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Synthesis And Application Of RP-chromatography Packing Bonding Agents

Posted on:2011-08-04Degree:MasterType:Thesis
Country:ChinaCandidate:S H WangFull Text:PDF
GTID:2231330395457862Subject:Physical chemistry
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After years of developing, chromatography has become an indispensable mean of separation in many areas. Chromatographic packing, as a core component of the chromatography, is not only a wide range of preparation techniques and becomes more sophisticated and applied. Silica gel chromatography to matrix has many advantages is the mainstream of liquid chromatography packing.Chemical bond liquid chromatography stationary phase is the mainstream, therefore the chemical bond with silica gel as a substrate mixture of great significance. This paper summarizes some of the synthesis rotes, the most commonly used method is through hydrosilylation or Grignard reagent, bonding agent using the additional reaction of olefins is more difficult and the cost is high. Grignard reagent method is the low cost synthetic method, and the production is high purity, it is an ideal synthesis. However, the reaction conditions are harsh, Grignard reagents currently used bonding agent in the literature very few, if we use this method to synthetic bonding agent, we should optimize the synthesis conditions.The paper also introduces the reaction process, by optimizing the reaction conditions; we wish to find the process of industrialization. Considering of all factors, we synthesized in ethanol as the initial chlorosilane-base bonding agents, through experimental inquiry we have prepared of Grignard reagents, using distillation and ethyl bromide in the experiment to remove water, can greatly improve the operability. Alkyl formats and through different reagents and reaction of dimethyldichlorosilane, silicone bonding agents are different.Through experiments we insure the n-butyl, phenyl, octadecyl alkyl dimethyl chlorosilane synthetic routes; the yield of C4bonding agent can reach99.4%. Phenyl bonding agent can reach70%yield, C18of the bonding agent reaction with silica gel, and that product insured by infrared spectroscopy.
Keywords/Search Tags:RP chromatography, silica gel, bonding agent, chlorosilanes, Grignard reaction
PDF Full Text Request
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