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Method for preparing crown ether functionalized porous microsphere adsorbent by one-step double-emulsion template method

A technology of porous microspheres and double emulsions, applied in chemical instruments and methods, inorganic chemistry, alkali metal compounds, etc., can solve the problems of unimproved adsorption performance, complex preparation, poor stability, etc., and achieve the effect of high-efficiency and selective separation of lithium

Pending Publication Date: 2021-04-13
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there are many ways to extract lithium from salt lakes, among which the adsorption method has broad application prospects, but the existing adsorbents for lithium extraction are often poor in stability, complicated to prepare, and the adsorption performance needs to be improved

Method used

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  • Method for preparing crown ether functionalized porous microsphere adsorbent by one-step double-emulsion template method
  • Method for preparing crown ether functionalized porous microsphere adsorbent by one-step double-emulsion template method
  • Method for preparing crown ether functionalized porous microsphere adsorbent by one-step double-emulsion template method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Preparation of Porous Multichamber Microspheres Rich in Epoxy Groups on the Surface (PMCB) and Microspheres with Capability of Recognizing and Trapping Lithium Ions (PMCB-B12C4)

[0031] (1) First, 5 mg of phenylselenium bromide and 6 mg of PS-b-P4VP were added to 5 mL of dichloromethane solution for 2 min for uniform dissolution and reaction to obtain an amphiphilic surfactant solution;

[0032] (2) Add 400 μL amphiphilic surfactant solution, 10 μL glycidyl methacrylate, 20 μL ethylene glycol dimethacrylate, and 10 μL Irgacure-1173 photoinitiator to the centrifuge tube, and then Add 1600 μL of deionized water dropwise under high-speed stirring at 1200 r, and after 2 minutes, prepare the water-in-oil-in-water (W / O / W) double emulsion;

[0033](3) The water-in-oil-in-water (W / O / W) double emulsion obtained in (2) was polymerized under ultraviolet light for 2 hours, and finally washed with ethanol and distilled water several times, and dried in a vacuum oven at 45°C for 6 h...

Embodiment 2

[0036] (1) First, 5 mg of phenylselenium bromide and 6 mg of PS-b-P4VP were added to 5 mL of dichloromethane solution for 2 min for uniform dissolution and reaction to obtain an amphiphilic surfactant solution;

[0037] (2) Add 400 μL amphiphilic surfactant solution, 10 μL glycidyl methacrylate, 20 μL ethylene glycol dimethacrylate, and 10 μL Irgacure-1173 photoinitiator to the centrifuge tube, and then Add 1600 μL of deionized water dropwise under high-speed stirring at 1200 r, and after 2 minutes, prepare the water-in-oil-in-water (W / O / W) double emulsion;

[0038] (3) The water-in-oil-in-water (W / O / W) double emulsion obtained in (2) was polymerized under ultraviolet light for 2 hours, and finally washed with ethanol and distilled water several times, and dried in a vacuum oven at 45°C for 6 hours to obtain PMCB .

[0039] (4) 500mg PMCB and 500mg B12C4-NH 2 The crown ether was mixed and added to 50mL of DMF solution, uniformly dispersed by ultrasonic waves for 4 minutes, a...

Embodiment 3

[0041] Preparation of Porous Multichamber Microspheres Rich in Epoxy Groups on the Surface (PMCB) and Microspheres with Capability of Recognizing and Trapping Lithium Ions (PMCB-B12C4)

[0042] (1) First, 5 mg of phenylselenium bromide and 6 mg of PS-b-P4VP were added to 5 mL of dichloromethane solution for 2 min for uniform dissolution and reaction to obtain an amphiphilic surfactant solution;

[0043] (2) Add 400 μL amphiphilic surfactant solution, 10 μL glycidyl methacrylate, 20 μL ethylene glycol dimethacrylate, and 10 μL Irgacure-1173 photoinitiator to the centrifuge tube, and then Add 1600 μL of deionized water dropwise under high-speed stirring at 1200 r, and after 2 minutes, prepare the water-in-oil-in-water (W / O / W) double emulsion;

[0044] (3) The water-in-oil-in-water (W / O / W) double emulsion obtained in (2) was polymerized under ultraviolet light for 2 hours, and finally washed with ethanol and distilled water several times, and dried in a vacuum oven at 45°C for 6 ...

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Abstract

The invention belongs to the technical field of preparation of chemical separation functional materials, and relates to a preparation method of a crown ether modified porous microsphere adsorbent. A water-in-oil-in-water double emulsion prepared by dynamically adjusting amphipathy of a block copolymer through one-step stirring is used as a template and is combined with an ultraviolet-induced polymerization way to obtain porous multi-cavity microspheres, and porous microspheres with the surfaces rich in crown ether active sites are prepared through an interface post-modification strategy; and a series of treatment is carried out to obtain a functional adsorbent, and the adsorbent is used for selective adsorption separation on Li<+> in salt lake brine. The crown ether modified porous multi-cavity microsphere adsorbent prepared by the preparation method disclosed by the invention has rapid adsorption kinetics and stable thermodynamic properties, and has excellent acid-base response characteristics.

Description

technical field [0001] The invention belongs to the technical field of preparation of chemical separation functional materials, and relates to a method for preparing a crown ether functionalized porous microsphere adsorbent by a one-step double emulsion template method. Background technique [0002] Lithium, a valuable alkali metal, is widely known for its wide applications in ceramics, aircraft alloys, lubricants, nuclear energy, pharmaceuticals and especially in the field of electrical storage. In recent years, the upsurge of new energy has driven the rapid growth of global lithium consumption, and the topic of how to efficiently extract raw material lithium has attracted widespread attention. However, lithium is an important commercial product and strategic resource. Except for a small part existing in mineral resources in the form of compounds, most of the known lithium resources mainly exist in relatively low concentrations in salt lakes and other complex environments w...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J20/30C22B26/12C22B3/24
CPCB01J20/268B01J20/28021B01J20/3057B01J20/3085C22B26/12C22B3/24Y02P10/20
Inventor 杨光潘建明
Owner JIANGSU UNIV
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