Transition metal salt impregnated carbon

• US 5,482,915 A
• Filed: 09/20/1993
• Issued: 01/09/1996
• Est. Priority Date: 09/20/1993
• Status: Expired due to Fees

• Current Assignee: Air Products and Chemicals Incorporated (Linde Plc)
• Original Assignee: Air Products and Chemicals Incorporated (Linde Plc)
• Inventors: Sciple, James F., Wang, Andrew W., Golden, Timothy C.
• Primary Examiner(s): MCFARLANE, ANTHONY R
• Application Number:
  US08/123,952
• Time in Patent Office: 841 Days
• Field of Search: 502/417, 502/406, 502/423, 502/424, 502/427, 502/437
• US Class Current: 502/417
• CPC Class Codes: B01D 2257/104 Oxygen
• 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: B01J 20/20 comprising free carbon; comprising carbon obtained by carbonising processes

Abstract

The present invention is a synthesis, product and process for activated carbon and preferably carbon molecular sieve separation of air to produce a nitrogen product wherein a carbon is partially pyrolyzed, impregnated with a transition metal salt and further pyrolyzed to develop enhanced microporosity. The resulting microporous carbon can then be activated with carbon dioxide or steam and then pore-sized by cracking of hydrocarbons on the carbon to produce a carbon molecular sieve.

Claims

1. A process for preparing an activated carbon impregnated with a transition metal salt with enhanced microporosity, comprising:

(a) impregnating a transition metal salt on a thermally generated pre-char carbon so as to impart approximately 0.5 to 15 weight percent of said transition metal salt on to said pre-char carbon based upon said pre-char carbon after impregnating said transition metal salt; and

(b) pyrolyzing said carbon at a temperature in the range of at least approximately 800°

C. to produce a transition metal salt impregnated activated carbon.

2. The process of claim 1 wherein said transition metal is selected from the group consisting of iron, nickel, manganese and copper.

3. The process of claim 1 wherein said impregnation is performed with a solution of said transition metal salt in an amount no greater than sufficient to wet said carbon.

4. The process of claim 1 wherein said transition metal salt is selected from the group consisting of iron chloride, nickel chloride, copper chloride, manganese chloride and iron nitrate.

5. The process of claim 1 wherein said pyrolysis is performed in an oxidative atmosphere selected from the group consisting of carbon dioxide, air, steam and mixtures thereof.

6. The process of claim 1 wherein said pyrolysis is performed in an oxygen deficient atmosphere.

7. The process of claim 6 wherein said oxygen deficient atmosphere has no more than 0.5 percent oxygen.

8. The process of claim 1 wherein said pre-char carbon is formed by the pyrolysis of a carbon in an oxygen deficient atmosphere at a temperature in the range of approximately 300°

to 600°

C.

9. The process of claim 8 wherein said carbon is selected from the group consisting of wood, coal, fruit pits, nut shells, bone and coconut shell.

10. The process of claim 1 wherein after said pyrolysis said carbon is activated by heating in the presence of an oxidation agent selected from the group consisting of carbon dioxide, air, steam and mixtures thereof.

11. The process of claim 1 wherein said carbon is further subjected to cracking of hydrocarbons on pores of said activated carbon to restrict the size of said pores in said carbon to produce a transition metal salt impregnated carbon molecular sieve adsorbent having enhanced microporosity.

12. A process for preparing a transition metal salt impregnated carbon molecular sieve adsorbent having enhanced microporosity, comprising:

(a) pyrolyzing a carbon in an inert atmosphere at a temperature in the range of approximately 300°

to 600°

C. to partially pyrolyze the carbon to a pre-char carbon;

(b) impregnating a solution of a transition metal salt on said partially pyrolyzed pre-char carbon so as to just wet said pre-char carbon to impart an approximately 0.5 to 15 weight percent increase in said pre-char carbon;

(c) drying said impregnated pre-char carbon at a temperature no greater than 200°

C.;

(d) further pyrolyzing said impregnated pre-char carbon in an inert atmosphere at a temperature in the range of approximately 800°

to 1000°

C. to produce a char;

(e) activating said char by heating the char in the presence of an oxidation agent selected from the group consisting of carbon dioxide, air, steam and mixtures thereof; and

(f) cracking hydrocarbons on pores of said activated char to restrict the size of said pores in said char to produce a transition metal salt impregnated carbon molecular sieve adsorbent having enhanced microporosity.