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A method for surface photoinitiated preparation of porous adsorbent with high density crown ether sites

A porous adsorbent, high-density technology, applied in chemical instruments and methods, process efficiency improvement, other chemical processes, etc., can solve problems such as selectivity to be improved, low site density, poor adsorption performance, etc., to avoid binding The effect of instability, improved kinetics, simplified preparation process

Active Publication Date: 2021-12-21
合肥九州龙腾科技成果转化有限公司
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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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  • A method for surface photoinitiated preparation of porous adsorbent with high density crown ether sites
  • A method for surface photoinitiated preparation of porous adsorbent with high density crown ether sites
  • A method for surface photoinitiated preparation of porous adsorbent with high density crown ether sites

Examples

Experimental program
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Effect test

Embodiment 1

[0041] (1) Preparation of 2AM12C4;

[0042] Mix 9 mmol of 30% potassium hydride dispersion in mineral oil with 1.9 mmol of 2-hydroxymethyl-12-crown-4 (2M12C4) in 30 mL of DMF for 30 min at room temperature, then add 10 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 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 of 4-VBC, 0.5mL of EGDMA, and 30mg of 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 Hy...

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-necked 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, a...

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 of 4-VBC, 0.83mL of EGDMA, and 50mg of AIBN into a 100mL three-necked flask, and sonicate for 10.0min to completely dissolve AIBN. Slowly add 1.67mL Hypermer 2296 dropwise to the flask under mechanical stirring at 1000rpm, ...

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Abstract

The invention belongs to the technical field of preparation of adsorption and separation functional materials, and specifically relates to a method for preparing a porous adsorbent with high-density crown ether sites by surface photoinitiation; the steps are as follows: firstly, 2AM12C4 and PVBC are prepared; PVBC is added to the mixed solution of water and DMF, Add anhydrous Na after ultrasonic dissolution 2 S 2 o 3 , after washing in water bath, ethanol, and vacuum drying, PVBC‑S 2 o 3 , and then add 2AM12C4 into the quartz bottle, seal it, pass nitrogen gas and put it under the condition of ultraviolet light irradiation, in PVBC‑S 2 o 3 The graft polymerization of the monomer 2AM12C4 is initiated on the surface of the surface, and finally, PVBC-g-PCE is obtained by ethanol cleaning and vacuum drying; the present invention makes the base material itself have a large amount of chloromethyl groups by participating in the polymerization of 4-VBC, avoiding subsequent modification The phenomena such as unstable combination are caused, the preparation process is simplified, and the kinetic 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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Patent Type & Authority Patents(China)
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 合肥九州龙腾科技成果转化有限公司
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