WO2020230638A1 - Procédé de commande de système - Google Patents

Procédé de commande de système Download PDF

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Publication number
WO2020230638A1
WO2020230638A1 PCT/JP2020/018210 JP2020018210W WO2020230638A1 WO 2020230638 A1 WO2020230638 A1 WO 2020230638A1 JP 2020018210 W JP2020018210 W JP 2020018210W WO 2020230638 A1 WO2020230638 A1 WO 2020230638A1
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WIPO (PCT)
Prior art keywords
ammonia
exhaust gas
nox
catalyst
zeolite
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PCT/JP2020/018210
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English (en)
Japanese (ja)
Inventor
北村　武昭
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株式会社 Ａｃｒ
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Publication of WO2020230638A1 publication Critical patent/WO2020230638A1/fr

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    • 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
    • B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • 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
    • B01J29/00—Catalysts comprising molecular sieves
    • B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
    • B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
    • B01J29/76—Iron group metals or copper
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
    • C01B39/04—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
    • 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
    • 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
    • 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 NOx purification system control of an exhaust gas aftertreatment device corresponding to automobile load driving.
  • One embodiment of the present invention relates to a copper zeolite catalyst and its control in an exhaust gas system designed to reduce nitrogen oxides (NOx).
  • certain embodiments relate to controlling the supply of urea and ammonia as NOx selective reducing agents.
  • the NOx purification catalyst for diesel vehicles uses ammonia obtained by spraying urea water with an exhaust gas aftertreatment device and hydrolyzing the urea water as a reducing agent (selective catalytic reduction, generally referred to as an SCR catalyst).
  • SCR catalyst selective catalytic reduction
  • synthetic zeolite is known because it has a high ability to adsorb ammonia at the solid acid point.
  • reaction formula (1) In the exhaust gas aftertreatment device, several chemical reactions occur, all of which reduce NOx to nitrogen.
  • the dominant reaction is represented by the reaction formula (1) in which NO and NH 3 proceed in equal amounts.
  • Patent Document 1 The CuCHA catalyst represented by Patent Document 1 is SSZ-13 in which copper is ion-exchanged.
  • Patent Document 2 As an SCR catalyst other than the above, it is disclosed that an iron and / or copper ion-exchange zeolite of SAPO-34 having a CHA-type crystal structure containing phosphor oxide, alumina and silica as main components is used (Patent Document). 2).
  • the catalyst represented by Patent Document 2 is SAPO-34 in which copper is ion-exchanged.
  • the CuCHA catalyst has excellent low temperature activity from an exhaust gas temperature of 200 ° C. to 350 ° C. and durability activity after aging in hot water.
  • the NOx purification rate decreases as the exhaust gas temperature rises from 350 ° C. to 500 ° C.
  • the temperature of the exhaust gas cooling system such as EGR of the internal combustion engine is adjusted so that the exhaust gas temperature at the inlet of the SCR catalyst is 500 ° C or less. Need to control.
  • the exhaust gas becomes 500 ° C or higher, but since the oxygen concentration is low and the atmosphere is reduced, NOx is reduced without spraying urea, so the SCR system is controlled at 500 ° C or lower. , Not limited to this.
  • the present invention is an SCR system control method capable of uniformly maintaining the NOx reduction purification of urea water at 93% or more from a low temperature of 200 ° C. to a high temperature of 500 ° C. at the exhaust gas temperature under a vehicle running load.
  • urea and / or ammonia are used to select NOx.
  • the catalyst is a zeolite containing copper, and the consumption of ammonia due to partial oxidation is equal to that of NOx in the exhaust gas. It is a system control method characterized in that the amount of ammonia is controlled and supplied.
  • the present invention is to control the amount of ammonia supplied by taking into account the amount of ammonia consumed by the reaction formulas (2) and (3) regardless of NOx purification. Shown in (Equation 1).
  • the catalyst carrier used in the present invention is not particularly limited, but a zeolite having a CHA type and / or AEI type and AFX type crystal structure is preferable because of the characteristics peculiar to the material having high durability due to hot water.
  • the catalyst metal is preferably copper from the viewpoint of low temperature activity, and the copper is preferably contained in an amount of 2.0% by mass to 5.0% by mass in terms of CuO.
  • the present invention is a known exhaust gas aftertreatment system used in a general vehicle as shown in FIG. 3, wherein the exhaust gas temperature of (Equation 1) uses the measured value of the temperature sensor (9) of the SCR catalyst inlet.
  • (Equation 1) catalyst upstream NOx volume concentration uses the measured value of (2) upstream NOx sensor at the engine outlet to control the system.
  • the constant C (Equation 1) of the present invention is an eigenvalue that differs depending on the acidity of various zeolites in the Cu zeolite catalyst.
  • the constant C in the exhaust gas temperature is determined by the model gas performance test shown in the embodiment of the present invention, the exhaust gas temperature is measured by the (9) temperature sensor at the inlet of the SCR catalyst, and the system of the present invention is controlled.
  • the constant C is the catalyst inlet concentration of NO, NH 3 , NO 2 , N 2 O and NO, NH 3 , NO, NH 3 , at each exhaust gas temperature. Obtain the concentrations of the catalyst outlets of NO 2 and N 2 O from the measured values.
  • ion-exchanged water and pseudo-boehmite (Pural SB) are added to a glass container while stirring, and the mixture is stirred at room temperature for 20 minutes. Then, adamantyltrimethylammonium hydroxide (TMadaOH) is slowly added with stirring, and the mixture is kept at room temperature for 1 hour. Then, colloidal silica (Ludox AS40) was added, and stirring was continued for 5 minutes, and the suspension had a pH of 8.4, and the following composition was prepared.
  • TMadaOH adamantyltrimethylammonium hydroxide
  • colloidal silica Lidox AS40
  • the obtained suspension was transferred to an autoclave with stirring (pressure sterilizer), sealed, heated at 150 ° C. for 72 hours while stirring at a speed of 50 rpm, and then slowly cooled to room temperature.
  • the gel composition obtained from the autoclave was taken out and the supernatant was set aside, and the pH of the supernatant was 10.6.
  • An equal volume of ion-exchanged water was added to the gel composition from which the supernatant had been removed, the mixture was shaken, and washing and solid-liquid separation were repeated with a centrifuge.
  • CHA type synthetic zeolite The obtained gel composition was transferred to a heat-resistant container, dried at 120 ° C. for 12 hours, and then the particle size was adjusted through a 20-mesh sieve net. Based on the results of X-ray diffraction analysis of the obtained synthetic zeolite, the relative intensities (I) and lattice plane spacing (d) of the main diffraction peaks were determined by the X-ray diffraction pattern of the International Society for Synthetic Zeolite. In light of the database and the PDF of the ICDD, it was identified as a zeolite consisting of CHA-type SSZ-13 having a maximum oxygen ring number of 8 and a three-dimensional structure.
  • a CuCHA powder catalyst was produced by mixing 100 g of the CHA-type SSZ-13 synthetic zeolite with NH 4 + -like CHA in 400 mL of a 1.0 M copper (II) nitrate solution. The pH was adjusted to 3.5 with acetic acid. Slurry was stirred for 1 hour at 80 ° C., it was subjected to ion exchange reaction between the NH 4 + form CHA and the copper ions. The resulting mixture was then filtered and washed with 800 mL of deionized water until the filtrate was clear and colorless. The washed sample was then dried to 90 ° C.
  • the obtained CuCHA product was baked at 700 ° C. for 2 hours.
  • the obtained CuCHA catalyst contained 2.8% by mass of CuO as measured by ICP analysis.
  • the obtained suspension was transferred to an autoclave with stirring (pressure sterilizer), sealed, heated at 170 ° C. for 72 hours while stirring at a speed of 50 rpm, and then slowly cooled to room temperature.
  • the gel composition obtained from the autoclave was taken out and the supernatant was set aside, and the pH of the supernatant was 10.2.
  • An equal volume of ion-exchanged water was added to the gel composition from which the supernatant had been removed, the mixture was shaken, and washing and solid-liquid separation were repeated with a centrifuge.
  • CHA type synthetic zeolite The obtained gel composition was transferred to a heat-resistant container, dried at 120 ° C. for 12 hours, and then the particle size was adjusted through a 20-mesh sieve net. From the results of X-ray diffraction analysis of the obtained synthetic zeolite, the relative intensity (I) and lattice plane spacing (d) of the main diffraction peaks were determined by the X-ray diffraction pattern of the International Society of Synthetic Zeolite. In light of the database and the PDF of the ICDD, it was identified as a zeolite consisting of CHA-type SAPO-34 having a maximum oxygen ring number of 8 and a three-dimensional structure.
  • the composition of the obtained CHA-type synthetic SAPO-34 zeolite was 44.50 wt% for P 2 O 5 , 9.60 wt% for SiO 2 , 45.90 wt% for Al 2 O 3 , and SiO 2
  • the mol ratio (SAR) of / Al 2 O 3 was 0.355.
  • a CuCHA powder catalyst was produced by mixing 100 g of the CHA-type SAPO-34 synthetic zeolite with NH 4 + -like CHA with 400 mL of a 1.0 M copper (II) nitrate solution. .. The pH was adjusted to 3.5 with acetic acid. Slurry was stirred for 1 hour at 80 ° C., it was subjected to ion exchange reaction between the NH 4 + form CHA and the copper ions. The resulting mixture was then filtered and washed with 800 mL of deionized water until the filtrate was clear and colorless. The washed sample was then dried to 90 ° C.
  • the obtained CuCHA product was baked at 700 ° C. for 2 hours.
  • the obtained CuCHA catalyst contained 2.8% by mass of CuO as measured by ICP analysis.
  • zeolite raw material ion-exchanged water is placed in a glass container, and a predetermined amount of 1N NaOH and N, N-diethyl-cis-2,6-dimethylpiperadinium cation hydroxide (DEDMPOH) are added to the glass container while stirring. Stir at room temperature for 20 minutes. Then, NH 4 + form Y-type zeolite and colloidal silica (Ludox AS40) with a predetermined amount was added, stirring was continued for 5 minutes, the suspension is at a pH of 9.2, were prepared following composition.
  • DEDMPOH N-diethyl-cis-2,6-dimethylpiperadinium cation hydroxide
  • the obtained suspension was transferred to an autoclave with stirring (pressure sterilizer), sealed, heated at 140 ° C. for 7 days while stirring at a speed of 50 rpm, and then slowly cooled to room temperature.
  • the gel composition obtained from the autoclave was taken out and the supernatant was set aside, and the pH of the supernatant was 11.3.
  • An equal volume of ion-exchanged water was added to the gel composition from which the supernatant had been removed, the mixture was shaken, and washing and solid-liquid separation were repeated with a centrifuge.
  • AEI type synthetic zeolite The obtained gel composition was transferred to a heat-resistant container, dried at 120 ° C. for 12 hours, and then the particle size was adjusted through a 20-mesh sieve net. From the results of X-ray diffraction analysis of the obtained synthetic zeolite, the relative intensity (I) and lattice plane spacing (d) of the main diffraction peaks were determined by the X-ray diffraction pattern of the International Society of Synthetic Zeolite. In light of the database and the PDF of the ICDD, it was identified as a zeolite consisting of AEI type SSZ-39 having a maximum oxygen ring number of 8 and a three-dimensional structure.
  • the obtained CuAEI product was baked at 700 ° C. for 2 hours.
  • the obtained CuAEI catalyst contained 2.8% by mass of CuO as measured by ICP analysis.
  • Reference Example 4 a CuAEI catalyst in which copper was ion-exchanged was produced in the same manner as in Reference Example 1 except that the synthetic zeolite of the catalyst carrier was replaced with AEI type SAPO-18 synthetic zeolite.
  • the obtained suspension was transferred to an autoclave with stirring (pressure sterilizer), sealed, heated at 215 ° C. for 120 hours while stirring at a speed of 50 rpm, and then slowly cooled to room temperature.
  • the gel composition obtained from the autoclave was taken out and the supernatant was set aside, and the pH of the supernatant was 9.2.
  • An equal volume of ion-exchanged water was added to the gel composition from which the supernatant had been removed, the mixture was shaken, and washing and solid-liquid separation were repeated with a centrifuge.
  • AEI type synthetic zeolite The obtained gel composition was transferred to a heat-resistant container, dried at 120 ° C. for 12 hours, and then the particle size was adjusted through a 20-mesh sieve net. From the results of X-ray diffraction analysis of the obtained synthetic zeolite, the relative intensity (I) and lattice plane spacing (d) of the main diffraction peaks were determined by the X-ray diffraction pattern of the International Society of Synthetic Zeolite. In light of the database and the PDF of the ICDD, it was identified as a zeolite consisting of AEI-type SAPO-18 having a maximum oxygen ring number of 8 and a three-dimensional structure.
  • the composition of the obtained AEI type SAPO-18 zeolite was 61.00 wt% for P 2 O 5 , 1.80 wt% for SiO 2 , and 37.20 wt% for Al 2 O 3 , and SiO 2 /.
  • the mol ratio (SAR) of Al 2 O 3 was 0.082.
  • the pH was adjusted to 3.5 with acetic acid.
  • Slurry was stirred for 1 hour at 80 ° C., it was subjected to ion exchange reaction between the NH 4 + form AEI and copper ions.
  • the resulting mixture was then filtered and washed with 800 mL of deionized water until the filtrate was clear and colorless.
  • the washed sample was then dried to 90 ° C.
  • the obtained CuAEI product was baked at 700 ° C. for 2 hours.
  • the obtained CuAEI catalyst contained 2.8% by mass of CuO as measured by ICP analysis.
  • the copper-containing SCR catalyst powders of Reference Examples 1 to 4 were prepared into a colloidal silica binder (solid content 20% by mass) and a slurry liquid, and deposited on a known cordierite honeycomb flow-through type substrate.
  • the slurry liquid was dispersed by a ball mill and deposited at 200 g / L per volume of the honeycomb base material. Then, it was dried at 80 ° C. and calcinated at 500 ° C., and an exhaust gas purification performance test using the system control of the present invention was performed.
  • Table 1 shows the relationship between the NOx exhaust gas concentration and the NH 3 supply control concentration in Examples 1 to 4 and Comparative Examples 1 to 4 as ANR (NH 3 / NOx).
  • Table 2 shows the results of NOx purification performance in Examples 1 to 4 and Comparative Examples 1 to 4.
  • Table 3 shows the results of the NH 3 slip (SCR catalyst downstream leakage) concentration in Examples 1 to 4 and Comparative Examples 1 to 4.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Inorganic Chemistry (AREA)
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  • General Engineering & Computer Science (AREA)
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  • Environmental & Geological Engineering (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)
  • Catalysts (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Exhaust Gas After Treatment (AREA)

Abstract

La présente invention concerne des systèmes de post-traitement de gaz d'échappement SCR, dans lesquels il existe un problème selon lequel, quelle que soit la réduction sélective de NOx, la purification de NOx est réduite en raison de l'oxydation partielle d'ammoniac dans une plage de température élevée de gaz d'échappement de 350 à 500 °C. Le procédé de commande de système selon la présente invention est caractérisé par les étapes consistant à réguler, dans un système de réduction catalytique sélective purifiant les NOx en utilisant de l'urée et/ ou de l'ammoniac, la quantité d'ammoniac égale à une quantité molaire de NOx dans le gaz d'échappement et à fournir l'ammoniac, en tenant compte de la quantité de consommation due à l'oxydation partielle de l'ammoniac, une zéolite contenant du cuivre étant utilisée en tant que catalyseur.
PCT/JP2020/018210 2019-05-15 2020-04-30 Procédé de commande de système WO2020230638A1 (fr)

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JP2019092172A JP2020186690A (ja) 2019-05-15 2019-05-15 システム制御方法
JP2019-092172 2019-05-15

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009517210A (ja) * 2005-11-30 2009-04-30 キャタピラー インコーポレイテッド 選択的触媒還元用の多段システム
JP2009293605A (ja) * 2008-06-09 2009-12-17 Hino Motors Ltd 排気処理装置の制御装置
JP2015196115A (ja) * 2014-03-31 2015-11-09 株式会社キャタラー Ｓｃｒ用触媒及び排ガス浄化触媒システム
JP2017524520A (ja) * 2014-08-13 2017-08-31 ユミコア・アクチエンゲゼルシャフト・ウント・コムパニー・コマンディットゲゼルシャフトＵｍｉｃｏｒｅ ＡＧ ＆ Ｃｏ．ＫＧ 窒素酸化物を低減するための触媒系

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009517210A (ja) * 2005-11-30 2009-04-30 キャタピラー インコーポレイテッド 選択的触媒還元用の多段システム
JP2009293605A (ja) * 2008-06-09 2009-12-17 Hino Motors Ltd 排気処理装置の制御装置
JP2015196115A (ja) * 2014-03-31 2015-11-09 株式会社キャタラー Ｓｃｒ用触媒及び排ガス浄化触媒システム
JP2017524520A (ja) * 2014-08-13 2017-08-31 ユミコア・アクチエンゲゼルシャフト・ウント・コムパニー・コマンディットゲゼルシャフトＵｍｉｃｏｒｅ ＡＧ ＆ Ｃｏ．ＫＧ 窒素酸化物を低減するための触媒系

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