Method for preparing grafting type strong preservation anion chromatographic packing

An anion chromatography and branched technology, which is applied in the field of preparation of grafted strong retention anion chromatography packing, can solve the problems of limited development and poor acid and alkali resistance, and achieve the effect of strong retention, strong retention and good rigidity.

Inactive Publication Date: 2015-09-30
ZHEJIANG UNIV
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Problems solved by technology

Silica gel packing is only suitable for pH2~8, and its wea

Method used

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  • Method for preparing grafting type strong preservation anion chromatographic packing
  • Method for preparing grafting type strong preservation anion chromatographic packing
  • Method for preparing grafting type strong preservation anion chromatographic packing

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[0035] The invention discloses a high-polymer polystyrene-divinylbenzene-glycidyl methacrylate-dendrimer-2,3-epoxypropyltrimethylammonium chloride grafted strong retention The preparation method of anionic chromatographic filler, with polystyrene-divinylbenzene-glycidyl methacrylate (PSt-DVB-GMA) as substrate; With ethylenediamine and methyl acrylate as substrate, by Michael Addition reaction and aminolysis reaction to synthesize polyamide-amine dendrimers (PAMAM) of different generations; by controlling the reaction conditions, the dendrimers (PAMAM) are grafted to polystyrene-divinyl in the manner of Grafting to Benzene-glycidyl methacrylate microspheres (PSt-DVB-GMA); and then grafted onto PSt-DVB- The polyamide-amine dendrimers on the GMA microspheres are modified by quaternization to obtain an ion chromatography filler with strong retention effect, and the column is packed by the homogenization method. The specific implementation steps are as follows:

[0036] 1) Synthe...

Embodiment 1

[0044] Grafting to grafting method to prepare grafted anion chromatographic column manufacturing process is as follows, the steps are:

[0045] (1) First, 1.8 μm monodisperse linear polystyrene seeds were synthesized by dispersion polymerization, and then cross-linked monodisperse polystyrene-divinylbenzene-glycidyl methacrylate (PSt- DVB-GMA) microspheres. figure 1 It is a scanning electron micrograph of polystyrene-divinylbenzene-glycidyl methacrylate (PSt-DVB-GMA) (magnification 6000 times).

[0046] (2) With ethylenediamine as the initiator nucleus and methanol as the reaction medium, the first step reaction is to carry out Michael addition reaction with methyl acrylate to generate 0.5G polyamide-amine dendrimer (PAMAM); the second step reaction The 0.5G dendrimer obtained in the first step undergoes an amidation reaction with ethylenediamine to generate a 1.0G polyamidoamine dendrimer. 1.0G polyamidoamine dendrimers were grafted onto polystyrene-divinylbenzene-glycidyl ...

Embodiment 2

[0050] Embodiment 2: chromatographic performance test

[0051] Instruments: SHINEHA CIC-100 ion chromatograph, SHINEHA conductivity detector, SHINEHA SHY-A-III anion self-regenerating suppressor

[0052] Sample: F - , Cl - , acetate, oxalate (all analytically pure)

[0053] Eluent: 10mM / mol NaOH solution

[0054] Separation column: Self-made packing is filled in a 4.6×150mm stainless steel column (grafted with 1.0 generation dendrimers)

[0055] Flow rate: 1.00ml / min

[0056] image 3 Chromatogram for a mixed sample of conventional anions and organic acids

[0057] 1-F in the chromatogram - (5ppm), 2-acetate (15ppm), 3-Cl - (5ppm), 4-oxalate (20ppm).

[0058] image 3 Inorganic anions and organic acid ions can be completely separated, and the retention time is different, which shows that the chromatographic packing column has excellent separation effect on organic acids and inorganic anions.

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Abstract

The method provides a method for preparing grafting type strong preservation anion chromatographic packing made of polymer polystyrene-divinyl benzene-glycidyl methacrylate-dendrimer-2,3-glycidyl trimethyl ammonium chloride. The method comprises the steps of grafting polyamide-amine dendrimer compound to polymer base ball polystyrene-divinyl benzene-glycidyl methacrylate in a grafted mode, using active cationic reagent 2,3-glycidyl trimethyl ammonium chloride to perform quaterisation modification on the grafting type base ball, and obtaining quaternary ammonium type ion chromatographic column packing having high preservation effects on anions. The obtained quaternary ammonium type ion chromatographic packing undergoes packing through a homogenate method, and an obtained compound strong preservation anion chromatographic column has very high separation preservation effects on conventional anions such as F- and Cl- and organic acids such as oxalic acid.

Description

technical field [0001] The present invention relates to a strong retention type anion chromatographic column and a preparation method thereof, in particular to a Grafting to graft type strong retention anion chromatography packing involving high polymer (PSt-DVB-GMA)-dendrimer-EPTAC The preparation method, and the application method of active cationization reagent EPTAC and macromolecular material dendrimer PAMAM in the preparation of chromatographic packing. Background technique [0002] Ion chromatography is one of the most widely used and fastest-growing branches in the field of chromatographic analysis. Ion chromatography is a kind of high-performance liquid chromatography. It is a chromatographic analysis method for analyzing conventional anions and cations. It has superior sensitivity and selectivity sex. Ion chromatography has become an effective tool for analyzing anions, cations and some organic substances, as well as sugars, amino acids, peptides, proteins, etc. i...

Claims

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Application Information

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IPC IPC(8): C08G83/00C08F257/02C08F212/08C08F220/32C08F212/36C08F112/08B01J20/285B01J41/12B01D15/04G01N30/02B01J41/13
Inventor 楼超艳朱岩
Owner ZHEJIANG UNIV
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