IP Library Granted Patent US 8,465,833
Granted Patent B2
US 8,465,833 · App. 13/383,516 · Granted Jun 18, 2013

Ferrocene/carbon dioxide releasing system

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Quick Facts
Patent No.
US 8,465,833
App. No.
13/383,516
Granted
Jun 18, 2013
Kind
B2
Abstract

Microparticles that encapsulate a fire extinguishing agent or combination of fire extinguishing agents, methods for preparing these microcapsules, methods for using such microcapsules, and articles of manufacture including at least one of such microparticles either in a coating or in a matrix that makes up a structural component of the article of manufacture are disclosed.

Claims (64)

1. A microcapsule comprising:

an inorganic shell encapsulating a flame extinguishing mixture comprising:

at least one iron-containing compound; and

at least one source of an inert gas.

2. The microcapsule of claim 1 , wherein the inorganic shell has a diameter of about 5 μm to about 5000 μm.

3. The microcapsule of claim 1 , wherein the inorganic shell has a wall thickness of about 0.10 μm to about 100 μm.

4. The microcapsule of claim 1 , wherein the inorganic shell comprises glass, ceramic, glass-ceramic, alumina, zirconia, yttria, silica alumina, mullite, sillimanite, porcelain, polycrystalline materials, vitreous silica, vitreous germania, vitreous boric oxide, titanium silicate, aluminosilicate, alkali silicate, alkaline earth silicate, alkaline earth germinate, alkali borate, borosilicate, alkali aluminosilicate, alkali galliosilicate, soda-lime silicate, alkali borosilicate, phosphate, lithium aluminosilicate, lithium silicate, lithium metasilicate, lithium disilicate, zinc silicate, or combination thereof.

5. The microcapsule of claim 1 , wherein the inorganic shell is a sol gel material.

6. The microcapsule of claim 1 , wherein the at least one iron-containing compound comprises iron pentacarbonyl, iron hexacarbonyl, iron acetylacetonate, ferrocene, ferrocene derivatives, fixed ferrocene, fixed ferrocene derivative, or combination thereof.

7. The microcapsule of claim 1 , wherein the at least one iron-containing compound comprises a ferrocene of formula I:

wherein each of R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 , and R 10 are independently selected from H, alkyl, cycloalkyl, aryl, heteroaryl, heterocycle, —COOH, PR 11 2 , and NR 11 2 , wherein each R 11 is independently selected from H, alkyl, cycloalkyl, aryl, heteroaryl, heterocycle, and —COOH.

8. The microcapsule of claim 1 , wherein the at least one source of inert gas comprises an intumescent compound.

9. The microcapsule of claim 1 , wherein the at least one source of inert gas comprises carbonate, hydroxide, water vapor, carbon dioxide, nitrogen, MgCO 3 , CaCO 3 , NaOH, KOH, Mg(OH) 2 , Ca(OH) 2 , or combination thereof or a fuel and an oxidizer.

10. The microcapsule of claim 9 , wherein the fuel comprises 5-aminotetrazole or a salt thereof, bitetrazole or salts thereof, diazoaminotetrazole or salts thereof, diazotetrazole dimer or salts thereof, guanidine nitrate, aminoguanidine nitrates, nitroguanidine, 5-nitro-1,2,4-triazol-3-one, triaminoguanidinium, diaminoguanidinium, or combination thereof, and oxidizer comprises an alkali metal nitrate, alkaline earth nitrate, phase stabilized ammonium nitrate, perchlorate, iodate, bromate, or combination thereof.

11. The microcapsule of claim 1 , wherein the microcapsule has a core-shell structure or a core-shell-shell structure.

12. A fire resistant material comprising:

at least one substrate; and

at least one microcapsule comprising an inorganic shell encapsulating a flame extinguishing mixture comprising:

at least one iron containing compound; and

at least one source of an inert gas.

13. The fire resistant material of claim 12 , wherein the inorganic shell has a diameter of about 5 μm to about 5000 μm.

14. The fire resistant material of claim 12 , wherein the inorganic shell has a wall thickness of about 0.10 μm to about 100 μm.

15. The fire resistant material of claim 12 , wherein the inorganic shell comprises glass, ceramic, glass-ceramic, alumina, zirconia, yttria, silica alumina, mullite, sillimanite, porcelain, polycrystalline materials, vitreous silica, vitreous germania, vitreous boric oxide, titanium silicate, aluminosilicate, alkali silicate, alkaline earth silicate, alkaline earth germinate, alkali borate, borosilicate, alkali aluminosilicate, alkali galliosilicate, soda-lime silicate, alkali borosilicate, phosphate, lithium aluminosilicate, lithium silicate, lithium metasilicate, lithium disilicate, zinc silicate, or combination thereof.

16. The fire resistant material of claim 12 , wherein the inorganic shell is a sol gel material.

17. The fire resistant material of claim 12 , wherein the at least one iron-containing compound comprises iron pentacarbonyl, iron hexacarbonyl, iron acetylacetonate, ferrocene, ferrocene derivatives, fixed ferrocene, fixed ferrocene derivative, or combination thereof.

18. The fire resistant material of claim 12 , wherein the at least one iron-containing compound comprises a ferrocene of formula I:

wherein each of R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 , and R 10 are independently selected from H, alkyl, cycloalkyl, aryl, heteroaryl, heterocycle, —COOH, PR 11 2 , and NR 11 2 , wherein each R 11 is independently selected from H, alkyl, cycloalkyl, aryl, heteroaryl, heterocycle, and —COOH.

19. The fire resistant material of claim 12 , wherein the at least one source of inert gas comprises an intumescent compound.

20. The fire resistant material of claim 12 , wherein the at least one source of inert gas comprises carbonate, hydroxide, water vapor, carbon dioxide, nitrogen, MgCO 3 , CaCO 3 , NaOH, KOH, Mg(OH) 2 , Ca(OH) 2 , or combination thereof or a fuel and an oxidizer.

21. The fire resistant material of claim 20 , wherein the fuel comprises 5-aminotetrazole or a salt thereof, bitetrazole or salts thereof, diazoaminotetrazole or salts thereof, diazotetrazole dimer or salts thereof, guanidine nitrate, aminoguanidine nitrates, nitroguanidine, 5-nitro-1,2,4-triazol-3-one, triaminoguanidinium, diaminoguanidinium, or combination thereof, and oxidizer comprises an alkali metal nitrate, alkaline earth nitrate, phase stabilized ammonium nitrate, perchlorate, iodate, bromate, or combination thereof.

22. The microcapsule of claim 1 , wherein the microcapsule has a core-shell structure or a core-shell-shell structure.

23. The fire resistant material of claim 12 , wherein the substrate comprises polymers, putties, mastics, and paints, coatings, or shaped articles.

24. The fire resistance material of claim 12 , wherein the substrate comprises metal, wood, fabric, concrete, particle board, a polymer material, or combination thereof and the substrate is coated with a matrix material comprising at least one microcapsule.

25. The fire resistant material of claim 12 , wherein the substrate is an article of manufacture comprising at least one microcapsule.

26. The fire resistant material of claim 25 , wherein the at least one microcapsule is provided in a coating comprising a polymer, putty, mastic, or paint.

27. The fire resistant material of claim 25 , wherein the article of manufacture comprises a polyolefin, polyurea, polyurethane, polyester, polyamide, or combination thereof.

28. The fire resistant material of claim 25 , wherein the article of manufacture comprises a floor surface, textile fabric, floor covering, pillow, stretcher pad, seat covering, adhesive tape, garment, wipe, swab, pen, furniture, conveyor means, delivery truck, delivery cart, tool, packaging, container, machine casing, machine cover, electronic component carrier, wafer boat, wafer jar, battery, antenna, transistor, printer component, fuel pump, fuel pump handle, hose, hose covering, fuel pump wand, fuel pump nozzle, fuel piping component, vehicle seat upholstery, exterior vehicle paneling, interior vehicle paneling, vehicle console component, gasket, seal, o-ring, diaphragm, gear, valve, bushing, bumper, grommet, stopper, bellows, plug, vibration mount, veering, weather stripping, roller, tubing connector, computer casing, circuit board, through-hole plating of a circuit board, microprocessor, random access memory component, read only memory component, disc drive, electrode, or lithographic resist.

29. A method for preparing a microcapsule, the method comprising:

providing at least one iron containing compound;

providing at least one source of an inert gas;

providing at least one inorganic shell precursor;

combining the at least one iron containing compound, the at least one source of inert gas, and at least one inorganic shell precursor in an aqueous solution to form a suspension;

stirring the suspension;

maintaining a temperature and pH operable to precipitate the at least one inorganic shell precursor; and

isolating the microcapsules from the suspension.

30. The method of claim 29 , further comprising:

providing a template agent selected from the group consisting of a long-chain alkyl quaternary ammonium salts, surfactants, and combination thereof; and

combining the template agent with the at least one iron containing compound, the at least one source of inert gas, and at least one inorganic shell precursor in an aqueous solution to form a suspension.

31. The method of claim 29 , wherein the temperature is about 10° C. to about 200° C.

32. The method of claim 29 , wherein the pH is about 5 to about 12.

33. The method of claim 29 , wherein the at least one iron-containing compound iron pentacarbonyl, iron hexacarbonyl, iron acetylacetonate, ferrocene, ferrocene derivatives, fixed ferrocene, fixed ferrocene derivative, or combination thereof.

34. The method of claim 29 , wherein the at least one source of inert gas comprises carbonate, hydroxide, water vapor, carbon dioxide, nitrogen, MgCO 3 , CaCO 3 , NaOH, KOH, Mg(OH) 2 , Ca(OH) 2 , or combination thereof or a fuel and an oxidizer.

35. The method of claim 29 , wherein the inorganic shell comprises glass, ceramic, glass-ceramic, alumina, zirconia, yttria, silica alumina, mullite, sillimanite, porcelain, polycrystalline materials, yitreous silica, vitreous germania, vitreous boric oxide, titanium silicate, aluminosilicate, alkali silicate, alkaline earth silicate, alkaline earth germinate, alkali borate, borosilicate, alkali aluminosilicate, alkali galliosilicate, soda-lime silicate, alkali borosilicate, phosphate, lithium aluminosilicate, lithium silicate, lithium metasilicate, lithium disilicate, zinc silicate, or combination thereof.

36. A method for preparing fire resistant material, the method comprising:

providing a substrate;

providing at least one microcapsule comprising an inorganic shell encapsulating a flame extinguishing mixture comprising:

at least one iron containing compound; and

at least one source of an inert gas; and

combining the at least one substrate and the at least one microcapsule to form a fire resistant material.

37. The method of claim 36 , wherein the inorganic shell comprises glass, ceramic, glass-ceramic, alumina, zirconia, yttria, silica alumina, mullite, sillimanite, porcelain, polycrystalline materials, vitreous silica, vitreous germania, vitreous boric oxide, titanium silicate, aluminosilicate, alkali silicate, alkaline earth silicate, alkaline earth germinate, alkali borate, borosilicate, alkali aluminosilicate, alkali galliosilicate, soda-lime silicate, alkali borosilicate, phosphate, lithium aluminosilicate, lithium silicate, lithium metasilicate, lithium disilicate, zinc silicate, or combination thereof.

38. The method of claim 36 , wherein the substrate comprises a polymer, putty, mastic, or paint.

39. The method of claim 36 , wherein the at least one iron-containing compound comprises iron pentacarbonyl, iron hexacarbonyl, iron acetylacetonate, ferrocene, ferrocene derivatives, fixed ferrocene, fixed ferrocene derivatives, or combination thereof.

40. The method of claim 36 , wherein the at least one source of inert gas comprises carbonate, hydroxide, water vapor, carbon dioxide, nitrogen, MgCO 3 , CaCO 3 , NaOH, KOH, Mg(OH) 2 , Ca(OH) 2 , or combination thereof or a fuel and an oxidizer.

41. The method of claim 36 , wherein combining further comprises at least one of stirring, mixing, melt mixing, shaking, or combination thereof.

Assignments (1)
SECURITY INTEREST Recorded Jan 29, 2019
From: EMPIRE TECHNOLOGY DEVELOPMENT LLC
To: CRESTLINE DIRECT FINANCE, L.P.
Reel/Frame 048373/0217 →