Chemical heat source comprising metal nitride, metal oxide and carbon

• US 5,188,130 A
• Filed: 11/29/1989
• Issued: 02/23/1993
• Est. Priority Date: 11/29/1989
• Status: Expired due to Term

• Current Assignee: Philip Morris Incorporated (Altria Group, Inc.), Philip Morris Products Inc (Philip Morris Limited)
• Original Assignee: Philip Morris Incorporated (Altria Group, Inc.)
• Inventors: Watkins, Michael L., Ariprala, Sarojini D., Hajaligol, Mohammad R., Deevi, Seetharama C., Losee, Donald B., Waymack, Bruce E.
• Primary Examiner(s): Millin, V.
• Assistant Examiner(s): BAHR, JENNIFER DOYLE
• Application Number:
  US07/443,636
• Time in Patent Office: 1,182 Days
• Field of Search: 131/359, 131/364, 252/636, 252/640
• US Class Current: 131/359
• CPC Class Codes: A24B 15/165 comprising as heat source a carbon fuel or an oxidized or thermally degraded carbonaceous fuel, e.g. carbohydrates, cellulosic material
• CPC Class Codes: C09K 5/16 Materials undergoing chemical reactions when used

Abstract

A chemical heat source comprising metal nitride, metal oxide and carbon, particularly useful in smoking articles, and methods of making the heat source are provided. The metal nitride of the heat source has an ignition temperature substantially lower than conventional carbonaceous heat sources, while at the same time provides sufficient heat to release a flavored aerosol from a flavor bed for inhalation by the smoker. Upon combustion the heat source produces virtually no carbon monoxide. The metal nitride is prepared by pre-forming the starting materials into a desired shape, and converting them to metal nitride in situ, without substantially altering the shape of the starting materials.

Claims

1. A method of making metal nitride, comprising the steps of:

a) mixing a metal species and a carbon source to form a mixture;

b) supplying heat to the mixture; and

c) contacting the mixture with a nitriding material to form metal nitride.

3. The method of claim 1 or 2, wherein the metal species is an iron species.

4. The method of claim 3, wherein the iron species is selected from the group consisting of Fe₂ O₃, FeOOH, Fe₃ O₄ O, FeO, or Fe⁰.

5. The method of claim 1 or 2, wherein the carbon source is selected from the group consisting of colloidal graphite and activated carbon.

6. The method of claim 1 or 2, wherein the heat is supplied in an environment that will allow the reduction of the metal species.

7. The method of claim 6, wherein the environment comprises an inert gas selected from the group helium, argon, nitrogen, or mixtures thereof.

8. The method of claim 7, wherein carbon monoxide and carbon dioxide are added to the environment at a ratio of between about 0.16 and about 6.

9. The method of claim 7, wherein carbon monoxide and carbon dioxide are added to the environment at a ratio of between about 0.3 and about 2.5.

10. The method of claim 1 or 2, wherein the nitriding material is a nitrogenous gas.

11. The method of claim 10, wherein the nitrogenous gas is ammonia.

14. The method of claim 1 or 2, wherein the heat is supplied to the mixture in a plurality of intervals.

15. The method of claim 1 or 2, wherein the heat is supplied to this mixture at a constant rate of increase.

16. The method of claim 14, wherein the heat is supplied to the mixture within the interval at a constant rate of increase.

17. The method of claim 15, wherein the rate of increase is up to about 20°

C./min.

18. The method of claim 16, wherein the rate of increase is up to about 20°

C./min.

19. The method of claim 15, wherein the heat is supplied to the mixture until a temperature of between about 650°

C. and about 900°

C. is reached.

20. The method of claim 16, wherein the heat is supplied to the mixture until a temperature of between about 650°

C. and about 900°

C. is reached.

21. The method of claim 16, wherein the heat is supplied to the mixture in two intervals.

22. The method of claim 21, wherein the heat is supplied to the mixture in the first interval at a first rate of increase and in the second interval at a second rate of increase.

23. The method of claim 22, wherein the first rate of increase is between about 0.1°

C./min. and about 10°

C./min.

24. The method of claim 22, wherein heat is supplied to the mixture in the first interval until a temperature of between about 100°

C. and about 200°

C. is reached.

25. The method of claim 22, wherein the first rate of increase is between about 0.2°

C./min and about 5°

C./min and heat is supplied to the mixture in the first interval until temperature of about 125°

C. is reached.

26. The method of claim 22, wherein the second rate of increase is between about 1°

C./min. and about 20°

C./min.

27. The method of claim 22, wherein heat is supplied to the mixture in the second interval until a temperature of between about 650°

C. and about 900°

C. is reached.

28. The method of claim 22, wherein the second rate of increase is between about 5°

C./min to about 10°

C./min and heat is supplied to the mixture in the second interval until a temperature of between about 675°

C. and about 825°

C. is reached.

30. The method of claim 1 or 2, wherein the metal species and carbon source are combined in a polar solvent.

31. The method of claim 30, wherein the polar solvent is water.

32. The method of claim 1 or 2, wherein the metal species is in particulate form having a particle size of up to about 300 microns.

33. The method of claim 1 or 2, wherein the metal species is in particulate form having a particle size of between about submicron and about 20 microns.

34. The method of claim 1 or 2, wherein the metal species has a surface area of between about 0.2 m² /g and about 300 m² /g.

35. The method of claim 1 or 2, wherein the metal species has a surface area of between about 1 m² /g and about 150 m² /g.

36. The method of claim 1 or 2, wherein the carbon source is in particulate form having a particle size of up to about 300 microns.

37. The method of claim 1 or 2, wherein the carbon source is in particulate form having a particle size of between about submicron and about 40 microns.

38. The method of claim 1 or 2, wherein the carbon source has a surface area of between about 0.5 m² /g and about 2000 m² /g.

39. The method of claim 1 or 2, wherein the carbon source has a surface area of between about 100 and about 600 m² /g.

40. The method of claim 1 or 2, wherein the nitriding material is contacted with the mixture at a temperature of between about 400°

C. to about 600°

C.

41. The method of claim 1 or 2, wherein the nitriding material is contacted with the mixture for up to about 150 min.

42. The method of claim 1 or 2, wherein the nitriding material is contacted with the mixture at a temperature of between about 450°

C. and about 500°

C. for between about 30 min and about 120 min.

2. A method of making a heat source comprising metal nitride, comprising the steps of:

a) mixing a metal species and a carbon source to form a mixture;

b) combining the mixture from step a) with a binder;

c) forming the mixture from step b) into a shape;

d) supplying heat to the mixture; and

e) contacting the mixture with a nitriding material to form metal nitride.

12. The method of claim 2, wherein the binder comprises a carbonaceous material.

13. The method of claim 2, wherein the carbonaceous material comprises a mixture comprising flour, sugar, and a vegetable oil.

29. The method of claim 2, wherein in step c) the mixture is formed into a cylindrical rod.

43. A heat source comprising metal nitride, wherein the heat source is substantially in the form of a cylindrical rod and has one or more fluid passages therethrough.

44. The heat source of claim 43, wherein the cylindrical rod has a diameter of between about 3.0 mm and about 8.0 mm, and a length of between about 8 mm and about 20 mm.

45. The heat source of claim 43, wherein the cylindrical rod has a diameter of between about 4.0 mm and 5.0 mm.

46. The heat source of claim 43, wherein the cylindrical rod has a length of between about 10 mm and 14 mm.

47. The heat source of claim 43, wherein the fluid passages are formed in the shape of a multi-pointed star.

48. The heat source of claim 43, wherein the fluid passages are formed as grooves around the circumference of the cylindrical rod.

49. A heat source for use in a smoking article comprising metal nitride, low valency metal oxide and carbon.

50. The heat source of claim 49, wherein the metal nitride is iron nitride and the low valency metal oxide is FeO.

51. The heat source of claim 49, wherein the heat source has an ignition temperature of between about 175°

C. and about 450°

C.

52. The heat source of claim 49, wherein the heat source has an ignition temperature of between about 190°

C. and 400°

C.

53. The heat source of claim 49, wherein, upon combustion, the heat source reaches a maximum temperature of between about 600°

C. and about 950°

C.

54. The heat source of claim 49, wherein, upon combustion, the heat source reaches a maximum temperature of between about 650°

C. and about 850°

C.

55. A heat source comprising metal nitride, low valency metal oxide, and carbon.

56. A smoking article comprising a heat source, wherein the heat source comprises metal nitride.