CN115957621A - Application of manganese oxide in catalytic decomposition of mixed mercaptan - Google Patents
Application of manganese oxide in catalytic decomposition of mixed mercaptan Download PDFInfo
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- CN115957621A CN115957621A CN202310044687.8A CN202310044687A CN115957621A CN 115957621 A CN115957621 A CN 115957621A CN 202310044687 A CN202310044687 A CN 202310044687A CN 115957621 A CN115957621 A CN 115957621A
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- mercaptan
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- manganese oxide
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- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 title claims abstract description 44
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 title claims abstract description 27
- 238000003421 catalytic decomposition reaction Methods 0.000 title claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 239000002244 precipitate Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 3
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- SUVIGLJNEAMWEG-UHFFFAOYSA-N propane-1-thiol Chemical compound CCCS SUVIGLJNEAMWEG-UHFFFAOYSA-N 0.000 claims description 12
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 2
- -1 methyl-ethyl Chemical group 0.000 description 10
- 239000012159 carrier gas Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000012495 reaction gas Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000003077 lignite Substances 0.000 description 3
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 150000003573 thiols Chemical class 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- LOCHFZBWPCLPAN-UHFFFAOYSA-N butane-2-thiol Chemical compound CCC(C)S LOCHFZBWPCLPAN-UHFFFAOYSA-N 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
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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
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Abstract
The invention discloses an application of manganese oxide in catalytic decomposition of mixed mercaptan, wherein the manganese oxide is prepared by dissolving potassium permanganate and ammonium oxalate in deionized water, uniformly stirring, reacting at 80-100 ℃ for 22-26 h, centrifuging, collecting precipitate, washing and drying the precipitate; introducing the mixed mercaptan into the tank containing MnO 2 In the reactor of the catalyst, the space velocity is 5000-50000 h ‑1 The method is simple, easy to operate and suitable for industrial production and market popularization and application.
Description
Technical Field
The invention relates to application of manganese oxide in catalytic decomposition removal of mixed mercaptan, belonging to the technical field of removal of sulfur-containing volatile organic pollutants.
Background
Lignite has abundant reserves in China, lignite gasification is a main clean coal technology, a large amount of sulfur-containing volatile organic pollutants are generated in the lignite gasification process, and mercaptan is mainly used. The mercaptan has the characteristics of extremely low odor threshold, unpleasant odor, high volatility, high toxicity, high corrosiveness and the like, is incorporated into the odor pollutant array, and has strict emission standards in national standard of the people's republic of China (emission Standard of odor pollutants) (GB-14554-93). In recent years, researchers at home and abroad attach more and more importance to the removal of mercaptan.
The research on mercaptans in the past has focused mainly on the removal of methyl mercaptan and has led to very important results. However, in addition to methyl mercaptan, there are some other organic mercaptans such as ethyl mercaptan, propyl mercaptan, etc. in sulfur-containing volatile organic pollutants, and there is little research on them. Furthermore, there are many studies on single thiols in the current study, but few studies on mixed thiol removal.
Disclosure of Invention
The invention provides MnO 2 A new use of, i.e. MnO 2 The manganese oxide is prepared by dissolving potassium permanganate and ammonium oxalate in deionized water, uniformly stirring, reacting at 80-100 ℃ for 22-26 h, centrifuging reaction products, collecting precipitate, washing the precipitate, and drying, wherein the dosage of the potassium permanganate is 18-22 mmol, and the dosage of the ammonium oxalate is 8-12 mmol.
The mixed mercaptan is methyl mercaptan (CH) 3 SH), ethanethiol (CH) 3 CH 2 SH), propanethiol (CH) 3 CH 3 CH 2 SH), wherein the concentration of methyl mercaptan, ethyl mercaptan and propyl mercaptan is 50-10000 ppm respectively.
The method is specifically operated byIntroduction of mixed mercaptans into the atmosphere containing MnO 2 In the reactor of the catalyst, the space velocity is 5000-50000 h -1 The reaction is carried out at normal pressure and 30-400 ℃, and the mixed mercaptan is removed simultaneously.
Advantages and technical effects of the invention
1. The invention explores MnO 2 The function in the mixed mercaptan can lay a certain foundation for the research of the subsequent mixed mercaptan, and can provide some ideas for the research of mixed systems of other polluted gases;
2. MnO prepared by the invention 2 The catalyst has a good removing effect on methyl-ethyl mixed mercaptan and methyl-propyl mixed mercaptan, and can completely remove the mercaptan in a mixed system;
the preparation process of the manganese oxide is simple and is suitable for industrial production and market popularization and application.
Drawings
FIG. 1 shows MnO prepared according to the present invention 2 XRD contrast with other manganese oxides;
FIG. 2 shows MnO prepared according to the present invention 2 The shape of the manganese oxide is compared with other manganese oxides, and A picture is MnO prepared by the method 2 The morphology of (2); b is alpha-MnO 2 The shape (nano rod shape) of the C picture is beta-MnO 2 Morphology (nanorod-like);
FIG. 3 shows MnO in example 1 2 A catalytic activity diagram of methyl-ethyl mixed mercaptan at different temperatures;
FIG. 4 shows MnO in example 2 2 A catalytic activity diagram of methyl-propyl mixed mercaptan at different temperatures;
FIG. 5 shows MnO in example 3 2 A stability profile for methyl ethyl mixed mercaptans;
FIG. 6 shows MnO in example 4 2 Stability profile for methyl propyl mixed thiol.
Detailed description of the preferred embodiments
The present invention is further illustrated in detail by the following examples, but the scope of the present invention is not limited to the above-described contents, and the methods in the examples are all conventional methods unless otherwise specified, and reagents are all conventional reagents or reagents prepared by conventional methods unless otherwise specified;
example 1: in thatMnO at different temperatures 2 Catalytic activity on methyl-ethyl mixed mercaptan
1. 20mmol of KMnO 4 、10mmol (NH 4 ) 2 C 2 O 4 Dissolving in 80mL of water, mixing, placing the mixture in a hydrothermal reaction kettle, carrying out hydrothermal reaction at 90 ℃ for 24h, centrifuging the reaction product, collecting precipitate, washing the precipitate with deionized water for 3 times, drying the washed precipitate in an oven at 105 ℃ for 12h, tabletting the obtained powder, crushing and sieving to obtain 40-60 mesh MnO 2 Catalyst, mnO prepared in this example 2 The XRD of the catalyst is shown in FIG. 1, from which it can be seen that MnO was prepared according to the present invention 2 The crystallinity of the manganese oxide is greatly different from that of other manganese oxides, and the manganese oxide has lower crystallinity and is of an amorphous structure; mnO made in this example 2 The morphology of the catalyst is shown in figure 2, and the MnO prepared by the method can be seen from the figure 2 The morphology of (a) is mainly spherical.
2. Take 0.1g MnO 2 The catalyst is loaded into a tubular furnace reactor, and CH with the volume concentration of 100ppm is introduced 3 SH、100ppm CH 3 CH 2 Mixed reaction gas (N) of SH 2 As carrier gas), the pressure of the reaction system is normal pressure, and the space velocity of the feeding is 36000h -1 The results of decomposition of methyl and ethyl mixed mercaptans at a temperature of 30 to 400 ℃ are shown in FIG. 3, and show that the conversion of methyl and ethyl mercaptans in the mixed system is 100% in the temperature range of 30 to 400 ℃.
Example 2: mnO (MnO) 2 Catalytic activity of methyl-propyl mixed mercaptan at different temperatures
1. 18mmol of KMnO 4 、11mmol (NH 4 ) 2 C 2 O 4 Dissolving in 90mL of water, mixing uniformly, placing the mixture in a hydrothermal reaction kettle, carrying out hydrothermal reaction for 22 hours at 100 ℃, then centrifuging the reaction product, collecting precipitate, washing the precipitate with deionized water for 4 times, drying the washed precipitate in an oven at 105 ℃ for 12 hours, tabletting the obtained powder, crushing and sieving to obtain 40-60 mesh MnO 2 A catalyst, and a water-soluble organic solvent,
2. taking 0.1g of MnO 2 The catalyst is loaded into a tubular furnace reactor, and CH with the volume concentration of 100ppm is introduced 3 SH、100ppm CH 3 CH 3 CH 2 Mixed reaction gas (N) of SH 2 As carrier gas), the pressure of the reaction system is normal pressure, and the feeding airspeed is 36000h -1 The results of decomposition of methyl and ethyl mixed mercaptans at a temperature of 30 to 400 ℃ are shown in FIG. 4, and show that the conversion rates of methyl mercaptan and propyl mercaptan in the mixed system are 100% in the temperature range of 30 to 400 ℃.
Example 3: mnO 2 Stability experiment for catalytic decomposition of methyl-ethyl mixed mercaptan
1. MnO in this embodiment 2 The preparation process of the catalyst was the same as in example 1;
2. taking 0.1g of MnO 2 The catalyst is loaded into a tubular furnace reactor, and CH with the volume concentration of 100ppm is introduced 3 SH、100ppm CH 3 CH 2 Mixed reaction gas (N) of SH 2 As carrier gas), the pressure of the reaction system is normal pressure, and the space velocity of the feeding is 36000h -1 The reaction temperature is 30 ℃, the stability test of methyl mercaptan is carried out, the result is shown in fig. 5, the result shows that the catalytic decomposition of the catalyst in the mixed system on methyl mercaptan and ethyl mercaptan starts to be inactivated after 23h, the conversion rate of ethyl mercaptan is reduced to about 30% after 44h along with the time extension, and the conversion rate of methyl mercaptan is about 60%.
Example 4: mnO 2 Stability test for catalytic decomposition of methyl-propyl mixed mercaptan
1. MnO in this embodiment 2 The preparation process of the catalyst is the same as that of example 2;
2. taking 0.1g of MnO 2 The catalyst is loaded into a tubular furnace reactor, and CH with the volume concentration of 100ppm is introduced 3 SH、100ppm CH 3 CH 3 CH 2 Mixed reaction gas (N) of SH 2 As carrier gas), the pressure of the reaction system is normal pressure, and the space velocity of the feeding is 36000h -1
And the reaction temperature is 30 ℃, the stability test of methyl propyl mercaptan is carried out, the result is shown in figure 6, and the result shows that the catalytic decomposition of methyl mercaptan and propyl mercaptan in the mixed system begins to be inactivated after 38 hours.
Claims (4)
1. The use of manganese oxide for the catalytic decomposition of mixed mercaptans.
2. Use according to claim 1, characterized in that: the manganese oxide is prepared by dissolving potassium permanganate and ammonium oxalate in deionized water, uniformly stirring, reacting at 80-100 ℃ for 22-26 h, centrifuging reaction products, collecting precipitate, washing the precipitate and drying.
3. Use according to claim 1, characterized in that: the mixed mercaptan is gas containing several of methyl mercaptan, ethyl mercaptan and propyl mercaptan.
4. Use according to claim 1, characterized in that: introducing the mixed mercaptan into the tank containing MnO 2 In the reactor of the catalyst, the space velocity is 5000-50000 h -1 The reaction is carried out at normal pressure and 30-400 ℃, and the mixed mercaptan is removed simultaneously.
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