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Method for preparing magnetic lithium-ion imprinted microspheres by surface polymerization using macrocyclic polyether olefins as functional monomers

A technology of macrocyclic polyethers and functional monomers, applied in chemical instruments and methods, and other chemical processes, can solve the problems that no one has prepared lithium-ion imprinted polymers, and achieve controllable morphology, good selectivity, highly specific effect

Active Publication Date: 2016-01-13
SHANGRAO DINGXIN METAL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But so far, no one has made lithium-ion imprinted polymers

Method used

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  • Method for preparing magnetic lithium-ion imprinted microspheres by surface polymerization using macrocyclic polyether olefins as functional monomers
  • Method for preparing magnetic lithium-ion imprinted microspheres by surface polymerization using macrocyclic polyether olefins as functional monomers

Examples

Experimental program
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Effect test

Embodiment 1

[0025] (1) Fe 3 o 4 Preparation: 13.5g of FeCl 3 ·6H 2 O was dissolved in a 250mL three-neck flask, nitrogen gas was introduced for 10min, and then 6.95g of Fe was added 2 SO 4 ·7H 2 O, continue to pass nitrogen for 10min, stir rapidly, and slowly add 50mL of concentrated ammonia water to the solution, react at 90°C for 2h, and vacuum dry to obtain Fe 3 o 4 .

[0026] (2) Fe 3 o 4 SiO 2 Preparation: 5.00gFe 3 o 4 Add 250mL of isopropanol and 20mL of high-purity water to the mixed solution, stir evenly and ultrasonically treat for 15min, then add 20mL of ammonia water and 33.3mL of ethyl orthosilicate in sequence. After stirring and reacting at room temperature for 12 hours, the product was separated by a magnet and washed with ultrapure water to neutrality to obtain Fe 3 o 4 SiO 2 .

[0027] (3) MH-Fe 3 o 4 SiO 2 Preparation: take 5.00gFe 3 o 4 SiO 2 The suspension was sonicated for 20min, then stirred rapidly to make the Fe 3 o 4 SiO 2 The particles a...

Embodiment 2

[0032] (1) Fe 3 o 4 Preparation: 13.5g of FeCl 3 ·6H 2 O was dissolved in a 250mL three-neck flask, nitrogen gas was introduced for 5min, and then 6.95g of Fe was added 2 SO 4 ·7H 2 O, continue to pass nitrogen gas for 20 minutes, stir rapidly, and slowly add 50 mL of concentrated ammonia water to the solution, react at 90 ° C for 4 hours, and dry in vacuum to obtain Fe 3 o 4 .

[0033] (2) Fe 3 o 4 SiO 2 Preparation: 5.00gFe 3 o 4 Add 250mL of isopropanol and 20mL of high-purity water to the mixed solution, stir evenly and ultrasonically treat for 15min, then add 20mL of ammonia water and 33.3mL of ethyl orthosilicate in sequence. After stirring and reacting at room temperature for 12 hours, the product was separated by a magnet and washed with ultrapure water to neutrality to obtain Fe 3 o 4 SiO 2 .

[0034] (3) MH-Fe 3 o 4 SiO 2 Preparation: take 5.00gFe 3 o 4 SiO 2 The suspension was sonicated for 20min, then stirred rapidly to make the Fe 3 o 4 SiO...

Embodiment 3

[0039] (1) Fe 3 o 4 Preparation: 13.5g of FeCl 3 ·6H 2 O was dissolved in a 250mL three-neck flask, nitrogen gas was introduced for 8min, and then 6.95g of Fe was added 2 SO 4 ·7H 2 O, continue nitrogen gas for 15min, stir rapidly, and slowly add 50mL concentrated ammonia water dropwise to the solution, at 90 ℃ Under the conditions of reaction for 2h, vacuum drying to obtain Fe 3 o 4 .

[0040] (2) Fe 3 o 4 SiO 2 Preparation: 5.00gFe 3 o 4 Add 250mL of isopropanol and 20mL of high-purity water to the mixed solution, stir evenly and ultrasonically treat for 15min, then add 20mL of ammonia water and 33.3mL of ethyl orthosilicate in sequence. After stirring and reacting at room temperature for 12 hours, the product was separated by a magnet and washed with ultrapure water to neutrality to obtain Fe 3 o 4 SiO 2 .

[0041] (3) MH-Fe 3 o 4 SiO 2 Preparation: take 5.00gFe 3 o 4 SiO 2 The suspension was sonicated for 20min, then stirred rapidly to make the Fe 3...

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Abstract

The invention discloses a method for preparing magnetic lithium ionic imprinting microspheres by using a surface polymerization method implemented by taking macrocyclic polyethers as a functional monomer, which comprises the following steps: (1) by taking FeCl3 and FeCl2 as raw materials, preparing magnetic nano Fe3O4 particles by using a microwave coprecipitation method; (2) enabling Fe3O4 to react with tetraethoxysilane and 3-(trimethoxysilyl) allyl trimethyl, so that MH-Fe3O4 @ SiO2 is obtained; (3) by taking a macrocyclic polyether compound with hydroxyl functional groups as raw materials, enabling the MH-Fe3O4 @ SiO2 and bromopropylene to have a nucleophilic substitution reaction; (4) by taking lithium ions as a template, carrying out imprinted polymerization on the surface of the MH-Fe3O4 @ SiO2 so as to obtain a polymer; and (5) carrying out eluting and vacuum drying on the polymer so as to obtain a lithium ionic imprinting polymer. The novel lithium ionic imprinting polymer synthesized according to the invention has the characteristics of simple preparation, large adsorption capacity, high selectivity and good regenerability.

Description

technical field [0001] The invention relates to a method for preparing ion-imprinted microspheres, in particular to a method for preparing magnetic lithium ion-imprinted microspheres by surface polymerization using macrocyclic polyether olefins as functional monomers. technical background [0002] Lithium is a common alkali metal. In addition to its high electrode potential and electrochemical equivalent, its compounds are used as active materials in lithium-ion batteries, and are also widely used in catalysts, intermediates and metal alloys for the synthesis of drugs. Aerosol etc. With the widespread use of lithium batteries, the demand for metal lithium has increased significantly. However, after hundreds of charge and discharge cycles of lithium-ion batteries, the electrodes will swell and the layered structure of the active material will be blocked. [0003] And inactivation, the battery capacity drops sharply until it is scrapped; the service life of lithium-ion batter...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F216/14C08F222/14C08J9/26B01J20/26B01J20/30
Inventor 罗旭彪郭斌邓芳罗胜联
Owner SHANGRAO DINGXIN METAL CHEM
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