IP Library Granted Patent US 8,357,728
Granted Patent B2
US 8,357,728 · App. 10/566,873 · Granted Jan 22, 2013

Porous material and method of production thereof

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Quick Facts
Patent No.
US 8,357,728
App. No.
10/566,873
Granted
Jan 22, 2013
Kind
B2
Abstract

The present invention relates to a method for producing a porous material comprising the steps of; (a) providing a C/W emulsion comprising an aqueous phase, a matrix building material, a surfactant and liquid CO 2 phase; (b) at least partially freezing the aqueous phase; (c) gasifying CO 2 from the liquid CO 2 phase to form an intermediate porous material; (d) venting gasified CO 2 from the intermediate porous material; and (e) freeze drying the intermediate porous material at least substantially to remove the aqueous phase and form the porous material. The present invention also relates to a porous material obtainable by the method.

Claims (32)

1. A method for producing a water-soluble porous, polymeric material comprising the steps of:

(a) providing a C/W emulsion comprising an aqueous phase, a matrix building material in the form of a water-soluble polymeric material, a surfactant and a liquid CO 2 phase;

(b) at least partially freezing the aqueous phase;

(c) gasifying CO 2 from the liquid CO 2 phase to produce an intermediate porous material;

(d) venting the gasified CO 2 from the intermediate porous material; and

(e) freeze drying the intermediate porous material at least substantially to remove the aqueous phase and to form the water-soluble porous material; wherein said water-soluble polymeric material is one or more chosen from the group consisting of water-soluble polysaccharides and water-soluble vinyl polymers, and is substantially free of cross-linking such that said water-soluble porous material is able to substantially fully dissolve in water at 20° C.

2. A method for producing a porous material as claimed in claim 1 , wherein the emulsion further comprises a dopant.

3. A method for producing a porous material as claimed in claim 2 , wherein the dopant is substantially water-soluble.

4. A method for producing a porous material as claimed in claim 2 , wherein the dopant is selected from one or more of the following dopants: pharmaceutical actives, pharmaceutical salts, enzymes, dyes, oxidising agents, reducing agents, cleaning agents, reagents for organic synthesis, agrochemicals, fabric softeners, clothes care agents, bleaches, flavours, fragrances, vitamins or nutraceuticals, metal nanoparticles (e.g., metal hydrosols), inorganic nanoparticles, biological polymers (e.g., DNA, RNA), growth factors/cofactors, and live cells (e.g., stem cells).

5. A method for producing a porous material as claimed in claim 1 , wherein a substantially water-soluble inorganic or organic additive is additionally used.

6. A method for producing a porous material as claimed in claim 5 , wherein the additive is selected from one or more of the following additives: partially hydrolysed silica precursors (i.e., a silica sol), other alkoxide sols, hydroxyapatite salts, and sodium silicate.

7. A method for producing a porous material as claimed in claim 1 , wherein the water-soluble polymeric material is selected from one or more of the following group of materials: poly(vinyl alcohol) and dextran.

8. A method for producing a porous material as claimed in claim 1 , wherein the temperature of the emulsion is reduced to a temperature in the range of −5° C. to −30° C.

9. A method for producing a porous material as claimed in claim 1 , wherein the CO 2 is gasified by means of depressurisation of the intermediate porous material.

10. A method for producing a porous material as claimed in claim 1 , wherein the surfactant is selected from one or more of the following list of surfactant: CTAB (cetyltrimethylammonium bromide), SDS (sodium dodecyl sulphate), pluronic surfactants, Brij 30 and Tween 40.

11. A method for producing a porous material as claimed in claim 1 , wherein the matrix building material is contained within the aqueous phase of the emulsion.

12. A method for producing a porous material as claimed in claim 1 , wherein the constituents of the emulsion are in the following quantities: the matrix building material is in the range of 5-20% w/v and the surfactant is in the range of 5-20% w/v in respect of H 2 O and the CO 2 is in the range of 65-95% v/v.

13. A method for producing a porous material as claimed in claim 1 , wherein the porous material is produced in the form of a monolithic block.

14. A method for producing a porous material as claimed in claim 1 , wherein the porous material is produced in the form of porous particles or beads.

15. A method for producing a porous material as claimed in claim 1 , wherein the emulsion further comprises an active ingredient for incorporation into the porous material.

16. A method for producing a porous material as claimed in claim 15 , wherein the active ingredient is selected from one or more from the following group; pharmaceutical actives, pharmaceutical salts, enzymes, dyes, oxidising agents, reducing agents, cleaning agents, reagents for organic synthesis, agrochemicals, fabric softeners, clothes care agents, bleaches, flavours, fragrances, vitamins or nutraceuticals, metal nanoparticles (e.g., metal hydrosols), inorganic nanoparticles, biological polymers (e.g., DNA, RNA), growth factors/cofactors, and live cells (e.g., stem cells).

17. A water-soluble porous material obtained by the method according to claim 1 , wherein the material is characterised by having

(a) a median pore diameter within the range of 5-100 microns;

(b) a total pore volume in the range of 8-15 cm 3 /g when approximately 80% v/v CO 2 is used; and

(c) a bulk density typically in the range 0.02-0.06 g/cm 3 , and being able to substantially fully dissolve in water at 20° C.

18. A water-soluble porous material according to claim 17 , characterised by having substantially no solvent residue remaining in the material that arises from the internal template phase.

19. A water-soluble porous material according to claim 17 , being produced in the form of a moulded, monolithic block that substantially conforms to the shape of a vessel in which it is produced.

20. A water-soluble porous material comprising a water-soluble polymer matrix, wherein the water-soluble porous material is produced according to the method of claim 1 , and wherein said matrix comprises substantially no residual organic solvent.

21. A water-soluble porous material according to claim 20 obtainable by a method which utilises substantially no organic solvent, hence the matrix being substantially free from any residual organic solvent component.

22. A water-soluble porous material according to claim 20 comprising surfactant moieties entangled with the polymeric matrix.

23. A water-soluble porous material according to claim 22 , wherein the presence of surfactant moieties results from the formation of the porous material from a C/W emulsion comprising the surfactant moieties.

24. A water-soluble porous material as claimed in claim 20 , wherein the material is used for one or more of the following applications: biomaterials, food materials, DNA storage, controlled release matrices, agrochemical release, reagent release (e.g., for chemical reactions), molecular separations and diagnostic reagent release.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 22, 2011
From: CONOPCO, INC. D/B/A UNILEVER
To: IOTA NANOSOLUTIONS LIMITED
Reel/Frame 026485/0862 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 2, 2011
From: CONOPCO, INC. D/B/A UNILEVER
To: IOTA NANOSOLUTIONS LIMITED
Reel/Frame 025886/0872 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 24, 2007
From: BUTLER, RACHEL; COOPER, ANDREW IAN
To: CONOPCO, INC. D/B/A UNILEVER
Reel/Frame 019342/0771 →