Synthetic method of superficially pellicular packing stuffing for strong-acid cation chromatographic column and product

A technology of strong acid cation and synthesis method, which is applied in the field of synthesizing filler for surface thin-shell type strong acid cation chromatographic column, can solve the problems of poor resistance to organic solvents, easy cracking of resin, and high sulfonation temperature, and achieves resistance to The effect of good organic solvent performance, strong organic solvent resistance performance and low sulfonation degree

Inactive Publication Date: 2009-04-15
QINGDAO SHENGHAN CHROMATOGRAPH TECH CO LTD
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In "A Novel Ion Exchange Chromatography Using a Conductivity Detector" published by Analytical Chemistry (ANAL.CHEM.47 (1975) 1801), Small of the United States proposed the use of styrene-divinylbenzene copolymers with a cross-linking degree of 2%. The sulfonation reaction is carried out at 90-100°C for 1-10 minutes, and then the reactants are poured into cold deionized water. This technology has a high sulfonation temperature, and the resin is easily broken when poured into cold deionized water, resulting in The degree of dispersion of the resin becomes larger, and there is no exchange group at the broken interface, which reduces the separation effect and reduces the strength of the cracked resin.
In addition, this technology has a low degree of crosslinking and poor resistance to organic solvents. In organic solvents, styrene-divinylbenzene resin is easy to swell and lose its exchange capacity.

Method used

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  • Synthetic method of superficially pellicular packing stuffing for strong-acid cation chromatographic column and product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1. Two-step dispersion polymerization and swelling method to synthesize monodisperse spherical styrene-divinylbenzene resin with a particle size of 12um and a crosslinking degree of 10%.

[0018] 2. Low temperature sulfonation

[0019] Functionalization of monodisperse spherical styrene-divinylbenzene resin microspheres with a particle size of 12 μm and a crosslinking degree of 10%, that is, low-temperature sulfonation

[0020] Get 10 g of the monodisperse spherical styrene-divinylbenzene resin microspheres with a particle size of 12 μm and a crosslinking degree of 10% obtained above, and add it to a 250 ml three-necked flask equipped with a stirrer, an addition funnel and a reflux condenser, and add 100ml dichloroethane, start the stirrer to stir. Take 10ml of chlorosulfonic acid, dissolve it in 100ml of dichloromethane, add it to the addition funnel, place the whole device in an ice-water bath, slowly add dichloromethane dissolved in chlorosulfonic acid dropwise, aft...

Embodiment 2

[0027] The difference between the synthesis process and Example 1 lies in the low-temperature sulfonation step: Weigh 10 g of monodisperse spherical styrene-divinylbenzene resin microspheres with a particle size of 12 μm and a crosslinking degree of 10% into a 250 ml flask equipped with a stirrer Add 100ml of concentrated sulfuric acid, under slow stirring, heat up to 30°C, keep warm for 15 minutes, take out and quickly pour the reactant into deionized water in a large amount of ice-water bath to terminate the reaction, filter and wash the reactant, and then evenly Slurry column packing.

Embodiment 3

[0029] The difference between the synthesis process and Example 1 is that 1. a styrene-divinylbenzene resin with a crosslinking degree of 6% and a particle size of 30 μm is synthesized by suspension polymerization;

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Abstract

The invention provides a method for synthesizing fillers for a surface-pellicular highly-acidic cationic chromatographic column. The method comprises the following steps: synthetic shape-crosslinking aromatic olefin organic matrix resin is sulphonated and then packed into a column, and the synthetic shape-crosslinking aromatic olefin organic matrix resin reacts with concentrated sulphuric acid or chlorosulfonic acid at a temperature between 5 and 40 DEG C, so as to perform sulfonation treatment. The synthetic shape-crosslinking aromatic olefin organic matrix resin is subjected to the sulfonation treatment under the condition of low temperature, thereby ensuring that the sulfonation degree is low and the resin can not be damaged when the reaction is stopped. The aromatic olefin organic matrix resin with high synthetic shape-crosslinking degree is high in strength and strong in the performance of tolerating organic solvents. A resin product produced by the synthesis method has good integrity. When having higher crosslinking degree, the synthetic resin is good in the performance of tolerating the organic solvents.

Description

technical field [0001] The invention relates to a chromatographic column filler, in particular to a synthesis method and a product of a surface thin-shell type strongly acidic cation chromatographic column filler. Background technique [0002] In "A Novel Ion Exchange Chromatography Using a Conductivity Detector" published by Analytical Chemistry (ANAL.CHEM.47 (1975) 1801), Small of the United States proposed the use of styrene-divinylbenzene copolymers with a cross-linking degree of 2%. The sulfonation reaction is carried out at 90-100°C for 1-10 minutes, and then the reactants are poured into cold deionized water. This technology has a high sulfonation temperature, and the resin is easily broken when poured into cold deionized water, resulting in The degree of dispersion of the resin becomes larger, and there is no exchange group at the broken interface, which reduces the separation effect and reduces the strength of the cracked resin. In addition, this technology has a l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J39/26B01J39/18B01J39/17
Inventor 崔成来王金平荆建增王群朱新勇
Owner QINGDAO SHENGHAN CHROMATOGRAPH TECH CO LTD
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