Regenerable system for the removal of sulfur compounds from a gas stream

Patent metadata

Field	Value
Publication number	US-2016279595-A1
Application number	US-201415036315-A
Country	US
Kind code	A1
Filing date	Nov 10, 2014
Priority date	Nov 15, 2013
Publication date	Sep 29, 2016
Grant date	—

Abstract

The disclosure relates to copper oxide-based sorbents, and processes for preparing and using them. The sorbents are preferably used to remove one or more sulfur species from gas streams. The sorbents comprise a porous silica support material impregnated with CuO nanoparticles. The nanoparticles are uniformly distributed throughout the porous silica support and sulfur compounds are adsorbed on the nanoparticles.

First claim

1 . A sulfidized sorbent composition comprising a porous silica support material impregnated with CuO nanoparticles, wherein the nanoparticles are essentially uniformly distributed throughout the porous silica support and sulfur compounds are adsorbed on the nanoparticles.

2 . (canceled)

3 . The sulfidized sorbent composition of claim 1 , wherein the silica support material has a median pore diameter of about 5 to about 15 nm.

4 . (canceled)

5 . (canceled)

6 . The sulfidized sorbent composition of claim 1 , wherein the nanoparticles have an average diameter of about 1 to about 8 nm.

7 . (canceled)

8 . (canceled)

9 . (canceled)

10 . The sulfidized sorbent composition of claim 1 , wherein the CuO nanoparticles further comprise Zn.

11 . The sulfidized sorbent composition of claim 10 , wherein the Cu/Zn molar ratio is in the range of about 20:1 to about 1:1.

12 . The sulfidized sorbent composition of claim 1 , wherein the porous silica support has a pore volume in the range of about 0.3 to about 3.0 ml/g.

13 . The sulfidized sorbent composition of claim 1 , wherein an average interparticle distance between the nanoparticles is at the theoretical maximum distance.

14 . (canceled)

15 . (canceled)

16 . The sulfidized sorbent composition of claim 1 , wherein the silica support material comprises SBA silica, MCM silica, FDU silica, KIT silica or silica gel.

17 . The sulfidized sorbent composition of claim 1 , wherein the sulfur compounds comprise H 2 S.

18 . A method of preparing a sulfidized sorbent composition comprising a porous silica support material impregnated with Cu—ZnO nanoparticles, wherein the nanoparticles are essentially uniformly distributed throughout the porous silica support and sulfur compounds are adsorbed on the nanoparticles, the method comprising:
impregnating the silica support material with an aqueous solution of zinc salt and copper salt having a molar ratio of Cu:Zn of about 2:1;
drying the impregnated support material;
calcinating the impregnated support material; and
passing a gaseous stream of sulfur compounds through the impregnated support material.

19 . The method of claim 18 , wherein the zinc salt is selected from the group consisting of zinc nitrate, zinc acetate, and a mixture thereof; and the copper salt is selected from the group consisting of copper nitrate, copper acetate, and a mixture thereof.

20 . The method of claim 18 , wherein the step of impregnating is performed by incipient wetness impregnating.

21 . (canceled)

22 . (canceled)

23 . The method of claim 18 , wherein the calcinating is performed by heating the dried particles to a temperature range of about 200-600 ° C.

24 . (canceled)

25 . The method of claim 18 , wherein the calcinating is performed in an inert gas.

26 . The method of claim 18 , wherein the sulfur compounds comprise H 2 S.

27 . A method of removing sulfur compounds adsorbed to the sulfidized sorbent composition of claim 1 comprising heating the sulfidized sorbent composition to a temperature between about 100-700 ° C. and passing an oxidizing agent over the sorbent composition.

28 . (canceled)

29 . (canceled)

30 . (canceled)

31 . (canceled)

32 . The method of claim 27 , further comprising passing a reducing agent over the sorbent composition after the oxidation step.

33 . The method of claim 32 , wherein the reducing agent is selected from the group consisting of hydrogen, methane, and carbon monoxide gas, or a mixture thereof.

34 . The method of claim 33 wherein the hydrogen gas comprises 1-10 mol % hydrogen in an inert carrier gas.

35 . The method of claim 32 , further comprising passing an oxidizing agent over the sorbent composition after the reduction step.

36 . (canceled)

37 . (canceled)

38 . (canceled)

39 . A method for removing sulfur compounds from a gas stream, the method comprising passing the gas stream through an effective amount of a sorbent composition for an effective amount of time to produce a sulfidized sorbent composition and to reduce sulfur compounds in the gas stream to a level of less than about 1 ppm, the sorbent composition comprising a porous silica support material impregnated with CuO nanoparticles, wherein the nanoparticles are essentially uniformly distributed throughout the porous silica support.

40 - 69 . (canceled)

Assignees

• Univ Minnesota

Inventors

• Tsapatsis Michael
• Elyassi Bahman
• Al Wahedi Yasser
• Al Hashimi Saleh

Classifications

• B01J20/3433

  of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425 · CPC title

• B01D2253/1124

  Metal oxides · CPC title

• B01D2253/304

  Linear dimensions, e.g. particle shape, diameter · CPC title

• B01D2257/302

  Sulfur oxides · CPC title

• B01J20/3483

  by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling · CPC title