CN115672313A - Preparation method of cerium manganese carbon smoke particulate catalyst - Google Patents
Preparation method of cerium manganese carbon smoke particulate catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- -1 cerium manganese carbon Chemical compound 0.000 title claims abstract description 14
- 239000000779 smoke Substances 0.000 title claims abstract description 12
- 238000004448 titration Methods 0.000 claims abstract description 66
- 239000003513 alkali Substances 0.000 claims abstract description 63
- 239000000243 solution Substances 0.000 claims abstract description 63
- 239000004071 soot Substances 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 41
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- YOSLGHBNHHKHST-UHFFFAOYSA-N cerium manganese Chemical compound [Mn].[Mn].[Mn].[Mn].[Mn].[Ce] YOSLGHBNHHKHST-UHFFFAOYSA-N 0.000 claims abstract description 25
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- 239000011572 manganese Substances 0.000 claims abstract description 18
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- 239000002245 particle Substances 0.000 claims abstract description 12
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- 239000007788 liquid Substances 0.000 claims description 53
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- 238000003756 stirring Methods 0.000 claims description 32
- 230000007306 turnover Effects 0.000 claims description 28
- 238000007789 sealing Methods 0.000 claims description 19
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 238000007667 floating Methods 0.000 claims description 8
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 6
- 239000001099 ammonium carbonate Substances 0.000 claims description 6
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 6
- 229940071125 manganese acetate Drugs 0.000 claims description 6
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 6
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 230000000149 penetrating effect Effects 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- HKVFISRIUUGTIB-UHFFFAOYSA-O azanium;cerium;nitrate Chemical compound [NH4+].[Ce].[O-][N+]([O-])=O HKVFISRIUUGTIB-UHFFFAOYSA-O 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 10
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- 239000007789 gas Substances 0.000 description 6
- 229910000510 noble metal Inorganic materials 0.000 description 6
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- 229910002651 NO3 Inorganic materials 0.000 description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 4
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
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- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
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- FMMWHPNWAFZXNH-UHFFFAOYSA-N Benz[a]pyrene Chemical compound C1=C2C3=CC=CC=C3C=C(C=C3)C2=C2C3=CC=CC2=C1 FMMWHPNWAFZXNH-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
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- JQVDAXLFBXTEQA-UHFFFAOYSA-N N-butyl-butylamine Natural products CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 1
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- ACNPLWSLUUSFTH-UHFFFAOYSA-N [K][Ce][Mn] Chemical compound [K][Ce][Mn] ACNPLWSLUUSFTH-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
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Images
Classifications
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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 discloses a preparation method of a cerium manganese carbon smoke particle catalyst, which comprises the following steps: step one, preparation of a salt solution, namely weighing a rare earth cerium precursor and a transition metal manganese precursor and dissolving the rare earth cerium precursor and the transition metal manganese precursor by using deionized water to obtain a salt solution I; step two, preparation of a precipitator, namely preparing an alkali solution as the precipitator to obtain a precipitator I; step three, preparing a precipitate, namely adding the salt solution I and the precipitant I into a titration precipitation device, dropwise adding the precipitant I into the salt solution I, and controlling the final pH value after titration to be eight to nine to obtain the precipitate I; and step four, post-treatment of the precipitate, namely putting the precipitate I into a water bath for aging, and performing suction filtration, stir-frying and roasting after aging to obtain a finished product. The cerium-manganese catalyst prepared by the invention has the characteristics of high oxidation-reduction performance and good texture performance, and is more favorable for improving the low-temperature catalytic purification performance of the soot particles discharged by a diesel engine compared with the cerium-manganese catalyst prepared by the traditional coprecipitation method.
Description
Technical Field
The invention mainly relates to the technical field of preparation of catalytic materials and the technical field of diesel engine tail gas purification, in particular to a preparation method of a cerium manganese carbon smoke particulate catalyst.
Background
Compared with a gasoline engine, the diesel engine is more excellent in aspects of dynamic property, fuel economy, durability and the like, although the hydrocarbon and carbon monoxide discharged by the diesel engine are only about 1/5 of that of a gasoline engine with the same discharge capacity, the quantity of the discharged soot particulate matters is far higher than that of the gasoline engine, the soot particulate matters can adsorb a plurality of organic compounds such as phenol, benzopyrene, dibutyl phthalate, amine and the like, the carcinogenicity is strong, cardiovascular diseases, respiratory diseases and skin cell changes can be caused, and the health is harmed. At present, the diesel particulate trap is adopted to solve the problem of the external purification of diesel engine discharged particulate, the trapping efficiency of the trap to particulate can reach more than 90%, but the inner wall of the trap needs to be coated with a high-activity soot catalytic combustion catalyst, so that the combustion of the soot particulate can be realized within the exhaust temperature range of the diesel engine tail gas, the trap is regenerated, otherwise, the back pressure is increased along with the increase of the trapped particulate, and the blockage occurs. The noble metal catalyst has good soot catalytic combustion activity, so the noble metal catalyst is the catalyst which is most widely commercially applied at present. However, noble metals are scarce resources and expensive, and the development of base metal catalysts with activity comparable to that of noble metal catalysts has great significance.
China is the first major country of world rare earth export and has extremely rich rare earth resources, the rare earth element cerium has a unique 4f electron layer structure and cannot be occupied by all electrons, the oxygen storage/release capacity is very excellent, and the released active oxygen is very beneficial to soot oxidation. The d orbital electron of the transition metal manganese is not filled, so that the transition metal manganese has a plurality of valence states, and oxygen vacancy is formed due to the valence state conversion when the catalytic soot is combusted, so that the catalytic activity is high. The prepared cerium-manganese catalyst is considered to have the potential of replacing a noble metal catalyst by combining the advantages of cerium and manganese.
However, in previous reports, although cerium-manganese catalysts show excellent soot catalytic activity in base metal catalysts, the performance of the cerium-manganese catalysts is still in a certain gap compared with that of noble metal catalysts, which restricts the commercial application of the cerium-manganese catalysts. Therefore, the activity of the base metal cerium manganese catalyst needs to be further improved from the aspects of texture performance, oxidation-reduction performance and the like, and meanwhile, the application cost of the catalyst needs to be reduced on the premise that the emission concentration meets the national standard by taking a simple process into consideration.
In the aspect of developing low-temperature high-activity soot particulate catalytic combustion, the patent document of application No. 202110074661.9 relates to a gold-modified manganese-based oxide catalyst and preparation and application thereof, and the catalyst mainly comprises a precious metal active component Au and an oxide carrier Mn 3 O 4 . Using Au/Mn 3 O 4 The composite catalyst is favorable for improving the activity of soot combustion, can greatly reduce the combustion temperature of soot particles and enables the soot particles to be combusted into CO 2 The temperature of the catalyst is reduced to be within the exhaust temperature range of the diesel vehicle tail gas, but the catalyst uses the precious metal Au, and the preparation cost is high. The patent document CN201510004640.4 relates to a catalyst of 3DOM supported potassium-manganese-cerium composite oxide, and preparation and application thereof, the catalyst is prepared by taking three-dimensional ordered oxide as a carrier and taking composite oxide of alkali metal, transition metal and rare earth metal as an active component, and the unique macroporous channel structure of the catalyst is beneficial to allowing soot to enter pores from all directions and provides the best diffusion for the soot particlesThe catalyst needs a specific three-dimensional ordered macroporous structure, and the preparation requirement of the catalyst is high. The patent document CN201410217081.0, and a preparation method and application of a catalyst for eliminating soot in diesel vehicle exhaust, the catalyst comprises a mixture of manganese-based oxide and cerium-based oxide, the preparation method comprises the steps of preparing an ammonium carbonate solution with a certain concentration, reversely dripping a salt solution into the ammonium carbonate solution under stirring at room temperature, drying in the air to obtain a precursor solid, and roasting to obtain the catalyst.
Disclosure of Invention
The invention mainly provides a preparation method of a cerium manganese carbon smoke particulate catalyst, which is used for solving the technical problems in the background technology.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a cerium manganese carbon smoke particulate catalyst comprises the following steps:
step one, preparing a salt solution, namely weighing corresponding rare earth cerium precursors and transition metal manganese precursors according to a stoichiometric ratio and dissolving the precursors by using deionized water to obtain a salt solution I;
step two, preparation of a precipitator, namely preparing an alkali solution as the precipitator to obtain a precipitator I;
step three, preparing a precipitate, namely adding the salt solution I and the precipitant I into a titration precipitation device, dropwise adding the precipitant I into the salt solution I, and controlling the final pH value after titration to be eight to nine to obtain the precipitate I;
and step four, post-treatment of the precipitate, namely putting the precipitate I into a water bath for aging, performing suction filtration, stir-frying and roasting after aging, and obtaining a finished cerium manganese catalyst after roasting.
In the first step, the mole fractions of cerium and manganese in the rare earth cerium precursor and the transition metal manganese precursor are added to form one, the rare earth cerium precursor is one or more of ammonium ceric nitrate and cerium nitrate, and the transition metal manganese precursor is one or more of manganese acetate and manganese nitrate, so that the precursors can be rapidly dissolved in deionized water.
In the second step, the alkali solution is at least one of ammonium carbonate solution, ammonia water, sodium hydroxide solution and sodium carbonate solution, the concentration of the alkali solution is three mol per liter, and the salt solution is precipitated by the alkali solution and then separated out in a hydroxide form.
The titration temperature in step three is thirty to ninety degrees celsius. In the preferred embodiment, the titration temperature is set to facilitate the improvement of the low-temperature catalytic purification performance of the catalyst.
The aging condition in the fourth step is that the time is two to eight hours, the temperature is sixty to one hundred ℃, the frying condition is that the time is six to twenty-four hours, the temperature is seventy to one hundred twenty ℃, the roasting condition is that the time is four to six hours, and the temperature is four hundred fifty to six hundred ℃. In the preferred embodiment, the catalytic soot combustion catalyst with high oxidation-reduction performance and good texture performance can be conveniently obtained through the post-treatment processes of aging, suction filtration, stir-drying and roasting.
The titration and precipitation device comprises a tank body, wherein the bottom of the tank body is provided with a stirring component of which an execution end extends into the tank body, the top of the tank body is provided with an alkaline liquid box, and the top of the alkaline liquid box is provided with a top cover;
the utility model discloses a titration apparatus for alkali lye box, including titration apparatus, base lye box inner wall bottom linear array, titration apparatus, base lye box, titration apparatus, box top, the bottom of titration apparatus, box inner wall and lie in be equipped with first sealed arch in the weeping mouth, the internal articulated returning face plate of titration apparatus, the returning face plate is close to first sealed bellied one side bottom is equipped with the sealed arch of second, the returning face plate is kept away from the bottom of the sealed protruding one side of second is connected the weeping mouth through the film and is kept away from first sealed bellied one side, the titration apparatus is internal and is located the returning face plate is kept away from the sealed protruding one side of second is equipped with the elasticity pulling part that is used for pulling the returning face plate, returning face plate lateral wall symmetry is equipped with the breakwater, the breakwater lateral wall is worn to be equipped with first inlet, the titration apparatus lateral wall wear to be equipped with the second inlet that first inlet position corresponds, the breakwater lateral wall is equipped with the buoyancy blocking part, the top is equipped with the execution end and extends to the stirring part of shifting the cover lye box is used for stirring the shifting the plate. In the preferred embodiment, the titration and precipitation device is convenient for the alkali liquor to quantitatively drip the metal salt solution, and the energy consumption is low.
The stirring component comprises a positioning box arranged at the bottom of the tank body, a motor arranged in the positioning box, a shaft lever arranged in the tank body and arranged at the execution end of the motor and extending to the outer wall of the shaft lever and positioned on a plurality of stirring blades in the tank body. In the preferred embodiment, the stirring element facilitates the homogeneous mixing of the lye with the metal salt solution.
The elastic pulling part comprises a positioning plate arranged on the inner wall of the titration box and a tension spring with one end connected with the side wall of the positioning plate and the other end connected with the outer wall of the turnover plate. In the preferred embodiment, the pulling of the flipping panel is facilitated by a resilient pulling member.
The buoyancy liquid blocking component comprises a liquid leakage box arranged on the outer wall of the water baffle, a through hole penetrating through the liquid leakage box and corresponding to the first liquid inlet, and a floating block arranged in the liquid leakage box. In the preferred embodiment, the buoyancy liquid-blocking component is used for facilitating the control of the amount of the alkali liquor entering the titration box.
The poking plate component comprises a miniature linear guide rail arranged at the top of the cover plate, a movable plate arranged at the execution end of the miniature linear guide rail, a positioning groove embedded in the side wall of the movable plate, and a poking plate hinged to the top of the side wall and arranged on the inner wall of the positioning groove. In the preferred embodiment, the flipping of the flipping panel one by one is facilitated by the flipping panel assembly.
Compared with the prior art, the invention has the beneficial effects that:
the high-activity cerium-manganese catalyst obtained by the preparation method of the carbon smoke particulate catalyst is applied to reducing the combustion temperature of carbon smoke in the tail gas of a diesel engine and purifying the atmospheric environment.
The traditional coprecipitation method is modified, the method adopts a titration precipitation device to dropwise add an alkali solution into a metal salt solution, and controls conditions in the preparation process of the catalyst, so that the operation is simple, the repeatability is good, the texture performance of the obtained product is good, the contact performance of the catalyst and soot is good, the activity is high, the soot can be ignited and burnt out at lower temperature, the ash accumulation resistance of the particulate trap is improved, the backpressure performance of the DPF is good, the regeneration time of the trap is shortened, and the industrial large-scale production is facilitated;
in the preparation process, ammonium ceric nitrate, cerium nitrate, manganese acetate and manganese nitrate are used as raw materials, can be quickly dissolved in deionized water, a salt solution is precipitated by an alkali solution and then is separated out in a hydroxide form, the low-temperature catalytic purification performance of the catalyst is conveniently improved by the set titration temperature, and the catalytic soot combustion catalyst with high oxidation-reduction performance and good texture performance is conveniently obtained by the post-treatment process of aging, suction filtration, parching and roasting;
it drips into metal salt solution to be convenient for alkali lye ration through titrating the sediment device, and the power consumption is low, titrates the homogeneous mixing that the sediment device passes through stirring part be convenient for alkali lye and metal salt solution, hinders the volume of liquid part be convenient for control entering the alkali lye in the titration box through buoyancy, stimulates the part through elasticity and is convenient for spur the returning face plate, is convenient for stir the returning face plate one by one through dialling the board part to the tank body is got into through titration box to the quantitative alkali lye of returning face plate rotation back.
The present invention will be explained in detail below with reference to the drawings and specific embodiments.
Drawings
FIG. 1 is an overall process flow diagram of the present invention;
FIG. 2 is an isometric view of the titration precipitation apparatus of the present invention;
FIG. 3 is an exploded view of the titration precipitation apparatus of the present invention;
FIG. 4 is an exploded view of the inner structure of the lye tank of the present invention;
FIG. 5 is an exploded view of the interior structure of the titration flask of the present invention;
FIG. 6 is a cross-sectional view of the structure of the titration precipitation apparatus of the present invention;
FIG. 7 is an enlarged view of the structure at A of the present invention;
FIG. 8 is an enlarged view of the structure of the present invention at B;
FIG. 9 is a graph of DTG (curves obtained by first differentiating a thermogravimetric curve) for examples 1-5 of the present invention;
FIG. 10 is a DTG graph of comparative examples 1-5 of the present invention;
FIG. 11 is a DTG graph of comparative examples 6 to 7 of the present invention.
FIG. 12 shows temperature programmed reduction (H) of examples 1 and 5 and comparative examples 1 and 5 2 -TPR) graph.
FIG. 13 is a Scanning Electron Microscope (SEM) image of comparative examples 1-5.
FIG. 14 is a Scanning Electron Microscope (SEM) image of examples 1-5.
Description of the drawings: 10. a titration and precipitation device; 11. a tank body; 111. an alkaline solution box; 112. a top cover; 113. a titration box; 1131. a liquid leakage port; 1132. a first seal projection; 1133. a second liquid inlet; 114. a cover plate; 12. a stirring member; 121. a positioning box; 122. a motor; 123. a shaft lever; 124. a stirring blade; 13. a turnover plate; 131. a second seal projection; 14. a film; 15. an elastic pulling member; 151. positioning a plate; 152. a tension spring; 16. a water baffle; 161. a first liquid inlet; 17. a buoyancy liquid-resistant member; 171. a liquid leakage box; 172. a through hole; 173. floating blocks; 18. a paddle member; 181. a micro linear guide rail; 182. moving the plate; 183. positioning a groove; 184. a poking plate.
Detailed Description
In order to facilitate an understanding of the invention, the invention will now be described more fully hereinafter with reference to the accompanying drawings, in which several embodiments of the invention are shown, but which may be embodied in different forms and not limited to the embodiments described herein, but which are provided so as to provide a more thorough and complete disclosure of the invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may be present, and when an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present, as the terms "vertical", "horizontal", "left", "right" and the like are used herein for descriptive purposes only.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and the terms used herein in the specification of the present invention are for the purpose of describing particular embodiments only and are not intended to limit the present invention, and the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, in a preferred embodiment of the present invention, a method for preparing a cerium manganese carbon soot particle catalyst comprises the following steps: step one, preparing a salt solution, namely weighing corresponding rare earth cerium precursors and transition metal manganese precursors according to a stoichiometric ratio and dissolving the precursors by using deionized water to obtain a salt solution I; step two, preparation of a precipitator, namely preparing an alkali solution as the precipitator to obtain a precipitator I; step three, preparing a precipitate, namely adding the salt solution I and the precipitant I into a titration precipitation device 10, dropwise adding the precipitant I into the salt solution I, and controlling the final pH value after titration to be eight to nine to obtain the precipitate I; and step four, post-treatment of the precipitate, namely putting the precipitate I into a water bath for aging, performing suction filtration, stir-drying and roasting after aging, and obtaining a finished product of the cerium-manganese catalyst after roasting is completed.
It should be noted that, in this embodiment, during preparation, corresponding ammonium cerium nitrate, manganese acetate, and manganese nitrate are weighed according to a stoichiometric ratio and dissolved in deionized water, after dissolution, a dissolving solution is filled into the tank 11, one or more of an ammonium carbonate solution, ammonia water, a sodium hydroxide solution, and a sodium carbonate solution are selected to prepare an alkali solution, the concentration of the alkali solution is three mol per liter, the prepared alkali solution is put into the alkali solution box 111, the alkali solution is dropped into the dissolving solution by the titration precipitation device 10, the temperature at the dropping time is controlled to be thirty to ninety degrees celsius, the final pH value after the completion of the titration is controlled to be eight to nine, at this time, a solid is separated out from the dissolving solution, the solid is put into a water bath for aging, the aging condition is two to eight hours, the temperature is sixty to one hundred celsius, suction filtration, drying, and baking are performed after the titration, a finished cerium manganese catalyst is obtained after baking, the drying condition is six to twenty four hours, the temperature is seventy to twenty-hundred celsius, the baking condition is four to six hours, and six to six-hundred celsius degrees.
Referring to fig. 2-8 again, in the preferred embodiment of the present invention, the titration settling device 10 includes a tank 11, a stirring member 12 having an execution end extending into the tank 11 is disposed at the bottom of the tank 11, an alkaline solution box 111 is disposed at the top of the tank 11, and a top cover 112 is disposed at the top of the alkaline solution box 111;
the bottom of the inner wall of the lye box 111 is provided with a plurality of titration boxes 113 with the bottoms penetrating through the lye box 111 in a linear array, the top of the titration box 113 is provided with a cover plate 114, the bottom of the titration box 113 is provided with a liquid leakage port 1131, the inner wall of the titration box 113 is provided with a first sealing protrusion 1132 in the liquid leakage port 1131, the titration box 113 is internally hinged with a turnover plate 13, the bottom of one side of the turnover plate 13 close to the first sealing protrusion 1132 is provided with a second sealing protrusion 131, the bottom of one side of the turnover plate 13 far away from the second sealing protrusion 131 is connected with one side of the liquid leakage port 1131 far away from the first sealing protrusion 1132 through a film 14, the titration box 113 is internally provided with a second liquid inlet 1133 corresponding to the position of the first liquid inlet 161, the side wall of the turnover plate 13 is provided with an elastic pulling component 15 for pulling the turnover plate 13, the side wall of the turnover plate 13 is symmetrically provided with a water baffle 16, the side wall of the water baffle 16 is provided with a first liquid stirring component 161, the side wall of the titration box 16 is provided with a buoyancy liquid blocking component 17, the stirring component is provided with a stirring and an actuating component, the stirring component 122 connected with a tank body actuating shaft rod 121, the stirring motor 121 and the stirring motor 121, the stirring motor 121 are provided with a stirring positioning component, the stirring motor 121, the stirring positioning component and the stirring motor 121, the buoyancy liquid-blocking component 17 is including locating the weeping box 171 of 16 outer walls of breakwater wears to locate weeping box 171 and with the through hole 172 that first inlet 161 position corresponds, and locate the floating block 173 in the weeping box 171, dial the board part 18 including locating the miniature linear guide 181 at cover plate 114 top is located the movable plate 182 of miniature linear guide 181 execution end inlays and locates the constant head tank 183 of movable plate 182 lateral wall, and the lateral wall top is articulated the group board 184 of constant head tank 183 inner wall.
It should be noted that, in this embodiment, a heating plate, a temperature sensor, and a PH sensor may be disposed in the tank 11, so as to heat the liquid in the tank 11 and to know the temperature information and the PH information in the tank 11 at the same time, the alkali solution is put into the alkali solution box 111 before titration, and the solution is put into the tank 11;
when in dripping, the plate-pulling part 18 pulls the turnover plate 13 one by one, the first liquid inlet 161 and the second liquid inlet 1133 are staggered after the turnover plate 13 rotates, so as to prevent alkali liquor in the alkali liquor box 111 from entering the titration box 113, the first sealing protrusion 1132 is separated from the second sealing protrusion 131, and the liquid in the titration box 113 can enter the tank body 11 through the liquid leakage port 1131, or can enter the tank body 11 through the liquid leakage port 1131 after flowing through the through hole on the side wall of the turnover plate 13;
when the turning plate 13 rotates to the position that the top of the turning plate 13 is lower than the execution end of the plate shifting part 18, the elastic pulling part 15 drives the turning plate 13 to reset, after the turning plate 13 is reset, the first sealing protrusion 1132 is abutted to the second sealing protrusion 131, the film 14 is pulled and unfolded by the turning plate 13 to block the liquid leakage port 1131, the first liquid inlet 161 and the second liquid inlet 1133 are reset to coincide, the alkali liquor in the alkali liquor box 111 enters the titration box 113 through the second liquid inlet 1133, the first liquid inlet 161 and the liquid leakage box 171, the alkali liquor drives the floating block 173 to move upwards, after the through hole 172 is blocked by the floating block 173, the alkali liquor cannot enter the titration box 113, so that the quantification of the alkali liquor is completed, and the next shifting of the plate shifting part 18 is waited;
further, when the toggle plate component 18 works, the execution end of the micro linear guide 181 drives the moving plate 182 to move, the moving plate 182 drives the toggle plate 184 to rotate, when the toggle plate 184 toggles the turnover plate 13, the moving plate 182 gives a supporting force to the toggle plate 184, when the toggle plate 184 resets and contacts with the turnover plate 13, the toggle plate 184 rotates around the hinged position of the toggle plate 184 and the moving plate 182;
further, when the elastic force pulling member 15 works, the tension spring 152 gives an elastic tension to the turnover plate 13;
further, when the stirring component 12 works, the execution end of the motor 122 drives the shaft rod 123 to rotate, and the shaft rod 123 drives the stirring blade 124 to rotate, so as to stir the solution, and to accelerate the mixing.
Evaluating the catalytic combustion activity of soot particulate matters:
the TGA/DSC thermogravimetric analyzer of the company METTLER, switzerland is selected to evaluate the soot catalytic combustion activity of the catalyst, and the Printex-U carbon black of the company Degussa, germany is used for simulating the soot discharged by a diesel engine. 10mg of soot particles and 100mg of catalyst sample are carefully ground in a mortar for 10min according to the mass ratio of 1. Heating about 10mg of the mixture from 30 deg.C to 600 deg.C for temperature programmed reaction at a heating rate of 10 deg.C/min under a reaction atmosphere of 10% 2 /N 2 Velocity of gas flowIs 30ml/min. Carrying out first differential on the thermogravimetric TG curve to obtain a DTG curve, and defining the temperature corresponding to the maximum weight loss of the carbon smoke particles as T m (peak of DTG curve), which was used as a standard for evaluating catalyst activity. Delta T is comparative example and example T using the same precipitant m The difference of (a).
Example 1:
(1) 56.6g of Ce (NO) are weighed out 3 ) 2 ·6H 2 O is dissolved in 280ml of deionized water, and 17.1ml of Mn (NO) is measured 3 ) 2 Solution with Ce (NO) 3 ) 2 ·6H 2 And mixing the O solution uniformly. Preparation of (NH) 4 ) 2 CO 3 And NH 3 ·H 2 An alkaline solution with the molar volume ratio of O being 3mol/L to 3mol/L is used as a precipitating agent.
(2) Dropwise adding the alkali solution into the mixed salt solution by adopting a titration precipitation device (10) at the temperature of 30 ℃ until the pH value reaches 8.5-8.8, and obtaining a mud-like hydroxide precipitate.
(3) Aging the obtained mud-like precipitate at 90 deg.C for 6h, washing with water, vacuum filtering until pH is 7, placing the precipitate in a crucible, parching at 80 deg.C for 20h, and calcining at 600 deg.C for 3h in a muffle furnace.
Example 2:
a cerium manganese soot catalytic combustion catalyst was prepared by following the procedure of example 1 except that only 3mol/L of (NH) was used instead in the procedure of step (1) 4 ) 2 CO 3 As an alkaline solution.
Example 3:
a cerium manganese soot catalytic combustion catalyst was prepared by following the procedure of example 1 except that only 3mol/L NH was used instead in the procedure of step (1) 3 ·H 2 O is used as an alkali solution.
Example 4:
a cerium manganese soot catalytic combustion catalyst was prepared by following the procedure of example 1 except that 3mol/L NaOH was used as an alkali solution in the step (1).
Example 5:
a cerium manganese soot catalytic combustion catalyst was prepared according to the procedure of example 1Meanwhile, 3mol/L of Na is used instead in the step (1) 2 CO 3 As an alkaline solution.
Comparative example 1:
a cerium manganese soot catalytic combustion catalyst was prepared by following the procedure of example 1, except that in the step (2), an alkali solution and a mixed salt solution were added dropwise together to perform coprecipitation.
Comparative example 2:
a cerium manganese soot catalytic combustion catalyst was prepared by following the procedure of comparative example 1, except that only 3mol/L of (NH) was used instead in step (1) 4 ) 2 CO 3 As an alkaline solution.
Comparative example 3:
a cerium manganese soot catalytic combustion catalyst was prepared by following the procedure of comparative example 1, except that only 3mol/L NH was used instead in step (1) 3 ·H 2 O is used as an alkali solution.
Comparative example 4:
a cerium manganese soot catalytic combustion catalyst was prepared according to the procedure of comparative example 1, except that 3mol/L NaOH was used as an alkali solution instead in the procedure of step (1).
Comparative example 5:
a cerium manganese soot catalytic combustion catalyst was prepared by following the procedure of comparative example 1 except that 3mol/L Na was used instead in step (1) 2 CO 3 As an alkaline solution.
Comparative example 6:
a cerium manganese soot catalytic combustion catalyst was prepared according to the procedure of comparative example 1, except that the mixed salt solution was dropwise added to the alkali solution in step (2).
Comparative example 7:
the cerium manganese carbon soot catalytic combustion catalyst was prepared according to the procedure of comparative example 1, except that in the procedure (2), the mixed salt solution and the alkali solution were mixed and poured into a beaker together to be stirred.
And (3) testing the texture performance:
the texture properties (specific surface and pore volume) were measured for examples 1 to 5 and comparative examples 1 to 7, and the results are shown in Table 1.
TABLE 1
It can be seen from table 1 that after the co-precipitation method is modified, the texture performance of the catalyst is significantly enhanced, and the large specific surface and pore volume are favorable for solid-solid contact between the catalyst and soot, so that the activity of the catalyst in catalyzing soot combustion is improved.
Evaluation of catalytic soot combustion activity of the catalyst:
the activity evaluation was performed on examples 1 to 5 and comparative examples 1 to 5 according to the catalyst activity evaluation method described above, as shown in fig. 9 and 10. It can be seen from the figure that after the salt-alkali coprecipitation method is changed into the method of dropwise adding salt into alkali by adopting a titration precipitation device (10), no matter which alkali solution is used, the activity of the catalyst is greatly improved, and the promotion range is 10-50 ℃ (the types of precipitants are different, and the promotion degree is different). The preparation method is simple and easy to operate, and can reduce the combustion temperature of the soot discharged by the diesel engine (the T of the soot particles without the catalyst) to a great extent m 657 deg.C), has great commercial application prospect.
The results of the activity evaluation of comparative example 6 and comparative example 7 are shown in fig. 11, and a comparison of fig. 9 and fig. 10 shows that the catalyst prepared by the method of dropping a salt solution into an alkali solution and the method of pouring a salt solution and an alkali solution together into a beaker, when the same alkali solution is used, has an activity superior to that of the conventional dropwise coprecipitation method, but the activity is not superior to that of the method of adding an alkali solution dropwise into a salt solution.
FIG. 12 compares H of examples 1 and 5, comparative examples 1 and 5 prepared by a modified precipitation method in which a base is dropped into a salt and a co-precipitation method by co-titration 2 The TPR map can show that when the adopted precipitator is the same as other preparation conditions, the cerium-manganese catalyst prepared by adopting the modified coprecipitation method has lower reduction temperature and larger reduction peak area, and good reduction performance plays an important role in improving the catalytic combustion activity of soot particles.
Fig. 13 and 14 compare the microscopic morphologies of the comparative examples and examples, and all examples except example 4 form a porous structure with better particle uniformity on the micron level, which facilitates sufficient contact of the catalyst with soot particles and accelerates the rate of solid-solid reaction.
The specific process of the invention is as follows:
the high-activity cerium-manganese catalyst obtained by the preparation method of the carbon smoke particulate catalyst is applied to reducing the combustion temperature of carbon smoke in the tail gas of a diesel engine and purifying the atmospheric environment.
The preparation method comprises the steps of weighing corresponding ammonium ceric nitrate, cerium nitrate, manganese acetate and manganese nitrate according to a stoichiometric ratio, dissolving the ammonium ceric nitrate, cerium nitrate, manganese acetate and manganese nitrate by using deionized water, filling a dissolving solution into a tank body 11 after the dissolving is finished, selecting one or more of an ammonium carbonate solution, ammonia water, a sodium hydroxide solution and a sodium carbonate solution to prepare an alkali solution, wherein the concentration of the alkali solution is three mol/L, putting the prepared alkali solution into an alkali solution box 111, dropping the alkali solution into the dissolving solution by using a titration precipitation device 10, controlling the temperature at the dropping time to be thirty-ninety ℃, controlling the final pH value after the dropping to be eight-nine, separating out a solid from the dissolving solution at the time, putting the solid into a water bath for aging, wherein the aging condition is two to eight hours, the temperature is sixty to one hundred ℃, performing suction filtration, stir-drying and roasting after the aging, obtaining a finished cerium-manganese catalyst product after the roasting is finished, the stir-drying condition is six to twenty-four hours, the temperature is seventy to twenty-hundred ℃, and the roasting condition is four-six-hundred hours;
a heating plate, a temperature sensor and a PH value sensor can be arranged in the tank body 11, so that the liquid in the tank body 11 can be heated conveniently, the temperature information and the PH value information in the tank body 11 can be known conveniently, alkali liquor is put into the alkali liquor box 111 before titration, and dissolved liquor is put into the tank body 11;
when in dripping, the plate-pulling part 18 pulls the turnover plate 13 one by one, the first liquid inlet 161 and the second liquid inlet 1133 are staggered after the turnover plate 13 rotates, so as to prevent alkali liquor in the alkali liquor box 111 from entering the titration box 113, the first sealing protrusion 1132 is separated from the second sealing protrusion 131, and the liquid in the titration box 113 can enter the tank body 11 through the liquid leakage port 1131, or can enter the tank body 11 through the liquid leakage port 1131 after flowing through the through hole on the side wall of the turnover plate 13;
when the turning plate 13 rotates to the position that the top of the turning plate 13 is lower than the execution end of the plate shifting part 18, the elastic pulling part 15 drives the turning plate 13 to reset, after the turning plate 13 is reset, the first sealing protrusion 1132 is abutted to the second sealing protrusion 131, the film 14 is pulled and unfolded by the turning plate 13 to block the liquid leakage port 1131, the first liquid inlet 161 and the second liquid inlet 1133 are reset to coincide, the alkali liquor in the alkali liquor box 111 enters the titration box 113 through the second liquid inlet 1133, the first liquid inlet 161 and the liquid leakage box 171, the alkali liquor drives the floating block 173 to move upwards, after the through hole 172 is blocked by the floating block 173, the alkali liquor cannot enter the titration box 113, so that the quantification of the alkali liquor is completed, and the next shifting of the plate shifting part 18 is waited;
when the shifting plate part 18 works, the execution end of the micro linear guide rail 181 drives the moving plate 182 to move, the moving plate 182 drives the shifting plate 184 to rotate, when the shifting plate 184 shifts the turnover plate 13, the moving plate 182 gives a supporting force to the shifting plate 184, when the shifting plate 184 resets and contacts with the turnover plate 13, the shifting plate 184 rotates around the hinged position of the shifting plate 182 and the shifting plate 184;
when the elastic force pulling part 15 works, the tension spring 152 gives elastic tension to the turnover plate 13;
when the stirring component 12 works, the execution end of the motor 122 drives the shaft rod 123 to rotate, and the shaft rod 123 drives the stirring blade 124 to rotate so as to stir the solution and accelerate the mixing.
The invention is described above with reference to the accompanying drawings, it is obvious that the invention is not limited to the above-described embodiments, and it is within the scope of the invention to adopt such insubstantial modifications of the inventive method concept and solution, or to apply the inventive concept and solution directly to other applications without modification.
Claims (10)
1. The preparation method of the cerium manganese carbon smoke particle catalyst is characterized by comprising the following steps of:
step one, preparation of a salt solution, namely weighing corresponding rare earth cerium precursors and transition metal manganese precursors according to a stoichiometric ratio and dissolving the precursors by using deionized water to obtain a salt solution I;
step two, preparation of a precipitator, namely preparing an alkali solution as the precipitator to obtain a precipitator I;
step three, preparing a precipitate, namely adding the salt solution I and the precipitant I into a titration precipitation device (10), dropwise adding the precipitant I into the salt solution I, and controlling the final pH value after titration to be eight to nine to obtain the precipitate I;
and step four, post-treatment of the precipitate, namely putting the precipitate I into a water bath for aging, performing suction filtration, stir-frying and roasting after aging, and obtaining a finished cerium-manganese catalyst after roasting.
2. The method according to claim 1, wherein the molar fractions of cerium and manganese in the rare earth cerium precursor and the transition metal manganese precursor in the first step are added to form one, wherein the rare earth cerium precursor is one or more of ammonium cerium nitrate and cerium nitrate, and the transition metal manganese precursor is one or more of manganese acetate and manganese nitrate.
3. The method of claim 1, wherein the alkali solution in step two is at least one of ammonium carbonate solution, ammonia water, sodium hydroxide solution, and sodium carbonate solution, and the concentration of the alkali solution is three mol/l.
4. The method of claim 1, wherein the titration temperature in step three is thirty to ninety degrees celsius.
5. The method of claim 1, wherein the aging in step four is performed for a period of two to eight hours at a temperature of sixty to one hundred degrees celsius, the parching is performed for a period of six to twenty-four hours at a temperature of seventy to one hundred twenty degrees celsius, and the calcining is performed for a period of four to six hours at a temperature of four hundred fifty to six hundred degrees celsius.
6. The preparation method of the cerium manganese carbon particulate catalyst according to claim 1, wherein the titration precipitation device (10) comprises a tank body (11), the bottom of the tank body (11) is provided with a stirring component (12) of which an execution end extends into the tank body (11), the top of the tank body (11) is provided with an alkaline liquid box (111), and the top of the alkaline liquid box (111) is provided with a top cover (112);
the alkali liquor box (111) inner wall bottom linear array is provided with a plurality of titration boxes (113) with bottoms penetrating through the alkali liquor box (111), the top of the titration box (113) is provided with a cover plate (114), the bottom of the titration box (113) is provided with a liquid leakage port (1131), the inner wall of the titration box (113) is provided with a first sealing protrusion (1132) in the liquid leakage port (1131), the titration box (113) is internally hinged with a turnover plate (13), the turnover plate (13) is close to one side bottom of the first sealing protrusion (1132) and is provided with a second sealing protrusion (131), the turnover plate (13) is far away from the bottom of one side of the second sealing protrusion (131) and is connected with the liquid leakage port (1131) through a film (14) and is far away from one side of the first sealing protrusion (1132), the titration box (113) is internally provided with a water baffle (16), the turnover plate (13) is far away from one side of the second sealing protrusion (131) and is provided with an elastic pulling part (15) for pulling the turnover plate (13), the side wall of the turnover plate (13) is symmetrically provided with a water baffle (16), the water baffle (16) side wall of the water baffle (161) is provided with a first buoyancy part (161), and a first water inlet (161) and a first buoyancy part (161) is arranged on one side wall, and a first water baffle (161) for passing through, and a first water inlet (16) is arranged, and a second buoyancy part (17) is arranged on the water inlet (16), the top of the cover plate (114) is provided with a plate shifting component (18) of which the execution end extends to the cover plate (114), and the plate shifting component (18) is used for shifting the turnover plate (13).
7. The method for preparing a cerium manganese carbon soot particulate catalyst according to claim 6, wherein the stirring member (12) comprises a positioning box (121) disposed at the bottom of the tank (11), a motor (122) disposed in the positioning box (121), a shaft (123) disposed at an executing end of the motor (122) and extending into the tank (11), and a plurality of stirring blades (124) disposed on an outer wall of the shaft (123) and located in the tank (11).
8. The method for preparing the cerium manganese carbon soot particulate catalyst according to claim 6, wherein the elastic pulling member (15) comprises a positioning plate (151) arranged on the inner wall of the titration box (113), and a tension spring (152) with one end connected with the side wall of the positioning plate (151) and the other end connected with the outer wall of the turnover plate (13).
9. The preparation method of the cerium manganese carbon soot particulate catalyst according to claim 6, wherein the buoyancy liquid-blocking member (17) comprises a liquid leakage box (171) arranged on the outer wall of the water baffle (16), a through hole (172) penetrating through the liquid leakage box (171) and corresponding to the first liquid inlet (161), and a floating block (173) arranged in the liquid leakage box (171).
10. The method for preparing a cerium-manganese-carbon soot particulate catalyst as claimed in claim 6, wherein said pick-up plate member (18) comprises a micro linear guide (181) disposed on the top of said cover plate (114), a moving plate (182) disposed at the execution end of said micro linear guide (181), a positioning groove (183) embedded in the side wall of said moving plate (182), and a pick-up plate (184) hinged to the inner wall of said positioning groove (183) at the top of the side wall.
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