Storage and stabilization of acetylene

Patent metadata

Field	Value
Publication number	US-9630895-B2
Application number	US-201314390784-A
Country	US
Kind code	B2
Filing date	Apr 13, 2013
Priority date	Apr 13, 2012
Publication date	Apr 25, 2017
Grant date	Apr 25, 2017

Abstract

A carbon adsorbent adapted for adsorptive storage and subsequent desorptive release of a decomposition-susceptible gas is described. Such carbon adsorbent comprises porosity in which mesopore volume is less than 0.25 cm 3 /gm of carbon adsorbent, in which the porosity comprises at least 80% by volume micropores, and at least 65% by volume of the micropores have pore diameter in a range of from 0.3 to 0.72 nm. The carbon adsorbent has a nitrogen adsorption BET surface area greater than 800 m 2 /g of carbon adsorbent, measured at 77° K, and a bulk density that is greater than 0.55 g/cc of carbon adsorbent. The carbon adsorbent can be utilized in gas storage and dispensing packages of varying type, to provide a safe and reliable source of decomposition-susceptible gas, e.g., acetylene for applications such as gas welding/cutting applications, atomic absorption spectroscopy applications, chemical synthesis and microelectronic products manufacturing.

First claim

What is claimed is:

1. A carbon adsorbent adapted for adsorptive storage and subsequent desorptive release of decomposition-susceptible gas, said carbon adsorbent comprising porosity in which mesopore volume is less than 0.25 cm 3 /gm of carbon adsorbent, in which said porosity comprises at least 80% by volume micropores, and at least 65% by volume of said micropores have pore diameter in a range of from 0.3 to 0.72 nm, wherein said carbon adsorbent has a nitrogen adsorption BET surface area greater than 800 m 2 /g of carbon adsorbent, as measured at 77° K, and a bulk density that is greater than 0.55 g/cc of carbon adsorbent.

2. The carbon adsorbent of claim 1 , comprising a pyrolyzate of polyvinylidene chloride.

3. The carbon adsorbent of claim 1 , having a fill density measured for acetylene gas at 25° C. and pressure of 650 Torr (86.7 kPa), of greater than 100 g acetylene/liter of carbon adsorbent.

4. The carbon adsorbent of claim 1 , having decomposition-susceptible gas adsorbed thereon.

5. The carbon adsorbent of claim 4 , wherein said decomposition-susceptible gas comprises gas selected from the group consisting of: formaldehyde; acetylene compounds of the formula R 1 —C≡C—R 2 in which each of R 1 and R 2 is independently selected from H, C 1 -C 12 alkyl, C 6 -C 10 aryl, C 6 -C 12 cycloalkyl, amino, alkylamino, dialkylamino, alkylaryl wherein alkyl is C 1 -C 12 alkyl and aryl is C 6 -C 10 aryl, arylalkyl wherein alkyl is C 1 -C 12 alkyl and aryl is C 6 -C 10 aryl, silyl, and R 3 Si— wherein each R 3 is independently selected from H and C 1 -C 12 alkyl; other non-saturated straight chain hydrocarbons; methylene; ethylene; diborane; boranes; germane; fluorogermanes; carboranes; alanes; aluminium hydrides; silane; chlorosilanes; digallane; chlorogallanes; and stannane.

6. The carbon adsorbent of claim 4 , wherein said decomposition-susceptible gas comprises acetylene.

7. The carbon adsorbent of claim 1 , which has been treated by a treatment that is effective to passivate or deactivate adsorbent surface thereof so that interaction of decomposition-susceptible gas with said surface is restricted to physical adsorption without chemical reaction.

8. The carbon adsorbent of claim 7 , wherein said treatment is selected from the group consisting of:
(i) chemical treatment to remove Lewis acid sites of the adsorbent;
(ii) surface neutralization treatment;
(iii) a process comprising: (a) cyclically purging the carbon adsorbent with an inert gas; (b) heating the carbon adsorbent under vacuum to elevated temperature; (c) subsequently cyclically purging the carbon adsorbent with an inert gas; (d) contacting the carbon adsorbent with a low concentration of an intended storage gas at elevated temperature; (e) removing the storage gas; and (f) cooling the carbon adsorbent under vacuum to ambient temperature; and
(iv) a process comprising: (a) cyclically purging the carbon adsorbent with an inert gas; (b) heating the carbon adsorbent under vacuum to elevated temperature; (c) cooling the carbon adsorbent under vacuum to ambient temperature; (d) gradually contacting the carbon adsorbent with a low concentration of an intended storage gas; (e) warming the vessel containing the gas to a temperature in a range of from 35° C. to 180° C.; (f) allowing the vessel pressure to stabilize; (g) evacuating and cycle purging the carbon adsorbent; and (h) cooling the carbon adsorbent under vacuum to ambient temperature.

9. A decomposition-susceptible gas storage and dispensing package, comprising a gas storage and dispensing vessel comprising an interior volume, and carbon adsorbent of claim 1 disposed in said interior volume.

10. The decomposition-susceptible gas storage and dispensing package of claim 9 , further comprising a deflagration suppression component or assembly that is configured to suppress deflagration of decomposition-susceptible gas deriving from the gas storage and dispensing vessel.

11. The decomposition-susceptible gas storage and dispensing package of claim 9 , as integrated with a transport vehicle.

12. The decomposition-susceptible gas storage and dispensing package of claim 9 , wherein the gas storage and dispensing vessel comprises a tube trailer vessel.

13. The decomposition-susceptible gas storage and dispensing package of claim 9 , comprising decomposition-susceptible gas adsorbed on said carbon adsorbent, wherein said decomposition-susceptible gas comprises gas selected from the group consisting of: formaldehyde; acetylene compounds of the formula R 1 —C≡C—R 2 in which each of R 1 and R 2 is independently selected from H, C 1 -C 12 alkyl, C 6 -C 10 aryl, C 6 -C 12 cycloalkyl, amino, alkylamino, dialkylamino, alkylaryl wherein alkyl is C 1 -C 12 alkyl and aryl is C 6 -C 10 aryl, arylalkyl wherein alkyl is C 1 -C 12 alkyl and aryl is C 6 -C 10 aryl, silyl, and R 3 Si— wherein each R 3 is independently selected from H and C 1 -C 12 alkyl; other non-saturated straight chain hydrocarbons; methylene; ethylene; diborane; boranes; germane; fluorogermanes; carboranes; alanes; aluminium hydrides; silane; chlorosilanes; digallane; chlorogallanes; and stannane.

14. The decomposition-susceptible gas storage and dispensing package of claim 13 , wherein said decomposition-susceptible gas comprises acetylene.

15. The decomposition-susceptible gas storage and dispensing package of claim 9 , wherein the carbon adsorbent has been treated by a treatment that is effective to passivate or deactivate adsorbent surface thereof so that interaction of decomposition-susceptible gas with said surface is restricted to physical adsorption without chemical reaction.

16. The decomposition-susceptible gas storage and dispensing package of claim 15 , wherein said treatment is selected from the group consisting of:
(i) chemical treatment to remove Lewis acid sites of the adsorbent;
(ii) surface neutralization treatment;
(iii) a process comprising: (a) cyclically purging the carbon adsorbent with an inert gas; (b) heating the carbon adsorbent under vacuum to elevated temperature; (c) subsequently cyclically purging the carbon adsorbent with an inert gas; (d) contacting the carbon adsorbent with a low concentration of an intended storage gas at elevated temperature; (e) removing the storage gas; and (f) cooling the carbon adsorbent under vacuum to ambient temperature; and
(iv) a process comprising: (a) cyclically purging the carbon adsorbent with an inert gas; (b) heating the carbon adsorbent under vacuum to elevated temperature; (c) cooling the carbon adsorbent under vacuum to ambient temperature; (d) gradually contacting the carbon adsorbent with a low concentration of an intended storage gas; (e) warming the vessel containing the gas to a temperature in a range of from 35° C. to 180° C.; (f) allowing the vessel pressure to stabilize; (g) evacuating and cycle purging the carbon adsorbent; and (h) cooling the carbon adsorbent under vacuum to ambient temperature.

17. The decomposition-susceptible gas storage and dispensing package of claim 9 , coupled in dispensing relationship to a process tool adapted for utilizing said decomposition-susceptible gas.

18. A method of packaging decomposition-susceptible gas for use in supplying same at a point of use, said method comprising adsorbing the decomposition-susceptible gas on a carbon adsorbent according to claim 1 , to enable the decomposition-susceptible gas to be provided in absorbed form on said carbon adsorbent at the point of use, for desorption at said point of use, wherein said decomposition-susceptible gas comprises acetyle

Assignees

• Advanced Tech Materials
• Entegris Inc

Inventors

• Sturm Edward A
• Baum Thomas H
• Carruthers J Donald

Classifications

• B01D2259/4525

  for storage and dispensing systems · CPC title

• B01D53/02

  by adsorption, e.g. preparative gas chromatography {(solid sorbent compositions B01J20/00, preparation of inorganic compounds or elements C01)} · CPC title

• C07C11/24

  Acetylene (production of acetylene gas by wet methods C10H) · CPC title

• B01J20/28011

  Other properties, e.g. density, crush strength · CPC title

• B01J20/28057

  Surface area, e.g. B.E.T specific surface area · CPC title