Cellulose chromatography support

• US 5,245,024 A
• Filed: 12/30/1991
• Issued: 09/14/1993
• Est. Priority Date: 06/30/1989
• Status: Expired due to Term

• Current Assignee: Loyola University Chicago
• Original Assignee: Loyola University Chicago
• Inventors: Beavins, Anita, Scarpa, Ioannis
• Primary Examiner(s): Nutter, Nathan M.
• Application Number:
  US07/778,188
• Time in Patent Office: 624 Days
• Field of Search: 536/56, 536/57, 536/84, 536/92, 536/98, 525/54.21, 525/54.1, 530/403, 530/404, 530/405, 530/814, 436/530
• US Class Current: 536/56
• CPC Class Codes: B01J 20/24 Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
• CPC Class Codes: B01J 20/28004 Sorbent size or size distribution, e.g. particle size
• CPC Class Codes: B01J 20/28011 Other properties, e.g. density, crush strength
• CPC Class Codes: B01J 20/28019 Spherical, ellipsoidal or cylindrical
• CPC Class Codes: B01J 20/286 Phases chemically bonded to a substrate, e.g. to silica or to polymers
• CPC Class Codes: B01J 20/3092 Packing of a container, e.g. packing a cartridge or column of chromatography columns B01D15/206
• CPC Class Codes: B01J 20/3212 consisting of a polymer obtained by reactions otherwise than involving only carbon to carbon unsaturated bonds
• CPC Class Codes: B01J 20/3217 Resulting in a chemical bond between the coating or impregnating layer and the carrier, support or substrate, e.g. a covalent bond
• CPC Class Codes: B01J 20/3248 the functional group or the linking, spacer or anchoring group as a whole comprising at least one type of heteroatom selected from a nitrogen, oxygen or sulfur, these atoms not being part of the carrier as such
• CPC Class Codes: B01J 20/3251 comprising at least two different types of heteroatoms selected from nitrogen, oxygen or sulphur
• CPC Class Codes: B01J 20/3253 comprising a cyclic structure not containing any of the heteroatoms nitrogen, oxygen or sulfur, e.g. aromatic structures
• CPC Class Codes: B01J 20/3255 comprising a cyclic structure containing at least one of the heteroatoms nitrogen, oxygen or sulfur, e.g. heterocyclic or heteroaromatic structures
• CPC Class Codes: B01J 20/3272 Polymers obtained by reactions otherwise than involving only carbon to carbon unsaturated bonds
• CPC Class Codes: B01J 20/3274 Proteins, nucleic acids, polysaccharides, antibodies or antigens
• CPC Class Codes: B01J 20/3425 of sorbents or filter aids comprising organic materials
• CPC Class Codes: B01J 2220/54 Sorbents specially adapted for analytical or investigative chromatography
• CPC Class Codes: B01J 2220/58 Use in a single column
• CPC Class Codes: C08B 16/00 Regeneration of cellulose
• CPC Class Codes: C08J 2301/00 Characterised by the use of cellulose, modified cellulose or cellulose derivatives
• CPC Class Codes: C08J 3/16 by coagulating dispersions C08J3/122 takes precedence
• CPC Class Codes: Y10S 530/814 : Cellulose or derivatives thereof

Abstract

This invention relates to an improved cellulose chromatography support and, in particular, to substantially spherical, high density cellulose particles. This invention also relates to a method of making these spherical, high density cellulose particles and, in particular, to a method for forming spherical cellulose from a high molecular weight viscose in a stable emulsion of a liquid carrier and emulsifying agents.

Claims

1. A chromatographic support comprising substantially spherical, non-cross-linked, high density cellulose particles wherein said particles have a bulk dry apparent density of about 0.65 to 0.85 g/ml, wherein said particles have an average diameter in the range of from about 25 microns to about 200 microns, and wherein said particles are essentially nonswelling in aqueous or organic solutions.

2. The cellulose particles according to claim 1 wherein said particles are stable in aqueous solutions of up to at least 3.0 M potassium chloride and 8 M urea.

3. The cellulose particles according to claim 1 further comprising chromatographic ligands covalently bound to said particles.

4. The cellulose particles according to claim 3 comprising polar chromatographic ligands covalently bound to said particles.

5. The cellulose particles according to claim 3 comprising nonpolar chromatographic ligands covalently bound to said particles.

6. The cellulose particles according to claim 4 wherein said covalently bound ligands are selected from the group consisting of aminoethyl, diethylaminoethyl, epichlorohydrin triethanolamine, polyethyleneimines, methyl polyethyleneimines, benzyl diethylamine ether, diethyl-[2-hydroxypropyl]aminoethyl, triethylaminoethyl, sulphopropyl, carboxymethyl, sulphonate, quaternary ammonium ethyl, antigens and antibodies.

7. The cellulose particles according to claim 1 wherein said particles are stable at pressures up to 120 psi.

8. The cellulose particles according to claim 1 wherein said particles are mechanically stable.

9. A method of making substantially spherical, high density cellulose particles comprising the steps of:

forming a stable emulsion of viscose in the presence of at least one emulsifying agent and a liquid carrier, wherein the temperature of said viscose during the formation of said emulsion does not thermally decompose said viscose;

regenerating cellulose from said viscose in the absence of acid over a period of time with continuous agitation under stationary hydrodynamic conditions to yield a dispersion of uniformly sized, deformable particles;

contacting said dispersion of deformable particles with a solvent suitable to cause a partial extraction of said liquid carrier from said emulsion, wherein said deformable particles begin to partially harden; and

hardening said deformable particles whereby high density particles having an average diameter in the range of from about 25 microns to about 200 microns are produced.

10. The method according to claim 9 wherein said temperature is above the freezing point of said emulsion, but less than 30°

.

11. The method according to claim 10 wherein said temperature is about 20°

to 30°

C.

12. The method according to claim 9 wherein said liquid carrier has a viscosity greater than 150 cSt at temperatures of about 20°

to 30°

C.

13. The method according to claim 12 wherein said liquid carrier is polypropylene glycol having an average molecular weight of about 1200 and a viscosity of about 160 cSt at temperatures of about 20°

to 30°

C.

14. The method according to claim 9 wherein said emulsion is formed in the presence of at least two emulsifying agents.

15. The method according to claim 14 wherein said emulsifying agents are neutral surfactants selected from the group consisting of sorbitan, polyoxyethylene (20) sorbitan monooleate and a castor oil ethoxylate.

16. The method according to claim 9 wherein said particle hardening comprises stirring said deformable particles in an acidic alcoholic solution.

17. The method according to claim 9 further comprising adding a salt solution to the viscose emulsion.

18. Spherical, high density cellulose particles made by a method comprising the steps of:

forming a stable emulsion of viscose in the presence of at least one emulsifying agent and a liquid carrier, wherein the temperature of said viscose during the formation of said emulsion does not thermally decompose said viscose;

regenerating cellulose from said viscose in the absence of acid over a period of time with continuous agitation under stationary hydrodynamic conditions to yield a dispersion of uniformly sized, deformable particles;

contacting said dispersion of deformable particles with a solvent suitable to cause a partial extraction of said liquid carrier from said emulsion, wherein said deformable particles begin to partially harden; and

hardening said deformable particles to produce high density particles having an average diameter in the range of from about 25 microns to about 200 microns.