Preparation method and application of covalently-modified high-density crown ether functionalized porous adsorbent

A porous adsorbent and covalent modification technology, which is applied in chemical instruments and methods, and other chemical processes, can solve the problems that the modification density of the adsorbent ligand needs to be improved, it is difficult to meet the high-efficiency lithium extraction, and the modification density affects the adsorption capacity. Achieve short adsorption equilibrium time, increase adsorption capacity and mass transfer efficiency, and increase the effect of high-density sites

Active Publication Date: 2019-09-13
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

At present, relevant studies have selected crown ethers with 12-14 membered rings as Li + Selective ligands, using high internal phase surface to carry out Li by copolymerization or surface modification + Ligand immobilization, such as Huang et al., used porous polymer foam as the substrate and synthesized 2-hydroxymethyl-12-crown-4 derivatives as ligands to immobilize the crown ether on the porous polymer by surface chemical modification. surface; although such materials have good Li + Selectivity and adsorption kinetics performance, but in order to meet the needs of low concentration, high magnesium lithium ratio brine to extract lithium, we believe that the modification density of the existing adsorbent ligands needs to be improved
Due to the relatively high quality of the substrate material and the limited contact area on the surface, the modification density of the ligand will have a huge impact on the adsorption capacity, and simple mixed copolymerization or surface modification has become increasingly difficult to meet the needs of efficient lithium extraction.

Method used

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  • Preparation method and application of covalently-modified high-density crown ether functionalized porous adsorbent
  • Preparation method and application of covalently-modified high-density crown ether functionalized porous adsorbent
  • Preparation method and application of covalently-modified high-density crown ether functionalized porous adsorbent

Examples

Experimental program
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Effect test

Embodiment 1

[0043] (1) Preparation of porous polymer (PVBC);

[0044] Add 0.5mL EGDMA, 3.0mL4-VBC, 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 to the flask, after mixing well, slowly add 16mL 0.2 M K 2 SO 4 solution; increase the mechanical stirring speed to 800rpm and stir for 2.0min to obtain milky white HIPEs. The prepared HIPEs were transferred into glass ampoules and sealed. The ampoule was polymerized in an oil bath at 70°C for 24 hours, and the obtained porous polymer (PVBC) was purified by a Soxhlet extractor. The solvent used for purification was acetone to remove the internal phase of HIPEs and residual reactants. After purification, Put the PVBC foam into a vacuum oven at 60°C for drying;

[0045] (2) Preparation of a porous polymer (PVBC-g-PGMA) grafted with polyglycidyl methacrylate (PGMA) on the surface;

[0046] Mix methanol, DMF and anisole at a vo...

Embodiment 2

[0050] (1) Preparation of porous polymer (PVBC);

[0051] Add 0.5mL of EGDMA, 2.5mL of 4-VBC, and 25mg of AIBN into a 100mL three-neck flask, and ultrasonicate for 5.0min to completely dissolve AIBN; under mechanical stirring at a speed of 500rpm, slowly add 1.0mL of Hypermer 2296 into the flask, mix well, and add Slowly add 15 mL of 0.2 M K to the flask 2 SO 4 solution, increase the mechanical stirring speed to 800rpm and stir for 2.0min to obtain milky white HIPEs. The prepared HIPEs were transferred into glass ampoules and sealed. The ampoule was placed in an oil bath at 70°C for 24 hours, and the obtained porous polymer (PVBC) was purified by a Soxhlet extractor (solvent was acetone) to remove the internal phase of HIPEs and residual reactants, and the purified PVBC foam Transfer to 60°C vacuum oven for drying for later use;

[0052] (2) Preparation of a porous polymer (PVBC-g-PGMA) grafted with polyglycidyl methacrylate (PGMA) on the surface;

[0053] Mix methanol, D...

Embodiment 3

[0057] (1) Preparation of porous polymer (PVBC);

[0058] Add 0.5mL EGDMA, 3.5mL4-VBC, and 35mg AIBN into a 100mL three-necked flask, and sonicate for 5.0min to completely dissolve AIBN. Under mechanical stirring at 500rpm, slowly add 1.0mL Hypermer 2296 dropwise to the flask, after mixing well, slowly add 17mL 0.2 M K 2 SO 4solution. Increase the mechanical stirring speed to 800rpm and stir for 2.0min to obtain milky white HIPEs; transfer the prepared HIPEs into a glass ampoule and seal, place the ampoule in a 70°C oil bath for polymerization for 24h, and obtain the porous polymer (PVBC) Purify by Soxhlet extractor (solvent is acetone) to remove the internal phase of HIPEs and residual reactants, and the purified PVBC foam is transferred to 60°C vacuum oven for drying for later use;

[0059] (2) Preparation of a porous polymer (PVBC-g-PGMA) grafted with polyglycidyl methacrylate (PGMA) on the surface;

[0060] Mix methanol, DMF and anisole at a volume ratio of 1:1:1 to ob...

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Abstract

The invention belongs to the technical field of preparation of specific separation functional materials, and relates to a preparation method and an application of a covalently-modified high-density crown ether functionalized porous adsorbent. The preparation method comprises the following steps: preparing a porous polymer PVBC and a glycidyl methacrylate surface-grafted porous polymer recorded asPVBC-g-PGMA; mixing the PVBC-g-PGMA with DMF, and adding 2AB12C4 after the PVBC-g-PGMA is dispersed in the DMF; and carrying out a water bath reaction, sequentially washing the obtained product with DMF, ethanol and double distilled water, and performing vacuum drying to obtain the porous adsorbent modified with aminoethylbenzo-12-crown-4. The prepared porous adsorbent effectively improves the adsorption capacity and the mass transfer efficiency, solves the problems of low density and deep embedding of acting sites of existing lithium adsorbents, and provides a new idea for the development ofefficient lithium adsorbents.

Description

technical field [0001] The invention belongs to the technical field of preparation of specific separation functional materials, and in particular relates to a preparation method of a covalently modified high-density crown ether functionalized porous adsorbent. Background technique [0002] Lithium (Li) is an important energy metal and has been widely used in lithium batteries, ceramics, glass, metallurgy, medicine and other fields. Among them, the application of lithium battery industry accounted for the highest proportion, reaching 56%, the application of ceramic and glass industry accounted for 23%, the production of lubricating grease accounted for 6%, the production of polymer accounted for 4%, and the powder of casting mold flux accounted for 3% %, air treatment accounts for about 2%, and other fields account for about 6%. At present, the common methods for obtaining lithium include precipitation, solvent extraction, and adsorption, but the precipitation method depends...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/30
CPCB01J20/262B01J20/30
Inventor 王盼潘建明陈学平黄伟
Owner 合肥九州龙腾科技成果转化有限公司
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