IP Library Granted Patent US 7,223,473
Granted Patent B2
US 7,223,473 · App. 10/744,598 · Granted May 29, 2007

Porous inorganic/organic hybrid particles for chromatographic separations and process for their preparation

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Quick Facts
Patent No.
US 7,223,473
App. No.
10/744,598
Granted
May 29, 2007
Kind
B2
Abstract

Novel material for chromatographic separations, processes for its preparation, and separations devices containing the chromatographic material. In particular, the disclosure describes porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry, which desirably may be surface modified, and that offer more efficient chromatographic separations than that known in the art.

Claims (25)

1. A porous inorganic/organic hybrid material, comprising porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry, wherein said particles have been surface modified with a surface modifier having the formula Z a (R′) b Si—R, where Z=Cl, Br, I, C 1 –C 5 alkoxy, dialkylamino or trifluoromethanesulfonate; a and b are each an integer from 0 to 3 provided that a+b=3; R′ is a C 1 –C 6 straight, cyclic or branched alkyl group, and R is a functionalizing group.

2. The hybrid material-of claim 1 , wherein said particles have been further surface modified by coating with a polymer.

3. The hybrid material of claim 1 wherein R′ is selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl, t-butyl, sec-butyl, pentyl, isopentyl, hexyl and cyclohexyl.

4. The hybrid material of claim 1 wherein the functionalizing group R is selected from the group consisting of alkyl, alkenyl, alkynyl, aryl, cyano, amino, diol, nitro, ester, a cation or anion exchange group, and an alkyl or aryl group containing an embedded polar functionality.

5. The hybrid material of claim 4 , wherein said functionalizing group R is a C 1 –C 30 alkyl group.

6. The hybrid material of claim 4 , wherein said functionalizing group R is a C 1 –C 20 alkyl group.

7. The hybrid material of claim 1 , wherein said surface modifier is selected from the group consisting of octyltrichlorosilane, octadecyltrichlorosilane, octyldimethylchlorosilane, and octadecyldimethylchlorosilane.

8. The hybrid material of claim 7 , wherein said surface modifier is selected from the group consisting of octyltrichlorosilane and octadecyltrichlorosilane.

9. The hybrid material of claim 1 , wherein said particles have been surface modified by a combination of organic group and silanol group modification.

10. The hybrid material of claim 1 , wherein said particles have been surface modified by a combination of organic group modification and coating with a polymer.

11. The hybrid material of claim 1 , wherein said particles have been surface modified by a combination of silanol group modification and coating with a polymer.

12. The hybrid material of claim 1 , wherein said particles have been surface modified via formation of an organic covalent bond between the particle's organic group and the modifying reagent.

13. The hybrid material of claim 1 , wherein said particles have been surface modified by a combination of organic group modification, silanol group modification, and coating with a polymer.

14. The hybrid material of claim 1 , wherein said particles have been surface modified by silanol group modification.

15. A separations device having a stationary phase comprising porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry, wherein the particles have been surface modified with a surface modifier having the formula Z a (R′) b Si—R, where Z=Cl, Br, I, C 1 –C 5 alkoxy, dialkylamino or trifluoromethanesulfonate; a and b are each an integer from 0 to 3 provided that a+b=3; R′ is a C 1 –C 6 straight, cyclic or branched alkyl group, and R is a functionalizing group.

16. The separations device of claim 15 , wherein said surface modifier is selected from the group consisting of octyltrichlorosilane, octadecyltrichlorosilane, octyldimethylchlorosilane, and octadecyldimethylchlorosilane.

17. The separations device of claim 16 , wherein said surface modifier is selected from the group consisting of octyltrichlorosilane and octadecyltrichlorosilane.

18. The separations device of claim 15 , wherein said functionalizing group R is selected from the group consisting of alkyl, alkenyl, alkynyl, aryl, cyano, amino, diol, nitro, ester, a cation or anion exchange group, and an alkyl or aryl group containing an embedded polar functionality.

19. The separations device of claim 15 , wherein said functionalizing group R is a C 1 –C 30 alkyl group.

20. A chromatographic column having improved lifetime, comprising

a) column having a cylindrical interior for accepting a packing material, and

b) a packed chromatographic bed comprising porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry that have been surface modified with a surface modifier having the formula Z a (R′) b Si—R, where Z=Cl, Br, I, C 1 –C 5 alkoxy, dialkylamino or trifluoromethanesulfonate; a and b are each an integer from 0 to 3 provided that a+b=3; R′ is a C 1 –C 6 straight, cyclic or branched alkyl group, and R is a functionalizing group.

21. A chromatographic column having improved lifetime, comprising

a) column having a cylindrical interior for accepting a packing material, and

b) a packed chromatographic bed comprising porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry that have been surface modified with a surface modifier having the formula Z a (R′) b Si-R, where Z=Cl, Br, I, C 1 –C 5 alkoxy, dialkylamino or trifluoromethanesulfonate; a and b are each an integer from 0 to 3 provided that a+b=3; R′ is a C 1–C 6 straight, cyclic or branched alkyl group, and R is a functionalizing group.