Superficially porous materials comprising a substantially nonporous hybrid core having narrow particle size distribution; process for the preparation thereof; and use thereof for chromatographic separations

Patent metadata

Field	Value
Publication number	US-10092893-B2
Application number	US-201113638924-A
Country	US
Kind code	B2
Filing date	Jul 25, 2011
Priority date	Jul 26, 2010
Publication date	Oct 9, 2018
Grant date	Oct 9, 2018

Abstract

The present invention provides novel chromatographic materials, e.g., for chromatographic separations, processes for its preparation and separations devices containing the chromatographic material; separations devices, chromatographic columns and kits comprising the same; and methods for the preparation thereof. The chromatographic materials of the invention are chromatographic materials comprising having a narrow particle size distribution.

First claim

The invention claimed is:

1. A superficially porous material comprising superficially porous particles, wherein the superficially porous particles comprise an inorganic/organic hybrid core and one or more layers of a porous shell material surrounding the inorganic/organic hybrid core wherein the inorganic/organic hybrid core has a pore volume of less than 0.10 cc/g; and
wherein the inorganic/organic hybrid core has the formula:
(SiO 2 ) d /[R 2 ((R) p (R 1 ) q SiO t ) m ]  (I)

wherein,
R and R 1 are each independently C 1 -C 18 alkoxy, C 1 -C 18 alkyl, C 2 -C 18 alkenyl, C 2 -C 18 alkynyl, C 3 -C 18 cycloalkyl, C 1 -C 18 heterocycloalkyl, C 5 -C 18 aryl, C 5 -C 18 aryloxy, or C 1 -C 18 heteroaryl;
R 2 is C 1 -C 18 alkyl, C 2 -C 18 alkenyl, C 2 -C 18 alkynyl, C 3 -C 18 cycloalkyl, C 1 -C 18 heterocycloalkyl, C 5 -C 18 aryl, C 1 -C 18 heteroaryl, wherein R 2 is attached to two or more silicon atoms;
R, R 1 and R 2 are optionally substituted;
p and q are each independently 0.0 to 2.0,
t is 0.5, 1.0, or 1.5;
d is 0 to about 30; and
m=2-20,

t
=

(

3
-

(

p
+
q

)

)

2

,

and p+q≤2.

2. The superficially porous material of claim 1 , wherein the superficially porous material has chromatographically enhancing pore geometry.

3. The superficially porous material of claim 1 wherein the porous shell material is a porous inorganic/organic hybrid material.

4. The superficially porous material of claim 1 wherein the porous shell material is a porous silica.

5. The superficially porous material of claim 1 wherein the porous shell material is a porous composite material.

6. The superficially porous material of claim 1 , wherein the superficially porous particles comprise an inorganic/organic hybrid core and more than one layer of a porous shell material wherein each layer of the porous shell material is independently selected from a porous inorganic/organic hybrid material of formula (I) according to claim 1 , a porous silica, a porous composite material, or mixtures thereof.

7. The superficially porous material of claim 1 wherein the superficially porous material has a spherical core morphology, a rod shaped core morphology, a bent-rod shaped core morphology, a toroid shaped core morphology, or a dumbbell shaped core morphology.

8. The superficially porous material of claim 1 , wherein the inorganic/organic hybrid core has a particle size of 0.5-10 μm.

9. The superficially porous material of claim 1 , wherein the superficially porous particles comprise an inorganic/organic hybrid core and more than one layer of a porous shell material, wherein each layer of porous shell material is independently from 0.05 μm to 5 μm in thickness as measured perpendicular to an outer surface of the inorganic/organic hybrid core.

10. The superficially porous material of claim 1 , wherein the superficially porous material has an average particle size between 0.8-10.0 μm.

11. The superficially porous material of claim 1 , wherein the superficially porous material has an average pore diameter of about 25-600 Å.

12. The superficially porous material of claim 1 , wherein the superficially porous material has an average pore volume of about 0.11-0.50 cm 3 /g.

13. The superficially porous material of claim 1 , wherein pore surface area is between about 10 m 2 /g and 400 m 2 /g.

14. The superficially porous material of claim 1 , which has been further surface modified.

15. The superficially porous material of claim 1 , which has been further surface modified by:
coating with a polymer;
by coating with a polymer by a combination of organic group and silanol group modification;
a combination of organic group modification and coating with a polymer;
a combination of silanol group modification and coating with a polymer;
formation of an organic covalent bond between an organic group of the material and a modifying reagent; or
a combination of organic group modification, silanol group modification and coating with a polymer.

16. A separations device having a stationary phase comprising the superficially porous material of claim 1 .

17. A chromatographic column, comprising
a) a column having a cylindrical interior for accepting a packing material and
b) a packed chromatographic bed comprising the superficially porous material of claim 1 .

18. A chromatographic device, comprising
a) an interior channel for accepting a packing material and
b) a packed chromatographic bed comprising the superficially porous material of claim 1 .

19. A kit comprising the superficially porous material of claim 1 , and instructions for use.

20. The superficially porous material of claim 1 , wherein the superficially porous particles comprise an inorganic/organic hybrid core and one or more layer of a porous shell material; and wherein each layer of the porous shell material is independently selected from a porous inorganic/organic hybrid material of formula (I) according to claim 1 .

Assignees

• Wyndham Kevin D
• Muriithi Beatrice W
• Waters Technologies Corp

Inventors

• Wyndham Kevin D
• Muriithi Beatrice W

Classifications

• B01J20/3219

  involving a particular spacer or linking group, e.g. for attaching an active group · CPC title

• B01J20/3257

  the functional group or the linking, spacer or anchoring group as a whole comprising at least one of the heteroatoms nitrogen, oxygen or sulfur together with at least one silicon atom, these atoms not being part of the carrier as such · CPC title

• B01J20/28004

  Sorbent size or size distribution, e.g. particle size · CPC title

• B01J20/28057

  Surface area, e.g. B.E.T specific surface area · CPC title

• Y10T428/2991

  Coated · CPC title