Chloromethyl polystyrene resin immobilized 1-aminoethyl-3-methylimidazolium bromide solid-phase extractant and its preparation method and application

A technology of chloromethyl polystyrene and methyl imidazolium bromide, which is applied in chemical instruments and methods, extraction water/sewage treatment, preparation of test samples, etc., can solve the mechanism of reducing selective adsorption and adsorption of pollutants and different effects, different methods and mechanisms, etc., to achieve the effect of recyclable sensitivity, good industrial application value, and simple synthesis method

Active Publication Date: 2019-11-22
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] It can be seen from the above that the existing loaded phenolic extractants either have no ionic liquid structure and do not have the advantages of ionic liquids; Separation and enrichment; either the type of ionic liquid on the solid support is different from that of the present invention, and the prepared adsorbent has a different structure, so the mechanism and effect of adsorption are also different
The technologies related to the immobilization of amino-based ionic liquids are mainly immobilized on porous carriers such as activated carbon and silica gel. Not only are the loading methods and mechanisms different, but they also reduce the selective adsorption of materials to pollutants, and their applications are mainly as catalysts. or absorb CO 2 , did not investigate the separation and enrichment effect of phenolic compounds

Method used

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  • Chloromethyl polystyrene resin immobilized 1-aminoethyl-3-methylimidazolium bromide solid-phase extractant and its preparation method and application
  • Chloromethyl polystyrene resin immobilized 1-aminoethyl-3-methylimidazolium bromide solid-phase extractant and its preparation method and application
  • Chloromethyl polystyrene resin immobilized 1-aminoethyl-3-methylimidazolium bromide solid-phase extractant and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 5g chloromethyl polystyrene resin and add 40mL N-methylpyrrolidone to swell for 24h, add 13.5g 1-aminoethyl-3-methylimidazolium bromide (chloromethyl polystyrene resin and 1-aminoethyl -3-Methylimidazolium bromide molar ratio 1:3) and 2.5g anhydrous K 2 CO 3, and then add 60mL N-methylpyrrolidone, seal the mixture and place it in an oil bath at 80°C for 12 hours. After the reaction, cool to room temperature, and wash the product with deionized water and absolute ethanol in turn until no 1-aminoethyl ether can be detected. Based on the absorbance of 3-methylimidazolium bromide salt and N-methylpyrrolidone, put the product in a forced air drying oven and dry it until no obvious water sample can be seen, then place it at 45°C for 24 hours in vacuum, and finally obtain The pale yellow solid chloromethyl polystyrene resin is immobilized with 1-aminoethyl-3-methylimidazolium bromide ionic liquid solid-phase extractant, and the product is sealed in a bottle and stored i...

Embodiment 2

[0037] Weigh 0.5g of chloromethyl polystyrene resin and add 10mL of N-methylpyrrolidone to swell for 12h, then add 4.6g of 1-aminoethyl-3-methylimidazolium bromide (chloromethyl polystyrene resin and 1-aminoethyl base-3-methylimidazolium bromide molar ratio 1:10) and 0.2mL triethylamine, then add 20mL N-methylpyrrolidone, seal the mixture and put it in an oil bath at 100°C for 8 hours. After the reaction Cool to room temperature, wash the product successively with deionized water and absolute ethanol until the absorbance of 1-aminoethyl-3-methylimidazolium bromide and N-methylpyrrolidone cannot be detected, and place the product in a blast drying oven After drying until no obvious water sample can be seen, place it at 45°C for 24 hours in a vacuum to obtain a light yellow solid chloromethyl polystyrene resin immobilized 1-aminoethyl-3-methylimidazolium bromide salt ionic liquid Solid phase extraction agent, the product is sealed in a bottle and stored in a desiccator for later...

Embodiment 3

[0041] Weigh 1g of chloromethyl polystyrene resin and add 10mL N-methylpyrrolidone to swell for 24h, then add 5.6g of 1-aminoethyl-3-methylimidazolium bromide (chloromethyl polystyrene resin and 1-aminoethyl -3-Methylimidazolium bromide molar ratio 1:6) and 0.5g anhydrous Na 2 CO 3 , then add 20mL of N-methylpyrrolidone, seal the mixture and place it in a 70°C oil bath for 14 hours of reaction. After the reaction, cool to room temperature, and wash the product with deionized water and absolute ethanol in turn until no 1-aminoethyl ether can be detected. Based on the absorbance of 3-methylimidazolium bromide salt and nitrogen-methylpyrrolidone, the product was dried in a forced air drying oven until no obvious water samples were seen, and then placed in vacuum at 45°C for 24 hours, and finally obtained light The yellow solid chloromethyl polystyrene resin is immobilized with 1-aminoethyl-3-methylimidazolium bromide salt ionic liquid solid-phase extractant, and the product is s...

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Abstract

The invention discloses a chloromethyl polystyrene resin immobilized 1-aminoethyl-3-methylimidazole bromate solid-phase extracting agent as well as a preparation method and application thereof, and belongs to the technical fields of solid-phase extraction and the pretreatment of samples. The chloromethyl polystyrene resin immobilized 1-aminoethyl-3-methylimidazole bromate solid-phase extracting agent is characterized in that the solid-phase extracting agent is made through grafting 1-aminoethyl-3-methylimidazole bromate ionic liquid on the surface of chloromethyl polystyrene resin through chemical bonding; the structural formula of the chloromethyl polystyrene resin immobilized 1-aminoethyl-3-methylimidazole bromate solid-phase extracting agent is as shown in the following descriptions. The invention also specifically discloses the preparation method and the application of the chloromethyl polystyrene resin immobilized 1-aminoethyl-3-methylimidazole bromate solid-phase extracting agent to separation and enrichment as well as the removal of paranitrophenol in a sample. The solid-phase extracting agent provided by the invention has the advantages of being simple and convenient in synthesis method, high in adsorption capacity, good in selectivity, high in anti-interference ability and high in sensitivity and being capable of being recycled, and the like.

Description

technical field [0001] The invention belongs to the technical field of solid-phase extraction and sample pretreatment, and in particular relates to a chloromethyl polystyrene resin-immobilized 1-aminoethyl-3-methylimidazolium bromide solid-phase extraction agent and a preparation method and application thereof. Background technique [0002] With the rapid development of industrialization and urbanization, various organic pollutants are discharged into the environment, causing serious environmental problems. p-nitrophenol is an important industrial raw material and intermediate in the production process of medicine, pesticide, dyestuff, artificial resin, explosive and other fine chemicals, and it is easy to enter and pollute water bodies in these production processes. As a common phenolic pollutant in the water environment, p-nitrophenol has carcinogenic, teratogenic, and mutagenic potential toxicity and is difficult to degrade. Even a very low concentration can cause great h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/286B01J20/30C02F1/26G01N1/40G01N1/34C02F101/38C02F101/34
CPCB01J20/265B01J20/286C02F1/26C02F2101/345C02F2101/38G01N1/34G01N1/405
Inventor 樊静程萌师东阳杜亭如苏梦圆赵扬扬刘闯马梦迪张晓迪吴甜
Owner HENAN NORMAL UNIV
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