Inorganic porous material and process for making same

• US 5,624,875 A
• Filed: 01/18/1996
• Issued: 04/29/1997
• Est. Priority Date: 07/19/1993
• Status: Expired due to Term

• Current Assignee: Merck Patent GmbH (Merck & Co., Inc.)
• Original Assignee: Merck Patent GmbH (Merck & Co., Inc.)
• Inventors: Nakanishi, Kazuki, Soga, Nachiro
• Primary Examiner(s): GROUP, KARL E
• Application Number:
  US08/586,632
• Time in Patent Office: 467 Days
• Field of Search: 501/12, 501/39, 65/17.2, 65/21.4, 65/22
• US Class Current: 501/39
• CPC Class Codes: B01J 20/103 comprising silica
• CPC Class Codes: B01J 20/28042 Shaped bodies; Monolithic structures
• CPC Class Codes: B01J 20/28083 being in the range 2-50 nm, i.e. mesopores
• CPC Class Codes: B01J 20/28085 being more than 50 nm, i.e. macropores
• CPC Class Codes: B01J 20/28092 Bimodal, polymodal, different types of pores or different pore size distributions in different parts of the sorbent
• CPC Class Codes: B01J 20/291 Gel sorbents
• CPC Class Codes: B01J 2220/54 Sorbents specially adapted for analytical or investigative chromatography
• CPC Class Codes: C03C 11/00 Multi-cellular glass ; Porous or hollow glass or glass particles
• CPC Class Codes: G01N 2030/525 surface properties, e.g. porosity
• CPC Class Codes: G01N 2030/528 Monolithic sorbent material

Abstract

A process for producing inorganic porous materials is disclosed. The materials prepared by this process are favorably applied to producing columns for chromatography, porous filters for separating blood, porous catalysts, or enzyme supports. These materials have interconnected continuous macropores with a median diameter larger than 0.1 μm. A preferred embodiment of said materials contains additionally mesopores in the walls of said macropores, said mesopores having a median diameter between 2 and 100 nm.

Claims

1. An inorganic porous material comprising a glass or glass-ceramic having interconnected continuous macropores with a median diameter larger than 0.1 μ

m and having mesopores with a median diameter of 2 to 100 nm on the walls of said macropores.

2. The inorganic porous column of claim 1, wherein the glass or glass-ceramic contains silica as the primary component.

3. The inorganic porous column of claim 1, wherein the percentage of macropore volume to total pore volume is from 20-90%.

4. The inorganic porous column of claim 1, wherein the percentage of mesopore volume to total pore volume is more than 10%.

5. The inorganic porous column of claim 1, wherein the percentage of mesopore volume to total pore volume is more than 50%.

6. The inorganic porous material of claim 1 in the form of a column.

7. The inorganic porous material of claim 1 in the form of a flat sheet.

8. The inorganic porous material of claim 1, wherein the macropores have a median diameter of 0.1 to 50 μ

m.

9. The inorganic porous material of claim 1, wherein the macropores have a median diameter of 0.2 to 20 μ

m.

10. The inorganic porous material of claim 1, wherein the surface of the macropores mesopores or both are modified by a functional organic ligand, an enzyme or a catalyst metal.

11. The inorganic porous material of claim 1, wherein the median diameter of the mesopores is 2 to 50 nm.

12. A process for chromatographic separation of a mixture of two substances which comprises passing said mixture through the inorganic porous material of claim 1.

13. A process for the preparation of an inorganic porous material comprising a glass or glass-ceramic having interconnected continuous macropores with a median diameter larger than 0.1 μ

m and having mesopores with a median diameter of 2 to 100 nm in the walls of said macropores, which comprises;

(a) preparing a gel having three dimensional interconnected phase domains, one phase domain being predominantly solvent and another phase domain being predominantly inorganic material with surface pores;

(b) immersing the gel in a liquid capable of dissolving the inorganic material;

(c) removing the liquid by evaporation drying and heat treatment; and

(d) calcining the gel to form the inorganic porous material.

14. The process of claim 13, wherein the inorganic material is silica and the liquid is an aqueous ammonia solution.

15. The process of claim 14, wherein the concentration of the aqueous ammonia solution is 10 mmol/l to 10 mol/l.

16. The process of claim 15, wherein the inorganic material is silica and the liquid is an aqueous solution containing fluoride ions.