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Preparation method for porous polymer microsphere anion filling material

A technology of polymer microspheres and anions, used in chemical instruments and methods, other chemical processes, etc., can solve the problems of unreliable particle size control methods, uneven particle size distribution, and easily broken microspheres, and achieve uniform particle size. And controllable, increase retention time, and the effect of less solvent consumption

Inactive Publication Date: 2017-06-20
PEKING UNIV SHENZHEN GRADUATE SCHOOL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above method has the following disadvantages: the particle size is too narrow, and the particle size control method is unreliable; the particle size distribution is not uniform; the microspheres are easily broken and unstable during the swelling process; there are many cumbersome steps in operation

Method used

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  • Preparation method for porous polymer microsphere anion filling material
  • Preparation method for porous polymer microsphere anion filling material
  • Preparation method for porous polymer microsphere anion filling material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Dissolve 5g of polystyrene / divinylbenzene microspheres in 50ml of toluene, stir and swell at room temperature for 3h, cool to room temperature, add 20ml of chloromethyl ether and 2ml of tin chloride, continue stirring at room temperature for 3h, add deionized water to terminate the reaction , washed with hydrochloric acid, tetrahydrofuran, acetone, set aside.

[0034] Take 5.4g of the above-mentioned chloromethylated microspheres, add them into 108ml of chloroform, add 40ml of ethylenediamine, stir and heat to 150°C, and react for 6h. Cool down to room temperature, treat with acetone, water, methanol, and dry in vacuo.

[0035] Take 2.4 g of the above-mentioned ethylenediamine microspheres in 120 ml of toluene, add 6 g of triethylamine, 1.5 g of acetic anhydride, and 15 g of 4-dimethylaminopyridine, and stir overnight at room temperature. Treat with methanol, water, acetone and dry in vacuo.

[0036] image 3 Electron micrographs of polymer microspheres with various ...

Embodiment 2

[0038] Dissolve 5g of polystyrene / divinylbenzene microspheres in 100ml of toluene, stir and swell at room temperature for 3h, cool to room temperature, add 20ml of chloromethyl ether and 4ml of tin chloride, continue stirring at room temperature for 3h, add deionized water to terminate the reaction , washed with hydrochloric acid, tetrahydrofuran, acetone, set aside.

[0039]Take 5.4g of the above-mentioned chloromethylated microspheres, add them into 216ml of chloroform, add 40ml of ethylenediamine, stir and heat to 150°C, and react for 6h. Cool down to room temperature, treat with acetone, water, methanol, and dry in vacuo.

[0040] Take 2.4 g of the above-mentioned ethylenediamine microspheres in 120 ml of toluene, add 6 g of triethylamine, 1.5 g of acetic anhydride, and 30 g of 4-dimethylaminopyridine, and stir overnight at room temperature. Treat with methanol, water, acetone and dry in vacuo.

Embodiment 3

[0042] Dissolve 5g of polystyrene / divinylbenzene microspheres in 100ml of toluene, stir and swell at room temperature for 3h, cool to room temperature, add 30ml of chloromethyl ether and 2ml of tin chloride, continue stirring at room temperature for 3h, add deionized water to terminate the reaction , washed with hydrochloric acid, tetrahydrofuran, acetone, set aside.

[0043] Take 5.4g of the above-mentioned chloromethylated microspheres, add them into 54ml of chloroform, add 40ml of ethylenediamine, stir and heat to 150°C, and react for 6h. Cool down to room temperature, treat with acetone, water, methanol, and dry in vacuo.

[0044] Take 2.4 g of the above-mentioned ethylenediamine microspheres in 100 ml of toluene, add 6 g of triethylamine, 1.5 g of acetic anhydride, and 45 g of 4-dimethylaminopyridine, and stir overnight at room temperature. Treat with methanol, water, acetone and dry in vacuo.

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Abstract

The invention discloses a preparation method for a porous polymer microsphere anion filling material. The preparation method comprises the following steps: a chloromethyl group is introduced at first, and then ethene diamine is introduced onto the surfaces of microspheres by using a surface grafting method. According to the invention, monodisperse polystyrene / divinyl benzene microspheres are used as a substrate which reacts with chloromethyl ether for introduction of a chloromethyl functional group and then reacts with ethene diamine via the surface grafting method so as to form the anion filling material. The anion filling material obtained in the invention has the characteristics of controllable microsphere size and controllable varieties of surface function groups; and the preparation method has the characteristics that the method is simple and easily practicable in process, low in cost for raw materials, easy to operate and easy for industrial application.

Description

technical field [0001] The invention relates to the technical field of anion fillers, in particular to a method for preparing porous polymer microsphere anion fillers. Background technique [0002] With the rapid development of economic globalization and the continuous expansion of food trade, in order to avoid the recurrence of the tragedy of "Sanlu" milk powder, waste oil and clenbuterol, it is particularly important to strengthen the research on food testing. With more and more detection items of organic chemical hazards in food, only relying on the existing detection technology and detection efficiency cannot meet the demand of simultaneous detection of hundreds of organic chemical hazards. The difficulties in the detection of organic chemical residues in food, The most time-consuming steps and the main source of error are concentrated in the pre-treatment stage of the sample. Therefore, the establishment of a sample pre-treatment method that matches the rapid and high-t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F212/36C08F8/32C08F8/24B01J20/26B01J20/30
CPCB01J20/22B01J20/265B01J2220/44B01J2220/4812C08F8/32C08F8/24C08F212/08C08F212/36
Inventor 王勇朱丽丽何洁滕超任连兵洪梅
Owner PEKING UNIV SHENZHEN GRADUATE SCHOOL
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