WO2013073032A1 - 排ガス処理触媒、排ガス処理触媒の製造方法、及び排ガス処理触媒の再生方法 - Google Patents

排ガス処理触媒、排ガス処理触媒の製造方法、及び排ガス処理触媒の再生方法 Download PDF

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WO2013073032A1
WO2013073032A1 PCT/JP2011/076500 JP2011076500W WO2013073032A1 WO 2013073032 A1 WO2013073032 A1 WO 2013073032A1 JP 2011076500 W JP2011076500 W JP 2011076500W WO 2013073032 A1 WO2013073032 A1 WO 2013073032A1
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Prior art keywords
exhaust gas
gas treatment
catalyst
coating layer
treatment catalyst
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PCT/JP2011/076500
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English (en)
French (fr)
Japanese (ja)
Inventor
米村　将直
野地　勝己
正志 清澤
昌則 出本
享平 高倉
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Mitsubishi Heavy Industries Ltd
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Mitsubishi Heavy Industries Ltd
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Priority to IN2243CHN2014 priority Critical patent/IN2014CN02243A/en
Priority to CA2848367A priority patent/CA2848367C/en
Priority to EP11875762.4A priority patent/EP2781252A4/en
Priority to JP2013544058A priority patent/JP5769814B2/ja
Priority to PCT/JP2011/076500 priority patent/WO2013073032A1/ja
Priority to US14/347,775 priority patent/US9249706B2/en
Priority to CN201180073708.4A priority patent/CN103826727B/zh
Publication of WO2013073032A1 publication Critical patent/WO2013073032A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
    • F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
    • F01N3/18—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control
    • 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
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8625—Nitrogen oxides
    • B01D53/8628—Processes characterised by a specific catalyst
    • 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
    • B01D53/96—Regeneration, reactivation or recycling of reactants
    • 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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/053—Sulfates
    • 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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/20—Carbon compounds
    • B01J27/232—Carbonates
    • 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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/28—Regeneration or reactivation
    • B01J27/30—Regeneration or reactivation of catalysts comprising compounds of sulfur, selenium or tellurium
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0215—Coating
    • 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
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
    • B01J38/485—Impregnating or reimpregnating with, or deposition of metal compounds or catalytically active elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/40—Alkaline earth metal or magnesium compounds
    • B01D2251/404—Alkaline earth metal or magnesium compounds of calcium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/204—Alkaline earth metals
    • B01D2255/2045—Calcium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20707—Titanium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20723—Vanadium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20776—Tungsten
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/30—Silica
    • 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
    • B01J2235/00—Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties
    • B01J2235/15—X-ray diffraction
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/19—Catalysts containing parts with different compositions
    • 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
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
    • B01J38/60—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using acids

Definitions

  • the present invention relates to an exhaust gas treatment catalyst, in particular, an exhaust gas treatment catalyst for removing nitrogen oxide from exhaust gas discharged from a combustion apparatus such as a high-concentration sulfur-containing fuel-fired boiler, a method for producing an exhaust gas treatment catalyst, and an exhaust gas treatment catalyst Relates to the playback method.
  • ammonia As a method for removing nitrogen oxides (NOx) in combustion exhaust gas from a combustion apparatus such as a boiler, ammonia (NH 3 ) is used as a reducing agent in the presence of a nitrogen oxide removal catalyst (hereinafter referred to as “denitration catalyst”).
  • a nitrogen oxide removal catalyst hereinafter referred to as “denitration catalyst”.
  • the vanadium is an active component of a denitration catalyst.
  • it is a substance that promotes the SO 2 oxidation reaction as a side reaction. Due to the deposited vanadium, in the actual machine, the SO 2 oxidation reaction rate increased with time, and the corrosive SO 3 discharged to the downstream flow was further increased.
  • a VOSO 4 film is deposited on the surface of the catalyst, resulting in a decrease in the denitration performance of the denitration catalyst by suppressing gas diffusion into the denitration catalyst.
  • Patent Document 1 Japanese Patent No. 3224708
  • Patent Document 2 Japanese Patent No. 4436124
  • the present invention has been made in view of the above circumstances, and it is possible to easily remove the deposited VOSO 4 and restore the denitration performance while effectively suppressing the penetration of the VOSO 4 into the denitration catalyst. It is an object of the present invention to provide an exhaust gas treatment catalyst, a method for producing the exhaust gas treatment catalyst, and a method for regenerating such an exhaust gas treatment catalyst.
  • an exhaust gas treatment catalyst comprises a coating layer containing at least one selected from the group consisting of alkali metal carbonates and alkaline earth metal carbonates on the surface of a denitration catalyst.
  • the present invention is a method for producing an exhaust gas treatment catalyst, the production method comprising at least one selected from the group consisting of alkali metal carbonates and alkaline earth metal carbonates.
  • the present invention in yet another aspect, is a method for regenerating an exhaust gas treatment catalyst.
  • the surface of the denitration catalyst is formed of a group consisting of an alkali metal carbonate and an alkaline earth metal carbonate.
  • Only the above-mentioned coating layer of the denitration catalyst in which VOSO 4 is deposited on the coating layer containing at least one selected from the above-mentioned layer is removed using an acid.
  • the covering layer is removed using an acid, and after the removal of the covering layer, selected from the group consisting of an alkali metal carbonate and an alkaline earth metal carbonate.
  • a coating layer containing at least one of the above is provided again.
  • alkaline earth metal carbonate that can be employed in the coating layer
  • calcium carbonate is suitable.
  • calcium carbonate is suitable as the alkaline earth metal carbonate that can be employed for the coating layer to be provided again.
  • acid hydrochloric acid, nitric acid, and sulfuric acid can be used, and hydrochloric acid is most preferable.
  • the present invention while effectively suppressing the VOSO 4 penetrates into the interior of the denitration catalyst, the VOSO 4 deposited with easily removed and to be able to recover the denitration performance exhaust gas treatment catalyst, An exhaust gas treatment catalyst manufacturing method and an exhaust gas treatment catalyst regeneration method are provided.
  • FIG. 1 is a conceptual diagram schematically showing a cross-sectional structure of an exhaust gas treatment catalyst according to the present invention.
  • FIG. 2 is a flowchart showing a flow of a regeneration test of the exhaust gas treatment catalyst according to the present invention.
  • FIG. 3 is a graph showing a surface X-ray diffraction chart after the catalyst B according to the embodiment of the present invention is exposed to exhaust gas.
  • FIG. 4 is a graph showing a surface X-ray diffraction chart after the catalyst C according to the comparative example of the present invention is exposed to exhaust gas.
  • FIG. 5 is a graph showing a surface X-ray diffraction chart after the catalyst B according to the embodiment of the present invention is exposed to exhaust gas and then washed with water.
  • FIG. 6 is a graph showing a surface X-ray diffraction chart after the catalyst B according to the embodiment of the present invention is exposed to exhaust gas and then washed with an HCl solution.
  • an exhaust gas treatment catalyst an exhaust gas treatment catalyst manufacturing method, and an exhaust gas treatment catalyst regeneration method according to the present invention will be described.
  • a coating layer containing at least one selected from the group consisting of an alkali metal carbonate and an alkaline earth metal carbonate is provided on the surface of the denitration catalyst.
  • the exhaust gas denitration catalyst that is the subject of the present invention is not particularly limited.
  • a tungsten component including a vanadium-tungsten component supported on a support containing silica and / or titania is used.
  • tungsten component supported on a support containing silica and / or titania is used.
  • vanadium-molybdenum component supported, and other active components supported are various examples.
  • the shape of the denitration catalyst it is preferable to adopt a honeycomb shape.
  • a coating layer containing at least one selected from the group consisting of alkali metal carbonates and alkaline earth metal carbonates is provided on the surface of the above denitration catalyst. Manufactured by.
  • the coating layer is required to have a performance that effectively suppresses VOSO 4 from penetrating into the denitration catalyst. And it is necessary to provide the performance which can remove the deposited VOSO 4 easily.
  • a washcoat slurry containing at least one selected from the group consisting of alkali metal carbonates and alkaline earth metal carbonates is prepared.
  • the denitration catalyst is immersed in the prepared slurry for washcoat. After removing the denitration catalyst, excess slurry is removed, dried at 80 ° C. to 150 ° C., and calcined at 300 ° C. to 600 ° C., whereby an exhaust gas detreatment catalyst having a desired coating layer can be obtained. .
  • the coating amount of the coating layer is preferably 20 g to 100 g per 1 m 2 in terms of the surface area.
  • the exhaust gas treatment catalyst according to the present invention is intended for super heavy oils such as orimulsion, asphalt, vacuum residual oil (VOR), or coal containing high-concentration sulfur.
  • the present invention is applied to a treatment catalyst for exhaust gas discharged from a combustion apparatus such as a boiler that burns such high-concentration sulfur-containing fuel.
  • VOSO 4 is deposited on the coating layer of the denitration catalyst.
  • FIG. 1 is a sectional view showing an embodiment of an exhaust gas treatment catalyst according to the present invention.
  • the exhaust gas treatment catalyst 1 includes a denitration catalyst layer 2 shown as a particle layer, and a coating layer 3 on the surface thereof.
  • the molecules 4 of VOSO 4 are blocked by the coating layer 3 and the penetration into the denitration catalyst layer 2 is suppressed.
  • molecules to be treated such as NO, NH 3 and SO 2 can diffuse to the inside of the denitration catalyst layer 2.
  • VOSO 4 is deposited on the coating layer 3 after a long period of use.
  • the coating layer on which VOSO 4 is deposited is removed using an acid.
  • washing with an acid is suitable.
  • the acid used include hydrochloric acid, sulfuric acid, and nitric acid.
  • hydrochloric acid a concentration range of 0.01 N to 5 N is preferable.
  • sulfuric acid a concentration range of 0.01 N to 5 N is preferable.
  • the denitration catalyst from which the coating layer has been removed includes a coating containing at least one selected from the group consisting of alkali metal carbonates and alkaline earth metal carbonates.
  • the layer is to be provided again.
  • the method of providing the coating layer may be the same method as the removed coating layer.
  • Example 1 Production of honeycomb catalyst
  • reagent grade 1 manufactured by Hayashi Junyaku
  • calcium carbonate 1500 g was added to 4884 g of water, and thoroughly stirred, pulverized and adjusted in a ball mill to prepare a slurry for 13 wt% calcium carbonate washcoat.
  • a honeycomb substrate having a composition of 96 wt% TiO 2 —SiO 2 ⁇ 1 wt% V 2 O 5 -3 wt% WO 3 (lattice spacing: 7.0 mm, wall thickness: 1.0 mm) for the above wash coat
  • excess slurry was removed and dried at 150 ° C.
  • the coating amount was 25 g per 1 m 2 of the base material, and this coated product was designated as a prototype honeycomb catalyst B.
  • This slurry was charged into a 20 liter autoclave, 500 g of tetrapropylammonium bromide was further added, hydrothermal synthesis was performed at 160 ° C. for 72 hours, washed with water and dried, and further fired at 500 ° C. for 3 hours to obtain crystallinity.
  • Silicate F was obtained.
  • This crystalline silicate F was represented by the following composition formula in terms of the molar ratio of oxide (excluding crystallization water), and the crystal structure was shown in Table 1 by X-ray diffraction. 0.5Na 2 O ⁇ 0.5H 2 O ⁇ [0.8Al 2 O 3 ⁇ 0.2Fe 2 O 3 ⁇ 0.25CaO ] ⁇ 25SiO 2
  • the crystalline silicate F was stirred in a 4N NH 4 Cl aqueous solution at 40 ° C. for 3 hours for NH 4 ion exchange. After ion exchange, the substrate was washed and dried at 100 ° C. for 24 hours, and then calcined at 400 ° C. for 3 hours to obtain H-type crystalline silicate F. Using the obtained crystalline silicate F, 1500 g of this powder was added to 4884 g of water, and sufficiently stirred, pulverized and adjusted in a ball mill to prepare a slurry for washcoat of 13 wt% catalyst powder.
  • a honeycomb substrate having a composition of 96 wt% TiO 2 —SiO 2 ⁇ 1 wt% V 2 O 5 -3 wt% WO 3 (lattice spacing: 7.0 mm, wall thickness: 1.0 mm) for the above wash coat
  • excess slurry was removed and dried at 150 ° C.
  • the coating amount was 25 g per 1 m 2 of the base material, and this coated product was designated as a prototype honeycomb catalyst C.
  • Example 2 About the honeycomb catalysts B and C manufactured in Example 1 and Comparative Example 1, the high-sulfur oil-fired power plant A was exposed to actual gas for about 6000 hours, and then the prototype catalyst B and the prototype catalyst C were placed in 5 holes ⁇ 5 holes. The catalyst was cut into a length of 70 mm and subjected to a catalyst cleaning test using water, 1N-HCl (1N-hydrochloric acid) as a cleaning solution.
  • FIG. 1 shows a cleaning flow of the catalyst.
  • washing was performed at a washing liquid / catalyst volume ratio of 3.0, a temperature of 40 ° C. (when using water), and 60 ° C. (when using an acid solution) for 4 hours (step 102). ). Then, it was dried at a temperature of 100 ° C. for 8 hours or more (step 103). Thereafter, diffraction analysis was performed on the catalyst surface visually or by X-ray (step 104).
  • Prototype catalyst C is a so-called metallosilicate coating layer, and VOSO 4 remained even after washing.
  • the exhaust gas treatment catalyst and the regeneration method of the exhaust gas treatment catalyst according to the present invention are intended for super heavy oil such as orimarsion, asphalt, vacuum residual oil (VOR), or coal containing high-concentration sulfur. It is suitable for the treatment of exhaust gas discharged from a combustion apparatus such as a boiler that burns such high-concentration sulfur-containing fuel.
  • super heavy oil such as orimarsion, asphalt, vacuum residual oil (VOR), or coal containing high-concentration sulfur.

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  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Environmental & Geological Engineering (AREA)
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PCT/JP2011/076500 2011-11-17 2011-11-17 排ガス処理触媒、排ガス処理触媒の製造方法、及び排ガス処理触媒の再生方法 Ceased WO2013073032A1 (ja)

Priority Applications (7)

Application Number Priority Date Filing Date Title
IN2243CHN2014 IN2014CN02243A (https=) 2011-11-17 2011-11-17
CA2848367A CA2848367C (en) 2011-11-17 2011-11-17 Exhaust gas treatment catalyst, method for producing exhaust gas treatment catalyst, and method for regenerating exhaust gas treatment catalyst
EP11875762.4A EP2781252A4 (en) 2011-11-17 2011-11-17 EXHAUST TREATMENT CATALYST, PROCESS FOR PREPARING THE EXHAUST TREATMENT CATALYST AND METHOD FOR REGENERATING THE EXHAUST TREATMENT CATALYST
JP2013544058A JP5769814B2 (ja) 2011-11-17 2011-11-17 排ガス処理触媒、排ガス処理触媒の製造方法、及び排ガス処理触媒の再生方法
PCT/JP2011/076500 WO2013073032A1 (ja) 2011-11-17 2011-11-17 排ガス処理触媒、排ガス処理触媒の製造方法、及び排ガス処理触媒の再生方法
US14/347,775 US9249706B2 (en) 2011-11-17 2011-11-17 Method for regenerating exhaust gas treatment catalyst
CN201180073708.4A CN103826727B (zh) 2011-11-17 2011-11-17 废气处理催化剂、制造废气处理催化剂的方法和用于再生废气处理催化剂的方法

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PCT/JP2011/076500 WO2013073032A1 (ja) 2011-11-17 2011-11-17 排ガス処理触媒、排ガス処理触媒の製造方法、及び排ガス処理触媒の再生方法

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US (1) US9249706B2 (https=)
EP (1) EP2781252A4 (https=)
JP (1) JP5769814B2 (https=)
CN (1) CN103826727B (https=)
CA (1) CA2848367C (https=)
IN (1) IN2014CN02243A (https=)
WO (1) WO2013073032A1 (https=)

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BR112016001465A2 (pt) * 2013-07-26 2017-08-29 Johnson Matthey Plc Artigo catalisador para tratar um gás de escape, e, métodos para tratar um gás de escape e para regenerar um artigo catalítico
CN108472644A (zh) 2016-01-22 2018-08-31 康明斯排放处理公司 用于再制造选择性催化还原系统的系统和方法
CN108144656A (zh) * 2017-11-23 2018-06-12 浙江天蓝环保技术股份有限公司 一种用于中毒脱硝催化剂的再生液及再生方法

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EP2781252A1 (en) 2014-09-24
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JP5769814B2 (ja) 2015-08-26
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