Filter including a porous discriminating layer on a fused single crystal acicular ceramic support, and method for making the same

• US 5,198,007 A
• Filed: 12/05/1991
• Issued: 03/30/1993
• Est. Priority Date: 12/05/1991
• Status: Expired due to Term

• Current Assignee: The Dow Chemical Company (Dow, Inc.)
• Original Assignee: The Dow Chemical Company (Dow, Inc.)
• Inventors: Moyer, John R., Hughes, Neal N.
• Primary Examiner(s): Sever, Frank
• Application Number:
  US07/803,292
• Time in Patent Office: 481 Days
• Field of Search: 210/510.1, 55/523, 55/DIG. 5, 55/DIG. 3, 156/89, 428/116-118, 501/53, 501/55, 501/80, 501/68, 501/94, 501/133, 501/153, 501/154
• US Class Current: 55/523
• CPC Class Codes: B01D 2201/46 Several filtrate discharge conduits each connected to one filter element or group of filter elements
• CPC Class Codes: B01D 2239/0478 on a layer of the filter
• CPC Class Codes: B01D 2239/0654 Support layers
• CPC Class Codes: B01D 2239/10 Filtering material manufacturing
• CPC Class Codes: B01D 2239/1216 Pore size
• CPC Class Codes: B01D 29/31 Self-supporting filtering elements
• CPC Class Codes: B01D 29/52 in parallel connection
• CPC Class Codes: B01D 39/1692 Other shaped material, e.g. perforated or porous sheets
• CPC Class Codes: B01D 39/2075 sintered or bonded by inorganic agents
• CPC Class Codes: B01D 46/0039 with flow guiding by feed or discharge devices
• CPC Class Codes: B01D 46/2429 of the honeycomb walls or cells
• CPC Class Codes: B01D 46/24492 Pore diameter
• CPC Class Codes: C04B 14/047 Zeolites
• CPC Class Codes: C04B 2111/00612 as one or more layers of a layered structure
• CPC Class Codes: C04B 2111/00793 as filters or diaphragms
• CPC Class Codes: C04B 2111/00801 Membranes; Diaphragms
• CPC Class Codes: C04B 35/185 Mullite 3Al2O3-2SiO2
• CPC Class Codes: C04B 38/00 Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof treating slag with gases or gas generating material C04B5/06 ; expanded graphite C04B35/536
• CPC Class Codes: C04B 38/0006 Honeycomb structures from one or more corrugated sheets by winding or stacking C04B38/0083
• CPC Class Codes: C04B 38/0051 characterised by the pore size, pore shape or kind of porosity
• CPC Class Codes: C04B 41/4582 : Porous coatings, e.g. coating containing porous fillers
• CPC Class Codes: C04B 41/48 : Macromolecular compounds
• CPC Class Codes: C04B 41/5031 : Alumina
• CPC Class Codes: Y10S 55/05 : Methods of making filter
• CPC Class Codes: Y10S 55/30 : Exhaust treatment

Abstract

A filter useful for separating contaminants from fluids includes a fused single crystal acicular ceramic support having a discriminating layer thereon, such as a sintered, porous alpha-alumina membrane, on at least part of the support. The support is preferably composed of a non-stoichiometric acicular mullite of about 76 percent by weight Al₂ O₃ and about 24 percent by weight SiO₂. The support can be any one of a variety of shapes, but is conveniently elongated in form and preferably includes a plurality of parallel channels through it. The support may be in either a dead-end or cross-flow configuration. In the dead-end configuration, half of the channel holes at each end are plugged in a checkerboard arrangement with the holes open at one end and plugged at the other end. In the cross-flow configuration, all channels are connected by a series of shallow slits cut in the filter, and no end plugs are used.

Claims

1. A filter useful for separating at least one contaminant from a fluid passed through said filter, comprising:

a porous support composed of a fused interlocked single crystal acicular ceramic material having properties sufficient to provide high mechanical strength, high impact strength, heat resistance and good resistance to thermal cycling; and

a porous discriminating layer on at least part of said support.

2. The filter of claim 1, wherein said ceramic material is non-stoichiometric acicular mullite.

3. The filter of claim 2, wherein said non-stoichiometric acicular mullite is composed of about 76 percent by weight alumina and about 24 percent by weight silica.

4. The filter of claim 1, wherein said support is formed as a honeycomb extrusion of plural parallel channels.

5. The filter of claim 4, further comprising porous plugs of said ceramic material interlocked with said extrusion, disposed in single, alternating ends of said channels.

6. The filter of claim 1, wherein said support is formed as a disk having a face on which said discriminating layer is disposed.

7. The filter of claim 1, wherein said support is formed as a cylinder.

8. The filter of claim 7, Wherein said cylinder has a hollow interior and an external surface, and wherein said discriminating layer is disposed on said external surface of said cylinder.

9. The filter of claim 8, further comprising means permitting fluid passing through said discriminating layer and said cylinder to exit said interior of said cylinder.

10. The filter of claim 1, wherein said support includes an extrusion having a fluid inlet end and a porous end cap positioned over said fluid inlet end, said end cap being composed of said ceramic material interlocked with said extrusion.

11. The filter of claim 1, wherein said support includes an extrusion having a fluid outlet end and a porous end cap positioned over said fluid outlet end, said end cap being composed of said ceramic material interlocked with said extrusion.

12. The filter of claim 1, wherein said support has a theoretical density of about 15 to 50 percent.

13. The filter of claim 1, wherein the average pore size of said support is about 10 to about 25 micrometers.

14. The filter of claim 1, wherein said discriminating layer is a sintered ceramic layer, a layer of a polymeric organic compound, a molecular sieve, a gel filtration gel, or a microporous gaseous diffusion barrier.

15. The filter of claim 1, wherein said discriminating layer is a sintered alpha-alumina membrane.

16. The filter of claim 1, wherein said discriminating layer has a pore size between about 0.5 nanometers and about 50 micrometers.

17. The filter of claim 1, further comprising an external, fluid-impermeable glaze substantially covering said filter.

18. The filter of claim 17, wherein said glaze includes a mixture of glass frit and clay.

19. A filter useful for separating at least one contaminant from a fluid passed through said filter, comprising:

a support including a porous honeycomb extrusion composed of a non-stoichiometric acicular mullite having properties sufficient to provide high mechanical strength, high impact strength, heat resistance and good resistance to thermal cycling, having a plurality of parallel channels and including a fluid inlet end and a fluid outlet end;

a plurality of plugs disposed in single alternating ends of said parallel channels, said plugs also being made of non-stoichiometric acicular mullite and interlocked with said honeycomb extrusion; and

end caps positioned over said fluid inlet and fluid outlet ends, said end caps also being made of non-stoichiometric acicular mullite and interlocked with said honeycomb extrusion;

said extrusion, said plugs and one of said end caps including surfaces defining an inlet chamber in said filter;

an external fluid-impermeable glaze covering said support; and

a sintered porous alpha-alumina membrane on said inlet chamber-defining surfaces of said support, said membrane acting as a discriminating layer for filtering and separating.

20. A method of forming a filter useful for separating at least one contaminant from a fluid passed through said filter, comprising:

forming a green support composed of a ceramic material capable of being converted in situ into fused, interlocked, single crystal, acicular ceramic particles;

converting said ceramic material in situ into fused, interlocked, single crystal, acicular ceramic particles, thereby forming a rigid and porous ceramic support having high mechanical strength, high impact strength, heat resistance and good resistance to thermal cycling; and

applying a porous discriminating layer on at least part of said support.

21. The method of claim 20, wherein said ceramic material is a non-stoichiometric mullite yielding acicular mullite upon said converting step.

22. The method of claim 21, wherein said non-stoichiometric mullite is composed of about 76 percent by weight alumina and 24 percent by weight silica.

23. The method of claim 20, wherein said applying step is accomplished by coating at least one surface of said support with a slurry of alpha-alumina, and sintering said support and said alpha-alumina so as to form a thin, continuous membrane of porous alpha-alumina on said at least one surface of said support.

24. The method of claim 20, wherein said step of forming a support is accomplished by abutting together at least two support pieces, and wherein said pieces become interlocked with one another during said converting step.

25. The method of claim 24, wherein one of said at least two pieces includes a honeycomb extrusion of plural parallel channels.

26. The method of claim 25, wherein the other of said at least two pieces includes a plurality of porous plugs disposed in single alternating ends of said parallel channels.

27. The method of claim 25, wherein said extrusion includes at least one of a fluid inlet end and a fluid outlet end, and wherein the other of said at least two pieces includes an end cap over one of said inlet and outlet ends of said extrusion.

28. The method of claim 20, further comprising the step of firing a fluid-impermeable enamel glaze on said support, substantially covering said support, prior to applying said discriminating layer to said support.

29. The method of claim 20, wherein said ceramic material is a non-stoichiometric mullite composed of alumina and silica, and wherein said converting step is accomplished by heating said support at 500°

to 950°

C. in the presence of silicon tetrafluoride for a time sufficient to form fluorotopaz from said alumina and silica, and then heating said support at 1100°

to 1150°

C. for a time sufficient to transform said fluorotopaz into non-stoichiometric acicular mullite.

30. A method of forming a filter useful for separating at least one contaminant from a fluid passed through said filter, said filter including a porous ceramic support, and said method comprising:

abutting at least two support pieces together, said pieces each being composed of a ceramic material capable of being converted in situ into fused, interlocked, single crystal, acicular particles having properties sufficient to provide high mechanical strength, high impact strength, heat resistance and good resistance to thermal cycling; and

converting said ceramic material in situ into fused, interlocked, single crystal, acicular particles;

whereby said two support pieces become unified and interlocked by said acicular particles.

31. The method of claim 30, wherein said ceramic material is a non-stoichiometric mullite, and said converting step is carried out so as to convert said pieces into non-stoichiometric acicular mullite.

32. The method of claim 31, wherein said non-stoichiometric mullite is composed of about 76 percent by weight alumina and 24 percent by weight silica.

33. The method of claim 30, wherein said at least two support pieces include an extrusion and end caps on the ends of said extrusion.

34. The method of claim 30, wherein said at least two support pieces include a honeycomb extrusion having channels defined therein, and plugs closing the ends of at least some of said channels.

35. The method of claim 34, wherein said plugs are composed of a paste or slurry of said ceramic material.

36. The method of claim 30, wherein said at least two pieces are abutted by joining said pieces with a paste or slurry including said ceramic material.