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Synthesis method of hydrophilic ion pair chromatography packing

A technology of ion-pair chromatography and synthesis method, which is applied in the field of ion-pair chromatography packing, which can solve the problems of difficult sulfonation reaction control, poor product consistency, and low success rate, and achieves surface hydrophilic capacity that is easy to control, low in cost, and successful high rate effect

Active Publication Date: 2015-07-22
QINGDAO SHENGHAN CHROMATOGRAPH TECH CO LTD
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention aims to solve the problem of adding a large amount of organic solvents to modify styrene-divinylbenzene. The components of the ion chromatography analysis system need to have high organic solvent tolerance requirements, and the modification is carried out by concentrated sulfuric acid sulfonation, and the sulfonation of the surface The reaction control is difficult, the product consistency is poor, screening is required, the success rate is low, and the technical problems are high cost. To provide a hydrophilic ion-pair chromatography with low production cost, high efficiency, high success rate and easy control of surface hydrophilic capacity Synthesis method of filler

Method used

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  • Synthesis method of hydrophilic ion pair chromatography packing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 3 g of protective colloid reagent polyvinyl alcohol to 500 ml of deionized water and stir to dissolve. Divinyl benzene with a content of 80% and initiator (di)benzoyl peroxide dissolved in toluene were packed into a brown bottle, filled with nitrogen gas and sealed, and stored at 4 degrees Celsius for later use.

[0015] In the 1000 ml three-neck flask equipped with a stirrer and reflux condenser, add the polyvinyl alcohol solution dissolved in 1, and add 1 g of potassium styrene sulfonate, and then add 5 ml of the mixed monomer and seeds in 1 , under a nitrogen atmosphere, first stirred and swelled at 30 degrees Celsius for 24 hours, then stirred and reacted at 80 degrees Celsius for 4 hours, and finally matured and reacted at 90 degrees Celsius for 10 hours.

[0016] The presence of potassium styrene sulfonate makes the ethylstyrene-divinylbenzene polymer microspheres with a crosslinking degree of 80% synthesized by swelling polymerization become highly crossl...

Embodiment 2

[0020] The difference from 1 in Example 1 is that the protective colloid reagent is gelatin, 500 milliliters of deionized water is dissolved in 5 grams of protective colloid reagent gelatin, the content of 70% divinylbenzene and the initiator are lauryl peroxide.

[0021] The difference from 2 in Example 1 is that the gelatin solution dissolved in 1 was added to the three-necked bottle; under nitrogen atmosphere, first stirred and swelled at 25 degrees Celsius for 25 hours, then stirred and reacted at 77.5 degrees Celsius for 4.5 hours, and finally matured at The reaction was stirred at 87.5 degrees Celsius for 10.5 hours.

[0022] The presence of potassium styrene sulfonate makes the ethylstyrene-divinylbenzene polymer microspheres with a crosslinking degree of 70% synthesized by the swelling polymerization method become highly crosslinked hydrophilic ethylstyrene-divinylbenzene polymer microspheres containing sulfonic acid groups on the surface. divinylbenzene filler. T...

Embodiment 3

[0025] The difference with Example 1 is that the protective colloid reagent is light calcium carbonate, 500 milliliters of deionized water, add 10 grams of protective colloid reagent light calcium carbonate, the divinylbenzene and initiator of content 85% are n-octyl peroxide acyl.

[0026] The difference from 2 in Example 1 is that the light calcium carbonate solution dissolved in 1 is added to the three-necked bottle; under nitrogen atmosphere, first stir and swell at 35 degrees Celsius for 23 hours, then stir and react at 82.5 degrees Celsius for 3.5 hours, Finally, ripen and react at 92.5 degrees Celsius for 9.5 hours with stirring.

[0027] Potassium styrene sulfonate makes the ethylstyrene-divinylbenzene polymer microspheres with a crosslinking degree of 85% synthesized by swelling polymerization method become highly cross-linked hydrophilic ethylstyrene-divinylbenzene containing sulfonic acid groups on the surface Benzene filler. The filler is washed and dried, ex...

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Abstract

The invention relates to a synthesis method of hydrophilic ion pair chromatography packing, which is used for preparing the chromatography packing. The method adopts the technical scheme that a mixture of monomers ethylstyrene and divinylbenzene reacts with an ion monomer, namely potassium styrene sulfonate on the surface to generate the high-crosslinking hydrophilic ethylstyrene-divinylbenzene packing containing a sulfonic acid group on the surface. The method solves the technical problems that when a large number of organic solvents are added for modifying styrene-divinylbenzene, other components of an ion chromatography analysis system are required to have high organic solvent tolerance; and when concentrated sulfuric acid sulfonation is adopted for modification, the control difficulty of a sulfonation reaction on the surface is high, the product consistency is poor, screening is required, a success rate is low and the cost is high.

Description

technical field [0001] The invention relates to an ion-pair chromatographic filler, in particular to a method for synthesizing a hydrophilic ion-pair chromatographic filler. Background technique [0002] Ion-pair chromatography is an excellent tool for the analysis of surfactants. Crosslinked styrene-divinylbenzene packing is a commonly used ion-pair chromatography packing, although the synthesized high cross-linking styrene-divinylbenzene packing has a wider range of tolerance to pH than octadecylsilane bonded silica packing without It will be decomposed, high pressure resistance, and good controllability of synthetic particle size, etc., but its surface has strong hydrophobicity, and it needs to be modified by adding a large amount of organic solvents to shorten the analysis time, which affects other components of the ion chromatography analysis system. Higher organic solvent resistance requirements are proposed. The most common method for hydrophilic modification of hig...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/36C08F212/06C08F212/14B01J20/285B01J20/30B01D15/08
Inventor 崔成来许爱华张彬彬史振举
Owner QINGDAO SHENGHAN CHROMATOGRAPH TECH CO LTD
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