CN113731450B - Doped cesium-vanadium alkali metal catalyst - Google Patents
Doped cesium-vanadium alkali metal catalyst Download PDFInfo
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- CN113731450B CN113731450B CN202111109341.9A CN202111109341A CN113731450B CN 113731450 B CN113731450 B CN 113731450B CN 202111109341 A CN202111109341 A CN 202111109341A CN 113731450 B CN113731450 B CN 113731450B
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- 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
- B01J27/055—Sulfates with alkali metals, copper, gold or silver
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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
- F01N3/24—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 constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
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- 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
Abstract
The invention provides two doped cesium-vanadium alkali metal catalysts, wherein the promoting layer alkali metal compound of the first doped cesium-vanadium alkali metal catalyst is Cs 2 SO 4 Also comprises active ingredient Cs 2 V 4 O 11 Base coating gamma-Al 2 O 3 ，Cs 2 V 4 O 11 The mass fraction of the catalyst is 18-26wt% and Cs 2 SO 4 The mass fraction of the catalyst is 4-12wt%, and gamma-Al 2 O 3 The mass fraction of the catalyst is 62-78 wt%, and the catalyst is called 7GB2; the alkali metal compound of the second doped cesium-vanadium alkali metal catalyst promoting layer is Cs 2 SO 4 Also comprises an active ingredient CsVO 3 Base coat CePO 4 ，CsVO 3 The mass fraction of the catalyst is 20-28wt% and Cs 2 SO 4 The mass fraction of the CePO is 6-14wt% 4 The mass fraction of the cesium-vanadium alkali metal catalyst is 58-74 wt%, and the cesium-vanadium alkali metal catalyst is called 8G. The cesium-vanadium alkali metal catalyst with lower PM light-off temperature can be obtained by doping any one impurity in Fe/Sb/P/Co/Ge into the cesium-vanadium alkali metal catalyst.
Description
Technical Field
The invention relates to a catalyst and the preparation field thereof. In particular to a doped cesium-vanadium alkali metal catalyst.
Background
The particles in the tail gas of the diesel engine mainly comprise carbon and organic substances adsorbed on the carbon, the weight is lighter, the particles can be suspended in the air for a long time, the suspension time is longer when the particle size is smaller, the influence on the environment is caused for a long time, and the particles contain cancerogenic substances, so that the influence on the health of a human body is great. In 7 months of the present year, china will comprehensively implement the national six-emission standard of heavy-duty diesel vehicles, marks that the national automobile standard comprehensively enters the national six-age, and has more severe emission standard, so that the diesel vehicle tail gas post-treatment technology faces more challenges and opportunities.
The diesel particulate filter (DPF: diesel Particulate Matter) in the exhaust gas treatment system is used for capturing carbon and other granular substances (PM: particulate Matter) in the exhaust gas of the diesel engine, preventing the carbon and other granular substances from being discharged into the atmosphere, and as the granular substances are deposited in the DPF, the exhaust back pressure is increased, the exhaust gas temperature needs to be periodically increased to burn the granular substances, and the temperature needs to reach the normal burning temperature of the PM above 600 ℃, so that the mode is called active regeneration. DPFs are typically coated with a catalyst that catalyzes the combustion of the particulate matter, which is known as passive regeneration, when the normal combustion temperature is not reached. The development of a high performance PM combustion catalyst is critical to solving the soot pollution problem.
The soot combustion catalyst generally comprises three types of noble metal base, oxide base and alkali metal base, and the existing DPF catalyst basically comprises platinum noble metals such as platinum (Pt), palladium (Pd), rhodium (Rh) and the like, and has good PM combustion performance and durability. However, platinum group metals are expensive, and in order to reduce the price of the catalyst, researchers in various countries have been conducting researches on saving platinum groups and replacing platinum groups in the automobile exhaust gas purifying catalyst. ( Reference is made to non-patent document 1: feather Tian Zhengming et al, "reduction in the amount of platinum group metal used in exhaust gas purifying catalysts and substitution technique", automobile technology vol.63, pages 42-47, 2009 )
Patent CN 111804294A relates to a preparation method of a stable potassium-based carbon smoke combustion catalyst and an obtained product, and the invention prepares the stable potassium-based carbon smoke combustion catalyst (K-HWO) by immersing hexagonal phase tungsten trioxide (HWO) with a pore canal structure into potassium (K) salt solution. Compared with cesium-vanadium alkali metal catalysts, the catalyst has poor thermal stability and limited effect of reducing the ignition temperature of carbon smoke.
The patent CN 106807385A relates to a nest-shaped carbon smoke combustion catalyst, which contains transition metal elements Cu+Ce+Zr and has poor effect of reducing the ignition temperature of carbon smoke.
Japanese patent JP 3821357B2 reports a type of metal nitrate-fused salt-type catalyst supported on an alkaline carrier, which is fused into a liquid phase near the temperature of reaction with PM, so that the contact surface with PM is increased, PM is removed by more efficient combustion, and PM is catalyzed to burn at a lower temperature if the melting point of the fused salt is lower. The molten salt catalyst may evaporate due to the low melting point, resulting in poor durability of the catalyst in this patent compared to the DPF noble metal catalyst. The molten salt type catalyst of the present invention of CN103501900a uses a 1 st complex metal oxide (CsV oxide) of cesium and vanadium and a sulfate containing cesium and an alkaline earth metal as catalyst components, and provides a molten salt type exhaust gas purifying catalyst with improved durability, but there is room for improvement in reducing the PM light-off temperature Tmax compared with a DPF catalyst to which a platinum noble metal is added.
Disclosure of Invention
The object of the present invention is to reduce the light-off temperature of PM while ensuring high durability of the catalyst by providing a CDPF catalyst that does not contain noble metals.
To achieve the above object, the present invention provides a first doped cesium-vanadium alkali metal catalyst, wherein the promoting layer alkali metal complex is Cs 2 SO 4 Also comprises active ingredient Cs 2 V 4 O 11 Base coating gamma-Al 2 O 3 ，Cs 2 V 4 O 11 The mass fraction of the catalyst is 18-26wt% and Cs 2 SO 4 The mass fraction of the catalyst is 4-12wt%, and gamma-Al 2 O 3 The mass fraction of the catalyst is 62-78 wt%, and the catalyst is called 7GB2.
Further, also comprises impurity source Fe 2 O 3 、Sb 2 O 5 Or NH 4 H 2 PO 4 One of the impurity sources is selected to be mixed with the raw materials according to a certain proportion, and then the mixture is burned for 3 hours at a certain temperature, wherein the Fe doped with the raw materials is recorded as 7GB2-1, the Sb doped with the raw materials is 7GB2-2, and the P doped with the raw materials is 7GB2-3.
Providing a second doped cesium-vanadium alkali metal catalyst, wherein the promoting layer alkali metal complex is Cs 2 SO 4 The method is characterized in that: also comprises an active ingredient CsVO 3 Base coat CePO 4 ，CsVO 3 The mass fraction of the catalyst is 20-28 wt%, cs 2 SO 4 The mass fraction of the CePO is 6-14wt% 4 The mass fraction of the cesium-vanadium alkali metal catalyst is 58-74 wt%, and the cesium-vanadium alkali metal catalyst is called 8G.
Further, the alloy also comprises any one of impurity sources Co and Ge, wherein Co is doped with 8G-1, and Ge is doped with 8G-2.
According to the invention, by doping any one impurity in Fe/Sb/P/Co/Ge into the cesium-vanadium alkali metal catalyst, the cesium-vanadium alkali metal catalyst with lower PM ignition temperature can be obtained, wherein 7GB2-2 doped with Sb is reduced in Tmax and improved in thermal stability, and the improved catalyst is more suitable for being used as a DPF catalyst. Tmax can be reduced by at most 25 ℃ for 7GB2 and at most 17 ℃ for 8G by doping.
Drawings
FIG. 1 is an XRD pattern of the thermal stability of a cesium vanadium alkali metal catalyst 7GB2;
FIG. 2 is an XRD pattern of 7GB2 of Fe-doped for peak transfer confirmation;
fig. 3 XRD pattern of Sb doped 7GB2 for confirming peak transfer;
FIG. 4 is an XRD pattern showing the effect of firing temperature on 7GB2 after doping with Sb;
fig. 5 XRD pattern of 7GB2 of doped P for confirming peak transfer;
FIG. 6 is a graph of the highest temperature versus various catalyst examples.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings and examples.
Adding an impurity source containing Fe/Sb/P into a manufacturing raw material of 7GB2, wherein the manufacturing raw material of 7GB2 comprises the following components: cs (cells) 2 SO 4 ，VOSO 4 TH100/150; the impurity sources are as follows: fe (Fe) 2 O 3 、Sb 2 O 5 、 NH 4 H 2 PO 4 One of the impurity sources is selected to be mixed with the raw materials according to a certain proportion, and then the mixture is burned for 3 hours at a certain temperature, wherein the impurity element is M, and the ratio of the impurity element to the V element substance is as follows: 0.5,1.0,2.0, V is elemental vanadium. Cesium vanadium alkali metal catalysts doped with any one of the impurities Fe, sb, P are obtained with a lower Tmax.
Co and Ge-containing impurities are added into the raw materials for manufacturing 8G, so that the ignition temperature Tmax of PM combustion catalyzed by 8G is reduced, and the catalyst has higher catalytic activity. The ratio of the amounts of impurity element to V element substance is preferably: 0.5,1.0,2.0, V is elemental vanadium.
Example 1
The preparation raw material of the cesium-vanadium alkali metal catalyst 7GB2 comprises: cs (cells) 2 SO 4 ，VOSO 4 TH100/150, sintered at 800 ℃,1000 ℃,1100 ℃ for three hours, respectively, to obtain the following components: cs (cells) 2 SO 4 ，Cs 2 V 4 O 11 ，γ-Al 2 O 3 And (3) carrying out XRD experiments on the sintered product to analyze the thermal stability of the cesium-vanadium alkali metal catalyst 7GB2.
As shown in FIG. 1, the 7GB2 catalyst produces a catalyst active Cs at 800 ℃ 2 V 4 O 11 While the XRD pattern of the sintered corresponding product at 1000℃and 1100℃shows a new peak in comparison with the XRD pattern at 800℃at which the active substance Cs is present 2 V 4 O 11 Conversion to CsVO 3 ，γ-Al 2 O 3 Conversion to alpha-Al 2 O 3 . 7GB2 at 800 ℃ also has a stable catalyst component, and the components of the 7GB2 catalyst at 1000 ℃ and 1100 ℃ are: cs (cells) 2 V 4 O 11 And Al 2 O 3 The catalyst was unstable at these two temperatures, as indicated by the start of the conversion to other materials.
Example 2
In the embodiment of the cesium-vanadium alkali metal catalyst doped with Fe impurities, fe is 2 O 3 And Cs 2 SO 4 ，VOSO 4 The TH100/150 catalyst preparation raw materials are mixed, the ratio of Fe to V substances is 2.0, wherein V is vanadium element, and the samples are sintered for 3 hours at 800 ℃,1000 ℃ and 1100 ℃ respectively.
As shown in fig. 2, the graph in the XRD pattern of the catalyst sintered product doped with Fe impurities is compared with the XRD pattern of the undoped catalyst sintered product, and no peak transfer occurs, and the addition of Fe impurities does not affect the generation of 7GB2 catalyst active ingredient.
Example 3
In the embodiment of the cesium-vanadium alkali metal catalyst doped with Sb impurities, sb is adopted 2 O 3 And Cs 2 SO 4 ，VOSO 4 TH100/150 catalyst preparation originThe materials were mixed and the ratio of the amounts of Sb and V was 2.0, and the samples were sintered at 800℃and 1000℃and 1100℃for 3 hours, respectively.
As shown in fig. 3, the graph in the XRD pattern of the sintered catalyst product doped with Sb impurity is compared with the XRD pattern of the sintered catalyst product undoped, no peak transfer occurs, and the addition of Sb impurity does not affect the generation of 7GB2 catalyst active ingredient.
As shown in FIG. 4, sb was sintered at 800℃and 1000 ℃ 2 O 3 With Al 2 O 3 Reaction to AlSbO 4 The thermal stability of the 7GB2-2 catalyst is improved compared with that of the 7GB2 catalyst.
Example 4
In the embodiment of the cesium-vanadium alkali metal catalyst doped with P impurities of the invention, NH 4 H 2 PO 4 And Cs 2 SO 4 ，VOSO 4 The TH100/150 catalyst-making materials were mixed, the ratio of the amounts of P and V matters was 2.0, and the samples were sintered at 800℃and 1100℃for 3 hours, respectively.
As shown in fig. 5, the XRD peak of the calcined sample at 1100 ℃ slightly shifted from the XRD pattern of the sintered product of the catalyst doped with P impurity, which was not affected by the addition of P impurity below 1100 ℃, did not affect the formation of the 7GB2 catalyst active ingredient.
Example 5
As shown in fig. 6, after doping in 7GB2, the generation of active substances is not affected, and after adding three impurities, the ignition temperature of catalytic soot is reduced, compared with the original 7GB2, the doping M: the Tmax of 7GB2-1,7GB2-2,7GB2-3 with V=2.0 is reduced by 16 ℃,19 ℃ and 25 ℃ respectively, and the effect of reducing the Tmax of 7GB2-3 doped with Fe is better.
Example 6
As shown in FIG. 6, the Ge-doped alkali metal catalyst 8G is doped with Ge, and the active material in the 8G catalyst is CsVO 3 After the Ge impurity is doped and heat treated, the catalyst active substance becomes CsV 0.95 Ge 0.05 O 3 Or CsV 0.90 Ge 0.10 O 3 . Tmax for 8G was 509℃and CsV 0.95 Ge 0.05 O 3 The catalyst Tmax as the catalytically active material was 495℃and CsV 0.90 Ge 0.10 O 3 The catalyst Tmax, which is a catalytically active material, was 497℃and the PM light-off temperature Tmax was significantly reduced after addition of Co impurities.
Example 7
As shown in FIG. 6, co impurity is doped in cesium-vanadium alkali metal catalyst 8G, and CsVO is the active material in the 8G catalyst 3 After the Co impurity is doped and heat treated, the active substance of the catalyst becomes CsV 0.95 Co 0.05 O 3 (Co 3 O 4 ) Or CsV 0.95 Co 0.05 O 3 (CoSO 4 ). Tmax for 8G was 509℃and CsV 0.95 Co 0.05 O 3 (Co 3 O 4 ) The catalyst Tmax as the catalytically active material was 500℃and CsV 0.95 Co 0.05 O 3 (CoSO 4 ) The catalyst Tmax, which is a catalytically active material, was 492℃and the PM light-off temperature Tmax was significantly reduced after addition of Co impurities.
Claims (1)
1. A doped cesium vanadium alkali metal catalyst characterized by: comprising a promoter layer of an alkali metal complex Cs 2 SO 4 Active ingredient Cs 2 V 4 O 11 Base coating gamma-Al 2 O 3 ，Cs 2 V 4 O 11 The mass fraction of the catalyst is 18-26wt% and Cs 2 SO 4 The mass fraction of the catalyst is 4-12wt%, and gamma-Al 2 O 3 The mass fraction of (2) is 62-78wt%; also comprises impurity source Sb 2 O 5 Or NH 4 H 2 PO 4 Mixing with raw materials according to the proportion of Sb to V or P to V elements of 2:1, sintering at 800 ℃ or 1100 ℃ for 3 hours, doping Sb of 7GB2-2 and doping P of 7GB2-3, and reducing the ignition temperature of catalytic carbon smoke after adding impurities.
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Citations (8)
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| JP2004290723A (en) * | 2003-03-25 | 2004-10-21 | Toyota Central Res & Dev Lab Inc | Exhaust gas purifying catalyst |
| CN103501900A (en) * | 2011-04-28 | 2014-01-08 | 松下电器产业株式会社 | Molten salt-type off gas purification catalyst and off gas purification filter |
| CN107308935A (en) * | 2016-04-27 | 2017-11-03 | 福特全球技术公司 | Three-way catalyst and the coating structure of resistance to phosphorus catalyst |
| CN107405603A (en) * | 2015-04-10 | 2017-11-28 | 松下知识产权经营株式会社 | Particle-like substance combustion catalyst and particle-like substance combustion catalyst filter |
| WO2018055894A1 (en) * | 2016-09-20 | 2018-03-29 | パナソニックＩｐマネジメント株式会社 | Particulate matter combustion catalyst and particulate matter combustion catalyst filter |
| JP2019136632A (en) * | 2018-02-07 | 2019-08-22 | パナソニックＩｐマネジメント株式会社 | Combustion catalyst |
| JP2019147071A (en) * | 2018-02-26 | 2019-09-05 | パナソニックＩｐマネジメント株式会社 | Exhaust gas purification catalyst and exhaust gas purification filter carrying the same |
-
2021
- 2021-09-22 CN CN202111109341.9A patent/CN113731450B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3784675A (en) * | 1971-08-02 | 1974-01-08 | Gulf Research Development Co | Process for reducing the content of nitrogen oxides in the exhaust gases from internal combustion engines |
| JP2004290723A (en) * | 2003-03-25 | 2004-10-21 | Toyota Central Res & Dev Lab Inc | Exhaust gas purifying catalyst |
| CN103501900A (en) * | 2011-04-28 | 2014-01-08 | 松下电器产业株式会社 | Molten salt-type off gas purification catalyst and off gas purification filter |
| CN107405603A (en) * | 2015-04-10 | 2017-11-28 | 松下知识产权经营株式会社 | Particle-like substance combustion catalyst and particle-like substance combustion catalyst filter |
| CN107308935A (en) * | 2016-04-27 | 2017-11-03 | 福特全球技术公司 | Three-way catalyst and the coating structure of resistance to phosphorus catalyst |
| WO2018055894A1 (en) * | 2016-09-20 | 2018-03-29 | パナソニックＩｐマネジメント株式会社 | Particulate matter combustion catalyst and particulate matter combustion catalyst filter |
| JP2019136632A (en) * | 2018-02-07 | 2019-08-22 | パナソニックＩｐマネジメント株式会社 | Combustion catalyst |
| JP2019147071A (en) * | 2018-02-26 | 2019-09-05 | パナソニックＩｐマネジメント株式会社 | Exhaust gas purification catalyst and exhaust gas purification filter carrying the same |
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| CN113731450A (en) | 2021-12-03 |
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