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A kind of preparation method of hydrophilic latex agglomeration type anion chromatographic filler

An anion chromatography and hydrophilic technology, which is applied in the field of preparation of hydrophilic latex agglomerated anion chromatography packing, can solve seven kinds of ion chromatography with poor peak shape, inaccurate detection results, negative peaks of fluoride ion and water Can not be completely separated and other issues

Active Publication Date: 2018-12-25
QINGDAO SHENGHAN CHROMATOGRAPH TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention solves the problem that the separation column made of the existing carbon nanotube latex agglomeration-type anion chromatographic filler cannot completely separate the negative peaks of fluorine ion and water, and the peak shape of the separated seven ion chromatograms is not good, and the broadening is serious, which leads to the detection results Inaccurate technical problems, provide a quaternized hydrophilic nano-spherical latex agglomeration agent, which is evenly adsorbed on the surface of sulfonated skeleton microspheres through electrostatic interaction, and obtain a hydrophilic latex agglomeration type anion chromatography The preparation method of the packing, the separation column filled with the ion chromatography packing can completely separate the negative peaks of the fluorine ion and the water, and the peak shape of the separated seven kinds of ion chromatography is sharp and symmetrical, the broadening is moderate, and the detection accuracy is high

Method used

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  • A kind of preparation method of hydrophilic latex agglomeration type anion chromatographic filler
  • A kind of preparation method of hydrophilic latex agglomeration type anion chromatographic filler
  • A kind of preparation method of hydrophilic latex agglomeration type anion chromatographic filler

Examples

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Effect test

Embodiment 1

[0027] Step 1, preparation of sulfonated polystyrene-divinylbenzene copolymer skeleton microspheres

[0028] Select polystyrene-divinylbenzene copolymer microspheres with a particle size of 5 μm and a crosslinking degree of 5% prepared by suspension polymerization, and wash them with hot water. Select 3 g dry weight of polystyrene-divinylbenzene copolymer microspheres washed with hot water, add 100 mL of concentrated sulfuric acid into a three-necked flask, raise the temperature to 50 ° C, and keep the reaction for 60 min. After the sulfonation reaction, close the water bath, slowly add 100mL 50% sulfuric acid from the dropping funnel, transfer the solution to deionized water after stirring, let it settle, and finally pour off the upper layer, and suction filter to obtain sulfonated polyphenyl Ethylene-divinylbenzene copolymer skeleton microspheres.

[0029] Step 2, microemulsion polymerization synthesis of polyglycidyl methacrylate-ethylene glycol dimethacrylate nano-spheric...

Embodiment 2

[0039] Step 1, preparation of sulfonated polyvinylstyrene-divinylbenzene copolymer skeleton microspheres

[0040] The difference from Step 1 of Example 1 is: select polyvinylstyrene-divinylbenzene copolymer microspheres with a particle size of 30 μm and a crosslinking degree of 15%. Add 100mL of concentrated sulfuric acid into the three-necked flask, raise the temperature to 90°C, and keep the reaction for 25min. The sulfonated polyvinylstyrene-divinylbenzene copolymer skeleton microspheres were prepared by suction filtration.

[0041] Step 2, microemulsion polymerization synthesis of polyglycidyl methacrylate-ethylene glycol dimethacrylate nano-spherical latex

[0042] The difference from step 2 of Example 1 is: 6.32g (water phase mass 5.00%) sodium dodecylbenzenesulfonate; warm up to 65°C, add 18mL of persulfuric acid that dissolves 0.5g of potassium persulfate in 30mL of deionized water in advance Potassium solution, the stirring speed is 200r / min, heat preservation react...

Embodiment 3

[0051] Step 1, preparation of sulfonated polystyrene-divinylbenzene copolymer skeleton microspheres

[0052] The difference from Step 1 of Example 1 is: select polystyrene-divinylbenzene copolymer microspheres with a particle size of 10 μm and a crosslinking degree of 8%; add 100 mL of concentrated sulfuric acid into a three-necked flask, raise the temperature to 65° C., and keep the reaction for 50 minutes.

[0053] Step 2, microemulsion polymerization synthesis of polyglycidyl methacrylate-ethylene glycol dimethacrylate nano-spherical latex

[0054] The difference from step 2 of Example 1 is: 0.36g (water phase mass 0.30%) sodium dodecylbenzenesulfonate; be warmed up to 50°C, add 15mL of potassium persulfate solution dissolved in deionized water in advance, and the stirring speed is 80r / min, keep warm for 3.5h, then add the remaining 15mL potassium persulfate solution, keep warm for 4.0h and then cool to room temperature. Synthesize polyglycidyl methacrylate-ethylene glyco...

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Abstract

The invention relates to a preparation method of hydrophilic latex-agglomerated anion chromatographic packing. Produced resin is used for filling a chromatographic column. The preparation method comprises: agglomerating a quaternizated polyglycidyl methacrylate-dimethyl acrylate glycol ether hydrophilic nano spherical latex agglomeration agent and surface-sulfonated copolymer skeleton microspheres to obtain the hydrophilic latex-agglomerated anion chromatographic packing resin, wherein the agglomeration agent is uniformly adsorbed onto a sulfonation layer on the surface of the skeleton microspheres, and the sulfonation layer is completely coated. Fluorine ions and water negative peaks of a sample detected by a packing filled chromatographic column are completely separated, the peak of seven ions is sharp and symmetric, the spread is moderate, and the accuracy of a detection result is high.

Description

technical field [0001] The invention relates to an anion chromatographic column filler, in particular to a method for preparing a hydrophilic latex agglomerated anion chromatographic filler. Background technique [0002] Chinese invention patent, application publication number CN 102935390 A, "Preparation method of carbon nanotube latex agglomeration type anion chromatographic filler" discloses a method for preparing carbon Nanotube latex, using ionic bonding, agglomerates a layer of carbon nanotube latex on the surface of sulfonated polystyrene-divinylphenyl spheres, as an anion exchange functional group of carbon nanotube latex agglomeration type Anion chromatography packing technology. Although the separation column made of the anion chromatographic filler of the invention has a certain hydrophilic property and can separate seven kinds of anions, in the chromatographic analysis, the tailing of these seven kinds of ions is serious, and the peak shape is not sharp and symm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/30B01J20/26B01J20/286B01D15/08
CPCB01D15/08B01J20/261B01J20/264B01J20/265B01J20/286B01J2220/445B01J2220/4812
Inventor 史振举崔承来黄蕾李彦商荣宁
Owner QINGDAO SHENGHAN CHROMATOGRAPH TECH CO LTD
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