CN117943043A - Mullite type catalyst for denitration of marine diesel engine tail gas and preparation method thereof - Google Patents
Mullite type catalyst for denitration of marine diesel engine tail gas and preparation method thereof Download PDFInfo
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- CN117943043A CN117943043A CN202311729795.5A CN202311729795A CN117943043A CN 117943043 A CN117943043 A CN 117943043A CN 202311729795 A CN202311729795 A CN 202311729795A CN 117943043 A CN117943043 A CN 117943043A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 59
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 29
- 239000007789 gas Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 5
- 230000001105 regulatory effect Effects 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 3
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims description 17
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000004134 energy conservation Methods 0.000 abstract description 2
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 abstract description 2
- 229940082328 manganese acetate tetrahydrate Drugs 0.000 abstract description 2
- CESXSDZNZGSWSP-UHFFFAOYSA-L manganese(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Mn+2].CC([O-])=O.CC([O-])=O CESXSDZNZGSWSP-UHFFFAOYSA-L 0.000 abstract description 2
- HDCOFJGRHQAIPE-UHFFFAOYSA-N samarium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Sm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HDCOFJGRHQAIPE-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000011572 manganese Substances 0.000 description 13
- 229910002651 NO3 Inorganic materials 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 238000010335 hydrothermal treatment Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000000539 dimer Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000010718 Oxidation Activity Effects 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of environmental protection, and particularly relates to a mullite catalyst for denitration of marine diesel engine tail gas and a preparation method thereof. Sequentially adding samarium nitrate hexahydrate, potassium permanganate and manganese acetate tetrahydrate into deionized water, stirring for the first time, adding ferric nitrate nonahydrate after stirring uniformly, and regulating the pH value of the solution by using ammonia water after continuing stirring; and (3) carrying out hydrothermal reaction on the solution with the pH adjusted, centrifuging to collect precipitate after the reaction, and carrying out washing, constant-temperature drying and roasting treatment to obtain the mullite catalyst. The synthesis steps provided by the invention are simple, and the prepared mullite catalyst can improve the acidity of the catalyst, is easy to oxidize and remove NOx, improves the oxygen adsorption content on the surface of the catalyst, improves the oxygen storage capacity and improves the activity of the catalyst; the method can be used for denitration of the tail gas of the marine diesel engine, achieves the purposes of energy conservation and emission reduction, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a mullite catalyst for denitration of marine diesel engine tail gas and a preparation method thereof.
Background
With the continuous development of world trade and further advanced integration of economic globalization, NO x emitted from marine diesel exhaust severely pollutes the atmosphere and marine environment, which is one of the important reasons for ozone pollution and severe haze weather. At present, the concentration of NO x (x=1-2) discharged in the tail gas of most marine diesel engines in China is generally higher than 3.4 g/kW.h required by Tier III. Therefore, effective control of NO x emissions in marine diesel exhaust is an important component of atmospheric pollution control, and is a technical problem to be solved at present.
At present, the technology for reducing the emission of NO x in marine diesel engine tail gas mainly comprises the following steps: an in-plane purification control method and an out-of-plane control method. From the prior art, the in-machine control method can meet the Tier II standard discharged by the marine diesel engine NO x, but if the Tier III standard is met, the conventional engine is changed into a dual-fuel engine, and the in-machine control method also needs to be adopted. The Selective Catalytic Reduction (SCR) method is the most effective technology for controlling the tail gas NO x of the marine diesel engine outside the machine at present due to mature technology, wide application range and stable treatment effect. The NO x control principle of the technology is that urea or NH 3 is used as a reducing agent, NO x in tail gas is catalytically reduced to harmless N 2 under the action of a catalyst, and the catalyst is the core of the technology. At present, the international widely used marine diesel engine tail gas NO x controls the catalyst to be V 2O5-WO3/TiO2. But its further industrial application is greatly limited by its poor low temperature activity, narrow activity temperature window (350-450 ℃), poor hydrothermal stability and resistance to alkali poisoning, and the biotoxicity possessed by the V species themselves. Therefore, with the stricter environmental regulations and the comprehensive implementation of Tier III standard, the China shipping industry is urgent to develop a green environmental protection non-V-based NH 3 -SCR catalyst with wider activity temperature window, higher low temperature NO x catalytic activity and excellent hydrothermal stability.
Mullite, because of its excellent oxidation activity, higher thermal stability and lower manufacturing cost, is widely considered to be the most promising alternative to the conventional V 2O5-WO3/TiO2 catalyst for SCR catalysts for stationary and mobile source (marine) diesel exhaust NO x purification. However, its weaker acidity and stronger oxidation properties greatly limit its NO x purification operating temperature window. Therefore, how to improve the low temperature NH 3 -SCR activity of mullite oxides based on the prior art has been the focus of researchers.
Disclosure of Invention
Aiming at the problems of poor activity, narrow active temperature window and the like of the low-temperature NH 3 -SCR of the existing mullite-type oxide, the invention aims to solve the problems, and provides a preparation method of a mullite-type catalyst, wherein the prepared mullite-type catalyst has excellent low-temperature catalytic activity and wide NO x operating temperature window, and meanwhile has the advantages of low preparation cost and simple operating method.
In order to achieve the technical purpose, the invention adopts the following technical scheme;
the preparation method of the mullite catalyst for denitration of marine diesel engine tail gas comprises the following steps:
Sequentially adding samarium nitrate hexahydrate (Sm (NO 3)·6H2 O), potassium permanganate (KMnO 4) and manganese acetate tetrahydrate (Mn (CH 3COO)2·4H2 O) into deionized water, stirring for the first time, adding ferric nitrate nonahydrate (Fe (NO 3)3·9H2 O) after stirring continuously, regulating the pH of the solution by ammonia water, performing hydrothermal reaction on the solution after regulating the pH, centrifuging to collect precipitate after reaction, washing with water, drying at constant temperature, and roasting to obtain the mullite-type catalyst, wherein the value range of y is less than or equal to 0.1, and the molar ratio of Fe (NO 3)3·9H2 O to Sm (NO 3)·6H2 O) is 0.000875-0.003500:0.002500.
Further, in the step, sm (NO 3)·6H2O、KMnO4、Mn(CH3COO)2·4H2 O and deionized water are used in an amount of 0.002500mol:0.001500mol:0.003500mol:40-80 mL).
Further, in the step, the first stirring is magnetic stirring, and the duration is 10-30min.
Further, in the step, an optimal ratio of Fe (molar ratio of NO 3)3·9H2 O to Sm (NO 3)·6H2 O is 0.001750:0.002500) is defined.
Further, in the step, the duration of continuous stirring is 30-60min.
Further, in the step, the ammonia water adjusts the pH of the solution to 7-9.
Further, in the step, the hydrothermal temperature is 180 ℃; the hydrothermal duration is 12-24h.
Further, in the step, the drying temperature is 100-150 ℃ and the drying time is 12 hours; the roasting temperature is
Roasting for 4 hours at 400-550 ℃.
The mullite catalyst prepared by the invention is used for denitration of tail gas, and is particularly used for denitration of marine diesel engine tail gas.
The invention has the following advantages and remarkable effects:
(1) The mullite catalyst (SmMnFeO 5-y) provided by the invention has simple synthesis steps, and the prepared mullite catalyst can improve the acidity of the catalyst, is easy to oxidize NO x, can improve the oxygen adsorption content on the surface of the catalyst, improve the oxygen storage capacity and the catalyst activity, is used for denitration of tail gas of a marine diesel engine, and achieves the purposes of energy conservation and emission reduction.
(2) The catalytic activity of the catalyst can be obviously improved by doping the B-site element into the mullite oxide, the acidity of the catalyst is obviously improved after doping the Fe element, and meanwhile, one Mn 4+ site in the Mn-Mn dimer is replaced, a stable Mn-Fe dimer structure is formed, and the activity of NO oxide is obviously improved.
(3) The NH 3 -SCR performance of the mullite catalyst is evaluated, and compared with the pure mullite phase oxide (215-265 ℃) and the V 2O5-WO3/TiO2 (350-450 ℃) catalyst, the mullite catalyst provided by the invention has the advantages that the low-temperature activity and the activity temperature window (50-425 ℃) are obviously improved, and the substantial technical effect is obtained.
Drawings
FIG. 1 shows the NO X absorption rate of the mullite-type catalyst obtained in example 3.
FIG. 2 shows the NO x absorbance comparison for the mullite-type catalysts obtained in examples 1-3.
Detailed Description
The invention will be further illustrated with reference to specific examples. Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Unless otherwise defined, 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. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
Example 1:
Sequentially adding 0.002500mol Sm(NO3)·6H2O、0.001500mol KMnO4、0.003500mol Mn(CH3COO)2·4H2O to 40mL of deionized water, magnetically stirring for 30min, adding 0.000875mol of Fe (NO 3)3·9H2 O) to the solution, continuously stirring for 30min, adjusting pH to 9 with ammonia water, performing hydrothermal treatment at 180 ℃ for 12h, performing centrifugal washing, drying at 100 ℃ for 12h, and roasting at 550 ℃ for 4h to obtain the mullite catalyst.
Example 2:
Sequentially adding 0.002500mol Sm(NO3)·6H2O、0.001500mol KMnO4、0.003500mol Mn(CH3COO)2·4H2O to 40mL of deionized water, magnetically stirring for 30min, adding 0.003500mol of Fe (NO 3)3·9H2 O) to the solution, continuously stirring for 30min, adjusting pH to 9 with ammonia water, performing hydrothermal treatment at 180 ℃ for 12h, performing centrifugal washing, drying at 100 ℃ for 12h, and roasting at 550 ℃ for 4h to obtain the mullite catalyst.
Example 3:
Sequentially adding 0.002500mol Sm(NO3)·6H2O、0.001500mol KMnO4、0.003500mol Mn(CH3COO)2·4H2O to 40mL of deionized water, magnetically stirring for 30min, adding 0.001750mol of Fe (NO 3)3·9H2 O) to the solution, continuously stirring for 30min, adjusting pH to 9 with ammonia water, performing hydrothermal treatment at 180 ℃ for 12h, performing centrifugal washing, drying at 100 ℃ for 12h, and roasting at 550 ℃ for 4h to obtain the mullite catalyst.
Example 4:
sequentially adding 0.002500mol Sm(NO3)·6H2O、0.001500mol KMnO4、0.003500mol Mn(CH3COO)2·4H2O to 40mL of deionized water, magnetically stirring for 30min, adding 0.001750mol of Fe (NO 3)3·9H2 O) to the solution, continuously stirring for 30min, adjusting pH to 7 with ammonia water, performing hydrothermal treatment at 180 ℃ for 12h, performing centrifugal washing, drying at 100 ℃ for 12h, and roasting at 550 ℃ for 4h to obtain the mullite catalyst.
Example 5:
Sequentially adding 0.002500mol Sm(NO3)·6H2O、0.001500mol KMnO4、0.003500mol Mn(CH3COO)2·4H2O to 40mL of deionized water, magnetically stirring for 30min, adding 0.001750mol of Fe (NO 3)3·9H2 O) to the solution, continuously stirring for 30min, adjusting pH to 9 with ammonia water, performing hydrothermal reaction at 180 ℃ for 24h, performing centrifugal washing, drying at 100 ℃ for 12h, and roasting at 550 ℃ for 4h to obtain the mullite catalyst.
Example 6:
And synthesizing SmMnFeO y a catalyst by a hydrothermal method. Sequentially adding 0.002500mol Sm(NO3)·6H2O、0.001500mol KMnO4、0.003500mol Mn(CH3COO)2·4H2O to 40mL of deionized water, magnetically stirring for 30min, adding 0.001750mol of Fe (NO 3)3·9H2 O) to the solution, continuously stirring for 30min, adjusting pH to 9 with ammonia water, hydrothermal for 12h at 180 ℃, centrifuging, washing with water, drying for 12h at 150 ℃, and roasting for 4h at 550 ℃ to obtain the mullite catalyst.
Example 7:
Sequentially adding 0.002500mol Sm(NO3)·6H2O、0.001500mol KMnO4、0.003500mol Mn(CH3COO)2·4H2O to 40mL of deionized water, magnetically stirring for 30min, adding 0.001750mol of Fe (NO 3)3·9H2 O) to the solution, continuously stirring for 30min, adjusting pH to 9 with ammonia water, performing hydrothermal treatment at 180 ℃ for 12h, performing centrifugal washing, drying at 100 ℃ for 12h, and roasting at 400 ℃ for 4h to obtain the mullite catalyst.
Example 8:
Sequentially adding 0.002500mol Sm(NO3)·6H2O、0.001500mol KMnO4、0.003500mol Mn(CH3COO)2·4H2O to 30mL of deionized water, magnetically stirring for 30min, adding 0.001750mol of Fe (NO 3)3·9H2 O) to the solution, continuously stirring for 60min, adjusting pH to 9 with ammonia water, performing hydrothermal treatment at 180 ℃ for 12h, performing centrifugal washing, drying at 100 ℃ for 12h, and roasting at 550 ℃ for 4h to obtain the mullite catalyst.
Example 9:
Sequentially adding 0.002500mol Sm(NO3)·6H2O、0.001500mol KMnO4、0.003500mol Mn(CH3COO)2·4H2O to 40mL of deionized water, magnetically stirring for 10min, adding 0.001750mol of Fe (NO 3)3·9H2 O) to the solution, continuously stirring for 30min, adjusting pH to 9 with ammonia water, hydrothermal for 12h at 180 ℃, centrifuging, washing with water, drying at 150 ℃ for 12h, and roasting at 550 ℃ for 4h to obtain the mullite catalyst.
The synthesized catalyst was tested for performance, exemplified by mullite catalyst prepared in example 3, designated SFMO #. As can be seen from FIG. 1, compared with the conventional catalyst (the activity temperature is not less than 200 ℃), the mullite catalyst synthesized by the example 3 shows better low-temperature activity in NH 3 -SCR, the reaction NO x absorbs more than 99% at 55 ℃, and the activity window is obviously widened.
As can be seen from FIG. 2, the mullite-type catalysts obtained in examples 1 to 3 were respectively designated SFMO 1#, SFMO 2# and SFMO 3#, in examples 1 to 3, by varying the addition amount of Fe (NO 3)3·9H2 O) to determine the optimum content of Fe source, and the addition amount of Fe (NO 3)3·9H2 O) had a direct effect on the result, and the activity window of the resulting catalyst was the widest and the overall activity was the optimum when the addition amount of Fe (NO 3)3·9H2 O) was 0.001750mol, and unexpected substantial effects were obtained.
Description: the above embodiments are only for illustrating the present invention and not for limiting the technical solution described in the present invention; thus, while the invention has been described in detail with reference to the various embodiments described above, it will be understood by those skilled in the art that the invention may be modified or equivalents; all technical solutions and modifications thereof that do not depart from the spirit and scope of the present invention are intended to be included in the scope of the appended claims.
Claims (10)
1. The preparation method of the mullite catalyst for denitration of marine diesel engine tail gas is characterized by comprising the following steps of:
Sequentially adding Sm (NO 3)·6H2O、KMnO4、Mn(CH3COO)2·4H2 O) into deionized water, stirring for the first time, adding Fe (NO 3)3·9H2 O, continuously stirring, regulating the pH of the solution with ammonia water, performing hydrothermal reaction on the solution with the pH regulated, centrifuging to collect precipitate after reaction, washing with water, drying at constant temperature, and roasting to obtain a mullite catalyst which is denoted as SmMnFeO 5-y, wherein the value range of y is less than or equal to 0.1, and the molar ratio of Fe (NO 3)3·9H2 O to Sm (NO 3)·6H2 O is 0.000875-0.003500:0.002500).
2. The method for preparing mullite-based catalyst for denitration of marine diesel exhaust gas according to claim 1, wherein the dosage relationship of Sm (NO 3)·6H2O、KMnO4、Mn(CH3COO)2·4H2 O and deionized water is 0.002500mol:0.001500mol:0.003500mol:40-80 mL).
3. The method for preparing mullite-based catalyst for denitration of marine diesel exhaust gas according to claim 1, wherein the molar ratio of Fe (NO 3)3·9H2 O to Sm (NO 3)·6H2 O) is 0.001750:0.002500.
4. The method for preparing the mullite catalyst for denitration of marine diesel engine tail gas according to claim 1, wherein the first stirring is magnetic stirring for 10-30min; the duration of continuous stirring is 30-60min.
5. The method for preparing mullite catalyst for denitration of marine diesel exhaust gas according to claim 1, wherein the ammonia water adjusts the pH of the solution to 7-9.
6. The method for preparing the mullite catalyst for denitration of marine diesel exhaust gas according to claim 1, wherein the hydrothermal temperature is 180 ℃; the hydrothermal duration is 12-24h.
7. The method for preparing the mullite catalyst for denitration of marine diesel exhaust gas according to claim 1, wherein the drying temperature is 100-150 ℃ and the drying time is 12 hours; the roasting temperature is 400-550 ℃, and the roasting time is 4 hours.
8. A mullite-type catalyst prepared according to the process of any one of claims 1-7.
9. Use of the mullite catalyst of claim 8 for the denitration of exhaust gases.
10. Use according to claim 9, characterized in that the mullite catalyst is used for denitration of marine diesel exhaust.
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