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Synthesis And Properties Of A New Porous Silica Gel By Sol-Gel/PS Template Method And The Application In Liquid Chromatographic

Posted on:2013-07-04Degree:MasterType:Thesis
Country:ChinaCandidate:Y ShaoFull Text:PDF
GTID:2251330392470389Subject:Materials science
Abstract/Summary:PDF Full Text Request
Chromatographic separation technology has become an important separation andpurification technology in the organic chemistry and biochemistry, andchromatographic column is the key to realize effective separation, so the separationperformance of chromatographic column largely depends on the performance of thechromatographic column packing. Because silica gel is rich in silicon hydroxy whichcan participate in reaction on its surface and for its good strength, porous structure,surface area which is easy to control and good chemical stability etc silica gel hasbecome one kind of the most widely used chromatographic column packing. Thispaper chooses porous silica gel as the research object, and tries to get a new kind ofliquid chromatography column packing which has good column efficiency and lowcolumn pressure. The main research content is as follows:(1) The preparation of polystyrene microsphere. The polymerizationmicrospheres respectively is prepared by using emulsion polymerization anddispersion, and then PS microspheres which have monodispersity and diameter of2μm are obtained through the adjustment of the parameters; PS microsphere surfacesuccessful gets positive charge through the polyimide (PEI) modification, and theeffects of the concentration of PEI on PS surface charge quantity are investigated.(2) The preparation of porous silica gel by sol-gel/PS template method. Withethyl silicate (TEOS) as precursor, Vinyl trimethoxy silane (VTMS) as the couplingagent, nitric acid as catalyst system, silicon sol is preparated, and the effects of theratio of TEOS and VTMS, water content on the the sol-gel process; by adding the PSmicrospheres which is modified by PEI in the sol and the further hydrolysis,polymerization and release processing the porous silica gel is obtained. By usinginfrared spectrum (IR), thermo-gravimetric (TG) and transmission electronmicroscopy (TEM), and the measured zeta CAD porous structure formation process istracked, and the corresponding template mechanism is put forward.(3) Surface alkylation of porous silicon. Using octadecyl trimethyl chlorosilane assilane reagents the obtained porous silicon realizes surface chemical modification. Byusing Infrared spectrum and transmission electron microscopy characterizationmethods the structure and morphology of bond silicon phase and the possible causeswhich lead to the nonideal result are analyzed. (4) Discussion of porous silica gel‘s chromatographic application. The poroussilica gel is filled in the chromatographic column which is long15cm and hasdiameter of5mm through the slurry loading column pump, and then using theobtained chromatographic column material separation is realized on liquidchromatograph (island sea LC-10AD) to test its separation effect as liquidchromatography column stationary phase.
Keywords/Search Tags:Sol-gel, Porous silica composites, Liquid chromatography
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