Process for the preparation of a molecular sieve adsorbent for selectively adsorbing methane from a gaseous mixture

• US 6,090,738 A
• Filed: 03/09/1998
• Issued: 07/18/2000
• Est. Priority Date: 03/10/1997
• Status: Expired due to Fees

• Current Assignee: Indian Petrochemicals Corp. Ltd. (Reliance Industries Limited)
• Original Assignee: Indian Petrochemicals Corp. Ltd. (Reliance Industries Limited)
• Inventors: Jasra, Raksh Vir, Choudary, Nettem Venkateshwarlu, Bhat, Sodankoor Garadi Thirumaleshwar
• Primary Examiner(s): Dunn, Tom
• Assistant Examiner(s): Nguyen, Cam N.
• Application Number:
  US09/037,153
• Time in Patent Office: 862 Days
• Field of Search: 502/62, 502/64, 502/65, 502/68, 502/73, 502/79, 95/902, 95/128, 95/143
• US Class Current: 502/62
• CPC Class Codes: B01J 20/183 Physical conditioning without chemical treatment, e.g. drying, granulating, coating, irradiation
• CPC Class Codes: B01J 20/186 Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
• CPC Class Codes: Y10S 95/902 Molecular sieve

Abstract

This invention relates to the manufacture of a molecular sieve adsorbent for selectively separating methane from its gaseous mixture with nitrogen. More particularly, the invention relates to the manufacture of novel molecular sieve adsorbents useful for the separation of methane-nitrogen gaseous mixture.

Claims

1. A process for preparing a molecular sieve adsorbent for selectively adsorbing methane from a gaseous mixture comprising methane and nitrogen, said process comprising:

(a) preparing a mixture of zeolite powder from a zeolite of the formula

space="preserve" listing-type="equation">Na.sub.m Al.sub.m Si.sub.48-m O.sub.96 nH.sub.2 O

where m is from 2 to 8, n is from 0 to 30, the value of n depends on the value of m and degree of hydration.

and, clay and an organic binder;

(b) shaping said zeolite mixture to obtain adsorbent bodies;

(c) subjecting said adsorbent bodies to calcination; and

(d) subjecting said adsorbent bodies either prior to or after calcination or both, to cationic exchange in the presence of an alkali metal solution to affect surface modification of said adsorbent bodies to obtain said molecular sieve adsorbent of the formula

space="preserve" listing-type="equation">Na.sub.a.M1.sub.b.M2.sub.c.Al.sub.x.Si.sub.48-x.O.sub.96.nH.sub.2 O

where the value of

a is from 0.1 to 1,

b and c are from 0 to 8

and x is from 2 to 8,

M1 is potassium or cesium or a mixture thereof and M2 is a rare earth metal ion, and n represents the moles of water.

2. The process as claimed in claim 1, wherein the alkali metal solution is a salt solution of potassium or cesium or a mixture thereof.

3. The process as claimed in claim 1, wherein said clay is bentonite clay.

4. The process as claimed in claim 1, wherein said clay is present in an amount of 2 to 40% by weight.

5. The process as claimed in claim 1, wherein said binder is selected from the group consisting of sodium lignosulfate, starch and polyvinyl alcohol.

6. The process as claimed in claim 1, wherein said zeolite mixture is subjected to ball milling to produce powders of particle size of less than 60 microns.

7. The process as claimed in claim 1, wherein the adsorbent bodies are dried at room temperature for about 6 to 12 hrs. followed by oven drying at a temperature of 110°

C. for 6to 18 hrs.

8. The process as claimed in claim 1, wherein said calcination is carried out at a temperature of 500 to 750°

C.

9. The process as claimed in claim 1, wherein said calcination is carried out for a period of from 2 to 12 hrs.

10. The process as claimed in claim 1, wherein said cation exchange is carried out at a concentration of 1 to 10% by weight of the cation in aqueous solution.

11. The process as claimed in claim 10, wherein said cation exchange is carried out at a temperature of 30 to 100°

C. for 4 to 48 hrs.

12. The process as claimed in claim 1 wherein said cation exchanged adsorbent bodies are thoroughly washed with hot water.

13. The process as claimed in claim 12, wherein the adsorbent bodies are oven dried at 110°

C. for 6 to 8 hours.

14. A molecular sieve adsorbent of the formula