A novel preparation method of grafted dendritic macromolecular microspheres
A technology of dendritic macromolecules and microspheres, which is applied in the field of ion chromatography preparation, can solve the problems of complicated process and limited quantity, and achieve the effects of uniform particle size, stable performance and long service life
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[0034] The invention discloses a preparation method of a dendrimer graft type ion chromatography stationary phase, comprising: preparation of 1.0G dendrimer, preparation of polystyrene divinylbenzene microspheres, dendrimer and microsphere The grafting of spheres, the quaternization modification of dendrimers and the preparation of quaternized dendrimer grafted anion chromatographic fillers, using polystyrene-divinylbenzene as the matrix, prepared by dispersion polymerization For the dispersed linear polystyrene microsphere seeds, after the seeds are activated, the polystyrene-divinylbenzene microspheres are synthesized by a single-step seed swelling method, and the porogen is removed by extraction. Then by chemical grafting method, polyamide-amine (PAMAM) dendrimers are grafted onto the surface of microspheres and modified by quaternization with 1,4-butanediol glycidyl ether; , the specific preparation steps are:
[0035] a. Preparation of 1.0GPAMAM dendrimers by divergent m...
Embodiment 1
[0045] Embodiment 1: The preparation process of 1.0GPAMAM grafted polystyrene-divinylbenzene anion chromatography stationary phase packing is as follows, and its steps are:
[0046] 1. Preparation of 0.5GPAMAM: Dissolve 2mL of ethylenediamine in 20mL of methanol, slowly add 23g of methyl acrylate under stirring in an ice-water bath, slowly raise the temperature to 25°C after the dropwise addition, and stir for 24 hours to obtain 0.5G of PAMAM .
[0047] 2. Preparation of 1.0 GPAMAM: Dissolve 5 g of 0.5 GPAMAM in 20 mL of methanol, slowly add 15 g of ethylenediamine dropwise under stirring in an ice-water bath, slowly raise the temperature to 25°C after the addition, and stir for 24 hours to obtain 1.0 g of PAMAM.
[0048] 3, the preparation of polystyrene seed, synthetic particle diameter 1~3 μ m monodisperse polystyrene seed by emulsion dispersion polymerization method, the concentration of monomeric styrene is 5% (m / m) of total amount, stabilizing agent polyvinylpyrrolidone ...
Embodiment 2
[0053] Embodiment 2: with reference to the method and steps of embodiment 1
[0054] 1. Preparation of 0.5GPAMAM: Dissolve 2mL of ethylenediamine in 20mL of methanol, slowly add 23g of methyl acrylate under stirring in an ice-water bath, slowly raise the temperature to 25°C after the dropwise addition, and stir for 24 hours to obtain 0.5G of PAMAM .
[0055] 2. Preparation of 1.0 GPAMAM: Dissolve 5 g of 0.5 GPAMAM in 20 mL of methanol, slowly add 15 g of ethylenediamine dropwise under stirring in an ice-water bath, slowly raise the temperature to 25°C after the addition, and stir for 24 hours to obtain 1.0 g of PAMAM.
[0056] 3, the preparation of polystyrene seed, synthetic particle diameter 1~3 μ m monodisperse polystyrene seed by emulsion dispersion polymerization method, the concentration of monomeric styrene is 5% (m / m) of total amount, stabilizing agent polyvinylpyrrolidone Consumption is 0.5% (m / v) of reaction medium, and initiator azobisisobutyronitrile consumption i...
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