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Preparation method and application of a selective dynamic solid phase extraction cerium ion imprinted polymer

A technology of imprinting polymers and cerium ions, which is applied in chemical instruments and methods, radioactive purification, water/sludge/sewage treatment, etc., can solve the problems of loss of exchange groups, low adsorption capacity, poor thermal stability, etc., and achieve superior The effect of cerium ion recognition performance, large specific surface area, good mechanical properties and thermal stability

Inactive Publication Date: 2015-12-09
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the thermal stability of ion exchange and adsorption solid phase extraction technology is poor, it is easy to lose the exchange group at high temperature, it will degrade under the action of radiation, and the adsorption capacity is low; solvent extraction technology uses a lot of organic solvents, which is easy to produce secondary pollution

Method used

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  • Preparation method and application of a selective dynamic solid phase extraction cerium ion imprinted polymer
  • Preparation method and application of a selective dynamic solid phase extraction cerium ion imprinted polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Put 0.25g of SBA-15 in a round bottom flask, add 150mL hydrochloric acid with a concentration of 3mol / L, reflux for 24h, then filter, wash repeatedly with deionized water twice until neutral, vacuum dry at 80°C for 6h and take it out.

[0043] (2) Add 0.25g of SBA-15 treated in step (1) and 0.25mL of 4-(chloromethyl)phenyltrimethoxysilane to a solution of 10mL of toluene in turn, and place the mixed solution at 90°C In an oil bath, under the protection of nitrogen, stir magnetically for 24 hours. After the reaction, the product is washed 5 times with toluene and methanol successively to elute unreacted 4-(chloromethyl)phenyltrimethoxysilane and toluene. The obtained chlorine-functionalized mesoporous material (SBA-15-Cl) was dried under vacuum.

[0044] (3) Add 8 mL of phenylmagnesium bromide (PMB) into a three-necked flask, preheat the oil bath to 40 ° C, and add 0.5 mL of dry carbon disulfide (CS 2 ), under the protection of nitrogen, maintain the temperature of ...

Embodiment 2

[0054] (1) Put 1g of SBA-15 in a round bottom flask, add 150mL hydrochloric acid with a concentration of 3mol / L, reflux for 24h, then filter, wash repeatedly with deionized water twice until neutral, vacuum dry at 80°C for 6h and take out.

[0055] (2) Add 0.5g of SBA-15 treated in step (1) and 0.5mL of 4-(chloromethyl)phenyltrimethoxysilane to a solution of 20mL of toluene in turn, and place the mixed solution at 90°C In an oil bath, under the protection of nitrogen, stir magnetically for 24 hours. After the reaction, the product is washed 5 times with toluene and methanol successively to elute unreacted 4-(chloromethyl)phenyltrimethoxysilane and toluene. The obtained chlorine-functionalized mesoporous material (SBA-15-Cl) was dried under vacuum.

[0056] (3) Add 16 mL of phenylmagnesium bromide (PMB) into a three-necked flask, preheat the oil bath to 50 ° C, and add 1 mL of dry carbon disulfide (CS) dropwise under nitrogen protection. 2 ), under the protection of nitrogen, ...

Embodiment 3

[0066] (1) Put 2.5g of SBA-15 in a round bottom flask, add 150mL hydrochloric acid with a concentration of 3mol / L, reflux for 24h, then filter, wash repeatedly with deionized water twice until neutral, vacuum dry at 80°C for 6h, and then take it out.

[0067](2) Add 1 g of SBA-15 treated in step (1) and 1.0 mL of 4-(chloromethyl)phenyltrimethoxysilane to a solution of 40 mL of toluene in sequence, and place the mixed solution in 90°C oil bath, under a nitrogen atmosphere, magnetically stirred for 24 h, and after the reaction, the product was washed 5 times with toluene and methanol successively to elute unreacted 4-(chloromethyl)phenyltrimethoxysilane and toluene. The obtained chlorine-functionalized mesoporous material (SBA-15-Cl) was dried under vacuum.

[0068] (3) Add 32 mL of phenylmagnesium bromide (PMB) into a three-necked flask, preheat the oil bath to 60 °C, and add 2 mL of dry carbon disulfide (CS) dropwise under nitrogen protection. 2 ), under the protection of nit...

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Abstract

The invention relates to a preparation method and application of a cerium ion imprinted polymer by virtue of selective dynamic solid phase extraction and belongs to the technical field of material preparation and separation. The invention particularly relates to a method for preparing a cerium ion imprinted polymer by using an ordered mesoporous material SBA-15 as a substrate, metal cerium ions as a template, 4-(chloromethyl)phenyltrimethoxysilane as a coupling agent, 4-vinylpyridine as a functional monomer, ethyleneglycol dimethacrylate as a cross-linking agent, azodiisobutyronitrile as an initiating agent and a reversible addition-fragmentation chain transfer (RAFT) polymerization as a polymerization mode. The selective identification performance of the prepared adsorbing material is researched by selecting a dynamic adsorption experiment. The RAFT polymerization is firstly adopted to synthesize the imprinted polymer by selective dynamic solid phase extraction and separation conditions of cerium ions in an aqueous solution are researched by using the dynamic adsorption experiment. Results show that a cerium ion imprinted polymer adsorbing material obtained by the invention has excellent adsorption and identification performances for the cerium ions.

Description

technical field [0001] The invention relates to a preparation method for synthesizing ion-imprinted polymers on the surface of mesoporous materials using reversible addition-fragmentation chain transfer polymerization technology, in particular to a preparation method for selective dynamic solid-phase extraction of cerium ion-imprinted polymers, and is applied to The invention relates to dynamic adsorption and separation of cerium ions in aqueous solution, belonging to the technical field of material preparation and separation. Background technique [0002] The development and utilization of nuclear materials has driven the development of the world, but at the same time, the harm caused is also becoming more and more serious. The mining and processing of nuclear fuel, the leakage of nuclear reactors, the reprocessing of nuclear fuel, and the use of nuclear weapons have become the main sources of radioactive elements in the environment. Europium, uranium, strontium, thorium, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F226/06C08F222/14C08J9/26B01J20/26B01J20/30C02F1/28C02F1/62G21F9/12
Inventor 刘燕孟祥国倪良陈瑞孟敏佳刘方方胡兆勇
Owner JIANGSU UNIV