Method for preparing high-density crown ether site porous adsorbent by surface photoinitiation

A porous adsorbent, high-density technology, applied in chemical instruments and methods, process efficiency improvement, alkali metal oxides/hydroxides, etc. It can improve the kinetic performance, avoid binding instability, and simplify the preparation process.

Active Publication Date: 2019-11-05
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the deficiencies in the prior art, the purpose of the present invention is to overcome the problems of low density of action sites, poor adsorption performance, and need to improve the selectivity of existing organic / composite adsorbents; to provide a surface photoinitiated preparation of high-density crown ether site porous Adsorbent method with 2AM12C4 as Li + Selective ligands, based on PolyHIPEs porous polymers, prepared a porous adsorbent (PVBC-g-PCE) grafted with crown ether polymer chains on the surface

Method used

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  • Method for preparing high-density crown ether site porous adsorbent by surface photoinitiation
  • Method for preparing high-density crown ether site porous adsorbent by surface photoinitiation
  • Method for preparing high-density crown ether site porous adsorbent by surface photoinitiation

Examples

Experimental program
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Effect test

Embodiment 1

[0041] (1) Preparation of 2AM12C4;

[0042] Mix 9mmol of 30% potassium hydride dispersion in mineral oil with 1.9mmol of 2-hydroxymethyl-12-crown-4 (2M12C4) in 30mL DMF for 30min at room temperature, then add 10mmol of allyl bromide , the reaction was quenched with methanol after stirring overnight, methanol was then evaporated under reduced pressure, the product was washed three times with water, and then washed with CH 2 Cl 2 Extraction with MgSO 4 Dry and filter. The solvent was removed by rotary evaporation and the residue was purified by column chromatography with SiO as stationary phase 2 , the mobile phase is hexane with a volume ratio of 1:2: EtOAc to obtain 2AM12C4;

[0043] (2) Preparation of porous polymer (PVBC) with chloromethyl groups on the surface;

[0044] Add 3.0mL 4-VBC, 0.5mL EGDMA, and 30mg AIBN into a 100mL three-neck flask, and sonicate for 5.0min to completely dissolve AIBN. Under mechanical stirring at 500rpm, slowly add 1.0mL Hypermer 2296 dropw...

Embodiment 2

[0055] (1) Preparation of 2AM12C4;

[0056] Mix 12 mmol of 30% potassium hydride dispersion in mineral oil with 2.2 mmol of 2-hydroxymethyl-12-crown-4 (2M12C4) in 40 mL of DMF for 30 min at room temperature, then add 12 mmol of allyl bromide , the reaction was quenched with methanol after stirring overnight, methanol was then evaporated under reduced pressure, the product was washed three times with water, and then washed with CH 2 Cl 2 Extraction with MgSO 4 Dry and filter. The solvent was removed by rotary evaporation and the residue was purified by column chromatography with SiO as stationary phase 2 , the mobile phase is hexane:EtOAc with a volume ratio of 1:2 to obtain 2AM12C4;

[0057] (2) preparation of porous polymer (PVBC);

[0058] Add 4.0mL of 4-VBC, 0.67mL of EGDMA, and 40mg of AIBN into a 100mL three-neck flask, and sonicate for 8.0min to completely dissolve AIBN. Under mechanical stirring at 700rpm, slowly add 1.34mL Hypermer 2296 dropwise to the flask, aft...

Embodiment 3

[0064] (1) Preparation of 2AM12C4;

[0065] Mix 15 mmol of 30% potassium hydride dispersion in mineral oil with 2.5 mmol of 2-hydroxymethyl-12-crown-4 (2M12C4) in 50 mL of DMF for 30 min at room temperature, then add 15 mmol of allyl bromide , the reaction was quenched with methanol after stirring overnight, methanol was then evaporated under reduced pressure, the product was washed three times with water, and then washed with CH 2 Cl 2 Extraction with MgSO 4 Dry and filter. The solvent was removed by rotary evaporation and the residue was purified by column chromatography with SiO as stationary phase 2 , the mobile phase is hexane:EtOAc with a volume ratio of 1:2 to obtain 2AM12C4;

[0066] (2) preparation of porous polymer (PVBC);

[0067] Add 5.0mL 4-VBC, 0.83mL EGDMA, and 50mg AIBN into a 100mL three-necked flask, and sonicate for 10.0min to completely dissolve AIBN. Under mechanical stirring at 1000rpm, slowly add 1.67mL Hypermer 2296 dropwise to the flask, after mi...

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Abstract

The invention belongs to the technical field of adsorption separation functional material preparation, and particularly relate to a method for preparing a high-density crown ether site porous adsorbent by surface photo initiation. The method includes the following steps that first, 2AM12C4 and PVBC are prepared and obtained; the PVBC is added into a mixed liquor of water and DMF, water-free Na2S2O3 after ultrasonic dissolution is added, and water bath, ethanol cleaning, and air drying are conducted to obtain PVBC-S2O3 which is added into a quartz bottle with the 2AM12C4, after being sealed, nitrogen is introduced under ultraviolet irradiation, the grafting polymerization of the monomer 2AM12C4 is initiated on the surface of the PVBC-S2O3 and at last, ethanol cleaning, and air drying are conducted to obtain PVBC-g-PCE; and a substrate material contains a large amount of chloromethyl group through participation of 4-VBC in polymerization, the unstable combination caused by subsequent modification is avoided, preparation processes are simplified, and the dynamic performance and adsorption capacity of the adsorbent are improved.

Description

technical field [0001] The invention belongs to the technical field of preparation of adsorption and separation functional materials, and in particular relates to a method for preparing a high-density crown ether site porous adsorbent induced by surface light. Background technique [0002] Lithium (Li), known as "white oil", as a new type of green energy, has important applications in national economy and national defense construction. With the continuous development of lithium batteries, ceramics, glass, metallurgy and other fields, the society's demand for lithium resources continues to increase. my country's lithium resources are mainly distributed in salt lake brine, and the production cost of extracting lithium from salt lake brine is low, the technology investment is small, and the profit is considerable. Therefore, extracting lithium from salt lake brine has great significance and application prospects. [0003] The commonly used methods for extracting lithium resou...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J20/30C22B26/12C22B3/24
CPCB01J20/262B01J20/28054B01J20/30C22B26/12C22B3/24Y02P10/20
Inventor 白雪潘建明陈学平黄伟
Owner JIANGSU UNIV
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