Organic amine impregnated activated carbon

• US 5,462,908 A
• Filed: 06/16/1993
• Issued: 10/31/1995
• Est. Priority Date: 06/16/1993
• Status: Expired due to Term

• Current Assignee: Her Majesty The Queen In Right of Canada As Represented By The Minister of National Defence
• Original Assignee: Her Majesty The Queen In Right of Canada As Represented By The Minister of National Defence
• Inventors: Harrison, Brian H., Pagotto, Jack, Liang, Septimus H.-C.
• Primary Examiner(s): Pal, Asok
• Assistant Examiner(s): PHAN, NHAT
• Application Number:
  US08/077,110
• Time in Patent Office: 867 Days
• Field of Search: 502/401, 502/416, 95/142
• US Class Current: 502/401
• CPC Class Codes: B01D 2253/102 Carbon
• CPC Class Codes: B01D 2253/25 Coated, impregnated or composite adsorbents
• CPC Class Codes: B01D 2257/2066 Fluorine
• CPC Class Codes: B01D 2259/4541 for portable use, e.g. gas masks
• CPC Class Codes: B01D 53/02 by adsorption, e.g. preparative gas chromatography solid sorbent compositions B01J20/00, preparation of inorganic compounds or elements C01
• CPC Class Codes: B01D 53/68 Halogens or halogen compounds
• CPC Class Codes: B01J 20/20 comprising free carbon; comprising carbon obtained by carbonising processes
• CPC Class Codes: Y02C 20/30 of perfluorocarbons [PFC], hydrofluorocarbons [HFC] or sulfur hexafluoride [SF6]

Abstract

A novel organic amine-impregnated activated carbon composition is disclosed which may be used in breathing gas filters to enhance removal of various toxic perfluorocarbons. Three processes for impregnating activated carbon with organic amines are also disclosed. One of these processes comprises the steps of placing the amine in contact with substantially dry activated carbon, subjecting the carbon and amine to an environment devoid of oxidizing gases or vapors (such as oxygen gas), and then heating the carbon and amine for an extended period while maintaining this oxidizer-free environment. Pretreatment procedures to enhance both the shelf-life and service-life of the amine-impregnated activated carbon are also disclosed.

Claims

1. A breathing gas filter composition providing protection against toxic perfluorocarbons, comprising substantially dry activated carbon and an organic amine impregnant, said organic amine being selected from the group consisting of substituted amines, amides and sulfonamides in an amount of 1.5 to 18% by weight, based on the weight of the carbon and additionally comprising 0.1 to 10% by weight, based on the weight of the carbon of an alkaline hydroxide.

2. A composition according to claim 1, wherein the organic amine is selected from the group consisting of aliphatic secondary and tertiary amines.

3. A process for impregnating activated carbon with a low vapour pressure organic amine, comprising the steps of placing the amine in contact with substantially dry activated carbon, subjecting the carbon and amine to positive pressure of 1-5 Pa in an oxygen-free inert gas atmosphere and then heating the carbon and amine for an extended period while maintaining the positive pressure of 1-5 Pa in an oxygen-free inert gas atmosphere, including the step of pre-treating the activated carbon with a compound selected from the group consisting of an alkaline hydroxide in an amount of 0.1 to 10% by weight, based on the weight of the carbon, a suitable halogen and a suitable halide salt.

4. A process according to claim 3, including the additional step of storing the amine-impregnated carbon in an oxidizer-free enclosure.

5. A process according to claim 3, wherein the heating step is effected at 40°

to 60°

C. for 1 to 72 hours.

6. A process according to claim 4, wherein the oxygen-free inert gas is selected from the group consisting of nitrogen, argon and helium.

7. A process according to claim 3, wherein the organic amine is included in an amount of 1.5 to 18% by weight, based on the weight of the carbon.

8. A process according to claim 7, wherein the amine is selected from the group consisting of aliphatic secondary and tertiary amines.

9. A process according to claim 8, wherein the amine is included in an amount of 4 to 7% by weight, based on the weight of the carbon.

10. A process according to claim 9, wherein the activated carbon is selected from the group consisting of carbon impregnated with copper, silver and chromium, unimpregnated base carbon, and carbon impregnated with copper, silver, chromium and triethylenediamine.

11. A process according to claim 10, wherein the activated carbon is carbon impregnated with copper, silver and chromium.

12. A process according to claim 11, wherein the amine is selected from dipropylamine and triethylamine.

13. A process according to claim 3, wherein the compound is selected from the group consisting of a suitable halogen and a suitable halide salt.

14. A process for impregnating activated carbon with a solid amine compound, comprising dissolving the amine in a solvent selected from water and organic solvents and adding the amine solution to the activated carbon, including the step of pre-treating the activated carbon with a compound selected from the group consisting of an alkaline hydroxide in an amount of 0.1 to 10% by weight, based on the weight of the carbon, a suitable halogen and a suitable halide salt.

15. A breathing gas filter composition providing protection against toxic perfluorocarbons, comprising substantially dry activated carbon and an organic amine impregnant, said organic amine being selected from the group consisting of ethylenediamine, dipropylamine, isopropylamine, aniline, N,N-diethyl-1,4-phenylenediamine, 4-phenylazoaniline, diisopropylamine, diethylamine, diethylenetriamine, diphenylamine, pyrrole, piperidine, triethylamine, triisobutylamine, tricotylamine, N,N-diethylaniline, 4-(4-nitrobenzyl)-pyridine, hexamethyleneamine, monoethanolamine, urea, N,N-dimethylformamide, o-toluenesulfonamide and p-toluenesulfonamide, in an amount of 1.5 to 18 percent by weight, based on the weight of the carbon and additionally comprising 0.1 to 10% by weight, based on the weight of the carbon of an alkaline hydroxide.

16. A composition according to claim 15, additionally comprising 0.1 to 10% by weight, based on the weight of the carbon of an alkaline hydroxide.

17. A composition according to claim 15, wherein the amine is selected from the group consisting of dipropylamine, diisopropylamine, pyrrole, piperidine, triethylamine, triisobutylamine and tricotylamine.

18. A composition according to claim 17, wherein the organic amine is included in an amount of 4 to 7% by weight, based on the weight of the carbon.

19. A composition according to claim 17, wherein the amine is triethylamine.

20. A composition according to claim 17, which the amine is dipropylamine.

21. A composition according to claim 17, claim the amine is piperidine.