CN113694931B - Composite catalyst, catalyst suspension, preparation method and application thereof - Google Patents
Composite catalyst, catalyst suspension, preparation method and application thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 279
- 239000000725 suspension Substances 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 229910001868 water Inorganic materials 0.000 claims abstract description 51
- 239000003960 organic solvent Substances 0.000 claims abstract description 42
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000011591 potassium Substances 0.000 claims abstract description 41
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 41
- 239000004094 surface-active agent Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims description 27
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 18
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical group CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910018921 CoO 3 Inorganic materials 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000005470 impregnation Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 41
- 238000000576 coating method Methods 0.000 abstract description 38
- 239000002904 solvent Substances 0.000 abstract description 18
- 239000000203 mixture Substances 0.000 abstract description 10
- 229910001414 potassium ion Inorganic materials 0.000 abstract description 10
- 239000006185 dispersion Substances 0.000 abstract description 8
- 238000004090 dissolution Methods 0.000 abstract description 6
- 230000001737 promoting effect Effects 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 description 22
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- 150000004706 metal oxides Chemical class 0.000 description 17
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 13
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 13
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000011148 porous material Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 239000002184 metal Substances 0.000 description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 6
- 239000002341 toxic gas Substances 0.000 description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
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- ZFPGARUNNKGOBB-UHFFFAOYSA-N 1-Ethyl-2-pyrrolidinone Chemical compound CCN1CCCC1=O ZFPGARUNNKGOBB-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000003618 dip coating Methods 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0213—Preparation of the impregnating solution
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
- B01J37/0219—Coating the coating containing organic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0234—Impregnation and coating simultaneously
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/024—Multiple impregnation or coating
-
- 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
- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
- F01N3/033—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices
- F01N3/035—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices with catalytic reactors, e.g. catalysed diesel particulate filters
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Catalysts (AREA)
Abstract
The invention relates to a composite catalyst, a catalyst suspension, a preparation method and application thereof. In the preparation method of the composite catalyst, a catalyst containing potassium is mixed with water, a water-soluble organic solvent and a surfactant to obtain a catalyst suspension; then, the carrier is immersed in the catalyst suspension and sintered again to obtain the composite catalyst; wherein the volume ratio of the water-soluble organic solvent to the water is (1-9): 1-9. By adding specific volume of water-soluble organic solvent into water, the catalyst K is inhibited + The dissolution of potassium ions in the catalyst is prevented from losing in the coating process, so that the stability of the structure and the composition of the catalyst is maintained, a specific solvent environment is provided for promoting the uniform dispersion of the catalyst, the catalyst in the prepared composite catalyst still maintains the original structure, and the catalytic efficiency of the composite catalyst is improved.
Description
Technical Field
The invention relates to the technical field of catalyst preparation, in particular to a composite catalyst, a catalyst suspension, a preparation method and application thereof.
Background
The problem of pollution is now becoming more and more interesting worldwide, with a significant portion of air pollution coming from the rapid development of the automotive industry. The exhaust gas of the diesel engine, the diesel generator, the boiler and the like contains a large amount of particulate matters and toxic gases, including carbon monoxide and nitrogen oxides, and a large amount of particulate matters and toxic gas nitrogen oxides bring about serious environmental pollution, wherein carbon monoxide is a toxic gas, which can cause death of people, and nitrogen oxide is not only a toxic gas but also acid rain, which pollutes the environment and even endangers life safety of people.
In the conventional technology, a wall-flow particulate filter (DPF) and other tail gas filters are often adopted to filter out particulate matters in tail gas, and toxic gas is catalyzed by a catalyst in the filter to be converted into pollution-free gas, namely carbon dioxide, water and nitrogen. The commonly used catalysts comprise noble metal catalysts and composite metal oxide catalysts, the wall-flow type particle filter adopting the noble metal catalysts is severely limited by cost, the composite metal oxide catalysts have low cost and are suitable for large-area application, and the composite metal oxide catalysts particularly containing potassium element have excellent catalytic performance. In general, in preparing an exhaust gas filter containing a composite metal oxide catalyst containing a potassium element, a suspension of the catalyst containing potassium is prepared by using water as a solvent, and then the exhaust gas filter having a support activation layer is impregnated with the catalyst suspension. However, the catalyst produced by this method is not efficient in catalysis.
Therefore, there is an urgent need to develop a method for preparing a catalyst capable of improving the catalytic efficiency of a catalyst coating layer containing potassium.
Disclosure of Invention
Based on the above, the invention provides a composite catalyst, a catalyst suspension, a preparation method and application thereof, wherein the preparation method of the composite catalyst can improve the catalytic efficiency of the prepared composite catalyst coating.
The technical scheme of the invention is as follows.
One aspect of the present invention provides a method for preparing a composite catalyst, comprising the steps of:
mixing a catalyst containing potassium with water, a water-soluble organic solvent and a surfactant to obtain a catalyst suspension; wherein the volume ratio of the water-soluble organic solvent to the water is (1-9);
and (3) immersing the carrier in the catalyst suspension, and sintering to obtain the composite catalyst.
In some embodiments, the volume ratio of the water-soluble organic solvent to the water is (3-5): 1.
In some embodiments, the water-soluble organic solvent is selected from at least one of methanol, ethanol, isopropanol, acetone, 2-butanone, dioxane, acetonitrile, tetrahydrofuran, N-dimethylformamide, N-ethyl pyrrolidone, and dimethyl sulfoxide.
In some of these embodiments, the water-soluble organic solvent is selected from at least one of 2-butanone, dioxane, and acetonitrile.
In some of these embodiments, the alumina carrier, silica gel carrier, and activated carbon carrier are at least one.
In some of these embodiments, the conditions of the impregnation are: dipping for 1-24 h at 15-30 ℃.
In some of these embodiments, the catalyst is present in a concentration of 1% to 20% by mass based on the total mass of the catalyst suspension.
In some of these embodiments, the potassium-containing catalyst is a composite metal oxide catalyst containing elemental potassium.
In some of these embodiments, the sintering conditions are: sintering for 1-24 h at 300-1000 ℃.
In a further aspect of the invention there is provided a process for preparing a catalyst suspension comprising the steps of:
mixing a catalyst containing potassium with water and a water-soluble organic solvent to obtain a catalyst suspension;
wherein the volume ratio of the water-soluble organic solvent to the water is (1-9).
In some of these embodiments, the surfactant is present in a concentration of 0.0001% to 0.02% by mass based on the total mass of the catalyst suspension.
The invention also provides a preparation method of the catalyst suspension, which comprises the following steps:
mixing a catalyst containing potassium with water and a water-soluble organic solvent to obtain a catalyst suspension;
wherein the volume ratio of the water-soluble organic solvent to the water is (1-9).
Further, the invention also provides a catalyst suspension, which is prepared by the preparation method of the catalyst suspension.
In another aspect, the invention also provides a composite catalyst, which is prepared by the preparation method of the composite catalyst.
The invention also provides an exhaust gas filter comprising the composite catalyst.
Advantageous effects
The inventionIn the preparation method of the composite catalyst provided by the invention, a catalyst containing potassium is mixed with water, a water-soluble organic solvent and a surfactant to obtain a catalyst suspension; then, the carrier is immersed in the catalyst suspension and sintered again to obtain the composite catalyst; and controlling the volume ratio of the water-soluble organic solvent to water to be (1-9). By adding a specific volume of a water-soluble organic solvent to water, the catalyst K can be suppressed as compared with a suspension prepared in pure water as a solvent + The dissolution of potassium ions in the catalyst is prevented from losing in the coating process, so that the stability of the structure and the composition of the catalyst is maintained, a specific solvent environment is provided for promoting the uniform dispersion of the catalyst, the catalyst in the prepared composite catalyst still maintains the original structure, and the catalytic efficiency of the composite catalyst coating is improved.
The invention also provides a catalyst prepared by the preparation method of the composite catalyst, and the catalyst in the prepared composite catalyst still keeps the original structure, and the catalytic efficiency of the catalyst coating is high.
The invention also provides an exhaust gas filter comprising the composite catalyst. The tail gas filter has high catalytic efficiency and can improve the efficiency of tail gas treatment.
Drawings
FIG. 1 is a graph showing the catalytic effect of the catalyst suspension prepared in example 1 after calcination;
FIG. 2 shows a catalyst La 0.9 K 0.1 FeO 3 Is a catalytic effect diagram of (1);
FIG. 3 is a graph showing the catalytic effect of the catalyst suspension prepared in comparative example 1 after sintering;
FIG. 4 is a graph showing the catalytic effect of the catalyst suspension prepared in example 4 after sintering;
FIG. 5 is a graph showing the catalytic effect of the catalyst suspension prepared in comparative example 2 after sintering;
FIG. 6 is a graph showing the catalytic effect of the catalyst suspension prepared in comparative example 4 after sintering.
Detailed Description
The present invention will be described more fully hereinafter in order to facilitate an understanding of the present invention, and preferred embodiments of the present invention are set forth. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
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. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
In the prior art, a wall-flow particulate filter (DPF) is often used for filtering out particulates in exhaust gas and catalytically treating toxic gases, wherein the catalytic performance of a composite metal oxide containing potassium is excellent, water is generally used as a solvent to prepare a suspension of a catalyst containing potassium, and then the suspension of the catalyst is used for impregnating the wall-flow particulate filter with a carrier activation layer. However, it was found that: due to K + Very water-soluble, K-containing catalysts in dip coating processes + Is easy to run off, and can have adverse effect on the atomic proportion and structure of the catalyst in the coating obtained by coating, thereby reducing the catalytic efficiency of the catalyst.
Based on this, the skilled person has been trying to start from both the development of a new catalyst or the development of a new coating method, in order to achieve a catalyst coating with high catalytic efficiency while reducing costs. The present inventors have been working on developing a method that prevents the loss of potassium ions in potassium-containing catalysts. In some techniques, the skilled artisan prevents loss of potassium ions by adding a specific binder to a mixed suspension of catalyst and water to form a slurry. Based on years of experience in the field of practice and scientific research, the present inventors break the limitations of the conventional technology and creatively propose to develop a catalyst inhibiting agent based on the solvent environment for regulating the catalyst suspensionChemical agent K + A coating method for preventing potassium ions in the catalyst from losing in the dip coating, thereby maintaining the stability of the structure and composition of the catalyst.
Those skilled in the art, after a number of experimental studies, have found that: when the catalyst is dispersed by adopting an organic solvent, the ionization capacity of the pure organic solvent is far weaker than that of water, so that the pure organic solvent can not be well contacted with the catalyst, and the dispersion of catalyst powder is not facilitated. Based on this, those skilled in the art creatively adopt water-soluble organic solvent and water as solvents and control the volume ratio of the two, thereby providing a specific solvent environment and inhibiting the catalyst K + The dissolution of potassium ions in the catalyst is prevented from losing in the coating process, so that the catalyst is uniformly dispersed while the stability of the structure and the composition of the catalyst is maintained. The technical scheme of the invention is obtained after a large number of tests.
An embodiment of the present invention provides a method for preparing a composite catalyst, which includes the following steps S10 to S20.
Step S10, mixing a catalyst containing potassium with water, a water-soluble organic solvent and a surfactant to obtain a catalyst suspension; wherein the volume ratio of the water-soluble organic solvent to the water is (1-9) to (1-9).
Step S20, immersing the carrier in the catalyst suspension obtained in the step S10, and sintering to obtain the composite catalyst.
In the preparation method of the composite catalyst, a catalyst containing potassium is mixed with water, a water-soluble organic solvent and a surfactant to obtain a catalyst suspension; then, the carrier is immersed in the catalyst suspension, and then sintered to obtain a composite catalyst; and controlling the volume ratio of the water-soluble organic solvent to water to be (1-9). By adding specific volume of water-soluble organic solvent into water, the catalyst K is inhibited + The dissolution of potassium ions in the catalyst is prevented from losing in the coating process, so that the stability of the structure and the composition of the catalyst is maintained, a specific solvent environment is provided for promoting the uniform dispersion of the catalyst, and the catalyst in the prepared composite catalyst is still maintainedThe original structure of the catalyst improves the catalytic efficiency of the composite catalyst coating.
In some of these embodiments, in step S10, the support is selected from at least one of an alumina support, a silica gel support, and an activated carbon support.
The carrier can provide a larger specific surface area, so that the catalytic efficiency of the prepared composite catalyst is improved. Further, the carrier alumina carrier is, in particular, gamma-Al 2 O 3 。
Preferably, in step S10, the volume ratio of the water-soluble organic solvent to water is (3-5): 1.
The solvent environment provided by the water-soluble organic solvent and water with the specific volume ratio is more favorable for inhibiting the catalyst K + The dissolution of potassium ions in the catalyst is prevented from losing in the coating process, so that the stability of the structure and the composition of the catalyst is maintained; meanwhile, the catalyst is more beneficial to promoting the uniform dispersion of the catalyst, so that the catalytic efficiency of the catalyst coating can be further improved.
The water-soluble organic solvent is an organic solvent which is miscible with water; including but not limited to: methanol, ethanol, isopropanol, ethylene glycol, acetone, 2-butanone, dioxane, acetonitrile, tetrahydrofuran, N-dimethylformamide, N-ethylpyrrolidone, and dimethyl sulfoxide.
In some embodiments, the water-soluble organic solvent is selected from at least one of methanol, ethanol, isopropanol, acetone, 2-butanone, dioxane, acetonitrile, tetrahydrofuran, N-dimethylformamide, N-ethyl pyrrolidone, and dimethyl sulfoxide.
Preferably, the above water-soluble organic solvent is selected from at least one of 2-butanone, dioxane and acetonitrile. The solvent environment provided by the water-soluble organic solvent and water is more favorable for inhibiting the catalyst K + The dissolution of potassium ions in the catalyst is prevented from losing in the coating process, so that the stability of the structure and the composition of the catalyst is maintained; meanwhile, the catalyst is more beneficial to promoting the uniform dispersion of the catalyst, so that the catalytic efficiency of the catalyst coating can be further improved.
In some of these embodiments, the mass concentration of the catalyst in the catalyst suspension is 1% to 20%, and further, the mass concentration is preferably 4% to 12%, based on the total mass of the catalyst suspension.
In some of these embodiments, the catalyst is a composite metal oxide catalyst containing a potassium element.
It is understood that the above-mentioned composite metal oxide catalyst is a catalyst containing two or more metal elements. Wherein the molar ratio of the potassium element in the total metal is 1-40%, and further the molar ratio of the potassium element in the total metal is 5-20%.
In step S10, the catalyst containing potassium, water and the water-soluble organic solvent are not in a specific order, and the catalyst containing potassium and water may be mixed first, then the water-soluble organic solvent may be added, or the water and the water-soluble organic solvent may be mixed first, and then the catalyst containing potassium may be added.
Further, the catalyst is at least one selected from the group consisting of a two-component composite metal oxide catalyst, a three-component composite metal oxide catalyst, a four-component composite metal oxide catalyst, and a five-component composite metal oxide catalyst.
In some of these embodiments, the metal element in the above-described catalyst includes at least one of a second main group element and a transition metal element in addition to the potassium element. The composite metal oxide catalyst containing potassium element is exemplified below, but the following ranges are not included.
Representative composite metal oxides are CuK composite metal oxides, laKCo composite metal oxides, laKCoFe composite metal oxides.
In some of these embodiments, in step S10, before mixing the potassium-containing catalyst with water and the water-soluble organic solvent, the catalyst may be pulverized by a jet mill or a ball mill to further reduce its particle size in order to facilitate dispersion of the catalyst.
In some of these embodiments, the particle size of the catalyst is controlled below 3 μm.
In some of these embodiments, the surfactant is present in a concentration of 0.0001% to 0.02% by mass based on the total mass of the suspension of catalyst.
Surfactants are used to enhance the stability of the suspension.
In some of these embodiments, in step S20, the conditions of impregnation are: dipping for 1-24 h at 15-30 ℃.
Further, the impregnation step of step S20 is performed under ultrasonic or stirring conditions.
Convection is promoted by ultrasonic or stirring methods, so that the dipping time is reduced. Further, the soaking time is 1-4 h.
In some of these embodiments, in step S20, after the carrier is immersed in the suspension of the catalyst and before the sintering step, the following steps are further included:
the impregnated support is purged with compressed air.
And removing redundant suspension in the carrier gaps by means of compressed air blowing and the like.
In some of these embodiments, in step S20, the conditions of the sintering step are: sintering for 1-24 h at 300-1000 ℃.
Further, in step S20, sintering conditions are as follows: sintering at 400-800 deg.c for 2-6 hr. An embodiment of the present invention also provides a composite catalyst, which is prepared by the preparation method of the composite catalyst.
The catalyst in the composite catalyst prepared by the preparation method of the composite catalyst still maintains the original structure, and the catalytic efficiency of the catalyst coating is high. The invention also provides an exhaust gas filter, which comprises the composite catalyst.
Further, the exhaust gas filter is a particulate filter. Specifically, the exhaust gas filter is a wall-flow type particulate filter. In some embodiments, the exhaust gas filter may be prepared by immersing a filter containing a carrier in the catalyst suspension and sintering the immersed filter. It will be appreciated that in other embodiments, the composite catalyst may be prepared outside the filter without being activated by the support and then placed in the filter.
Further, the preparation steps of the exhaust gas filter are as follows:
immersing the filter which is not activated by the carrier in sol of the carrier material, and sintering to prepare the filter containing the carrier; then, the filter containing the carrier was immersed in the above catalyst suspension and sintered again to obtain a gas filter.
In still other embodiments, the filter that has not been activated by the support is immersed in the sol of the support material for 1 to 6 hours, then removed, excess sol is leached, and then calcined.
Further, the conditions of the above calcination are: roasting for 1-5 h at 300-500 ℃.
The exhaust gas filter comprises the composite catalyst prepared by the preparation method of the composite catalyst. By adding specific volume of water-soluble organic solvent into water, the catalyst K is inhibited + The catalyst is dissolved, and the potassium ions in the catalyst are prevented from losing in the dip coating process, so that the stability of the structure and the composition of the catalyst is maintained, and meanwhile, a specific solvent environment is provided to promote the uniform dispersion of the catalyst, so that the catalyst in the catalyst coating obtained after the coating still maintains the original structure, the catalytic efficiency of the composite catalyst is improved, and the tail gas treatment efficiency of the particle filter is improved.
The invention will be described in connection with specific embodiments, but the invention is not limited thereto, and it will be appreciated that the appended claims outline the scope of the invention, and those skilled in the art, guided by the inventive concept, will appreciate that certain changes made to the embodiments of the invention will be covered by the spirit and scope of the appended claims.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
1) Immersing the wall-flow type particle filter which is not activated by the carrier in alumina sol with the solid content of 6% for 2 hours, taking out, and draining the carrier holes of the wall-flow type particle filterExcess alumina sol in the channel is then baked for 2 hours at 400 ℃ to form gamma-Al 2 O 3 A coated wall-flow particulate filter.
2) Selecting perovskite catalyst La containing potassium 0.9 K 0.1 FeO 3 Wherein the molar ratio of potassium element in the total catalyst metal is 5%, and the catalyst is crushed by adopting a ball milling method, so that the granularity of the catalyst is controlled below 3 mu m.
And (2) taking dioxane and water as solvents, mixing the dioxane and the water according to the volume ratio of 4:1 to obtain a mixed solvent, adding the crushed catalyst, adding a surfactant PVP (polyvinylpyrrolidone), and stirring to obtain a catalyst suspension. Wherein the solid content of the catalyst is 4% based on the total mass of the suspension of the catalyst; the mass percentage of the surfactant PVP is 0.01 percent.
3) Immersing the wall-flow type particle filter covered by the gamma-Al 2O3 coating obtained in the step 1) into the suspension obtained in the step 2), taking out after keeping for 1h, purging by adopting compressed air to remove the superfluous suspension carried on the surface of the DPF pore canal, and then placing the DPF pore canal in an air atmosphere at 400 ℃ for roasting for 6h to obtain the wall-flow type particle filter loaded with the potassium-containing catalyst coating.
4) The catalytic effect of the wall-flow particulate filter prepared by the coating method of the above steps was tested, and the specific steps were as follows:
taking out part of the catalyst suspension obtained in the step 2), airing, roasting at 400 ℃ for 6 hours to obtain a roasted catalyst, and testing the catalytic effect of the catalyst by adopting a TG method, wherein the specific steps are as follows:
the catalyst prepared in the step 4) and a raw material perovskite catalyst La 0.9 K 0.1 FeO 3 And respectively and uniformly mixing the mixed materials with simulated carbon smoke according to the mass ratio of 9:1, and respectively carrying out thermogravimetric analysis experiments under the air atmosphere to respectively obtain TG and DTG curves, wherein the TG and DTG curves are shown in figures 1 and 2. Wherein, the temperature of the intersection point between the tangent line of the TG curve and the baseline before weightlessness at the maximum weightlessness rate temperature (Tmax) is the ignition temperature (Tig) when the temperature is increased to 800 ℃ according to the program of 10 ℃/min. When the catalyst has a light-off temperatureThe lower the degree, the better the activity. With a raw material perovskite catalyst La 0.9 K 0.1 FeO 3 The catalyst in the catalyst coating layer prepared by the coating method of the above steps maintains high catalytic efficiency compared to the light-off temperature.
FIG. 1 is a graph of the catalytic effect of the catalyst prepared in step 4), with a light-off temperature (Tig) of 296 ℃; FIG. 2 shows a perovskite catalyst La as a starting material 0.9 K 0.1 FeO 3 The light-off temperature (Tig) was 304 ℃. From this, it can be seen that: the catalyst in the catalyst coating prepared by the coating method in the step has lower ignition temperature, the catalytic performance of the catalyst is not changed basically, and the catalyst loaded by the wall-flow type particle filter prepared in the step 3) keeps high catalytic efficiency.
Example 2
1) Immersing the wall-flow type particle filter which is not activated by the carrier in alumina sol with the solid content of 6 percent for 2 hours, taking out, draining the redundant alumina sol in the carrier pore canal of the wall-flow type particle filter, and roasting for 2 hours at 400 ℃ to form gamma-Al 2 O 3 A coated wall-flow particulate filter.
2) Selecting perovskite catalyst La containing potassium 0.6 K 0.4 CoO 3 Wherein the molar ratio of potassium element in the total catalyst metal is 20%, and the catalyst is crushed by adopting a ball milling method, so that the granularity of the catalyst is controlled below 3 mu m.
The preparation method comprises the steps of selecting dioxane, 2-butanone and water as solvents, mixing the dioxane, the 2-butanone and the water in a volume ratio of 1:1 and a volume ratio of 3:1 to obtain a mixed solvent, adding a crushed catalyst, adding a surfactant PVP (polyvinylpyrrolidone), and stirring to obtain a catalyst suspension. Wherein the solid content of the catalyst is 12% based on the total mass of the suspension of the catalyst; the mass percentage of the surfactant PVP is 0.01 percent.
3) Immersing the wall-flow type particle filter covered by the gamma-Al 2O3 coating obtained in the step 1) into the suspension obtained in the step 2), taking out after keeping for 1h, purging by adopting compressed air to remove the superfluous suspension carried on the surface of the DPF pore canal, and then placing the DPF pore canal in an air atmosphere at 400 ℃ for roasting for 6h to obtain the wall-flow type particle filter loaded with the potassium-containing catalyst coating.
4) The catalytic effect of the wall-flow particulate filter prepared by the coating method of the above steps was tested, and the specific steps were as follows:
taking out part of the catalyst suspension obtained in the step 2), airing, roasting at 400 ℃ for 6 hours to obtain a roasted catalyst, and testing the catalytic effect of the catalyst by adopting a TG method, wherein the specific steps are as in the step 4 of the example 1
The results show that: the light-off temperature (Tig) of the catalyst prepared in the step 4) is 299 ℃; raw material perovskite catalyst La 0.6 K 0.4 CoO 3 The light-off temperature (Tig) of (C) was 304 ℃. From this, it can be seen that: the wall-flow particulate filter supported catalyst produced in step 3) above maintains high catalytic efficiency.
Example 3
1) Immersing the wall-flow type particle filter which is not activated by the carrier in alumina sol with the solid content of 6 percent for 2 hours, taking out, draining the redundant alumina sol in the carrier pore canal of the wall-flow type particle filter, and roasting for 2 hours at 400 ℃ to form gamma-Al 2 O 3 A coated wall-flow particulate filter.
2) Selecting perovskite catalyst La containing potassium 0.6 K 0.4 CoO 3 Wherein the molar ratio of potassium element in the total catalyst metal is 20%, and the catalyst is crushed by adopting a ball milling method, so that the granularity of the catalyst is controlled below 3 mu m.
The preparation method comprises the steps of selecting dioxane, 2-butanone and water as solvents, mixing the dioxane, the 2-butanone and the water in a volume ratio of 1:1 and a volume ratio of the dioxane to the 2-butanone to the water of 5:1 to obtain a mixed solvent, adding a crushed catalyst, adding a surfactant PVP (polyvinylpyrrolidone), and stirring to obtain a catalyst suspension. Wherein the solid content of the catalyst is 12% based on the total mass of the suspension of the catalyst; the mass percentage of the surfactant PVP is 0.01 percent.
3) Immersing the wall-flow type particle filter covered by the gamma-Al 2O3 coating obtained in the step 1) into the suspension obtained in the step 2), taking out after keeping for 1h, purging by adopting compressed air to remove the superfluous suspension carried on the surface of the DPF pore canal, and then placing the DPF pore canal in an air atmosphere at 400 ℃ for roasting for 6h to obtain the wall-flow type particle filter loaded with the potassium-containing catalyst coating.
4) The catalytic effect of the wall-flow particulate filter prepared by the coating method of the above steps was tested, and the specific steps were as follows:
taking out part of the catalyst suspension obtained in the step 2), airing, roasting at 400 ℃ for 6 hours to obtain a roasted catalyst, and testing the catalytic effect of the catalyst by adopting a TG method, wherein the specific steps are as in the step 4 of the example 1
The results show that: the light-off temperature (Tig) of the catalyst prepared in the step 4) is 301 ℃; raw material perovskite catalyst La 0.6 K 0.4 CoO 3 The light-off temperature (Tig) of (C) was 304 ℃. From this, it can be seen that: the structure and the composition proportion of the catalyst in the catalyst coating prepared by the coating method in the step are basically consistent with those of the raw material catalyst, the catalytic performance of the catalyst is basically unchanged, and the catalyst loaded by the wall-flow type particle filter prepared in the step 3) keeps high catalytic efficiency.
Example 4
Example 4 is essentially the same as example 1 except that in step 2), the volume ratio of dioxane to water is 0.5:1, and the remaining steps and process conditions are the same as example 1.
The test results show that: the light-off temperature (Tig) of the catalyst obtained in step 4) was 303 ℃. FIG. 4 is a graph showing the catalytic effect of the catalyst prepared in example 4.
Example 5
Example 5 is essentially the same as example 1 except that in step 2), the volume ratio of dioxane to water is 7:1, and the remaining steps and process conditions are the same as example 1.
The test results show that: the light-off temperature (Tig) of the catalyst obtained in step 4) was 303 ℃.
Example 6
Example 6 is essentially the same as example 1 except that in step 2), methanol and water are selected as solvents, and the remaining steps and process conditions are the same as example 1.
The test results show that: the light-off temperature (Tig) of the catalyst obtained in step 4) was 303 ℃.
Comparative example 1
1) Immersing the wall-flow type particle filter which is not activated by the carrier in alumina sol with the solid content of 6 percent for 2 hours, taking out, draining the redundant alumina sol in the carrier pore canal of the wall-flow type particle filter, and roasting for 2 hours at 400 ℃ to form gamma-Al 2 O 3 A coated wall-flow particulate filter.
2) Selecting perovskite catalyst La containing potassium 0.9 K 0.1 FeO 3 Wherein the molar ratio of potassium element in the total catalyst metal is 5%, and the catalyst is crushed by adopting a ball milling method, so that the granularity of the catalyst is controlled below 3 mu m.
Water is selected as a solvent, then the crushed catalyst is added, and a surfactant PVP (polyvinylpyrrolidone) is added, and the mixture is stirred to obtain a catalyst suspension. Wherein the solid content of the catalyst is 4% based on the total mass of the suspension of the catalyst; the mass percentage of the surfactant PVP is 0.01 percent.
3) The gamma-Al obtained in the step 1) is reacted with 2 O 3 Immersing the wall-flow type particle filter covered by the coating into the suspension obtained in the step 2), keeping for 1h, taking out, adopting compressed air to sweep and remove redundant suspension carried on the surface of a DPF pore canal, and then placing the DPF pore canal in an air atmosphere at 400 ℃ for roasting for 6h to obtain the wall-flow type particle filter loaded with the potassium-containing catalyst coating.
4) The catalytic effect of the wall-flow particulate filter produced by the coating method of the above steps was tested, with the following steps being as in example 1, step 4).
The results show that: degree ratio 4 the light-off temperature (Tig) of the catalyst prepared in step 4) was 346 ℃, and the catalytic effect is shown in fig. 3. From this, it can be seen that: the catalytic performance of the catalyst in the catalyst coating layer prepared by the coating method of the above steps is significantly reduced.
Comparative example 2
Comparative example 2 is substantially the same as example 1 except that: in step 2), dioxane was used as a solvent, water was not added, and the other steps and process conditions were the same as in example 1.
The test results show that: the light-off temperature (Tig) of the catalyst obtained in step 4) was 314 ℃.
FIG. 5 is a graph showing the catalytic effect of the catalyst prepared in comparative example 2.
Comparative example 3
Comparative example 3 is substantially the same as example 1 except that: in step 2), the volume ratio of dioxane to water was 11:1, and the rest of the steps and process conditions were the same as in example 1.
The test results show that: the catalyst prepared in step 4) of comparative example 3 had a light-off temperature (Tig) of 342 ℃.
Comparative example 4
Example 7 was essentially the same as example 1 except that in step 2), no surfactant PVP was added, and the remaining steps and process conditions were the same as example 1.
The test results show that: the light-off temperature (Tig) of the catalyst prepared in step 4) of comparative example 4 was 346 ℃, and fig. 6 is a graph showing the catalytic effect of the catalyst prepared in comparative example 4.
The foregoing examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. A method for preparing a composite catalyst for an exhaust gas filter, comprising the steps of:
mixing a catalyst containing potassium with water, a water-soluble organic solvent and a surfactant to obtain a catalyst suspension; wherein the volume ratio of the water-soluble organic solvent to the water is 3:1; the water-soluble organic solvent is 2-butanone and dioxane, and the volume ratio of the dioxane to the 2-butanone is 1:1;
immersing the carrier in the catalyst suspension, and sintering to obtain a composite catalyst;
the catalyst containing potassium is La 0.6 K 0.4 CoO 3 。
2. The method for preparing a composite catalyst for an exhaust gas filter according to claim 1, wherein the carrier is at least one selected from the group consisting of an alumina carrier, a silica gel carrier and an activated carbon carrier.
3. The method for preparing a composite catalyst for an exhaust gas filter according to any one of claims 1 to 2, wherein the impregnation conditions are as follows: soaking for 1-24 h at 15-30 ℃.
4. The method for producing a composite catalyst for an exhaust gas filter according to any one of claims 1 to 2, wherein the mass concentration of the catalyst is 1% to 20% based on the total mass of the catalyst suspension.
5. The method for preparing a composite catalyst for an exhaust gas filter according to any one of claims 1 to 2, wherein the sintering conditions are as follows: sintering for 1-24 h at 300-1000 ℃.
6. The method for producing a composite catalyst for an exhaust gas filter according to any one of claims 1 to 2, wherein the mass concentration of the surfactant is 0.0001% to 0.02% based on the total mass of the catalyst suspension.
7. A method for preparing a catalyst suspension for an exhaust gas filter, comprising the steps of:
mixing a catalyst containing potassium with water and a water-soluble organic solvent to obtain a catalyst suspension, wherein the catalyst containing potassium is La 0.6 K 0.4 CoO 3 ；
The volume ratio of the water-soluble organic solvent to the water is 3:1, the water-soluble organic solvent is 2-butanone and dioxane, and the volume ratio of the dioxane to the 2-butanone is 1:1.
8. A catalyst suspension for an exhaust gas filter, characterized by being produced by the method for producing a catalyst suspension for an exhaust gas filter according to claim 7.
9. A composite catalyst for an exhaust gas filter, characterized by being produced by the method for producing a composite catalyst for an exhaust gas filter according to any one of claims 1 to 6.
10. An exhaust gas filter comprising the composite catalyst for an exhaust gas filter according to claim 9.
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