Mixed matrix membrane with super water washed silica containing molecular sieves and methods for making and using the same

• US 7,268,094 B2
• Filed: 08/18/2003
• Issued: 09/11/2007
• Est. Priority Date: 08/18/2003
• Status: Expired due to Fees

• Current Assignee: Chevron USA Incorporated (Chevron Corp.)
• Original Assignee: Chevron USA Incorporated (Chevron Corp.)
• Inventors: Miller, Stephen J., Yuen, Lun-Teh
• Primary Examiner(s): LORENGO, JERRY A
• Application Number:
  US10/643,555
• Publication Number:
  US 20050043167A1
• Time in Patent Office: 1,485 Days
• Field of Search: 502/4, 502/60, 502/62
• US Class Current: 502/4
• CPC Class Codes: B01D 2325/26 Electrical properties
• CPC Class Codes: B01D 67/00793 Dispersing a component, e.g. as particles or powder, in another component
• CPC Class Codes: B01D 67/0088 Physical treatment with compounds, e.g. swelling, coating or impregnation
• CPC Class Codes: B01D 69/148 Organic/inorganic mixed matrix membranes
• CPC Class Codes: B01D 71/027 Silicium oxide
• CPC Class Codes: B01D 71/0281 Zeolites
• CPC Class Codes: B01J 20/28026 Particles within, immobilised, dispersed, entrapped in or on a matrix, e.g. a resin
• CPC Class Codes: B01J 20/28033 Membrane, sheet, cloth, pad, lamellar or mat

Abstract

The present invention provides a method for preparing silica containing molecular sieves which may be mixed with an organic polymer to create a mixed matrix membrane. Further, this invention includes a method of making such a mixed matrix membrane and the membrane itself. A process for separating component gases from a mixture using the subject mixed matrix membrane is also described. The method for preparing silica containing molecular sieves comprises super water washing silica containing molecular sieves to produce water washed molecular sieves which are substantially free of surface remnants. Super water washing also ideally lowers the concentration of alkali metals in the molecular sieves. The water washed sieves are sufficiently free of surface remnants such that when the water washed sieves are subjected to a Sieve Wash Conductivity Test, a wash filtrate is produced having a conductivity of less than 110 micro mhos/cm, more preferably less than 80 micro mhos/cm, even more preferably less than 50 micro mhos/cm, and most preferably less than 30 micro mhos/cm. It is believed that super washing the sieves to this degree will enhance, compared to conventional preparation techniques, the ability of the molecular sieves to bond with an organic polymer to form a highly selective and permeable mixed matrix membrane.

Claims

1. A method for preparing silica containing molecular sieves which may be mixed with an organic polymer to create a mixed matrix membrane, the method comprising:

washing silica containing molecular sieves with a basic water solution having a pH of at least 9; and

water washing the silica containing molecular sieves sufficiently to produce water washed molecular sieves which are substantially free of surface remnants, such that when the water washed molecular sieves are subjected to a Sieve Wash Conductivity Test, a wash filtrate is produced having a conductivity of less than 110 micro mhos/cm.

2. The method of claim 1, wherein:

the conductivity is less than 80 micro mhos/cm.

3. The method of claim 1, wherein:

the conductivity is less than 50 micro mhos/cm.

4. The method of claim 1, wherein:

the conductivity is less than 30 micro mhos/cm.

5. The method of claim 1 wherein:

the basic water solution has a pH of at least 11.

6. The method of claim 1, wherein:

the water washing is performed continuously until the silica containing molecular sieves are substantially free of the surface remnants.

7. The method of claim 1, wherein:

the water washing is performed batch wise until the silica containing molecular sieves are substantially free of the surface remnants.

8. The method of claim 1, further comprising:

calcining the silica containing molecular sieves after the step of water washing has produced sieves which are substantially free of surface remnants.

9. The method of claim 1, further comprising:

silanating the water washed silica containing molecular sieves.

10. A method of making a mixed matrix membrane, the method comprising the steps of:

washing silica containing molecular sieves with a basic water solution having a pH of at least 9;

water washing the silica containing molecular sieves sufficiently to produce water washed molecular sieves which are substantially free of surface remnants, such that when the water washed molecular sieves are subjected to a Sieve Wash Conductivity Test, a wash filtrate is produced having a conductivity of less than 110 micro mhos/cm;

dispersing the water washed molecular sieves into a solvated organic polymer; and

allowing the organic polymer to dry thereby creating a mixed matrix membrane comprising an organic polymer with the water washed molecular sieves dispersed therein.

11. The method of claim 10 wherein, the wash filtrate has a conductivity of less than 80 micro mhos/cm.

12. The method of claim 10 wherein, the wash filtrate has a conductivity of less than 50 micro mhos/cm.

13. The method of claim 10 wherein, the wash filtrate has a conductivity of less than 30 micro mhos/cm.

14. The method of claim 10, further comprising the step of calcining the water washed silica containing molecular sieves.

15. The method of claim 10, further comprising the step of silanating the water washed silica containing molecular sieves.