CN101791560A - Method for improving activity of supported copper oxide-manganese oxide composite catalyst - Google Patents
Method for improving activity of supported copper oxide-manganese oxide composite catalyst Download PDFInfo
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- CN101791560A CN101791560A CN201010127514.5A CN201010127514A CN101791560A CN 101791560 A CN101791560 A CN 101791560A CN 201010127514 A CN201010127514 A CN 201010127514A CN 101791560 A CN101791560 A CN 101791560A
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- catalyst
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- gamma
- al2o3
- manganese oxide
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- 239000003054 catalyst Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000002131 composite material Substances 0.000 title claims abstract description 13
- 230000000694 effects Effects 0.000 title claims abstract description 11
- DLXAZYQCSSNEPD-UHFFFAOYSA-N [O-2].[Mn+2].[Cu]=O Chemical compound [O-2].[Mn+2].[Cu]=O DLXAZYQCSSNEPD-UHFFFAOYSA-N 0.000 title abstract 3
- 229910016978 MnOx Inorganic materials 0.000 claims abstract description 13
- 239000011572 manganese Substances 0.000 claims abstract description 13
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 238000001179 sorption measurement Methods 0.000 claims abstract description 3
- 238000001704 evaporation Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000007598 dipping method Methods 0.000 claims description 7
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 2
- 229910003158 γ-Al2O3 Inorganic materials 0.000 abstract 5
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 abstract 2
- 238000011278 co-treatment Methods 0.000 abstract 1
- 238000001514 detection method Methods 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 238000006555 catalytic reaction Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910052681 coesite Inorganic materials 0.000 description 4
- 229910052906 cristobalite Inorganic materials 0.000 description 4
- 230000008030 elimination Effects 0.000 description 4
- 238000003379 elimination reaction Methods 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 229910052682 stishovite Inorganic materials 0.000 description 4
- 229910052905 tridymite Inorganic materials 0.000 description 4
- 238000006424 Flood reaction Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 229910002451 CoOx Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910017566 Cu-Mn Inorganic materials 0.000 description 1
- 229910017871 Cu—Mn Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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Abstract
The invention provides a method for improving the activity of a supported copper oxide-manganese oxide composite catalyst. The method comprises the following steps: gamma-Al2O3 is calcined at 500 DEG C for 5 hours before being used as a carrier, BET of the gamma-Al2O3 is 162m<2>/g through N2 adsorption detection, 1 g of gamma-Al2O3 carrier is immersed with 0.1192g, 0.2383 g and 0.3973 gram of 0.05mol.L-1 Mn(CH3COO)2 respectively, is stirred for 1 hour, is evaporated at 100 DEG C in oil bath, is dried for 12 hours at 100 DEG C, and is calcined for 5 hours at 500 DEG C in air; the MnOx/gamma-Al2O3 carrier is immersed respectively with 9.4ml, 9.0ml and 8.5ml of 0.10mol.L-1 Cu(NO3)2 aqueous solution, is stirred for 1h, evaporated in oil bath at 100 DEG C, dried for 12h at 100 DEG C, and calcined for 5h at 500 DEG C under the air atmosphere; and after CuO/MnOx/gamma-Al2O3 catalyst is activated with N2 at 100 DEG C for 1 hour, CO-He gas is introduced to the catalyst for 1 hour after the catalyst is heated to 325 DEG C (the volume ratio of CO gas to He gas is 0.016:0.984) so as to prepare the high-activity supported copper oxide-manganese oxide composite catalyst. The treatment method adopted by the invention has the advantages that: CO treatment catalyst is simple and easy to implement, and after the catalyst is treated by CO, the catalytic activity is obviously improved.
Description
Technical field
The present invention relates to the processing method of support type cupric oxide-manganese oxide composite catalyst.
Background technology
NO
XThe elimination of compound research has become extremely important in the past more than 20 year.In recent years, a lot of methods has been used for the elimination of oxynitrides.In order to satisfy the discharge standard of strict environment Litter, catalysis is eliminated oxynitrides and has been caused world wide scientific research personnel's extensive concern.The CO reductive NO is the catalysis removing method of a kind of important elimination NO.
Show good performance because noble metal catalyst is eliminated NO in catalysis at present, people select Pt mostly for use, Rh, and noble metals such as Pd are eliminated NO as catalyst.The nineties in 20th century, Mergler YZ[Mergler YZ, Aalst AV, Delft JV, Nieuwenhuys BE.Promoted Pt catalysts for automotive pollution control:characterization of Pt/SiO2, Pt/CoOx/SiO2, and Pt/MnOx/SiO2 catalysts.J Catal1996; 161:310-8.] etc. the Pt/MnOx/SiO2 catalysis of people preparation in the reaction of CO reductive NO, demonstrate good catalytic activity.But because the noble metal fancy price makes its application be subjected to certain restriction, people have turned to sight cheap gradually, the research of the transition metal oxide that catalytic performance is good.Transition metal oxide is (as V
2O
5, Fe
2O
3, CuO, Cr
2O
3, Mn
2O
3, MnO
2) usually be applied to the research [G.Ramis, F.Berti, Appl.Catal.B 18 (1998) 1 for G.Busca, L.Lietti] of catalyst together with other oxidation.MnO in the transition metal
xIn the Mn element owing to have+2 ,+3 ,+4 ,+5 ,+6, more than+7 kind of valence state shows good activity and is subjected to extensive attention in oxidation-reduction catalyst.People are with simple MnO the earliest
xMake catalyst, studied NO and N as Yamashita and Vannice
2O is at MnO
xOn decomposition, find Mn
2O
3To NO and N
2O has higher activity [J.Catal.161 (1996) 254.T.Yamashita, A.Vannice, J.Catal.163 (1996) 158 for T.Yamashita, A.Vannice].Simultaneously, the copper base oxide is to NO
xThe elimination of compound also demonstrates good catalytic activity.People are again with MnO subsequently
xWith other metal such as Cu, Ce etc. prepare composite metal oxide as catalyst [I.Spassova, M.Khristova, D.Panayotov, D.Mehandjiev, J.Catal.185 (1999) 43.; K.Tikhomirov, O.
M.Elsener, A.Wokaun, Appl.Catal.B:Environ.64 (2006) 72.; D.Delimaris, T.Ioannides, Appl.Catal.B:Environ.84 (2008) 303.], prepared CuO-MnO as Spassova etc. [D.Panayotov, D.Mehandjiev, J.Catal.185 (1999) 43. for I.Spassova, M.Khristova]
xO composite metallic oxide catalyst is studied its activity in the NO-CO reaction, finds to generate CuMn
2O
4Spinelle is the high main cause of catalyst activity.What adopt mostly in the Cu-Mn system all is not have the composite metal oxide of carrier as catalyst, generates CuMn when high-temperature roasting
2O
4Spinelle.
In recent years, the method with atmosphere processing catalyst is in the news successively.Lu-Cun Wang[Lu-Cun Wang, Lin He, Yong-Mei Liu, Yong Cao, et al., Journal of Catalysis 264 (2009) 145-153] etc. the people use O respectively
2, H
2, He is to Au/a-Mn
2O
3Catalyst is handled.TEM result shows that the difference of handling atmosphere has very important influence to the size of gold particle.H
2Over reduction will obviously reduce catalytic activity.Therefore the selection of treatment temperature seems particularly important when catalyst is handled in selective reduction.
Summary of the invention
We prepare the CuO/MnOx/ γ-Al of CuO and MnOx high degree of dispersion by cheap raw material
2O
3Catalyst can be determined suitable treatment temperature very exactly by simple CO-TPR experiment, makes CuO/MnOx/ γ-Al
2O
3The catalytic activity of catalyst significantly improves, so the method for this atmosphere processing catalyst has good prospects for application.
Purpose of the present invention: a kind of processing CuO/MnOx/ γ-Al is provided
2O
3The method of catalyst is with the CuO/MnOx/ γ-Al after the CO processing
2O
3In the catalyst, Cu
2+Restore All has become Cu
0And Cu
+, Mn
3+Partial reduction has become Mn
2+, simultaneously at Cu
+And Mn
2+Between form collaborative oxygen room, surface, the decomposition of this highly beneficial NO.It is expected to be applied to the bimetal composite oxide catalytic oxidation and eliminates NO
X
Principle of the present invention is as follows: at first respectively MnOx and CuO are loaded to γ-Al by conventional step impregnation method
2O
3On, the sample that obtains is through high-temperature roasting.Determine that by the CO-TPR experiment CO handles the temperature of catalyst.Sample is through 100 ℃ of N
2Feed CO-He gas 1h. when temperature is elevated to 325 ℃ behind the activation processing 1h
The object of the present invention is achieved like this:
A kind of method that improves support type cupric oxide-manganese oxide composite catalyst activity, it is made up of following steps:
Step 1. is with γ-Al
2O
3Be used as carrier before through 500 ℃ of roasting 5h, through N
2Determining adsorption, its BET are 162m
2/ g uses 0.1192,0.2383,0.3973 gram Mn (CH respectively
3COO)
24H
2O aqueous solution dipping γ-Al
2O
3Carrier 1 gram stirs 1h, 100 ℃ of evaporating water of oil bath, and at 100 ℃ of dry 12h, the following 500 ℃ of roasting 5h of air atmosphere; Sample is recited as 03MnAl respectively; 06MnAl; 10MnAl.
The MnO that step 2. obtains with step 1
x/ γ-Al
2O
3Be carrier, use 9.40,9.00 respectively, the 0.10molL of 8.50ml
-1Cu (NO
3)
23H
2O aqueous solution dipping 03MnAl, 06MnAl, the 10MnAl carrier stirs 1h, 100 ℃ of evaporating water of oil bath, at 100 ℃ of dry 12h, the following 500 ℃ of roasting 5h of air atmosphere; Sample is recited as 06Cu03MnAl respectively; 06Cu 06MnAl; 06Cul0MnAl
CuO/MnOx/ γ-Al that step 3. is prepared with step 2
2O
3Catalyst is through 100 ℃ of N
2Behind the activation processing 1h, feed CO-He gas 1h (volume ratio of CO and He gas 0.016: 0.984) when temperature is elevated to 325 ℃, promptly obtain highly active support type cupric oxide-manganese oxide composite catalyst.
The advantage of processing method of the present invention is: CO handles the simple realization easily of catalyst, and catalyst is after CO handles, and catalytic activity is significantly improved.
Description of drawings
Fig. 1: CO-TPR lab diagram;
Fig. 2: the inventive method is handled the characterization result figure of catalyst,
(A) XRD figure of fresh sample (B) CO handles the XRD figure of back sample
Fig. 3: catalyst activity and selectivity comparison diagram before and after handling.
The specific embodiment
Preparation process is divided into two Main Stage:
1. Preparation of catalysts
Respectively MnOx and CuO are loaded to γ-Al by conventional step impregnation method
2O
3On, the sample that obtains is through 500 ℃ of high-temperature roasting 1h.
Embodiment 1 usefulness 0.1192 gram Mn (CH
3COO)
24H
2O floods γ-Al
2O
3Carrier 1 gram stirs 1h, 100 ℃ of evaporating water of oil bath, and at 100 ℃ of dry 12h, the following 500 ℃ of roasting 5h of air atmosphere; Sample is recited as 03MnAl respectively.With 03MnAl is carrier, with the 0.10molL of 9.4ml
-1Cu (NO
3)
23H
2O aqueous solution dipping stirs 1h, 100 ℃ of evaporating water of oil bath, and at 100 ℃ of dry 12h, the following 500 ℃ of roasting 5h of air atmosphere; Sample is recited as 06Cu03MnAl respectively;
Embodiment 2 usefulness 0.2383 gram Mn (CH
3COO)
24H
2O floods γ-Al
2O
3Carrier 1 gram stirs 1h, 100 ℃ of evaporating water of oil bath, and at 100 ℃ of dry 12h, the following 500 ℃ of roasting 5h of air atmosphere; Sample is recited as 03MnAl respectively.With 03MnAl is carrier, with the 0.10molL of 9.0ml
-1Cu (NO
3)
23H
2O aqueous solution dipping stirs 1h, 100 ℃ of evaporating water of oil bath, and at 100 ℃ of dry 12h, the following 500 ℃ of roasting 5h of air atmosphere; Sample is labeled as 06Cu06MnAl respectively;
Embodiment 3 usefulness 0.3973 gram Mn (CH
3COO)
24H
2O floods γ-Al
2O
3Carrier 1 gram stirs 1h, 100 ℃ of evaporating water of oil bath, and at 100 ℃ of dry 12h, the following 500 ℃ of roasting 5h of air atmosphere; Sample is recited as 03MnAl respectively.With 03MnAl is carrier, with the 0.10molL of 8.5ml
-1Cu (NO
3)
23H
2O aqueous solution dipping stirs 1h, 100 ℃ of evaporating water of oil bath, and at 100 ℃ of dry 12h, the following 500 ℃ of roasting 5h of air atmosphere; Sample is labeled as 06Cu03MnAl respectively;
2. the processing of catalyst
In quartzy microreactor, carry out, adopt thermal conductivity detector (TCD).Amount of samples 100mg, elder generation is through N before heating up
2Purge 1h at 100 ℃, be cooled to room temperature after, switch to CO+N
2Gaseous mixture, wherein CO accounts for 1.6% (percent by volume), its flow velocity 12mLmin
-1, heating rate is 2 ℃ of min
-1Catalyst after the processing is labeled as 06Cu03MnAl-CO respectively; 06Cu06MnAl-CO; 06Cul0MnAl-CO;
In order to ensure Cu
2+All become Cu
0And Cu
+, at first carry out CuO/ γ-Al
2O
3CO-TPR experiment.300-400 ℃ of temperature range, can produce Cu simultaneously when observing individualism CuO species
0And Cu
+Ion is so treatment temperature has been selected 325 ℃ of (see figure 1)s.
Embodiment 4.
The conversion ratio of table 1 NO
Table 2 N
2Conversion ratio
Claims (1)
1. method that improves support type cupric oxide-manganese oxide composite catalyst activity is characterized in that it is made up of following steps:
Step 1. is with γ-Al
2O
3Be used as carrier before through 500 ℃ of roasting 5h, through N
2Determining adsorption, its BET are 162m
2/ g uses 0.1192,0.2383,0.3973 gram Mn (CH respectively
3COO)
2Dipping γ-Al
2O
3Carrier 1 gram stirs 1h, 100 ℃ of evaporating water of oil bath, and at 100 ℃ of dry 12h, the following 500 ℃ of roasting 5h of air atmosphere;
The MnO that step 2. obtains with step 1
x/ γ-Al
2O
3Be carrier, use 9.4,9.0 respectively, the 0.10molL of 8.5ml
-1Cu (NO
3)
2Aqueous solution dipping MnO
x/ γ-Al
2O
3Carrier stirs 1h, 100 ℃ of evaporating water of oil bath, and at 100 ℃ of dry 12h, the following 500 ℃ of roasting 5h of air atmosphere;
CuO/MnOx/ γ-Al that step 3. is prepared with step 2
2O
3Catalyst is through 100 ℃ of N
2Behind the activation processing 1h, feed CO-He gas 1h (volume ratio of CO and He gas 0.016: 0.984) when temperature is elevated to 325 ℃, promptly obtain highly active support type cupric oxide-manganese oxide composite catalyst.
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|---|---|---|---|
| CN201010127514.5A CN101791560A (en) | 2010-03-18 | 2010-03-18 | Method for improving activity of supported copper oxide-manganese oxide composite catalyst |
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| Publication Number | Publication Date |
|---|---|
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Family
ID=42584605
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102671691A (en) * | 2012-05-28 | 2012-09-19 | 四川君和环保工程有限公司 | Low-temperature SCR (Selective Catalytic Reduction) denitrification catalyst, as well as preparation method and application thereof |
| CN102962076A (en) * | 2012-12-17 | 2013-03-13 | 南京大学 | Method for preparing supported type bimetal oxide nano catalyst |
| CN102974347A (en) * | 2012-12-03 | 2013-03-20 | 南京大学 | Method for preparing copper-based nano-catalyst with different valence states |
| CN105536804A (en) * | 2015-12-04 | 2016-05-04 | 重庆大学 | Mn and Ce doped Cu based methane combustion catalyst and preparation method thereof |
| CN108906075A (en) * | 2018-08-01 | 2018-11-30 | 兰州大学 | CuO-MnFe2O4Composite material and preparation method and catalyst and application |
| CN112044440A (en) * | 2019-06-06 | 2020-12-08 | 中南大学 | Catalyst for preparing chlorine gas by catalytic oxidation of hydrogen chloride and preparation method and application thereof |
-
2010
- 2010-03-18 CN CN201010127514.5A patent/CN101791560A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 《催化学报》 20091115 董林 "负载型催化剂的表面相互作用及其在大气分子污染物NO和CO消除中的应用基础研究" 第1.3节 1 第30卷, 第11期 2 * |
| 《无机化学学报》 20070310 张丽萍等 "CO预处理对CuO/gamma-Al2O3催化剂性能的影响" 第1.1节 1 第23卷, 第3期 2 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102671691A (en) * | 2012-05-28 | 2012-09-19 | 四川君和环保工程有限公司 | Low-temperature SCR (Selective Catalytic Reduction) denitrification catalyst, as well as preparation method and application thereof |
| CN102974347A (en) * | 2012-12-03 | 2013-03-20 | 南京大学 | Method for preparing copper-based nano-catalyst with different valence states |
| CN102974347B (en) * | 2012-12-03 | 2015-05-20 | 南京大学 | Method for preparing copper-based nano-catalyst with different valence states |
| CN102962076A (en) * | 2012-12-17 | 2013-03-13 | 南京大学 | Method for preparing supported type bimetal oxide nano catalyst |
| CN102962076B (en) * | 2012-12-17 | 2014-10-22 | 南京大学 | Method for preparing supported type bimetal oxide nano catalyst |
| CN105536804A (en) * | 2015-12-04 | 2016-05-04 | 重庆大学 | Mn and Ce doped Cu based methane combustion catalyst and preparation method thereof |
| CN108906075A (en) * | 2018-08-01 | 2018-11-30 | 兰州大学 | CuO-MnFe2O4Composite material and preparation method and catalyst and application |
| CN108906075B (en) * | 2018-08-01 | 2021-07-02 | 兰州大学 | CuO-MnFe2O4Composite material and preparation method thereof, catalyst and application |
| CN112044440A (en) * | 2019-06-06 | 2020-12-08 | 中南大学 | Catalyst for preparing chlorine gas by catalytic oxidation of hydrogen chloride and preparation method and application thereof |
| CN112044440B (en) * | 2019-06-06 | 2021-09-10 | 中南大学 | Catalyst for preparing chlorine gas by catalytic oxidation of hydrogen chloride and preparation method and application thereof |
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