Methods and devices using a shrinkable support for porous monolithic materials

• US 7,651,762 B2
• Filed: 03/13/2007
• Issued: 01/26/2010
• Est. Priority Date: 03/13/2007
• Status: Active Grant

• Current Assignee: Agilent Technologies, Inc.
• Original Assignee: Varian Incorporated (Agilent Technologies, Inc.)
• Inventors: Xu, Dengfeng, Grenz, Robert Lee
• Primary Examiner(s): XU, LING X
• Application Number:
  US11/717,317
• Publication Number:
  US 20080223786A1
• Time in Patent Office: 1,050 Days
• Field of Search: None
• US Class Current: 428/304.4
• CPC Class Codes: B01J 20/28042 Shaped bodies; Monolithic structures
• CPC Class Codes: B01J 20/28054 characterised by their surface properties or porosity
• CPC Class Codes: B01J 20/282 Porous sorbents ion exchange B01J39/00 - B01J41/00
• CPC Class Codes: B01J 2220/82 Shaped bodies, e.g. monoliths, plugs, tubes, continuous beds
• CPC Class Codes: B01J 35/56 Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
• CPC Class Codes: G01N 2030/528 Monolithic sorbent material
• CPC Class Codes: G01N 30/56 Packing methods or coating methods
• CPC Class Codes: G01N 30/6052 body
• CPC Class Codes: Y10T 428/22 Nonparticulate element embedded or inlaid in substrate and visible
• CPC Class Codes: Y10T 428/249953 Composite having voids in a component [e.g., porous, cellular, etc.]
• CPC Class Codes: Y10T 428/249967 Inorganic matrix in void-containing component
• CPC Class Codes: Y10T 428/24997 Of metal-containing material
• CPC Class Codes: Y10T 428/249987 With nonvoid component of specified composition
• CPC Class Codes: Y10T 428/24999 Inorganic

Abstract

Articles of manufacture and devices and methods of forming and using the same are provided, wherein the article comprises a porous inorganic substrate contained in or bounded by a support made from an inorganic material are provided, wherein said porous substrate and support are heated to a temperature effective to shrink the support onto the porous substrate such that liquid tight contact is formed between the porous substrate and the support. In a preferred aspect, the porous inorganic substrate has a porosity of at least 5%, and is a porous monolith formed using a sol-gel method. The articles thus formed provide a confined fluid flow through the porous substrate, providing superior performance in separations, catalysis, filtration, and the like.

Claims

1. An article comprising a porous inorganic substrate contained in a support made from an inorganic material, wherein said porous substrate and support are heated to a temperature effective to shrink but not melt the support onto the porous substrate such that liquid tight contact is formed between the porous substrate and the support, wherein said temperature is near or above the softening temperature for the inorganic material, and wherein the temperature effective to shrink the support onto the porous substrate has no affect or only limited affect on the pore distribution of the porous substrate.

2. The article of claim 1, wherein the porous inorganic substrate is a porous monolith.

3. The article of claim 1, further wherein a vacuum is applied to the support that is sufficient to lower the temperature at which shrinkage occurs.

4. The article of claim 1, wherein said article is adapted for use in chromatography, catalysis, adsorption, filtration, fuel cells, optoelectronics, sensor technologies, or hydrogen storage.

5. The article of claim 1, wherein said porous inorganic substrate comprises an inorganic material or an inorganic-organic hybrid material.

6. The article of claim 5, wherein said support comprises a metal or metalloid oxide.

7. The article of claim 1, wherein inorganic porous substrate is a porous monolith formed using a sol-gel method.

8. The article of claim 1, wherein the porosity, chemistry, adsorption or catalytic characteristics of the porous substrate are modified.

9. The article of claim 8, wherein said modifying is selected from the introduction of a bonded phase, introduction of a catalytic functionality, structure remodeling, or introduction of a sensor.

10. The article of claim 1, wherein said support made from an inorganic material comprises a glass or ceramic material.

11. The article of claim 1, further comprising a protective outer layer.

21. The article of claim 1, wherein the liquid tight contact between the porous inorganic substrate and the support is formed by a method comprising the steps of

a) assembling the porous inorganic substrate into a support comprising an inorganic material, and

b) shrinking the support onto the porous inorganic substrate by heating the article to a temperature that is effective to shrink but not melt the support onto the porous substrate

wherein said temperature is near or above the softening temperature for the inorganic material, and wherein the temperature effective to shrink the support onto the porous substrate has no affect or only limited affect on the pore distribution of the porous substrate.

12. A method of forming an article comprising a porous inorganic substrate in liquid tight contact with an inorganic support, comprising:

a) assembling a porous inorganic substrate into a shrinkable support comprising an inorganic material, and

b) shrinking the support onto the porous substrate by heating the article to a temperature that is effective to shrink but not melt the support onto the porous substrate, such that there is liquid tight contact between the porous substrate and the support, wherein said temperature is near or above the softening temperature for the inorganic material, and wherein the temperature effective to shrink the support onto the porous substrate has no affect or only limited affect on the pore distribution of the porous substrate.

13. The method of claim 12, wherein a vacuum is applied to the support that is sufficient to lower the temperature at which shrinkage occurs.

14. The method of claim 13, wherein said porous inorganic substrate comprises a metal or metalloid oxide selected from oxides of Si, Ge, Sn, Al, Ga, Mg, Mb, Co, Ni, Ga, Be, Y, La, Pb, V, Nb, Ti, Zr, Ta, W, Hf, or combinations thereof.

15. The method of claim 13, wherein said porous inorganic substrate is monolithic.

16. The method of claim 15, wherein said porous inorganic substrate is made using a sol-gel method.

17. The method of claim 15, wherein said porous monolith is formed from particles that are modified to form a monolith.

18. The method of claim 15, wherein said porous monolith is formed separately from said shrinkable support and inserted therein prior to shrinking.

19. The method of claim 15, wherein said porous monolith is formed inside said shrinkable support prior to shrinking.

20. The method of claim 13, wherein said shrinkable support is a glass or ceramic.

22. A chromatographic column comprising a porous inorganic monolith enclosed inside a glass tubing, the improvement comprising forming the porous inorganic monolith from a sol gel, calcining the porous inorganic monolith and assembling it into the glass tubing, and heating the assembly to shrink but not melt the glass tubing such that there is liquid tight contact between the porous inorganic monolith and the glass tubing wherein said heating is to near or above the softening temperature for the glass tubing, and wherein the temperature effective to shrink the glass tubing has no affect or only limited affect on the pore distribution of the porous inorganic monolith.

23. The chromatographic column of claim 22, wherein the porous inorganic monolith is formed and calcined inside the glass tubing prior to heating the assembly to shrink the glass tubing.

24. A method for separating a mixture of analytes in a sample, said method comprising the steps of

a) providing a chromatographic column comprising a porous inorganic substrate enclosed inside a glass tubing, wherein the column has been heated to shrink but not melt the glass tubing such that a liquid tight contact is formed between the porous inorganic substrate and the glass tubing, wherein said heating is to near or above the softening temperature for the glass tubing, and wherein the temperature effective to shrink the glass tubing has no affect or only limited affect on the pore distribution of the porous inornanic substrate;

b) applying the sample to the chromatographic column;

c) eluting the chromatographic column with a mobile phase; and

d) collecting the separated analytes eluting from the chromatographic column.