Special adsorbent for carbon dioxide acquisition on mars

• US 6,294,501 B1
• Filed: 03/02/1999
• Issued: 09/25/2001
• Est. Priority Date: 03/09/1998
• Status: Expired due to Fees

• Current Assignee: Alliedsignal Inc. (Honeywell International Inc.)
• Original Assignee: Alliedsignal Inc. (Honeywell International Inc.)
• Inventors: Chang, Chin-Hsiung
• Primary Examiner(s): Hendrickson, Stuart L.
• Application Number:
  US09/261,046
• Time in Patent Office: 938 Days
• Field of Search: 502/416, 502/418, 502/423, 502/437, 423/445.R, 951/39, 264/29.7
• US Class Current: 502/418
• CPC Class Codes: B01D 2253/306 Surface area, e.g. BET-specific surface
• CPC Class Codes: B01D 2253/308 Pore size
• CPC Class Codes: B01D 2253/311 Porosity, e.g. pore volume
• CPC Class Codes: B01D 2256/12 Oxygen
• CPC Class Codes: B01D 2257/504 Carbon dioxide
• CPC Class Codes: B01D 2257/80 Water
• CPC Class Codes: B01D 2259/416 involving cryogenic temperature treatment
• 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 53/053 with storage or buffer vessel
• CPC Class Codes: B01J 20/20 comprising free carbon; comprising carbon obtained by carbonising processes
• CPC Class Codes: B01J 20/28004 Sorbent size or size distribution, e.g. particle size
• CPC Class Codes: B01J 20/28014 characterised by their form
• CPC Class Codes: B01J 20/28042 Shaped bodies; Monolithic structures
• CPC Class Codes: B01J 20/28066 being more than 1000 m2/g
• CPC Class Codes: B01J 20/28073 being in the range 0.5-1.0 ml/g
• CPC Class Codes: B01J 20/2808 being less than 2 nm, i.e. micropores or nanopores
• CPC Class Codes: B01J 20/28088 Pore-size distribution
• CPC Class Codes: B01J 20/3007 Moulding, shaping or extruding
• CPC Class Codes: B01J 20/3021 Milling, crushing or grinding
• CPC Class Codes: B01J 20/3035 Compressing
• CPC Class Codes: B01J 20/3078 : Thermal treatment, e.g. calcining or pyrolizing
• CPC Class Codes: B01J 20/3416 : of sorbents or filter aids comprising free carbon, e.g. activated carbon
• CPC Class Codes: B01J 20/3483 : by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
• CPC Class Codes: B01J 20/3491 : by pressure treatment
• CPC Class Codes: B01J 2220/56 : Use in the form of a bed
• CPC Class Codes: Y02C 20/40 : of CO2

Abstract

A carbon dioxide adsorbent comprises a carbonized, shaped precursor material, with such material being characterized by a total micropore volume of at least about 0.525 cm³/g and a median pore diameter of at least about 0.439 nm, whereby the material has a carbon dioxide capacity of at least about 28.6% g/g at a carbon dioxide partial pressure of about 6 mm Hg and a temperature of about 196° K. Also provided is a method of making a carbon dioxide adsorbent, which includes the steps of polymerizing a monomer to produce a precursor material; shaping the precursor material to produce a shaped precursor material; and carbonizing the shaped precursor material to produce the adsorbent, whereby the adsorbent is characterized by a carbon dioxide capacity of at least about 28.6% g/g at a carbon dioxide partial pressure of about 6 mm Hg and a temperature of about 196° K.

Claims

1. A carbon dioxide adsorbent, comprising:

a carbonized precursor material, such that said adsorbent is characterized by a weight that is from about 0.0063 to 0.0092 g, a total micropore volume from about 0.525 to 0.580 cm³/g and a median pore diameter from about 0.439 to 0.453 nm, and

whereby said adsorbent has a carbon dioxide capacity of at least about 28.6% g/g at a carbon dioxide partial pressure of about 6 mm Hg and a temperature of about 196°

K.

2. The adsorbent of claim 1, wherein said material is further characterized by a BET surface area of at least about 1064 m²/g.

3. The adsorbent of claim 1, wherein said material is further characterized by a Langmuir surface area of at least about 1271 m²/g.

4. A carbon dioxide adsorbent, comprising:

a carbonized, shaped precursor material characterized by an absence of a cross-linking agent, and a length to diameter ratio of about 1 in a non-carbonized state,

whereby said adsorbent is characterized by a BET surface area not greater than about 1150 m²/g, a Langmuir surface area not greater than about 1407 m²/g, a total micropore volume not greater than about 0.580 cm³/g, a median pore diameter not greater than about 0.453 nm, and a carbon dioxide capacity of at least about 28.6% g/g at a carbon dioxide partial pressure of about 6 mm Hg and a temperature of about 196°

K.

5. The adsorbent of claim 4, wherein said BET surface area is about 1150 m²/g.

6. The adsorbent of claim 4, wherein said Langmuir surface area is about 1407 m²/g.

7. The adsorbent of claim 4, wherein said total micropore volume is about 0.580 cm³/g.

8. The adsorbent of claim 4, wherein said median pore diameter is about 0.453 nm.

9. A carbon dioxide adsorbent, comprising:

a carbonized precursor material characterized by a particle size between about 4 to about 100 micrometers in a non-carbonized state,

whereby said adsorbent is characterized by a BET surface area between about 1064 to 1150 m²/g, a Langmuir surface area between about 1271 to 1407 m²/g, a total micropore volume between about 0.525 to 0.580 cm³/g, a median pore diameter between about 0.439 to 0.443 nm, and a carbon dioxide capacity of at least about 28.6% g/g at a carbon dioxide partial pressure of about 6 mm Hg and a temperature of about 196°

K.

10. The adsorbent of claim 9, wherein said material is further characterized by a total micropore volume of about 0.580 cm³/g.

11. The adsorbent of claim 9, wherein said material is further characterized by a median pore diameter of about 0.439 nm.

12. The adsorbent of claim 9, wherein said material has a carbon dioxide capacity of about 32.6% g/g at a carbon dioxide partial pressure of about 6 mm Hg.

13. The adsorbent of claim 9, wherein said material is further characterized by a BET surface area of at least about 1064 m²/g.

14. The adsorbent of claim 9, wherein said material is further characterized by a Langmuir surface area of at least about 1271 m²/g.

15. A method of making a carbon dioxide adsorbent, comprising the step of:

polymerizing a monomer to produce a precursor material in the absence of a cross-linking agent; and

heating said precursor material in a stepped fashion;

carbonizing said shaped precursor material to produce said adsorbent,

whereby said adsorbent is characterized by a weight that is from 0.0063 to 0.0092 g, a total micropore volume of at least about 0.525 cm³/g, a median pore diameter between about 0.439 to 0.443 nm, and a carbon dioxide capacity of at least about 28.6% g/g at a carbon dioxide partial pressure of about 6 mm Hg and a temperature of about 196°

K.

16. The method of claim 15, wherein the step of polymerizing comprises one of the steps of suspension polymerization and bulk polymerization.

17. The method of claim 15, wherein said monomer is characterized by being essentially free of oxygen in its molecular structure and comprised of hydrogen, a halogen and carbon.

18. The method of claim 15, wherein the step of carbonization comprises the step of heating said shaped precursor material in the presence of an inert gas.

19. A method of making a carbon dioxide adsorbent, comprising the step of:

polymerizing a monomer in the absence of a cross-linking agent to produce a precursor material characterized by a particle size between about 4 to about 100 micrometers;

shaping said precursor material to produce a shaped precursor material characterized by a length to diameter ratio of about 1;

heating said shaped precursor material in a stepped fashion,

carbonizing said shaped precursor material to produce said adsorbent,

whereby said adsorbent is characterized by a BET surface area between about 1064 to 1150 m²/g, a Langmuir surface area between about 1271 to 1407 m²/g, a total micropore volume between about 0.525 to 0.580 cm³/g, a median pore diameter between about 0.439 to 0.443 nm, and a carbon dioxide capacity of at least about 28.6% g/g at a carbon dioxide partial pressure of about 6 mm Hg and a temperature of about 196°

K.

20. The method of claim 19, wherein said monomer is selected from the group consisting of acrylonitrile, vinylidene fluoride, chlorotrifluoroethylene, vinylidene chloride, mixtures of the foregoing, vinyl fluoride, vinyl bromide, chlorinated ethylene, chlorofluorinated ethylene, vinyl-chlorobenzene, vinylidene bromide and vinylidene-flouride-chlorotrifluoroethylene.

21. The method of claim 19, wherein the step of polymerizing occurs in the presence of a cross-linking agent and said cross-linking agent is selected from the group consisting of divinyl-benzene, trivinyl benzene, divinyl acetylene, and divinyl sulfide.

22. The method of claim 19, wherein the step of carbonization comprises the step of heating said shaped precursor material at a temperature between about 25 to 860°

C.

23. The method of claim 19, wherein said adsorbent is in the form of carbon molecular sieves and said sieves are characterized by a density between about 0.935 to 1.098 g/cm³.

24. The method of claim 19, wherein said adsorbent is in the form of carbon molecular sieves and said sieves are characterized by a weight between about 0.0063 to 0.0076 g.

25. The method of claim 19, wherein said adsorbent is in the form of carbon molecular sieves and said sieves are characterized by a diameter between about 2.00 to 2.10 nm.

26. The method of claim 19, wherein said adsorbent is in the form of carbon molecular sieves and said sieves are characterized by a length between about 1.95 to 2.10 nm.