US20180272318A1 - Denitration catalyst and method for producing the same - Google Patents

Denitration catalyst and method for producing the same Download PDF

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Publication number
US20180272318A1
US20180272318A1 US15/764,038 US201615764038A US2018272318A1 US 20180272318 A1 US20180272318 A1 US 20180272318A1 US 201615764038 A US201615764038 A US 201615764038A US 2018272318 A1 US2018272318 A1 US 2018272318A1
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Prior art keywords
denitration catalyst
catalyst
vanadium
vanadium pentoxide
specific surface
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US15/764,038
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English (en)
Inventor
Eiji KIYONAGA
Kenji Hikino
Keiichiro MORITA
Masatake Haruta
Toru Murayama
Makoto MINO
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chugoku Electric Power Co Inc
Tokyo Metropolitan Public University Corp
Original Assignee
Chugoku Electric Power Co Inc
Tokyo Metropolitan Public University Corp
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Application filed by Chugoku Electric Power Co Inc, Tokyo Metropolitan Public University Corp filed Critical Chugoku Electric Power Co Inc
Assigned to TOKYO METROPOLITAN UNIVERSITY, THE CHUGOKU ELECTRIC POWER CO., INC. reassignment TOKYO METROPOLITAN UNIVERSITY ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HARUTA, MASATAKE, HIKINO, KENJI, KIYONAGA, Eiji, MINO, Makoto, MORITA, Keiichiro, MURAYAMA, TORU
Publication of US20180272318A1 publication Critical patent/US20180272318A1/en
Abandoned legal-status Critical Current

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    • F01N2370/00—Selection of materials for exhaust purification
    • F01N2370/02—Selection of materials for exhaust purification used in catalytic reactors
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N2510/00—Surface coverings
    • F01N2510/06—Surface coverings for exhaust purification, e.g. catalytic reaction
    • F01N2510/068—Surface coverings for exhaust purification, e.g. catalytic reaction characterised by the distribution of the catalytic coatings
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N2570/00—Exhaust treating apparatus eliminating, absorbing or adsorbing specific elements or compounds
    • F01N2570/14—Nitrogen oxides
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N2590/00—Exhaust or silencing apparatus adapted to particular use, e.g. for military applications, airplanes, submarines
    • F01N2590/02—Exhaust or silencing apparatus adapted to particular use, e.g. for military applications, airplanes, submarines for marine vessels or naval applications
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N2610/00—Adding substances to exhaust gases
    • F01N2610/02—Adding substances to exhaust gases the substance being ammonia or urea
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E20/00—Combustion technologies with mitigation potential
    • Y02E20/12—Heat utilisation in combustion or incineration of waste
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00—Road transport of goods or passengers
    • Y02T10/10—Internal combustion engine [ICE] based vehicles
    • Y02T10/12—Improving ICE efficiencies

Definitions

  • the present invention relates to a denitration catalyst and a method for producing the denitration catalyst. More specifically, the present invention relates to a denitration catalyst used when exhaust gas generated through fuel combustion is cleaned up and a method for producing the denitration catalyst.
  • Nitrogen oxide causes, for example, acid rain, ozone depletion, and photochemical smog and seriously affects the environment and the human body, and therefore the treatment for nitrogen oxide has been an important issue.
  • a known technique of removing the nitrogen oxide is a selective catalytic reduction reaction (NH 3 -SCR) that uses ammonia (NH 3 ) as a reducing agent.
  • NH 3 -SCR selective catalytic reduction reaction
  • a catalyst in which vanadium oxide is supported on titanium oxide serving as a carrier is widely used as a catalyst for the selective catalytic reduction reaction.
  • Titanium oxide is the best carrier because titanium oxide has a low activity against sulfur oxide and has high stability.
  • vanadium oxide plays a key role in the NH 3 -SCR, but vanadium oxide cannot be supported in an amount of about 1 wt % or more because vanadium oxide oxidizes SO 2 into SO 3 . Therefore, vanadium oxide is typically used in an amount of 1 wt % or less relative to its carrier. Furthermore, in the current NH 3 -SCR, a catalyst in which vanadium oxide (and tungsten oxide in some cases) is supported on a titanium oxide carrier hardly reacts at low temperature and thus needs to be used at a high temperature of 350° C. to 400° C.
  • the present invention relates to a denitration catalyst containing 3.3 wt % or more of vanadium oxide in terms of vanadium pentoxide and having a BET specific surface area of 10 m 2 /g or more.
  • the denitration catalyst is preferably used for denitration at 200° C. or lower.
  • an amount of NH 3 desorbed by NH 3 -TPD is preferably 10.0 mmol/g or more.
  • the present invention relates to a method for producing the denitration catalyst, the method including a step of thermally decomposing a vanadate at a temperature of 300° C. to 400° C.
  • the present invention relates to a method for producing the denitration catalyst, the method including a step of dissolving a vanadate in a chelate compound, performing drying, and then performing firing.
  • the denitration catalyst according to the present invention exhibits a high denitration efficiency particularly at 200° C. or lower, which allows detoxification of NO into N 2 .
  • the selective catalytic reduction reaction that uses the denitration catalyst according to the present invention can be performed at 200° C. or lower, and therefore oxidation of SO 2 does not occur.
  • FIG. 1 illustrates the powder X-ray diffraction results of vanadium pentoxide catalysts produced in Examples 1 to 3 and Comparative Example 1.
  • FIG. 2 illustrates the powder X-ray diffraction results of vanadium pentoxide catalysts produced in Examples 3 to 8 and Comparative Examples 2 and 3.
  • FIG. 3 illustrates the NH 3 -SCR activity of vanadium pentoxide catalysts produced in Examples 1 to 3 and Comparative Examples 1 and 4.
  • FIG. 4 illustrates the relationship between the reaction temperature and the N 2 selectivity in a selective catalytic reduction reaction that uses vanadium pentoxide catalysts produced in Example 1 and Comparative Example 1.
  • FIG. 5 illustrates the space velocity dependency in the case where a vanadium pentoxide catalyst produced in Example 1 is used in a NH 3 -SCR reaction.
  • FIG. 6 illustrates a change in the NO conversion ratio over time in the case where a vanadium pentoxide catalyst produced in Example 1 is used in a selective catalytic reduction reaction in coexistence with water.
  • FIG. 7 illustrates changes in the NH 3 , NO, and SO 2 concentrations over time in the case where a vanadium pentoxide catalyst produced in Example 1 is used in a selective catalytic reduction reaction in coexistence with S.
  • FIG. 8 illustrates the relationship between the amount of vanadium pentoxide supported and the NO conversion ratio of a vanadium pentoxide catalyst produced in each of Examples at each reaction temperature.
  • FIG. 9 illustrates the relationship between the BET specific surface area and the NO conversion ratio of a vanadium pentoxide catalyst produced in each of Examples and Comparative Examples.
  • FIG. 10 illustrates the powder X-ray diffraction results of vanadium pentoxide catalysts produced in Examples 10 to 14.
  • FIG. 11 illustrates the NH 3 -SCR activity of vanadium pentoxide catalysts produced in Examples 10 to 14.
  • FIG. 12 illustrates the relationship between the specific surface area and the NO conversion ratio of vanadium pentoxide catalysts in Examples 1 and 2, Examples 10 to 13, and Comparative Example 1.
  • FIG. 13 illustrates the relationship between the BET specific surface area and the amount of NH 3 desorbed of vanadium pentoxide catalysts produced in Examples 1 and 2, Examples 11 and 12, and Comparative Example 1.
  • FIG. 14 illustrates the relationship between the amount of NH 3 desorbed and the NO conversion ratio of vanadium pentoxide catalysts produced in Examples 1 and 2, Examples 11 and 12, and Comparative Example 1.
  • a denitration catalyst of the present invention contains 3.3 wt % or more of vanadium oxide in terms of vanadium pentoxide and has a BET specific surface area of 10 m 2 /g or more. Such a denitration catalyst can exhibit a high denitration effect even in a low-temperature environment compared with known denitration catalysts such as a vanadium/titanium catalyst.
  • the NO conversion ratio is approximately 35% or more at a reaction temperature of 120° C. and approximately 60% or more at a reaction temperature of 150° C. Even at a reaction temperature of 100° C., the NO conversion ratio exceeds 20%.
  • the denitration catalyst contains only less than 3.3 wt % of vanadium oxide in terms of vanadium pentoxide, the NO conversion ratio is less than 20% at a reaction temperature of 120° C. and even at a reaction temperature of 150° C.
  • the denitration catalyst according to the present invention contains 3.3 wt % or more of vanadium oxide in terms of vanadium pentoxide, and may also contain titanium oxide as another component in addition to the vanadium oxide.
  • a noble metal, a base metal, and a main group metal may be contained.
  • tungsten oxide, chromium oxide, and molybdenum oxide can also be contained.
  • the denitration catalyst preferably contains 3.3 wt % or more of vanadium oxide in terms of vanadium pentoxide.
  • the denitration catalyst may contain 9 wt % or more of vanadium oxide in terms of vanadium pentoxide.
  • the denitration catalyst may contain 20 wt % or more of vanadium oxide in terms of vanadium pentoxide.
  • the denitration catalyst may contain 33 wt % or more of vanadium oxide in terms of vanadium pentoxide.
  • the denitration catalyst may contain 43 wt % or more of vanadium oxide in terms of vanadium pentoxide.
  • the denitration catalyst may contain 80 wt % or more of vanadium oxide in terms of vanadium pentoxide.
  • the content of vanadium oxide in the denitration catalyst may be 100%.
  • vanadium oxide includes vanadium(II) oxide (VO), vanadium(III) trioxide (V 2 O 5 ), vanadium(IV) dioxide (V 2 O 4 ), and vanadium(V) pentoxide (V 2 O 5 ), and the V element in vanadium pentoxide (V 2 O 5 ) may have a pentavalent, tetravalent, trivalent, or divalent form in the denitration reaction.
  • the NO conversion ratio exceeds 20%.
  • the NO conversion ratio exceeds 20%.
  • the NO conversion ratio exceeds 20%.
  • the NO conversion ratio exceeds 20%.
  • a denitration catalyst having a BET specific surface area of 4.68 m 2 /g which is a denitration catalyst having a BET specific surface area of less than 10 m 2 /g, the NO conversion ratio falls below 20%.
  • the BET specific surface area of the denitration catalyst is 10 m 2 /g or more and may be preferably 15 m 2 /g or more. More preferably, the BET specific surface area of the denitration catalyst may be 30 m 2 /g. More preferably, the BET specific surface area of the denitration catalyst may be 40 m 2 /g or more. More preferably, the BET specific surface area of the denitration catalyst may be 50 m 2 /g or more. More preferably, the BET specific surface area of the denitration catalyst may be 60 m 2 /g or more.
  • the BET specific surface area of the denitration catalyst is preferably measured in conformity with the conditions specified in JIS Z 8830:2013. Specifically, the BET specific surface area can be measured by a method described in Examples below.
  • the denitration catalyst of the present invention is used for denitration at 200° C. or lower.
  • the denitration catalyst is used for denitration at 160° C. or higher and 200° C. or lower.
  • oxidation of SO 2 into SO 3 does not occur during the NH 3 -SCR reaction.
  • the amount of NH 3 desorbed by NH 3 -TPD is 10.0 mmol/g or more.
  • the amount of NH 3 desorbed by NH 3 -TPD may be 20.0 mmol/g or more. More preferably, the amount of NH 3 desorbed by NH 3 -TPD may be 50.0 mmol/g or more. More preferably, the amount of NH 3 desorbed by NH 3 -TPD may be 70.0 mmol/g or more.
  • the denitration catalyst containing 3.3 wt % or more of vanadium oxide in terms of vanadium pentoxide and having a BET specific surface area of 10 m 2 /g or more can be produced by any of a thermal decomposition process, a sol-gel process, and an impregnation process.
  • a method for producing the denitration catalyst containing 3.3 wt % or more of vanadium pentoxide and having a specific surface area of 10 m 2 /g or more by a thermal decomposition process, a sol-gel process, or an impregnation process will be described.
  • the thermal decomposition process includes a step of thermally decomposing a vanadate.
  • vanadate examples include ammonium vanadate, magnesium vanadate, strontium vanadate, barium vanadate, zinc vanadate, tin vanadate, and lithium vanadate.
  • the vanadate is preferably thermally decomposed at 300° C. to 400° C.
  • the sol-gel process includes a step of dissolving a vanadate in a chelate compound, performing drying, and performing firing.
  • the chelate compound that may be used include compounds having a plurality of carboxy groups, such as oxalic acid and citric acid; compounds having a plurality of amino groups, such as acetylacetonate and ethylenediamine; and compounds having a plurality of hydroxy groups, such as ethylene glycol.
  • the sol-gel process preferably includes a step of dissolving a vanadate in a chelate compound such that the molar ratio of vanadium and the chelate compound is, for example, 1:1 to 1:5, though this is dependent on the chelate compound.
  • the molar ratio of the vanadate and the chelate compound may be 1:2 to 1:4.
  • the impregnation process includes a step of dissolving a vanadate in a chelate compound, adding a carrier, performing drying, and then performing firing.
  • the carrier include titanium oxide, aluminum oxide, and silica.
  • examples of the chelate compound that may be used include compounds having a plurality of carboxy groups, such as oxalic acid and citric acid; compounds having a plurality of amino groups, such as acetylacetonate and ethylenediamine; and compounds having a plurality of hydroxy groups, such as ethylene glycol.
  • xwt % V 2 O 5 /TiO 2 may be produced as a denitration catalyst according to an embodiment of the present invention by, for example, dissolving ammonium vanadate in an oxalic acid solution, adding titanium oxide (TiO 2 ) serving as a carrier, performing drying, and then performing firing.
  • the thus-produced denitration catalyst normally contains 3.3 wt % or more of vanadium pentoxide and has a specific surface area of 10 m 2 /g or more.
  • the denitration catalyst according to the above embodiment produces the following effects.
  • the denitration catalyst according to the above embodiment contains 3.3 wt % or more of vanadium oxide in terms of vanadium pentoxide and has a specific surface area of 10 m 2 /g or more.
  • a high denitration effect can be produced even in a selective catalytic reduction reaction at 200° C. or lower.
  • the denitration catalyst according to the above embodiment is preferably used for denitration at 200° C. or lower. This produces a high denitration effect in the selective catalytic reduction reaction that uses the denitration catalyst according to the above embodiment without oxidizing SO 2 .
  • the amount of NH 3 desorbed by NH 3 -TPD is preferably 10.0 mmol/g or more.
  • TPD temperature programed desorption
  • the method for producing a denitration catalyst according to the above embodiment preferably includes a step of thermally decomposing a vanadate at 300° C. to 400° C. This increases the specific surface area of the denitration catalyst according to the above embodiment, which improves a denitration effect in the selective catalytic reduction reaction that uses the denitration catalyst according to the above embodiment.
  • the method for producing a denitration catalyst according to the above embodiment preferably includes a step of dissolving a vanadate in a chelate compound, performing drying, and then performing firing. This increases the specific surface area of the denitration catalyst according to the above embodiment, which improves a denitration effect in the selective catalytic reduction reaction that uses the denitration catalyst according to the above embodiment.
  • V 2 O 5 vanadium pentoxide
  • the sample name of the denitration catalyst in Example 1 was “V 2 O 5 _ 300”.
  • Example 2 Ammonium vanadate was thermally decomposed in the air at 400° C. for 4 hours to obtain vanadium pentoxide.
  • the obtained vanadium pentoxide was used as a denitration catalyst in Example 2.
  • the sample name of the denitration catalyst in Example 2 was “V 2 O 5 _ 400”.
  • Ammonium vanadate was thermally decomposed in the air at 500° C. for 4 hours to obtain vanadium pentoxide.
  • the obtained vanadium pentoxide was used as a denitration catalyst in Comparative Example 1.
  • the sample name of the denitration catalyst in Comparative Example 1 was “V 2 O 5 _ 500”.
  • the vanadium pentoxide after firing was used as a denitration catalyst in Example 3.
  • the sample name of the denitration catalyst in Example 3 obtained by this sol-gel process was “V 2 O 5 _ SG_300”. Denitration catalysts obtained at different molar ratios of vanadium and oxalic acid when ammonium vanadate is dissolved in an oxalic acid solution will be described later.
  • the denitration catalyst after firing that was obtained by the same method as in Comparative Example 2 and contained 0.9 wt % of vanadium pentoxide was used as a denitration catalyst in Comparative Example 3.
  • the sample name of the denitration catalyst in Comparative Example 4 was “0.9 wt % V 2 O 5 /TiO 2 ”.
  • the denitration catalyst after firing that was obtained by the same method as in Comparative Example 2 and contained 3.3 wt % of vanadium pentoxide was used as a denitration catalyst in Example 4.
  • the sample name of the denitration catalyst in Example 4 was “3.3 wt % V 2 O 5 /TiO 2 ”.
  • the denitration catalyst after firing that was obtained by the same method as in Comparative Example 2 and contained 9 wt % of vanadium pentoxide was used as a denitration catalyst in Example 5.
  • the sample name of the denitration catalyst in Example 5 was “9 wt % V 2 O 5 /TiO 2 ”.
  • the denitration catalyst after firing that was obtained by the same method as in Comparative Example 2 and contained 20 wt % of vanadium pentoxide was used as a denitration catalyst in Example 6.
  • the sample name of the denitration catalyst in Example 5 was “20 wt % V 2 O 5 /TiO 2 ”.
  • the denitration catalyst after firing that was obtained by the same method as in Comparative Example 2 and contained 33 wt % of vanadium pentoxide was used as a denitration catalyst in Example 7.
  • the sample name of the denitration catalyst in Example 7 was “33 wt % V 2 O 5 /TiO 2 ”.
  • the denitration catalyst after firing that was obtained by the same method as in Comparative Example 2 and contained 43 wt % of vanadium pentoxide was used as a denitration catalyst in Example 8.
  • the sample name of the denitration catalyst in Example 8 was “43 wt % V 2 O 5 /TiO 2 ”.
  • the denitration catalyst after firing that was obtained by the same method as in Comparative Example 2 and contained 80 wt % of vanadium pentoxide was used as a denitration catalyst in Example 9.
  • the sample name of the denitration catalyst in Example 9 was “80 wt % V 2 O 5 /TiO 2 ”.
  • the existing catalyst is a catalyst in which, for example, tungsten oxide (WO 3 ) (content: 10.72 wt %) and silica (SiO 2 ) (content: 6.25 wt %) are supported on titanium oxide (TiO 2 ) (content: 79.67 wt %) and which contains about 0.5% of vanadium.
  • Powder X-ray diffraction analysis was performed with a Rigaku smart lab using Cu-Ka.
  • FIG. 1 illustrates powder XRD patterns of Example 1 (V 2 O 5 _ 300), Example 2 (V 2 O 5 _ 400), Example 3 (V 2 O 5 _ SG_300), and Comparative Example 1 (V 2 O 5 _ 500).
  • FIG. 2 illustrates powder XRD patterns of Example 3 (V 2 O 5 _ SG _ 300), and Examples 4 to 9 and Comparative Examples 2 and 3 (xwt % V 2 O 5 /TiO 2 ).
  • V 2 O 5 supported When the amount of V 2 O 5 supported was increased to 20 wt %, peaks for V 2 O 5 were observed at 22.2° and 27.4°, and the V 2 O 5 peak intensity increased as the amount of V 2 O 5 supported was increased. On the other hand, the TiO 2 peak intensity tended to decrease.
  • the BET specific surface area was measured with a MicrotracBEL BELSORP-max. Pretreatment was performed in an Ar atmosphere at 200° C. for 2 hours, and then measurement was performed at 196° C.
  • Example1 (V 2 O 5— 300) 16.6
  • Example2 (V 2 O 5— 400) 13.5 Comparative Example1 (V 2 O 5— 500) 4.68
  • Example3 (V 2 O 5— SG_300) 62.9 Comparative Example2 (0.3 wt % V 2 O 5 /TiO 2 ) 62.8 Comparative Example3 (0.9 wt % V 2 O 5 /TiO 2 ) 59
  • Example4 (3.3 wt % V 2 O 5 /TiO 2 ) 55.4
  • Example5 (9 wt % V 2 O 5 /TiO 2 ) 54.6
  • Example6 (20 wt % V 2 O 5 /TiO 2 ) 48.3
  • Example7 (33 wt % V 2 O 5 /TiO 2 ) 41.2
  • Example8 (43 wt % V 2 O 5 /TiO 2 ) 49.4
  • Example9 (80 w
  • Table 1 shows BET specific surface areas of Example 1 (V 2 O 5 _ 500), Example 2 (V 2 O 5 _ 400), Comparative Example 1 (V 2 O 5 _ 500), Example 3 (V 2 O 5 _ SG _ 300), Comparative Examples 2 and 3 and Examples 4 to 9 (xwt % V 2 O 5 /TiO 2 catalyst), and Comparative Example 4 (existing catalyst).
  • the vanadium pentoxide catalysts obtained by thermally decomposing ammonium vanadate the BET specific surface area decreased with increasing the thermal decomposition temperature. That is, the vanadium pentoxide in Example 1 (V 2 O 5 _ 500) in which the thermal decomposition was performed at 300° C.
  • NO in represents a NO concentration at an inlet of a reaction tube
  • NO out represents a NO concentration at an outlet of the reaction tube
  • N 2out represents a N 2 concentration at the outlet of the reaction tube
  • NH 3in represents a NH 3 concentration at the inlet of the reaction tube
  • NH 3out represents a NH 3 concentration at the outlet of the reaction tube.
  • NO ⁇ ⁇ CONVERSION ⁇ ⁇ RATIO NO in - NO out NO in ⁇ 100 [ Formula . ⁇ 1 ]
  • FIG. 3 illustrates the NH 3 -SCR activity of the vanadium pentoxide catalysts.
  • the NO conversion ratio increased as the thermal decomposition temperature was decreased.
  • the highest activity was exhibited in Example 1 (V 2 O 5 _ 300° C.) in which the catalyst was obtained at a thermal decomposition temperature of 300° C.
  • a NO conversion ratio of 80% or more was achieved when any of the catalysts in Example 1 (V 2 O 5 _ 300° C.), Example 2 (V 2 O 5 _ 400° C.), and Example 3 (V 2 O 5 _ SG_300° C.) was used.
  • the NO conversion ratio was higher in any of Examples than in Comparative Example 1 and Comparative Example 4.
  • the specific surface area of the vanadium pentoxide increases as the thermal decomposition temperature is decreased. Therefore, it is believed that the low-temperature NH 3 -SCR activity that uses a bulk vanadium pentoxide catalyst is attributable to the BET specific surface area.
  • the vanadium pentoxide was produced through a sol-gel process that uses oxalic acid in order to increase the BET specific surface area in Example 3.
  • the BET specific surface area of the vanadium pentoxide produced through this process is 62.9 m 2 g ⁇ 1 as shown in Table 1, which is about four times larger than the BET specific surface areas of the vanadium pentoxides produced through a thermal decomposition process.
  • the NO conversion ratio in Example 3 (V 2 O 5 _ SG_300° C.) was increased by 80% to 200% at 100° C. to 150° C. compared with the vanadium pentoxides produced through a thermal decomposition process.
  • FIG. 4 illustrates, as examples, the N 2 selectivities in Example 1 (V 2 O 5 _ 300° C.) and Comparative Example 1 (V 2 O 5 _ 500° C.).
  • FIG. 5 illustrates the measurement results.
  • FIG. 5( a ) illustrates the NO conversion ratio at a reaction temperature of 120° C.
  • FIG. 5( b ) illustrates the NO conversion ratio at a reaction temperature of 100° C.
  • the 80% NO detoxification was about 15 Lh ⁇ 1 g cat ⁇ 1 at 120° C. and about 11 Lh ⁇ 1 g cat ⁇ 1 at 100° C.
  • the N 2 selectivity was almost 100%.
  • FIG. 6 illustrates a change in the NO conversion ratio over time in the experiment.
  • the NO conversion ratio decreased from 64% to 50%.
  • the addition of H 2 O did not change the N 2 selectivity.
  • the N 2 selectivity was 100%.
  • the NO conversion ratio increased to 67%.
  • FIG. 7 illustrates the experimental results. No change occurred to the catalytic activity of NO. After the completion of the temperature increase to 150° C., the SO 2 concentration did not decrease though H 2 O and O 2 were constantly present. Consequently, SO 2 did not react. Accordingly, the denitration catalysts in Examples were found to have S resistance.
  • FIG. 8 illustrates the relationship between the amount of vanadium pentoxide supported and the NO conversion ratio at each reaction temperature.
  • FIG. 8( a ) illustrates the relationship between the amount of vanadium pentoxide supported and the NO conversion ratio at a reaction temperature of 120° C.
  • FIG. 8( b ) illustrates the relationship between the amount of vanadium pentoxide supported and the NO conversion ratio at a reaction temperature of 150° C.
  • FIG. 8( c ) illustrates the relationship at a reaction temperature of 100° C.
  • the catalyst in which the amount of vanadium pentoxide supported is 100 wt % is the denitration catalyst V 2 O 5 _ SG _ 300 produced in Example 3.
  • the points plotted using a square indicate a NO conversion ratio of the existing catalyst in Comparative Example 4. All the graphs showed that, on the whole, the NO conversion ratio increased as the amount of vanadium pentoxide supported was increased. Herein, all the graphs showed that the catalyst in which the amount of vanadium pentoxide supported was 3.3 wt % had a higher NO conversion ratio than the catalyst in which the amount of vanadium pentoxide supported was 9.0 wt %. Specifically, as illustrated in FIG. 8( a ) , in the NH 3 -SCR reaction at a reaction temperature of 120° C., the NO conversion ratio reached 80% when the amount of vanadium pentoxide supported was increased to 80 wt %. As illustrated in FIG.
  • FIG. 9( a ) illustrates the relationship between the BET specific surface area and the NO conversion ratio of the denitration catalysts in which vanadium pentoxide was supported on titanium oxide.
  • the BET specific surface area decreased, but the activity increased on the whole.
  • FIG. 9( b ) illustrates the relationship between the BET specific surface area and the NO conversion ratio of both the denitration catalysts in which vanadium pentoxide was supported on titanium oxide and the denitration catalysts in which vanadium pentoxide was not supported on titanium oxide. In the catalysts in which vanadium pentoxide was not supported on titanium oxide, the activity increased with increasing the BET specific surface area.
  • Example 3 of the above-described “1.1 Examples and Comparative Examples”, ammonium vanadate was dissolved in an oxalic acid solution such that the molar ratio of vanadium and oxalic acid was 1:3, then water was evaporated, drying was performed, and the resulting dried powder was fired. Thus, a denitration catalyst was produced.
  • the denitration catalysts of Examples 10 to 14 the molar ratios of vanadium and oxalic acid were set to 1:1, 1:2, 1:3, 1:4, and 1:5, respectively.
  • sample names were given as “V 2 O 5 SG_1:1” (Example 10), “V 2 O 5 _ SG_1:2” (Example 11), “V 2 O 5 _ SG_1:3” (Example 12), “V 2 O 5 _ SG_1:4” (Example 13), and “V 2 O 5 _ SG_1:5” (Example 14).
  • V 2 O 5 _ SG _ 300 in “Example 3” of “1.1 Examples and Comparative Examples” and “V 2 O 5 _ SG_1:3” in Example 12 were substantially the same, but the sample name “V 2 O 5 _ SG_1:3” in “Example 12” was used for the sake of convenience of description.
  • a surfactant may be added to the oxalic acid solution.
  • surfactant examples include anionic surfactants such as hexadecyltrimethylammonium bromide (CTAB), sodium lauryl sulfate (SDS), and hexadecylamine; cationic surfactants; amphoteric surfactants; and nonionic surfactants.
  • anionic surfactants such as hexadecyltrimethylammonium bromide (CTAB), sodium lauryl sulfate (SDS), and hexadecylamine
  • cationic surfactants such as hexadecyltrimethylammonium bromide (CTAB), sodium lauryl sulfate (SDS), and hexadecylamine
  • cationic surfactants such as hexadecyltrimethylammonium bromide (CTAB), sodium lauryl sulfate (SDS), and hexadecylamine
  • cationic surfactants such as hexadecy
  • FIG. 10 illustrates powder XRD patterns of Examples 10 to (V 2 O 5 _ SG).
  • vanadium pentoxides Examples 10, 11, and 14
  • examples having vanadium:oxalic acid ratios of 1:1, 1:2, and 1:5 only peaks for orthorhombic V 2 O 5 were detected.
  • vanadium pentoxides Examples 12 and 13
  • an unidentified peak was detected at 11° in addition to the peaks for orthorhombic V 2 O 5 .
  • the peak has not been identified yet.
  • the BET specific surface area was measured with a MicrotracBEL BELSORP-max. Pretreatment was performed in an Ar atmosphere at 200° C. for 2 hours, and then measurement was performed at 196° C.
  • Table 5 shows BET specific surface areas of Example 10 (V 2 O 5 _ SG_1:1), Example 11 (V 2 O 5 _ SG_1:2), Example 12 (V 2 O 5 _ SG_1:3), Example 13 (V 2 O 5 _ SG_1:4), and Example 14 (V 2 O 5 _ SG_1:5).
  • FIG. 11 illustrates the NH 3 -SCR activity of each V 2 O 5 _ SG catalyst.
  • FIG. 11( a ) illustrates the NO conversion ratio plotted against reaction temperature in the NH 3 -SCR reaction that uses each catalyst.
  • FIG. 11( b ) illustrates the relationship between the vanadium:oxalic acid ratio and the NO conversion ratio at a reaction temperature of 120° C.
  • the catalyst of Example 12 V 2 O 5 _ SG_1:3 having a vanadium:oxalic acid ratio of 1:3, the highest NO conversion ratio was achieved.
  • the NO conversion ratio decreased.
  • the NO conversion ratio in Example 13 (V 2 O 5 _ SG_1:4) was lower than that in Example 11 (V 2 O 5 _ SG_1:2) despite the fact that the specific surface area in Example 13 was larger than that in Example 11.
  • FIG. 12 illustrates the relationship between the BET specific surface area and the NO conversion ratio in Examples 10 to 13 (V 2 O 5 _ SG), Example 1 (V 2 O 5 _ 500), Example 2 (V 2 O 5 _ 400), and Comparative Example 1 (V 2 O 5 _ 500).
  • the point plotted using a square indicates the relationship between the BET specific surface area and the NO conversion ratio after the selective catalytic reduction reaction in Example 12 (V 2 O 5 _ SG_1:3).
  • the highest NO conversion ratio was achieved in the catalyst of Example 12 (V 2 O 5 _ SG_1:3) having a vanadium:oxalic acid ratio of 1:3.
  • the amount of acid sites on the surface of the catalyst can be estimated by NH 3 -TPD (TPD: temperature programed desorption).
  • TPD temperature programed desorption
  • 0.1 g of each of the catalysts in Example 1 (V 2 O 5 _ 500), Example 2 (V 2 O 5 _ 400), Comparative Example 1 (V 2 O 5 _ 500), Example 11 (V 2 O 5 _ SG_1:2), and Example 12 (V 2 O 5 _ SG_1:3) was pretreated at 300° C. for 1 hour while He (50 ml/min) was caused to flow.
  • the temperature was decreased to 100° C., and 5% ammonia/He (50 ml/min) was caused to flow for 30 minutes to adsorb ammonia.
  • the flow gas was changed to He (50 ml/min) and this state was kept for 30 minutes for stabilization.
  • the temperature was increased at 10° C./min and ammonia, which has a mass number of 16, was monitored with a mass spectrometer.
  • FIG. 13 is a graph obtained by plotting the amount of NH 3 desorbed as a function of the BET specific surface area of each catalyst. The graph in FIG. 13 showed that the amount of NH 3 desorbed increased substantially in proportion to the BET specific surface area of V 2 O 5 .
  • FIG. 13 shows that the amount of NH 3 desorbed increased substantially in proportion to the BET specific surface area of V 2 O 5 .
  • FIG. 14 is a graph obtained by plotting the NO conversion ratio as a function of the amount of NH 3 desorbed in each catalyst. The graph showed that the NO conversion ratio increased as the catalyst had a larger amount of NH 3 desorbed, that is, a larger amount of acid sites on the surface of the catalyst.
  • the denitration catalyst of the present invention that contains 3.3 wt % or more of vanadium oxide in terms of vanadium pentoxide and has a specific surface area of 10 m 2 /g or more exhibits a high denitration efficiency at a low temperature of 200° C. or lower in the selective catalytic reduction reaction that uses ammonia as a reducing agent. On the other hand, oxidation of SO 2 is not found.
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