Pb(II) after reaction is ended, so as to obtain a polymer layer with a lot of Pb(II) imprinting cavities distributed at the surfaces of the Fe3O4@SiO2 microspheres. The magnetic lead ion surface imprinting polymer disclosed by the invention can be applied to separation and removal of lead ions.

Description

technical field [0001] The invention relates to a preparation method of a magnetic lead ion surface imprinted polymer, in particular to a lead ion surface imprinted polymer with a core-shell structure and magnetic properties. Background technique [0002] Lead is mainly used as materials for cables, storage batteries, type alloys, X-ray and β-ray protection, etc. Lead alloys can be used for type casting and soldering. In recent years, with the rapid development of my country's industry, lead pollution has become increasingly serious and has become a major public hazard affecting human health. The acceptable maximum lead concentration in drinking water is 0.1-0.05mg / L. According to surveying and measuring, when blood lead concentration in the human body exceeds 0.3g / L, symptoms such as dizziness, insomnia, anemia and abdominal pain will occur. Therefore, it is of great significance to study the separation and removal of lead. At present, the common treatment methods includ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/14C08F220/06C08F2/44C08J9/26B01J20/26B01J20/28B01J20/30
Inventor 张惠欣窦倩
Owner HEBEI UNIV OF TECH
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