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Agglomerated high-hydrophilic strong anion exchanger, preparation method and application of anion exchanger in liquid chromatographic column filler

A technology of strong anion and exchanger, applied in the preparation, application of liquid chromatography column packing, agglomerated highly hydrophilic strong anion exchanger, can solve the problem of non-agglomeration of nanoparticles, difficulty in applying strong hydrophobicity, Difficult to agglomerate nanoparticles uniformly and other problems, so as to avoid the use of highly toxic reagents, the operation process is green and environmentally friendly, and the effect of overcoming uneven agglomeration

Active Publication Date: 2017-12-01
苏州明昊色谱技术有限公司
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Problems solved by technology

Although this method can obtain high-capacity quaternary ammonium-type chromatographic stationary phase fillers, its disadvantage is that it is difficult for nanoparticles to evenly agglomerate on the surface of micron-sized polymer microspheres due to the electrostatic repulsion between them, causing the surface to be partially exposed and No nanoparticle agglomeration
Moreover, because the surface of the polymer microsphere itself is strongly hydrophobic, the chromatographic packing obtained by this method lacks hydrophilicity.
Another disadvantage is that it is difficult to accurately control the particle size of nanoparticles, so the batch reproducibility of this type of chromatography packing preparation is insufficient
Therefore, this method is difficult to apply to polymer microspheres represented by chloromethylstyrene-divinylbenzene with strong hydrophobicity, thus limiting the type and development of the ion exchanger.
Even if the filler obtained by coating polymer microspheres with polyvinyl alcohol is still a neutral filler, it cannot be used for anion separation

Method used

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  • Agglomerated high-hydrophilic strong anion exchanger, preparation method and application of anion exchanger in liquid chromatographic column filler
  • Agglomerated high-hydrophilic strong anion exchanger, preparation method and application of anion exchanger in liquid chromatographic column filler

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preparation example Construction

[0036] 1) Preparation of polymer microspheres;

[0037] A suspension polymerization method is used to prepare polymer microspheres, and the polymer microspheres are chloromethylstyrene and divinylbenzene copolymer-based balls;

[0038] 2) Sulfonation of polymer microspheres;

[0039] Under the condition of an ice-water bath, disperse the chloromethylstyrene and divinylbenzene copolymer-based balls prepared in step 1) in a sulfuric acid solution; then continuously stir the reaction at room temperature to obtain a suspension, and the suspension Pour into the ice-water bath solution to terminate the reaction, and after suction filtration, wash the filter cake to neutrality to obtain sulfonated polymer microspheres;

[0040] 3) Preparation of quaternized polyvinyl alcohol;

[0041] Disperse polyvinyl alcohol in water, add sodium hydroxide and 3-chloro-2-hydroxypropyltrimethylammonium chloride at a temperature of 80-95°C, react continuously under the condition of magnetic stirrin...

Embodiment 1

[0045] 1) Preparation of polymer microspheres: Copolymer-based spheres of chloromethylstyrene and divinylbenzene with a particle size of about 8 μm were prepared by suspension polymerization.

[0046] 2) Sulfonation of polymer microspheres: Weigh 10 g of the prepared chloromethylstyrene and divinylbenzene copolymer-based balls and place them in a 50 mL round-bottomed flask. Add 20 mL of sulfuric acid solution with a mass percent content of 60%, and make the chloromethylstyrene and divinylbenzene copolymer-based balls completely dispersed in the sulfuric acid solution by magnetic stirring, and continuously stir for 30min at room temperature 30°C Finally, a suspension is obtained, which is poured into an ice-water bath solution to terminate the reaction, and the above-mentioned ice-water bath solution is suction-filtered, and the obtained filter cake is washed to neutrality to obtain the required sulfonated polymer microspheres.

[0047] 3) Quaternization of polyvinyl alcohol: T...

Embodiment 2

[0050] The highly hydrophilic strong anion exchanger obtained by agglomerating sulfonated polymer-based balls with quaternized polyvinyl alcohol is dispersed in the homogenate, and loaded into a chromatographic column under a hydraulic pressure of 5000 psi. The flow rate is 1mL / min, the mobile phase is 5mM potassium carbonate, and the IO is separated under the ultraviolet detection mode. 3 - , BrO 3 - , NO 2 - , NO 3 - , I - and SCN - ions, see the attached spectrum figure 1 . Obviously, the anion exchange chromatographic filler obtained by adopting the quaternized polyvinyl alcohol agglomerated sulfonated polymer microspheres proposed by the present invention in this example shows good separation performance for the above-mentioned ions.

[0051] Comparative test: In order to further highlight the separation effect of the chromatographic filler of the present invention, the method mentioned in the Chinese invention patent CN104226283 B, that is, the use of polyvinyl...

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Abstract

The invention belongs to the technical field of liquid chromatographic column filler preparation, and particularly relates to an agglomerated high-hydrophilic strong anion exchanger, a preparation method and application of the anion exchanger in liquid chromatographic column filler. The strong anion exchanger is prepared by agglomerating quaternized polyvinyl alcohol to sulfonated polymer microspheres. The quaternized polyvinyl alcohol is prepared by the following steps: dispersing polyvinyl alcohol into water, adding a sodium hydroxide solution and 3-chloro-2-hydroxypropyltrimethyl ammonium, continuously reacting under a stirring condition, pumping, filtering, rinsing and drying. The preparation method has the advantages that high-hydrophilic strong anion exchaner is prepared by agglomerating quaternized polyvinyl alcohol to polyolefine organic copolymer base spheres along with high preparation speed, simple operating process and environmental friendliness, monochloro-methyl-ether or dichloroethyl ether and other virulent reagents can be prevented from being applied, and the defect of hydrophilic shortage of anionic exchanger caused by modification with nanoparticles or carbon nano-tubes can be eliminated.

Description

technical field [0001] The invention belongs to the technical field of liquid chromatography column packing preparation, and in particular relates to an agglomerated highly hydrophilic strong anion exchanger, a preparation method and its application in liquid chromatography column packing. technical background [0002] Most of the highly hydrophilic and strong anion chromatography packings are based on organic polymer matrix, and the functional groups are mostly quaternary ammonium groups. However, to introduce quaternary ammonium groups on the surface of organic polymer-based spheres, the preparation process usually requires the use of chloromethyl ether and dichloro Hypertoxic reagents such as methyl ether chloromethylate organic polymers to introduce active chlorine, and then react with tertiary amine reagents to introduce quaternary amino groups. The preparation process is cumbersome, and chloromethyl ether and dichloromethyl Ether is extremely toxic to humans and the en...

Claims

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Application Information

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IPC IPC(8): B01J41/12G01N30/02C08F8/30C08F16/06C08F8/36C08F212/14C08F212/36
CPCB01J41/12C08F8/30C08F8/36G01N30/02C08F16/06C08F212/14C08F212/36
Inventor 侯彦杰杨丙成章飞勇
Owner 苏州明昊色谱技术有限公司
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