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Synthesis Method of Hydrophilic Ion Pair Chromatography Packing

A technology of ion-pair chromatography and synthesis method, applied in the field of ion-pair chromatography packing, can solve the problems of difficult control of sulfonation reaction, poor product consistency, low success rate, etc. high pressure effect

Active Publication Date: 2017-08-11
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 solves the problem of adding a large amount of organic solvents to modify styrene-divinylbenzene. Other parts 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. The technical problems of sulfonation reaction are difficult to control, poor product consistency, need to be screened, low success rate and high cost, and provide a hydrophilic ion with low production cost, high efficiency, high success rate and easy control of surface hydrophilic capacity Synthetic method for chromatographic packing

Method used

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  • Synthesis Method of Hydrophilic Ion Pair Chromatography Packing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 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.

[0022] In a 1000 ml three-neck flask equipped with a stirrer and a reflux condenser, add the dissolved polyvinyl alcohol solution in Part 1, then add 5 ml of the mixed monomer and seeds in Part 1, and first heat it at 30 degrees Celsius under a nitrogen atmosphere. Stir and swell for 24 hours, then stir and react at 80 degrees Celsius for 4 hours, and finally mature at 90 degrees Celsius and stir and react for 10 hours, take out, wash, filter and dry to obtain an ethylstyrene-divinylbenzene polymer with a crosslinking degree of 80%. Microspheres.

[0023] Get 10 grams after drying the ethylstyrene-divinylbenzene polymer microspheres prepared in 2, ...

Embodiment 2

[0029] The difference from 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, and the divinylbenzene with a content of 70% and the initiator are lauryl peroxide.

[0030] The difference between 2 and Example 1 is that the gelatin solution dissolved in 1 is added to the three-necked bottle; under nitrogen atmosphere, first stir and swell at 25 degrees Celsius for 25 hours, then stir and react at 77.5 degrees Celsius for 4.5 hours, and finally mature at 87.5 degrees Celsius The reaction was stirred for 10.5 hours at 100°C to obtain ethylstyrene-divinylbenzene polymer microspheres with a crosslinking degree of 70%.

[0031] The 3 difference from Example 1 is that the catalyst is anhydrous zinc chloride; the chloromethylation reaction temperature is 50 degrees Celsius with the chloromethylation reagent paroxymethylene and concentrated hydrochloric acid solution, and the...

Embodiment 3

[0036] 1 difference with embodiment one 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 of content 85% and initiator are n-octanoyl peroxide .

[0037] The difference between 2 and 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, and finally Aging was carried out at 92.5 degrees Celsius for 9.5 hours with stirring to prepare ethylstyrene-divinylbenzene polymer microspheres with a crosslinking degree of 85%.

[0038] The 3 difference from Example 1 is that the catalyst is anhydrous ferric chloride, and the chloromethylation reaction temperature is 70 degrees Celsius with the chloromethylation reagent paroxymethylene and concentrated hy...

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Abstract

The invention relates to a hydrophilic ion pair chromatography packing synthesis method which is used for manufacturing chromatography packing. The technical scheme includes that ethylstyrene-divinylbenzene polymer microspheres synthesized by a swelling polymerization method, chloromethylation reagent trioxymethylene and concentrated hydrochloric acid are subjected to chloromethylation reaction, chloromethylated ethylstyrene-divinylbenzene polymer microspheres are manufactured and then subjected to hydroxylation reaction together with sodium hydroxide to generate high cross-linked hydrophilic ethylstyrene-divinylbenzene packing with a hydroxyl group on the surface, or the chloromethylated ethylstyrene-divinylbenzene polymer microspheres and ammonia water are subjected to aminolysis reaction to generate high cross-linked hydrophilic ethylstyrene-divinylbenzene packing with a primary amino group on the surface. The synthesis method solves the technical problems that other parts of an ion chromatography system have high organic solvent tolerance requirements, or surface modified reaction control difficulty is high, product consistency is poor, screening is needed, success rate is low, and 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 has the advantages of being decomposed, high pressure resistance and good controllability of synthetic particle size, 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 will affect other components of the ion chromatography analysis system. Higher organic solvent resistance requirements are proposed. The most common method for hydrophilic mo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/285B01J20/30C08F218/12C08F212/36C08F8/24C08F8/32C08F8/00
Inventor 崔成来许爱华张彬彬史振举
Owner QINGDAO SHENGHAN CHROMATOGRAPH TECH CO LTD
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