Removal of occluded alkali metal cations from MSE-framework type molecular sieves

Patent metadata

Field	Value
Publication number	US-10226319-B2
Application number	US-201815882353-A
Country	US
Kind code	B2
Filing date	Jan 29, 2018
Priority date	Oct 14, 2014
Publication date	Mar 12, 2019
Grant date	Mar 12, 2019

Abstract

A method for reducing the level of occluded alkali metal cations from an MSE-framework type molecular sieve comprises either (a) contacting the molecular sieve with a solution containing ammonium ions at a temperature of at least about 50° C. to ammonium-exchange at least part of the occluded potassium ions or (b) contacting the molecular sieve with steam at a temperature of at least about 300° C. and then subjecting the steamed molecular sieve to ammonium exchange.

First claim

What is claimed is:

1. A method for reducing a level of occluded alkali metal cations from an MSE-framework type molecular sieve, the method comprising:
(a1) contacting an MSE framework-type molecular sieve containing a first amount of occluded potassium ions with a solution containing ammonium ions at a temperature of at least about 50° C. to ammonium-exchange at least part of the occluded potassium ions and produce a treated molecular sieve containing a second amount of occluded potassium ions, wherein the second amount is less than the first amount; and
exchanging the treated molecular sieve with cations of a rare earth element.

2. The method of claim 1 , wherein the MSE framework-type molecular sieve comprises MCM-68.

3. The method of claim 1 , wherein the MSE framework-type molecular sieve comprises an aluminosilicate.

4. The method of claim 3 , wherein the MSE framework-type molecular sieve has a silicon to aluminum atomic ratio in the range of from about 21 to about 1000.

5. The method of claim 1 , wherein the first amount of occluded potassium ions is at least about 0.25 wt % potassium by weight of the molecular sieve.

6. The method of claim 1 , wherein the second amount of occluded potassium ions in the treated molecular sieve is no more than about 0.10 wt % potassium.

7. The method of claim 1 , further comprising:
(b1) crystallizing a reaction mixture comprising a source of water, a source of an oxide of a tetravalent element, Y, a source of a trivalent element, X, a source of potassium and a source of organic structure directing agent effective to direct the crystallization of an MSE framework-type molecular sieve from the reaction mixture;
(c1) recovering crystals of MSE framework-type molecular sieve from the reaction mixture; and
(d1) supplying at least part of the recovered crystals or a product thereof to the contacting (a1).

8. The method of claim 7 , further comprising:
(e1) removing at least part of the organic structure directing agent contained by the recovered crystals prior to supplying the crystals to the contacting (a1).

9. The method of claim 7 , further comprising:
(f1) heating the treated molecular sieve to convert at least part of the exchanged ammonium ions to hydrogen ions.

10. The method of claim 1 , wherein the treated molecular sieve is converted to a hydrogen form prior to exchanging with the cations of the rare earth element.

11. A method for reducing a level of occluded alkali metal cations from an MSE-framework type molecular sieve, the method comprising:
(a2) contacting an MSE framework-type molecular sieve containing a first amount of occluded potassium ions with steam at a temperature of at least about 300° C. to produce a steamed molecular sieve; and
(b2) contacting the steamed molecular sieve with a solution containing ammonium ions to ammonium-exchange at least part of the potassium ions in the steamed molecular sieve thereby producing a treated molecular sieve containing a second amount of occluded potassium ions, wherein the second amount is less than the first amount; and
exchanging the treated molecular sieve with cations of a rare earth element.

12. The method of claim 11 , wherein the contacting (b2) is conducted with a solution containing ammonium ions at a temperature of at least about 10° C.

13. The method of claim 11 , wherein the MSE framework-type molecular sieve comprises an aluminosilicate.

14. The method of claim 13 , wherein the MSE framework-type molecular sieve has a silicon to aluminum atomic ratio of at least about 7.

15. The method of claim 11 , wherein the first amount of occluded potassium ions in the molecular sieve is at least about 0.25 wt % potassium.

16. The method of claim 11 , wherein the second amount of occluded potassium ions in the treated molecular sieve is less than about 0.10 wt % potassium.

17. The method of claim 11 , further comprising:
(c2) crystallizing a reaction mixture comprising a source of water, a source of an oxide of a tetravalent element, Y, a source of a trivalent element, X, a source of potassium and a source of organic structure directing agent effective to direct the crystallization of an MSE framework-type molecular sieve from the reaction mixture;
(d2) recovering crystals of MSE framework-type molecular sieve from the reaction mixture; and
(e2) supplying at least part of the recovered crystals or a product thereof to the contacting (a2).

18. The method of claim 17 , further comprising:
(f2) removing at least part of the organic structure directing agent contained by the recovered crystals prior to supplying the crystals to the contacting (a2).

19. The process of claim 17 , further comprising:
(g2) heating the treated molecular sieve to convert at least part of the exchanged ammonium ions to hydrogen ions.

20. The method of claim 11 , wherein the treated molecular sieve is converted to a hydrogen form prior to exchanging with the cations of the rare earth element.

Assignees

• Exxonmobil Res & Eng Co

Inventors

• Burton Allen W
• Strohmaier Karl G
• Weigel Scott J

Classifications

• A61B2017/00805

  Treatment of female stress urinary incontinence · CPC title

• C01B39/04

  using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound · CPC title

• A61B17/3403

  Needle locating or guiding means · CPC title

• B01D2253/112

  Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106 · CPC title

• B01D53/9486

  for storing hydrocarbons · CPC title