Liquid purification or separation – Processes – Liquid/liquid solvent or colloidal extraction or diffusing...
Patent
1996-07-16
1997-09-16
Therkorn, Ernest G.
Liquid purification or separation
Processes
Liquid/liquid solvent or colloidal extraction or diffusing...
210656, 2101982, 2105021, B01D 1508
Patent
active
056676921
DESCRIPTION:
BRIEF SUMMARY
The invention relates to an improved method for gel permeation chromatography and to support materials for this method.
BACKGROUND OF THE INVENTION
Gel permeation chromatography (GPC) for the size separation of macromolecules has become a standard method for the separation of biopolymers, especially proteins. This method requires support materials which possess a hydrophilic surface and which exhibit as little nonspecific adsorption behavior as possible. Furthermore, the supports used are to be pressure-stable in order to achieve high flow rates. This condition is particularly difficult to meet in the case of wide-pored supports.
The application DE 43 10 964 discloses oxirane-containing activated support materials in which monomers of the formula I are grafted onto a hydroxyl-containing base support ##STR2## in which R.sup.1, R.sup.2 and R.sup.3 independently of one another are H or CH.sub.3,
SUMMARY OF THE INVENTION
It has been found that these activated support materials can be reacted to give the crosslinked graft polymers according to the invention. In this reaction, cross-linking takes place onto the known graft polymer, having a linear polymer chain, by reaction, for example, with boron trifluoride etherate; the remaining epoxide groups are subsequently hydrolyzed if desired.
It was found that the separation properties of Fractogel.RTM. TSK HW 65 (S), a porous, vinyl-based copolymer containing aliphatic hydroxyl groups (1 meq of OH/g), were altered considerably if this base material was subjected to graft polymerization with glycidyl methacrylate followed by crosslinking. These measures provide access to gel permeation supports having improved separation properties.
The invention relates to support materials for gel permeation chromatography, based on hydroxyl-containing base supports on whose surfaces polymers are covalently bonded, characterized in that monomer unit, ##STR3## in which R.sup.1, R.sup.2 and R.sup.3 independently of one another are H or CH.sub.3,
The invention relates to processes for the preparation of support materials based on hydroxyl-containing base supports on whose surfaces polymers are covalently bonded by graft polymerization, characterized in that the hydroxyl-containing base support particles are suspended and polymerized in the presence of cerium(IV) ions in a solution comprising monomers of the formula I ##STR4## in which R.sup.1, R.sup.2 and R.sup.3 independently of one another are H or CH.sub.3 groups are converted to hydroxyl groups.
The invention relates to the use of a support material according to the invention for gel permeation chromatography, and to methods of separating at least two substances in a mixture by means of gel permeation chromatography using a support material according to the invention.
Base supports in the context of the present invention are particles onto which polymers are grafted. Base supports which can be employed are, in general, customary porous or nonporous support particles, provided they have primary or secondary aliphatic hydroxyl groups at their surface or can have aliphatic hydroxyl groups introduced into them by processes which are known per se. Particularly suitable base supports are polyvinyl alcohol-based polymers, or copolymers of (meth)acrylate derivatives and comonomers containing aliphatic hydroxyl groups, or diol-modified silica gels or polyvinyl-based copolymers containing aliphatic hydroxyl groups. Such base supports are obtainable commercially; one example is Fractogel.RTM. TKS HW 65 (S) (from E. Merck), a porous vinyl-based copolymer containing aliphatic hydroxyl groups (1 meq of OH/g).
It has surprisingly been found that (meth)acrylic esters containing an oxirane group can be grafted onto base supports comprising aliphatic hydroxyl groups on their surface. In this context, the polymerization is initiated in accordance with the invention using cerium(IV) ions: G. Mino and S. Kaizerman (1958) J. Polymer Science 31, 242-243; G. Mino et al. (1959) J. Polymer Science 38, 393-401. The activated support materials obtainab
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Merck Patent Gesellschaft mit beschrankter Haftung
Therkorn Ernest G.
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