Preparation method of magnetic zinc ion surface-imprinted polymer

A technology of surface imprinting and zinc ions, applied in the direction of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., can solve problems such as limited hydroxyl content, poor rigidity, and thermal instability, and achieve Effects of improving adsorption performance, increasing adsorption capacity, and improving introduction efficiency

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 zinc ion surface-imprinted polymer
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  • Preparation method of magnetic zinc ion surface-imprinted polymer

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0031] (1) Fe 3 o 4 Synthesis of: 2.78g FeSO 4 ·7H 2 O and 4.73 g FeCl 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 micro...

Embodiment 2

[0035] (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: 2g Fe 3 o 4 Ultrasonic dispersion of nanoparticles in a mixed solution consisting of 158g methanol and 40g distilled water, add 8g ammonia water and 14g 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 time...

Embodiment 3

[0037] (1) Fe 3 o 4 Synthesis of: 2.78g FeSO 4 ·7H 2 O and 4.73 g FeCl 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 g Fe 3 o 4 Ultrasonic dispersion of nanoparticles in a mixed solution consisting of 79g of absolute ethanol and 20g of distilled water, add 3g of ammonia water and 8g 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 a...

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Abstract

The invention relates to a preparation method of a magnetic zinc ion surface-imprinted polymer, which comprises the following steps: synthesizing magnetic Fe3O4@SiO2 microspheres by a coprecipitation process and a sol-gel process, and treating with acid to enhance the surface hydroxy content; introducing a polymerizable double bond onto the surface of the Fe3O4@SiO2 microspheres by a two-step process, i.e. grafting amino group onto the microsphere surface by using an aminosilane coupling agent, and reacting acid anhydride with the amino group to generate the double bond; and finally, carrying out polymerization reaction by using the Fe3O4@SiO2 microspheres as a carrier, Zn (II) as a template, ethylene glycol dimethacrylate as a crosslinking agent and methacrylic acid and salicylaldoxime as monomers, and after the reaction finishes, washing out the template Zn (II) to obtain the polymer layer in which abundant Zn (II) imprinted holes are distributed on the Fe3O4@SiO2 microsphere surface. The magnetic zinc ion surface-imprinted polymer can be used for separating and removing zinc ions.

Description

technical field [0001] The invention relates to a preparation method of a magnetic zinc ion surface imprinted polymer, in particular to a magnetic zinc ion surface imprinted polymer with a core-shell structure. Background technique [0002] Zinc is the fourth "most common" metal, after iron, aluminum and copper. In modern society, zinc is mainly used in metallurgy, machinery, chemical industry, light industry, medicine and military and other fields. Although zinc is an essential element for animals and plants, when the concentration of zinc exceeds 300mg / L, it can cause zinc poisoning in animals and affect the photosynthesis of plants. Therefore, the study on the separation and removal of zinc is of great significance. At present, the common treatment methods include ion exchange method, membrane separation method, chemical precipitation method and adsorption method, etc., and the adsorption method is considered to be an efficient and economical method. The specific recog...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08F220/06C08F222/14C08J9/26B01J20/26B01J20/28B01J20/30
Inventor 张惠欣窦倩
Owner HEBEI UNIV OF TECH
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