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A kind of preparation method of fast anion chromatographic column filler

A technology of anion chromatography and column packing, which is applied in the field of preparation of fast anion chromatography column packing, can solve the problems of large exchange capacity, uneven particle size distribution of latex, and slow separation speed, and achieve uniform particle size of latex, appropriate exchange capacity, and separation speed fast effect

Active Publication Date: 2019-07-30
QINGDAO SHENGHAN CHROMATOGRAPH TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention aims to solve the problem that in the preparation of the existing latex agglomerated anion chromatographic packing, the degree of sulfonation of the support matrix is ​​difficult to control, and it is difficult to achieve consistency between batches, which easily leads to too many sulfonic acid groups on the surface, resulting in a relatively large exchange capacity; The particle size distribution of latex synthesized by soap-free emulsion polymerization is uneven and the particles are large; the anion chromatographic column produced has relatively high column capacity and slow separation speed. It provides a support matrix for easy control of the sulfonation process, and the surface sulfonic acid groups Moderate quantity, suitable nano-emulsion exchange capacity, small and relatively uniform particle size, moderate anion chromatographic column capacity, and a preparation method for fast anion chromatographic column packing with fast separation speed

Method used

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  • A kind of preparation method of fast anion chromatographic column filler

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) 5 g of highly cross-linked hydrophilic ethylstyrene-divinylbenzene fillers containing sulfonic acid groups on the surface with a cross-linking degree of 70% were prepared by using the synthesis method disclosed in the Chinese invention patent application, application notification number CN 104788603 A. After washing with deionized water several times, dry at 40°C for later use.

[0017] (2) Dissolve 0.5g of sodium dodecylsulfonate in 100ml of deionized water, then add it into a 250ml three-necked flask, stir at 100r / min, and heat at 60°C. Add 10ml of chloromethylstyrene, 0.2ml of divinylbenzene and 0.4ml of vinyl acetate into the three-necked flask, and keep the nitrogen atmosphere for 30min. Dissolve 0.1g of potassium persulfate in 20ml of deionized water, then add it to the above-mentioned three-necked flask, keep stirring at 100r / min, heat at 60°C, and react for 20.0h to obtain a copolymer nanoemulsion with a particle size of 50nm and a crosslinking degree of 2%....

Embodiment 2

[0024] (1) 5 g of highly cross-linked hydrophilic ethylstyrene-divinylbenzene fillers containing sulfonic acid groups on the surface with a cross-linking degree of 85% were prepared by using the synthesis method disclosed in the Chinese invention patent application, application notification number CN 104788603 A. After washing with deionized water several times, dry at 40°C for later use.

[0025] (2) Dissolve 0.5g of sodium dodecylsulfonate in 100ml of deionized water, then add it into a 250ml three-necked flask, stir at 100r / min, and heat at 60°C. Add 10ml of chloromethylstyrene, 1ml of divinylbenzene and 1.05ml of vinyl acetate into the three-necked flask, and keep the nitrogen atmosphere for 30min. Dissolve 0.1g of potassium persulfate in 20ml of deionized water, then add it to the above-mentioned three-necked flask, keep stirring at 100r / min, heat at 60°C, and react for 20.0h to obtain a copolymer nanoemulsion with a particle size of 50nm and a crosslinking degree of 10%....

Embodiment 3

[0033] (1) 5 g of highly cross-linked hydrophilic ethylstyrene-divinylbenzene fillers containing sulfonic acid groups on the surface were prepared by using a Chinese invention patent application, application announcement number CN 104788603 A, through a synthetic method. After washing with deionized water several times, dry at 40°C for later use.

[0034] (2) Dissolve 0.5g of sodium dodecylsulfonate in 100ml of deionized water, then add it into a 250ml three-necked flask, stir at 100r / min, and heat at 60°C. Add 10ml of chloromethylstyrene, 0.4ml of divinylbenzene and 0.60ml of vinyl acetate into the three-necked flask, and keep the nitrogen atmosphere for 30min. Dissolve 0.1g of potassium persulfate in 20ml of deionized water, then add it into the above-mentioned three-necked flask, keep stirring at 100r / min, heat at 60°C, and react for 20.0h to obtain a 50nm copolymer nanoemulsion with a crosslinking degree of 4%.

[0035] (3) Pour 100ml of copolymer nanoemulsion prepared in...

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Abstract

The invention relates to a preparation method of a rapid anion chromatographic column packing material. The preparation method of the rapid anion chromatographic column packing material is applied to manufacturing rapid chromatographic columns. According to technical scheme of the rapid anion chromatographic column packing material, an support matrix is high-crosslinking hydrophilic ethylstyrene-divinylbenzene fillings with the surface provided with sulfonic acid groups; a functional matrix is a nano latex copolymerized from vinylbenzyl chloride monomers, divinyl benzene monomers and acetic acid vinyl ester monomers or glycidyl methacrylate through microemulsion polymerization, and the nano latex is hydrolyzed, demulsified, washed and quaternized to produce a quaternized copolymer nano latex; the support matrix and the functional matrix are agglomerated to obtain a rapid anion exchange resin. Therefore, the technical problems of existing latex agglomerated anion chromatographic packing materials that sulfonation of support matrixes are difficult to control and lacks batch-to-batch consistency, too much surface sulfonic acid groups exist, the exchange capacitance is relatively large, soap-free emulsion polymerized emulsion is non-uniform in latex particle size distribution and large in particle size, the column capacity of obtained anion chromatographic columns is relatively high and the separating speed is low can be solved.

Description

technical field [0001] The invention relates to an ion chromatographic column filler, in particular to a preparation method of a fast anion chromatographic column filler. Background technique [0002] Zeng Xueling, "Preparation and Evaluation of Latex Agglomerated Anion Chromatography Packing", Zhejiang University, 2016 master's thesis discloses a surface agglomeration of a surface sulfonated support matrix and quaternized nano latex particles to prepare latex agglomerated The preparation method of polyanion chromatographic filler. In the above papers, the support matrix is ​​prepared by sulfonating the surface of the styrene-divinylbenzene copolymer system. The disadvantage is that the degree of sulfonation is difficult to control, and it is difficult to achieve consistency between batches, which will easily lead to the number of surface sulfonate groups. Too much, resulting in a relatively large exchange capacity; latex is a styrene-methacrylate glycidyl ester system synt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J41/20B01J41/14B01D15/36
CPCB01D15/363B01J41/14B01J41/20
Inventor 张彬彬崔成来
Owner QINGDAO SHENGHAN CHROMATOGRAPH TECH CO LTD