WO2006096374B1 - Mercury removal sorbent - Google Patents

Mercury removal sorbent

Info

Publication number
WO2006096374B1
WO2006096374B1 PCT/US2006/006905 US2006006905W WO2006096374B1 WO 2006096374 B1 WO2006096374 B1 WO 2006096374B1 US 2006006905 W US2006006905 W US 2006006905W WO 2006096374 B1 WO2006096374 B1 WO 2006096374B1
Authority
WO
WIPO (PCT)
Prior art keywords
accordance
vanadium
tio
heavy metal
recited
Prior art date
Application number
PCT/US2006/006905
Other languages
French (fr)
Other versions
WO2006096374A2 (en
WO2006096374A3 (en
Inventor
Joseph B Cross
Glenn W Dodwell
Marvin M Johnson
Edward L Ii Sughrue
Jianhua Yao
Original Assignee
Conocophillips Co
Joseph B Cross
Glenn W Dodwell
Marvin M Johnson
Edward L Ii Sughrue
Jianhua Yao
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Conocophillips Co, Joseph B Cross, Glenn W Dodwell, Marvin M Johnson, Edward L Ii Sughrue, Jianhua Yao filed Critical Conocophillips Co
Priority to AU2006220978A priority Critical patent/AU2006220978B8/en
Priority to CA2600041A priority patent/CA2600041C/en
Priority to EP06736264.0A priority patent/EP1861191B1/en
Publication of WO2006096374A2 publication Critical patent/WO2006096374A2/en
Publication of WO2006096374A3 publication Critical patent/WO2006096374A3/en
Publication of WO2006096374B1 publication Critical patent/WO2006096374B1/en

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/64—Heavy metals or compounds thereof, e.g. mercury
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8665—Removing heavy metals or compounds thereof, e.g. mercury
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0214—Compounds of V, Nb, Ta
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204—Inorganic carriers, supports or substrates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234—Inorganic material layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234—Inorganic material layers
    • B01J20/3236—Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/60—Heavy metals or heavy metal compounds
    • B01D2257/602—Mercury or mercury compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/42—Materials comprising a mixture of inorganic materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S210/00—Liquid purification or separation
    • Y10S210/902—Materials removed
    • Y10S210/911—Cumulative poison
    • Y10S210/912—Heavy metal
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S210/00—Liquid purification or separation
    • Y10S210/902—Materials removed
    • Y10S210/911—Cumulative poison
    • Y10S210/912—Heavy metal
    • Y10S210/913—Chromium
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S210/00—Liquid purification or separation
    • Y10S210/902—Materials removed
    • Y10S210/911—Cumulative poison
    • Y10S210/912—Heavy metal
    • Y10S210/914—Mercury
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S502/00—Catalyst, solid sorbent, or support therefor: product or process of making
    • Y10S502/514—Process applicable either to preparing or to regenerating or to rehabilitating catalyst or sorbent
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S502/00—Catalyst, solid sorbent, or support therefor: product or process of making
    • Y10S502/515—Specific contaminant removal
    • Y10S502/516—Metal contaminant removal

Abstract

A sorbent composition comprising a vanadium compound and a TiO2 support material is disclosed. Methods of making and using the composition to rem heavy metals or heavy metal containing compounds from a fluid stream are also provided. Such methods are particularly useful in the removal of mercury and merc compounds from flue gas streams produced from the combustion of hydrocarbon-containing materials such as coal and petroleum fuels.

Claims

AMENDED CLAIMS received by the International Bureau on 22 August 2007 (22 -08.2007)
1. A method for forming a sorbent material comprising:
(a) incorporating into, onto, or into and onto a porous TiO2 support a mixture including a source of vanadate ions, a solvent capable of solubilizing said source of vanadate ions, and an oxidizing agent;
(b) drying said vanadate incorporated TiO2 material; and
(c) calcining said dried vanadium incorporated TiO2 material.
2. A method in accordance with claim 1 wherein said source of vanadate ions comprises NH4VO3.
3. A method in accordance with claim 1 wherein step (a) includes impregnating said TiO2 support with said source of vanadate ions.
4. A method in accordance with claim 1 wherein step (a) includes dissolving said source of vanadate ions in said solvent followed by the addition of said oxidizing agent so as to maintain the vanadium present in said vanadate ions in a +5 oxidation state.
5. A method in accordance with claim 1 wherein said solvent is selected from the group consisting of oxalic acid, HNO3, HCl, and mixtures thereof.
6. A method in accordance with claim 1 wherein said oxidizing agent is different from said solvent and selected from the group consisting of H2SO4, HNO3, permanganate, ozone, H2O2, and mixtures thereof.
7. A method in accordance with claim 1 wherein step (c) includes heating said dried vanadium incorporated TiO2 material to a temperature of between about 250 - 8000C (482-1472°F).
8. A method in accordance with claim 7 wherein step (c) includes heating said dried vanadium incorporated TiO2 material to a temperature of between about 300 - 6000C (572-1112°F).
9. A method in accordance with claim 1 wherein said vanadium oxide compound comprises V2O5 a hydrate of V2O5, a peroxo complex of vanadium oxide, or mixtures thereof.
10. A method in accordance with claim 1 wherein said calcined vanadium incorporated TiO2 material comprises from about 0.5-40% by weight vanadium on an elemental basis.
11. A method in accordance with claim 1 wherein said oxidizing agent is present in the vanadate ion containing mixture of step (a) at a level of about 0.01-25% by weight.
12 . A method for forming a sorbent material comprising:
(a) preparing a mixture comprising a source of vanadate ions and a solvent capable of solubilizing said source of vanadate ions;
(b) adding a quantity of an oxidizing agent to said mixture;
(c) intimately mixing said mixture with a quantity of TiO2 particles;
(d) drying said intimate mixture thereby forming a vanadium incorporated TiO2 material; and
(e) calcining said vanadium incorporated TiO2 material.
13. A method in accordance with claim 12 wherein said solvent is selected from the group consisting of oxalic acid, HNO3, HCl, and mixtures thereof.
14 A method in accordance with claim 12 wherein said oxidizing agent is different from said solvent and selected from the group consisting of H2SO4, HNO3, permanganate, ozone, H2O2, and mixtures thereof.
15. A method in accordance with claim 12 wherein said source of vanadate ions comprises NH4VO3.
16. A method in accordance with claim 12 wherein said oxidizing agent is added to said mixture in step (b) so as to provide from about 0.01-25% of the total weight of the mixture.
17. A method in accordance with claim 12 wherein step (c) includes impregnating said TiO2 particles with said vanadate ions.
18. A method in accordance with claim 12 wherein step (d) includes heating said mixture to a temperature of at least about 1000C (212°F).
19. A method in accordance with claim 12 wherein step (b) includes the drop wise addition of said oxidizing agent to said mixture.
20. A method in accordance with claim 12 wherein said oxidizing agent is added in a sufficient quantity so as to maintain the vanadium present in said vanadate ions in a +5 oxidation state.
21. A method in accordance with claim 12 wherein step (e) includes heating said vanadium incorporated TiO2 material to a temperature of between about 250 - 8000C (482- 1472°F).
22. A method in accordance with claim 21 wherein step (e) includes heating said vanadium incorporated TiO2 material to a temperature of between about 300 - 6000C (572- 1112°F).
23. A method in accordance with claim 12 wherein said vanadium oxide compound comprises V2O5 a hydrate of V2O5, a peroxo complex of vanadium oxide, or mixtures thereof.
24. A method in accordance with claim 12 wherein said vanadium incorporated TiO2 material comprises from about 0.5-40% by weight vanadium on an elemental basis.
25. A method of removing at least one elemental heavy metal from a fluid stream, said method comprising the step of:
(a) contacting said fluid stream with a vanadium incorporated TiO2 material comprising a porous TiO2 support material having incorporated onto, into, or onto and into a vanadium containing compound for sorption and removal of at least a portion of said at least one elemental heavy metal from said fluid stream.
26. A method in accordance with claim 25 wherein said vanadium incorporated support material oxidizes said elemental heavy metal into an oxidized heavy metal species .
27 A method in accordance with claim 25 wherein said vanadium containing compound comprises V2O5 a hydrate of V2O5, a peroxo complex of vanadium oxide, or mixtures thereof.
28 A method in accordance with claim 25 wherein said contacting step results in a pressure drop in said fluid stream of less than about 138 kPa (20 psia).
29 A method in accordance with claim 28 wherein said contacting step results in a pressure drop in said fluid stream of less than about 69 kPa (10 psia).
30 A method in accordance with claim 25 wherein said fluid stream has a temperature between about 10 - 2040C (50-400°F) during said contacting step.
31. A method in accordance with claim 25 wherein said fluid stream comprises at least one elemental heavy metal or selected from the group consisting of arsenic, beryllium, lead, cadmium, chromium, nickel, zinc, mercury, and barium.
32. A method in accordance with claim 31 wherein said at least one elemental heavy metal is mercury.
33. A method in accordance with claim 25 wherein said vanadium incorporated JJO2 material comprises divided particles that are suspended in said fluid stream during said contacting step, pelletized particles placed in a fixed or fluidized bed, monoliths, or combinations thereof.
34. A method in accordance with claim 25 wherein said contacting step results in the sorption of at least about 80% by weight of the at least one elemental heavy metal contained in said fluid stream.
35 A method in accordance with claim 25 wherein said vanadium incorporated TiO2 material is capable of sorbing at least about 1 atom of said elemental heavy metal per every 5 atoms of vanadium.
36. A method in accordance with claim 25 wherein said vanadium incorporated TiO2 material comprises from about 0.5-40% by weight vanadium on an elemental basis.
37. A process for the removal of at least one elemental heavy metal from a flue gas stream produced by the combustion of a hydrocarbon-containing fuel comprising the steps of: (a) contacting said flue gas stream with a first sorbent material comprising a vanadium incorporated TiO2 material comprising a porous TiO2 support material having incorporated onto, into, or onto and into a vanadium containing compound for sorbing and removing at least a portion of said at least one elemental heavy metal present in said flue gas stream from said flue gas stream; and
(b)contacting said flue gas stream with a second sorbent material different from said first sorbent material for sorbing and removing at least a portion of said at least one elemental heavy metal not sorbed during step (a).
38. A process as recited in claim 37 wherein said vanadium incorporated TiO2 material oxidizes said elemental heavy metal into an oxidized heavy metal species during step (a).
39 A process as recited in claim 37 wherein said second sorbent material comprises a material selected from the group consisting of porous zeolite materials, amorphous carbons, and combinations thereof.
40. A process as recited in claim 38 wherein said amorphous carbons are selected from the group consisting of activated charcoal, activated carbon, and combinations thereof.
41. A process as recited in claim 39 wherein said porous zeolite material comprises ZSM- 5 zeolite.
42. A process as recited in claim 37 wherein said flue gas stream comprises at least one elemental heavy metal selected from the group consisting of arsenic, beryllium, lead, cadmium, chromium, nickel, zinc, mercury, and barium.
43. A process as recited in claim 42 wherein said at least one elemental heavy metal is mercury.
44. A process as recited in claim 37 wherein said vanadium containing compound comprises V2O5 a hydrate of V2O5, a peroxo complex of vanadium oxide, or mixtures thereof.
45. A process as recited in claim 37 wherein step (a) results in a pressure drop in said flue gas stream of less than about 138 kPa (20 psia).
46. A process as recited in claim 37 wherein said flue gas stream has a temperature between about 10 - 2040C (50-400°F) during step (a).
47. A process as recited in claim 37 wherein said vanadium incorporated TiO2 material comprises divided particles that are suspended in said flue gas stream during step (a), pelletized particles placed in a fixed or fluidized bed, monoliths, or combinations thereof.
48. A process as recited in claim 37 wherein step (a) results in the sorption of at least about 80% by weight of said at least one elemental heavy metal contained in said flue gas stream.
49 A process as recited in claim 37 wherein step (b) results in the removal of at least about 80% by weight of said at least one elemental heavy metal compound from said flue gas stream leaving step (a).
50 A process as recited in claim 37 wherein said vanadium incorporated TiO2 material comprises from about 0.5-40% by weight vanadium on an elemental basis.
51. A process as recited in claim 37 wherein prior to step (a) said process includes removal of at least about 50% by weight of all NOx and SOx present in said flue gas.
52. A process as recited in claim 37 wherein said flue gas stream comprises less than about 400 ppm NOx and less than about 800 ppm SOx immediately prior to step (a).
PCT/US2006/006905 2005-03-03 2006-02-28 Mercury removal sorbent WO2006096374A2 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
AU2006220978A AU2006220978B8 (en) 2005-03-03 2006-02-28 Mercury removal sorbent
CA2600041A CA2600041C (en) 2005-03-03 2006-02-28 Method of making a sorbent comprising vanadium and tio2 and method of removing mercury using said sorbent
EP06736264.0A EP1861191B1 (en) 2005-03-03 2006-02-28 Method for mercury removal with a sorbent

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US11/071,633 US7404939B2 (en) 2005-03-03 2005-03-03 Mercury removal sorbent
US11/071,633 2005-03-03

Publications (3)

Publication Number Publication Date
WO2006096374A2 WO2006096374A2 (en) 2006-09-14
WO2006096374A3 WO2006096374A3 (en) 2007-09-13
WO2006096374B1 true WO2006096374B1 (en) 2007-10-18

Family

ID=36944300

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US2006/006905 WO2006096374A2 (en) 2005-03-03 2006-02-28 Mercury removal sorbent

Country Status (5)

Country Link
US (2) US7404939B2 (en)
EP (1) EP1861191B1 (en)
AU (1) AU2006220978B8 (en)
CA (1) CA2600041C (en)
WO (1) WO2006096374A2 (en)

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CN110756156A (en) * 2019-11-08 2020-02-07 浙江大学 Preparation method and application of bimetallic oxide demercuration adsorbent

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Also Published As

Publication number Publication date
CA2600041A1 (en) 2006-09-14
EP1861191A2 (en) 2007-12-05
US20080254979A1 (en) 2008-10-16
WO2006096374A2 (en) 2006-09-14
EP1861191B1 (en) 2014-12-24
AU2006220978B2 (en) 2010-07-08
EP1861191A4 (en) 2008-12-31
US20060198775A1 (en) 2006-09-07
US7498290B2 (en) 2009-03-03
US7404939B2 (en) 2008-07-29
WO2006096374A3 (en) 2007-09-13
AU2006220978B8 (en) 2010-10-28
AU2006220978A1 (en) 2006-09-14
CA2600041C (en) 2015-07-07

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