Molecular sieve adsorbent for gas purification and preparation thereof

• US 6,183,539 B1
• Filed: 07/01/1998
• Issued: 02/06/2001
• Est. Priority Date: 07/01/1998
• Status: Expired due to Fees

• Current Assignee: Zeochem
• Original Assignee: Zeochem, LLC
• Inventors: Rode, Edward J., Tsybulevskiy, Albert M.
• Primary Examiner(s): Spitzer, Robert H.
• Application Number:
  US09/108,518
• Time in Patent Office: 951 Days
• Field of Search: 951/17, 951/39, 959/02, 961/08, 502/68, 502/79
• US Class Current: 95/117
• 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: Y02C 20/40 of CO2
• CPC Class Codes: Y10S 95/902 Molecular sieve

Abstract

A molecular sieve adsorbent for the purification of gas streams containing water vapor and carbon dioxide and a process for its preparation. The adsorbent is a sodium form of a low-silica faujasite having a silica to alumina ratio of about 1.8:1 to about 2.2:1, a residual content of potassium ions less than about 8.0 percent (equiv.), a low content of crystalline and amorphous admixtures and crystal sizes generally within the range of 1-4 μm, blended with a binder.

Claims

1. A molecular sieve adsorbent for gas purification which comprises a sodium form of low-silica faujasite, having a silica:

alumina ratio of about 1.8-2.2 with a residual content of potassium ions less than about 8.0 percent (equiv.), and a binder, wherein at least about 80% of said low-silica faujasite, by weight, has a crystal size in the range of 1-4 μ

m and wherein the adsorbent has a volume of macropores with a radius from about 1000 to 10,000 Å

of at least about 0.4 cm³/g.

2. The molecular sieve adsorbent of claim 1 wherein the silica to alumina ratio is about 2.0 to about 2.2.

3. The molecular sieve adsorbent of claim 1 wherein the silica to alumina ratio is about 2.0 to about 2.1.

4. The molecular sieve adsorbent of claim 1 wherein the residual content of potassium ions is less than about 2.5 percent (equiv.).

5. The molecular sieve adsorbent of claim 1 wherein the residual content of potassium ions is less than about 1.0 percent (equiv.).

6. The molecular sieve adsorbent of claim 1 wherein the low silica faujasite comprises from about 60 to about 85 percent and the binder comprises from about 15 to about 40 percent of the adsorbent.

7. The adsorbent of claim 1 wherein the low-silica faujasite comprises less than 10.0 percent by weight zeolite A, high silica faujasite X and other crystalline and amorphous admixtures.

8. The adsorbent of claim 1 wherein the low-silica faujasite comprises of less than 2.0 percent by weight zeolite A, high silica faujasite X and other crystalline and amorphous admixtures.

9. The adsorbent of claim 1, wherein the low-silica faujasite has crystal sizes, wherein the crystal size of at least about 80 percent of the faujasite is in the range of about 1-3 μ

m.

10. The adsorbent of claim 1, wherein the low-silica faujasite has crystal sizes, wherein the crystal size of at least about 80 percent of the faujasite is in the range of about 1-2 μ

m.

11. The adsorbent of claim 1, wherein the binder is selected from the group consisting of kaolinite, bentonite, montmorillonite, and attapulgite clays, silica, alumina, alumosilicates, and cements.

12. The adsorbent of claim 1, wherein the adsorbent has a volume of macropores with a radius from about 1000 to 10000 Å

from about 0.4 to about 0.5 cm³/g.

13. A process for the adsorption of carbon dioxide and water from a gas stream comprising

passing the gas stream containing carbon dioxide and water over the molecular sieve adsorbent of claim 1, whereby substantial quantities of the carbon dioxide and water are adsorbed by the molecular sieve adsorbent.

14. A process for the production of a molecular sieve adsorbent comprising

preparing a sodium form of a low-silica faujasite, wherein the low-silica faujasite has a silica:

alumina ratio of about 1.8 to about 2.2 and a residual content of potassium ions less than about 8.0 percent (equiv.);

blending the resultant product with a binder and a peptizer, where in the blended product has a volume of macropores with a radius from about 1000 to 10000 Å

of at least about 0.4 cm³/g;

forming the blended product into a shaped article; and

drying and calcining the article to produce the adsorbent product.

15. The process of claim 14 wherein the low-silica faujasite is prepared by mixing sodium aluminate, sodium silicate and sodium and potassium hydroxide, wherein the ratio of the components expressed as mixtures of oxide are within the following ranges:

16. The process of claim 14 further comprising mixing a powder of montmorillonite in the amount of about 0.6 to about 1.5 percent, based on the final weight of the reaction product, with the prepared low-silica faujasite into a reaction mixture under intensive stirring for out 15 to 30 minutes, wherein the montmorillonite powder has a particle size of 0.4 to 0.8 μ

m and wherein the low-silica faujasite has a crystal-size in the range of about 1 to 4 μ

m.

17. The process of claim 14 further comprising ion exchanging the prepared, sodium form of low-silica faujasite with a sodium chloride solution.

18. The process of claim 17 wherein the sodium form of low silica faujasite is ion exchanged from about 1 to about 3 times.

19. The process of claim 17 wherein the sodium form of low silica faujasite is ion exchanged at a temperature from about 60°

C. to about 85°

C.

20. The process of claim 14 further comprising ion exchanging the prepared, sodium form of low-silica faujasite with a solution comprising sodium chloride and sodium hydroxide.

21. The process of claim 14 further comprising treating the prepared sodium form of low-silica faujasite and binder with a pore-forming additive.

22. The process of claim 21 wherein the pore-forming additive is selected from the group consisting of synthetic and natural materials including mineral acids, polyalkeneglycols, polyacrylamides, polycarboxylates, starch, molasses and lignin.

23. The process of claim 21 wherein the peptizer and pore-forming additives comprise from about 0.5 to about 2.0 percent of the adsorbent product, based on a total weight of the adsorbent product.

24. The process of claim 14 further comprising blending the low-silica faujasite with the peptizer.

25. The process of claim 14 further comprising blending the binder with the peptizer.