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1. (WO2019028519) PROCÉDÉ DE FORMATION D'UN ADSORBANT DE DIOXYDE DE CARBONE POUR UN APPAREIL DE RESPIRATION À CIRCUIT FERMÉ OU UN AUTRE APPAREIL RESPIRATOIRE
Note: Texte fondé sur des processus automatiques de reconnaissance optique de caractères. Seule la version PDF a une valeur juridique

CLAIMS

1 . A method of forming a carbon dioxide adsorbent of a rebreather apparatus for removing carbon dioxide from an individual user's breathing gas, the method comprising:

preparing a SIFSIX-3-Ni paste comprising a mixture of SIFSIX-3-Ni material and a solvent, the SIFSIX-3-Ni material substantially comprising 2-dimensional SIFSIX-3-Ni structure;

forming the SIFSIX-3-Ni paste into a shaped body having at least one mean dimension of greater than 0.5 mm; and

heat treating the shaped body in a reduced pressure environment comprising a pressure of less than 500 mbar at a temperature of at most 160 °C to substantially remove the solvent from the shaped body and form 3-dimensional SIFSIX-3-Ni crystal structure in the shaped body,

thereby producing a shaped adsorbent body for use in a rebreather apparatus.

2. A method according to claim 1 , wherein at least 60%, preferably at least 70%, more preferably at least 90%, yet more preferably at least 95%, yet even more preferably at least 99% of the 2-dimensional SIFSIX-3-Ni structure of the shaped body is transformed into 3-dimensional SIFSIX-3-Ni crystal structure in the heat treatment step.

3. A method according to claim 1 or 2, wherein the heat treatment step is conducted at a pressure of less than 100 mbar, preferably less than 50 mbar, more preferably less than 35 mbar.

4. A method according to any preceding claim, wherein the heat treatment step is conducted at a temperature of between 1 10 to 160 °C.

5. A method according to any preceding claim, wherein the heat treatment step is conducted for at least 5 hours, preferably at least 8 hours, more preferably at least 10 hours.

6. A method according to any preceding claim, wherein the heat treatment step comprises an initial heating step of:

heat treating the shaped body at least 80 °C, preferably about 80 °C at a pressure of less than 500 mbar, preferably less than 100 mbar for at least 12 hours, preferably at least 24 hours.

7. A method according to any preceding claim, wherein the heat treatment step comprises a temperature regime of:

a first heating step in which the temperature is kept from 140 °C to 160 °C, preferably 150 °C for less than 5 hours, preferably 2 to 5 hours; and

a second heating step in which the temperature is lowered to at most 130 °C for at least 5 hours, preferably at least 10 hours, more preferably at least 12 hours, and yet more preferably from 8 to 12 hours.

8. A method according to any preceding claim, wherein the inactivated SIFSIX-3-Ni material is synthesised from a mixture of a SiF6 precursor compound, a Ni precursor compound and pyrazine, in which the SiF6 precursor compound is selected from a salt of SiF6 and the Ni precursor compound is selected from at least one of a salt comprising Ni2+Ni(NO3)2.

9. A method according to any preceding claim, wherein forming the SIFSIX-3-Ni paste into a shaped body comprises at least one of extruding, palletising or moulding the SIFSIX-3-Ni paste into a desired 3-dimensional configuration.

10. A method according to any preceding claim, wherein the shaped body has at least one mean dimension of greater than 0.8 mm, preferably at least 1 mm, preferably at least 1 .2 mm, and yet more preferably at least 1 .5 mm.

1 1 . A method according to any preceding claim, wherein each of the mean width, mean depth and mean height of the shaped body are greater than 0.5 mm, and preferably greater than 1 mm.

12. A method according to any preceding claim, wherein in the forming step, the SIFSIX-3-Ni paste is extruded into an elongate body which is subsequently longitudinally divided.

13. A method according to any preceding claim, wherein the shaped body comprises an elongate body having a circular, or regular polygonal cross-sectional shape.

14. A method according to any preceding claim, wherein the solvent comprises a non-basic polar solvent or a non-self ionising polar solvent, preferably an alcohol.

15. A method according to any preceding claim, further comprising the step of:

drying the shaped body at a temperature of at least 20 °C for at least 1 hour prior to the heat treatment step.

16. A method according to any preceding claim, wherein the heat treatment step is conducted in a fluid tight housing, and the method further comprises the step of:

flushing an inert gas through the fluid tight housing.

17. A method according to any preceding claim, wherein after the heat treatment step further comprising the step of:

cooling the shaped body to at most 80 °C, preferably at most 60 °C under reduced pressure of at most 500 mbar, preferably at most 100 mbar.

18. A method according to any preceding claim, further comprising:

adsorbing carbon dioxide onto the surfaces of the SIFSIX-3-Ni shaped body; and

heating at a temperature of at least 80 °C, preferably 120 °C for at least 1 hour, preferably at least 2 hours at less than 100 mbar, preferably less than 50 mbar, thereby desorbing the carbon dioxide from the surfaces of the SIFSIX-3-Ni shaped body to produce a regenerated SIFSIX-3-Ni shaped body.

19. A method according to claim 18, wherein the heating step is conducted under inert gas flushing.

20. A method of forming a carbon dioxide filter of a rebreather apparatus for removing carbon dioxide from an individual user's breathing gas, the rebreathing apparatus, the method comprising:

producing a plurality of shaped adsorbent bodies according to any one of the preceding claims;

sealing a plurality of said shaped adsorbent bodies into a housing under an inert gas atmosphere.

21 . A method according to claim 20, wherein the inert gas atmosphere comprises at least one of nitrogen, or a Noble gas, preferably helium or argon.

22. A method according to claim 20 or 21 , wherein the housing includes two spaced apart support membranes configured to allow gas flow therethrough each membrane, the plurality of said shaped adsorbent bodies forming a packed bed therebetween and being compressed therebetween.

23. A method according to claim 22, wherein the housing includes an inner container housing the support membranes and packed bed, the inner container being seated within the housing using a fitted insert which at least friction fits the inner container within the inner walls of the housing.

24. A method according to claim 23, wherein the inner container is removably fitted within the housing.

25. A rebreathing apparatus for removing carbon dioxide from an individual user's breathing gas, the rebreathing apparatus including a carbon dioxide filter comprising:

a housing containing therein a packed bed of shaped adsorbent bodies,; wherein the shaped adsorbent bodies comprise SIFSIX-3-Ni having at least 60% 3-dimensional SIFSIX-3-Ni crystal structure, the balance being 2-dimensional SIFSIX-3-Ni structure, the shaped adsorbent bodies having at least one mean dimension of greater than 0.5 mm.

26. A rebreathing apparatus according to claim 25, wherein the housing includes an outlet that, in use, has a gas flow having about 0% CO2 gas stream for at least 1 hour.

27. A rebreathing apparatus according to claim 25 or 26, wherein at least 70%, preferably at least 90%, more preferably at least 95%, yet more preferably at least 99% the shaped adsorbent bodies comprises the 3-dimensional SIFSIX-3-Ni crystal structure.

28. A rebreathing apparatus according to any one of claims 25 to 27, wherein the adsorbent bodies are sealed within the housing in an inert gas atmosphere prior to use.

29. A rebreathing apparatus according to any one of claims 25 to 28, wherein the housing includes two spaced apart support membranes configured to allow gas flow therethrough each membrane, the plurality of said shaped adsorbent bodies forming a packed bed therebetween and being compressed therebetween.

30. A rebreathing apparatus according to claim 29, wherein the housing includes an inner container housing the support membranes and packed bed, the inner container being seated within the housing using a fitted insert which at least friction fits the inner container within the inner walls of the housing.

31 . A rebreathing apparatus according to claim 30, wherein the inner container is removably fitted within the housing.

32. A rebreathing apparatus according to claim 29, 30, or 31 , further including:

a first liquid free gas flow space that is in fluid communication with an inlet for the user's exhaled breathing gas, said exhaled breathing gas including carbon dioxide;

a second liquid free gas flow space that is in fluid communication with an outlet for fluid flow of gas that is substantially free of carbon dioxide;

wherein the first liquid free gas flow space is in fluid communication with the second liquid free gas flow space through the packed bed such that, in use, an exhaled gas stream can flow through the packed bed to facilitate adsorption of carbon dioxide from the user's exhaled breathing gas onto the adsorbent bodies.

33. A rebreathing apparatus according to any one of claims 25 to 32, wherein the shaped adsorbent bodies comprises elongate bodies having a circular, or regular polygonal cross-sectional shape.

34. A rebreathing apparatus according to any one of claims 25 to 33, wherein, the adsorbent bodies are configured to adsorb carbon dioxide from an individual user's exhaled gas, and be regenerated to a substantially carbon dioxide free state in situ, within the filter, by heat treatment.

35. A rebreathing apparatus according to claim 34, wherein heat treatment comprises heating the shaped adsorbent bodies at a temperature of at least 80 °C for at least 1 hour.

36. A rebreathing apparatus according to any one of claims 25 to 35, further including at least one breathing apparatus, a breathing mask, a breathing suit or other life support system in fluid connection to the carbon dioxide filter.