Silica monolithic supports preparation

Another recent trend focused on supports in the shape of monolithic columns having the goal to benefit from the high permeability and the improved mass transfer characteristics of such structures. With this goal in mind, Lubda and Lindner [75] prepared enantioselective silica monolith columns with tert-butylcarbamoylquinine surface modification. A commercial sol-gel-derived Chromolith Performance Si (100 X 4.6 mm ID) monolith (1.9 tim macropore diameter, 12.5 nm mesopore... 

Fields reported that continuous silica xerogels prepared from potassium silicate solutions could be used as highly permeable support media, and exhibit reasonable chromatographic efficiency in HPLC [23]. Minakuchi et al. reported the preparation and evaluation of continuous porous-silica columns that provide a much higher column efficiency in HPLC than do conventional columns packed with particles [13-16,18], The monolithic columns prepared in a capillary can also be used in CEC. 

The preparation of polymeric monoliths is relatively simple compared with those of the silica rods. A polymerization mixture consisting of monomer, cross-linker, initiator, and porogenic solvent is introduced into a sealed tube. The reaction can be temperature or redox initiated and in the case of transparent molds UV light can also be used to trigger the polymerization. At the end of the reaction the seals are removed and the tubes are attached to a pump, which flushes solvent through the monolith to remove the porogens and the unreacted components. The obtained monolith can be radial or axial compressed to prevent the formation of voids and further functionalized for different chromatographic modes. The majority of current monolithic supports... 

Monolith Column—Porous silica column prepared in situ to completely fill the column tube with a fully porous silica foam skelton. After the organic polymer support is heated off, the silica surface is silylated in place to product bonded-phase surface. Column is high resolution and can be used at high flow rates with relatively low back-pressure (see Chapter 16). 

Another group active in this field of research is led by Michael Buchmeiser, who has reported NHC-supported, catalyst systems anchored to both monolithic polymer and silica supports. The first example from this group involved the preparation of the norbornene-functionalized NHC salt 13, and the subsequent tethering of this molecule to a Runorbornene-derived monolithic material (14 Scheme 5.1) using ROMP [25]. The free carbene was then generated on the support and treated... 

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