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Ce(IV)-INITIATED GRAFT POLYMERISATION ON POLYMERS CONTAINING NO HYDROXYL GROUPS

a technology of hydroxyl group and polymerisation method, which is applied in the direction of anion exchangers, chemical/physical processes, peptides, etc., can solve the problems of limited number of oh group on the surface which are accessible to the reaction, limited stability to alkaline solutions, and complex process. time-consuming and labor-intensive problems

Inactive Publication Date: 2012-11-22
MERCK PATENT GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0010]The object of the present invention is therefore to provide a process which provides the possibility of preparing, in a simple and versatile manner, graft-polymerised chromatography materials on the basis of polymers which, although having no reactive hydroxyl groups on the surface, can, however, be derivatised in a simple manner in a graft polymerisation reaction which is initiated by Ce(IV) ions. A further object of the present invention is to provide a corresponding process which is simple and inexpensive to carry out and to provide chromatography materials having a broad application spectrum with respect to the possibility of separation of substance mixtures of a wide variety of origins, but also with respect to the stability to the influence of acids, bases, pressure or flow conditions.Subject-Matter of the Invention
[0026]Since it may be advantageous for separating off certain biomolecules for an interaction to take place with a hydrophobic component of the separating material, preference is also given to separating materials which have covalently bonded graft polymers on the surface and which are in turn prepared using at least one monomer unit having a pronounced hydrophobic content in the form of at least one alkyl or aryl group having a suitable number of carbon atoms and at least one further monomer unit which carries a charge. Separating materials of this type have proven particularly effective since they can interact with the biopolymer to be separated off both by means of the hydrophobic component and also by means of the charged component of the graft polymer.

Problems solved by technology

This method therefore appears only to be suitable for support materials which have hydroxyl groups on the surface under the given reaction conditions, but not for materials which lack these groups.
The ion exchangers prepared in this way exhibit good separation properties and good pressure stability, but have limited stability to alkaline solutions.
An essential disadvantage of graft polymerisations on support materials which have hydroxyl groups consists in that the number of OH groups on the surface which are accessible to the reaction is limited.
However, this process is complex and time-consuming to carry out.
Furthermore, the chromatography materials prepared on this basis are not suitable for all separation methods.

Method used

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  • Ce(IV)-INITIATED GRAFT POLYMERISATION ON POLYMERS CONTAINING NO HYDROXYL GROUPS
  • Ce(IV)-INITIATED GRAFT POLYMERISATION ON POLYMERS CONTAINING NO HYDROXYL GROUPS
  • Ce(IV)-INITIATED GRAFT POLYMERISATION ON POLYMERS CONTAINING NO HYDROXYL GROUPS

Examples

Experimental program
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Effect test

example 1

Synthesis of the Base Support Poly-MMA / EGDMA (Internal EGDMA-L01)

[0084]2.4 g of polyvinyl alcohol 40-88 (Merck), 5.28 g of sodium sulfate (Merck), 0.36 g of tributyl phosphate (Merck) and 0.48 g of emulsifier E30 (Leuna Tenside) are dissolved in 1200 ml of water. This aqueous phase is warmed to 40° C. 2.4 g of AIBN (Merck) are dissolved in 120 g of toluene (Merck), 160 g of n-heptanol (Merck), 1 g of methyl methacrylate (MMA, Merck) and 120 g of ethylene glycol dimethacrylate (EGDMA, Merck) at room temperature (organic phase). The organic phase is rapidly added to the aqueous phase in an inertised polymerisation vessel with vigorous stirring. The mixture is heated to 65° C. over the course of 50 min. This temperature is maintained for 2 h, and finally the mixture is polymerised at 80° C. for a further 4 h. The organic solvents are substantially removed by steam distillation. The resultant polymer is washed with acetone and water on a suction filter. The surface area of the polymer i...

example 2

Synthesis of the Base Support Poly-NVP / DVH (Internal: DVH-L06)

[0085]36 g of polyvinyl alcohol 40-88 (Merck), 36 g of sodium chloride (Merck) and 0.48 g of emulsifier E30 (Leuna Tenside) are dissolved in 1200 ml of water. This aqueous phase is warmed to 40° C. 1.2 g of AIBN (Merck) are dissolved in 260 g of butyl acetate (Merck), 1 g of N-vinylpyrrolidone (NVP, Merck) and 140 g of 1,3-divinylimidazolin-2-one (BASF) at room temperature (organic phase). The organic phase is rapidly added to the aqueous phase in an inertised polymerisation vessel with vigorous stirring. The mixture is heated to 65° C. over the course of 50 min. This temperature is maintained for 2 h, and finally the mixture is polymerised at 80° C. for a further 4 h. The resultant polymer is washed with acetone and water on a suction filter. The surface area of the polymer is 408 m2 / g.

example 3

Synthesis of the Base Support Poly-ES / DVB

[0086]19.8 g of magnesium hydroxide (Merck), 32 g of sodium sulfate (Merck) and 0.189 g of emulsifier E30 (Leuna Tenside) are dissolved in 1050 ml of water. This aqueous phase is warmed to 50° C. 1.05 g of AIBN (Merck) are dissolved in 185 g of toluene (Merck), 63 g of divinylbenzene (Aldrich) and 37 g of ethylstyrene (Aldrich) at room temperature (organic phase). The organic phase is rapidly added to the aqueous phase in an inertised polymerisation vessel with vigorous stirring. The mixture is heated to 72° C. over the course of 50 min. This temperature is maintained for 2 h, and finally the mixture is polymerised at 80° C. for a further 4 h. The organic solvents are substantially removed by means of steam distillation. The resultant polymer is washed with acetone and water on a suction filter. The surface area of the polymer is 596 m2 / g.

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Abstract

The invention relates to a process for the preparation of a separating material having improved binding capacity, and to materials prepared and to the use thereof for the separation of charged or uncharged biopolymers from liquids.

Description

[0001]The invention relates to a process for the preparation of a novel separating material, and to separating materials prepared and to the use thereof for the separation of charged biopolymers from liquids.PRIOR ART[0002]Chromatography is one of the most suitable methods for the isolation of bio-polymers from liquids. Polymer-based chromatography materials, in particular, are advantageous in the purification of biopharmaceuticals compared with silica-based materials, since polymers can be prepared in such a way that they survive the cleaning of the filled chromatography column by means of sodium hydroxide solution which is necessary in the course of processing.[0003]Besides hydrophobic interaction chromatography (HIC), size exclusion chromatography (SEC), mixed mode chromatography and affinity chromatography, ion exchange chromatography (IEX) is very frequently used. In addition, other types of chromatography, such as, for example, reversed phase chromatography, are also known. A ...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B01J39/20C07K1/18
CPCB01J20/285B01J20/3278B01J2220/82C08F4/52C08F257/02C08F265/00C08F271/00C08L51/003C08F271/02C08F283/06C08F290/06C08F291/00C08L2666/02
Inventor JOEHNCK, MATTHIAS
Owner MERCK PATENT GMBH
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