CN107519891A - A kind of preparation method of ternary metal oxide catalyst - Google Patents
A kind of preparation method of ternary metal oxide catalyst Download PDFInfo
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- CN107519891A CN107519891A CN201710845247.7A CN201710845247A CN107519891A CN 107519891 A CN107519891 A CN 107519891A CN 201710845247 A CN201710845247 A CN 201710845247A CN 107519891 A CN107519891 A CN 107519891A
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- metal oxide
- oxide catalyst
- ternary metal
- stirring
- added dropwise
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- 239000003054 catalyst Substances 0.000 title claims abstract description 19
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 12
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- AEJIMXVJZFYIHN-UHFFFAOYSA-N copper;dihydrate Chemical compound O.O.[Cu] AEJIMXVJZFYIHN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims abstract description 6
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims abstract description 6
- 229940099607 manganese chloride Drugs 0.000 claims abstract description 6
- 235000002867 manganese chloride Nutrition 0.000 claims abstract description 6
- 239000011565 manganese chloride Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 238000005119 centrifugation Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical group [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 229910052748 manganese Inorganic materials 0.000 abstract description 3
- 239000011572 manganese Substances 0.000 abstract description 3
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000000536 complexating effect Effects 0.000 abstract description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 42
- 239000007789 gas Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 150000002927 oxygen compounds Chemical class 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 244000248349 Citrus limon Species 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002912 waste gas Substances 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
- 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
- B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
-
- 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
- B01J37/08—Heat treatment
-
- 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
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation method of ternary metal oxide catalyst, step are as follows：4~5g Kocide SDs are added into 100~200mL water, stirring, 3~10g/L 20~100mL of citric acid solution is slowly added dropwise thereto simultaneously, after being added dropwise to complete, add 4~6g of 2~3g of manganese chloride and iron chloride, it is transferred to after stirring and dissolving in the hydrothermal reaction kettle of polytetrafluoroethylsubstrate substrate, reaction 18~24h after natural cooling is put into baking oven at 160~200 DEG C, solids is obtained after centrifugation to wash, dry by deionized water, 4~6h of calcining at 450~550 DEG C is placed in Muffle furnace again, produces a kind of ternary metal oxide catalyst.Molysite and manganese salt form Manganese Ferrite, citric acid and Kocide SD slow reaction under hydro-thermal, complex compound are progressively formed with the Manganese Ferrite of formation, three's complexing is abundant, forms uniformly compound ternary system.
Description
Technical field
The present invention relates to a kind of preparation method for the ternary metal oxide catalyst for handling nitrogen oxides, belong to catalysis material
Expect preparation field.
Background technology
Nitrogen oxides (NOx) is to cause one of major pollutants of atmosphere pollution.Wherein 57% comes from stationary source, such as steel
Waste gas caused by the combustion of fossil fuel such as iron, thermal power generation, cement, coal-burning boiler.Discharge capacity every year from national motor vehicle
Up to 583.3 ten thousand tons, more than 90% is nitric oxide (NO).The most frequently used NOx Treatment process is selective catalytic reduction
(SCR), but this method needs, with higher reaction temperature (being usually 200~400 DEG C), not being applied in hemi-closure space
NOx normal temperature eliminates.Using gas phase selective catalytic oxidation, i.e., by NO catalysis oxidations it is first NO2, then carry out absorption with alkali lye and disappear
Remove, be a kind of effective method.It is at most active carbon fibre that catalysis material currently used for NO room-temperature catalytic oxidations, which is reported,
Tie up (ACF), NACF or activated carbon (AC) of alkali lye coating or doping vario-property etc., such catalysis material has larger ratio
Surface area, more pore structure and surface functional group, mainly reacted by being reoxidized to NO absorption, but it is caused
NO2 is easily absorbing in carbon surface, with NO2Increase, Adsorption is reduced, activity decrease, can not meet it is actual should
With demand, therefore it is badly in need of developing the room-temperature catalytic oxidation NO catalyst that a kind of activity is high, stability is good, there is efficient stable
Property, the purification for pollutant in hemi-closure space.
The content of the invention
The purpose of the present invention is for the deficiency such as overcome existing catalyst activity low, there is provided a kind of ternary metal oxide catalysis
The preparation method of agent.
The technical solution adopted by the present invention is in turn include the following steps：
4~5g Kocide SDs, stirring are added into 100~200mL water, while 3~10g/L lemon is slowly added dropwise thereto
Lemon 20~100mL of acid solution, after being added dropwise to complete, 4~6g of 2~3g of manganese chloride and iron chloride is added, is transferred to after stirring and dissolving
In the hydrothermal reaction kettle of polytetrafluoroethylsubstrate substrate, reaction 18~24h after natural cooling is put into baking oven at 160~200 DEG C, from
Solids is obtained after the heart to wash, dry by deionized water, then is placed in Muffle furnace 4~6h of calcining at 450~550 DEG C, i.e.,
Obtain a kind of ternary metal oxide catalyst.
It is an advantage of the invention that：
Molysite and manganese salt form Manganese Ferrite, citric acid and Kocide SD slow reaction under hydro-thermal, progressively with the iron of formation
Sour manganese forms complex compound, and three's complexing is abundant, forms uniformly compound ternary system.
Embodiment
3 embodiments of the present invention are provided further below：
Embodiment 1
5g Kocide SDs, stirring are added into 200mL water, while 10g/L citric acid solution is slowly added dropwise thereto
100mL, after being added dropwise to complete, manganese chloride 3g and iron chloride 6g are added, the water of polytetrafluoroethylsubstrate substrate is transferred to after stirring and dissolving
In thermal response kettle, natural cooling after reaction 24h is put into baking oven at 200 DEG C, solids is obtained after centrifugation and passes through deionized water
Washing, dry, then be placed in Muffle furnace and calcine 4h at 550 DEG C, produce a kind of ternary metal oxide catalyst.
Using U-tube (internal diameter 4mm), continuously flowing reaction evaluating device, weighing 100mg synthesize obtained ternary metal oxygen
Compound catalyst is placed in pipe, and the flow velocity for adjusting air is 25mL/min, and air flow drives NO gases to enter U-tube reactor
In, the gas volume (i.e. air speed) for flowing through every liter of catalyst per hour is 6000h-1.Under the conditions of 30 DEG C, NO initial concentrations are
15ppm, NO conversion ratio are 97.1%.
Embodiment 2
4g Kocide SDs, stirring are added into 100mL water, while 3g/L citric acid solution is slowly added dropwise thereto
20mL, after being added dropwise to complete, manganese chloride 2g and iron chloride 4g are added, the hydro-thermal of polytetrafluoroethylsubstrate substrate is transferred to after stirring and dissolving
In reactor, natural cooling after reaction 18h is put into baking oven at 160 DEG C, solids is obtained after centrifugation and is washed by deionization
Wash, dry, then be placed in Muffle furnace and calcine 6h at 450 DEG C, produce a kind of ternary metal oxide catalyst.
Using U-tube (internal diameter 4mm), continuously flowing reaction evaluating device, weighing 100mg synthesize obtained ternary metal oxygen
Compound catalyst is placed in pipe, and the flow velocity for adjusting air is 25mL/min, and air flow drives NO gases to enter U-tube reactor
In, the gas volume (i.e. air speed) for flowing through every liter of catalyst per hour is 6000h-1.Under the conditions of 30 DEG C, NO initial concentrations are
17ppm, NO conversion ratio are 95.3%.
Embodiment 3
5g Kocide SDs, stirring are added into 150mL water, while 8g/L citric acid solution is slowly added dropwise thereto
70mL, after being added dropwise to complete, manganese chloride 2.5g and iron chloride 6g are added, the water of polytetrafluoroethylsubstrate substrate is transferred to after stirring and dissolving
In thermal response kettle, natural cooling after reaction 24h is put into baking oven at 200 DEG C, solids is obtained after centrifugation and passes through deionized water
Washing, dry, then be placed in Muffle furnace and calcine 5h at 550 DEG C, produce a kind of ternary metal oxide catalyst.
Using U-tube (internal diameter 4mm), continuously flowing reaction evaluating device, weighing 100mg synthesize obtained ternary metal oxygen
Compound catalyst is placed in pipe, and the flow velocity for adjusting air is 25mL/min, and air flow drives NO gases to enter U-tube reactor
In, the gas volume (i.e. air speed) for flowing through every liter of catalyst per hour is 6000h-1.Under the conditions of 30 DEG C, NO initial concentrations are
20ppm, NO conversion ratio are 96.8%.
Claims (1)
- A kind of 1. preparation method of ternary metal oxide catalyst, it is characterized in that in turn including the following steps：4~5g Kocide SDs, stirring are added into 100~200mL water, while 3~10g/L citric acid is slowly added dropwise thereto 20~100mL of solution, after being added dropwise to complete, 4~6g of 2~3g of manganese chloride and iron chloride is added, poly- four are transferred to after stirring and dissolving In the hydrothermal reaction kettle of PVF substrate, reaction 18~24h after natural cooling is put into baking oven at 160~200 DEG C, after centrifugation Obtain solids to wash, dry by deionized water, then be placed in Muffle furnace 4~6h of calcining at 450~550 DEG C, produce one Kind ternary metal oxide catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710845247.7A CN107519891A (en) | 2017-09-19 | 2017-09-19 | A kind of preparation method of ternary metal oxide catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710845247.7A CN107519891A (en) | 2017-09-19 | 2017-09-19 | A kind of preparation method of ternary metal oxide catalyst |
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| Publication Number | Publication Date |
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| CN107519891A true CN107519891A (en) | 2017-12-29 |
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| CN201710845247.7A Withdrawn CN107519891A (en) | 2017-09-19 | 2017-09-19 | A kind of preparation method of ternary metal oxide catalyst |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115920889A (en) * | 2022-11-07 | 2023-04-07 | 上海交通大学 | Preparation and application of foamed spinel catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101507928A (en) * | 2009-03-23 | 2009-08-19 | 华南理工大学 | Ferro manganese composite oxides catalyst and preparation method and use thereof |
| CN102500298A (en) * | 2011-11-24 | 2012-06-20 | 武汉大学 | Preparation method of metal oxides and composite microspheres of metal oxides |
| CN103768939A (en) * | 2013-12-31 | 2014-05-07 | 杭州天蓝环保设备有限公司 | Denitration synergist and SNCR (selective non-catalytic reduction) denitration synergism method |
| CN104028281A (en) * | 2014-06-27 | 2014-09-10 | 北京林业大学 | Multiphase catalytic ozone oxidation depollution technology based on enhanced ozone adsorption and application thereof |
| CN106076348A (en) * | 2016-06-12 | 2016-11-09 | 常州大学 | A kind of Fe-Al-Ce ternary metal oxide method for preparing catalyst |
-
2017
- 2017-09-19 CN CN201710845247.7A patent/CN107519891A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101507928A (en) * | 2009-03-23 | 2009-08-19 | 华南理工大学 | Ferro manganese composite oxides catalyst and preparation method and use thereof |
| CN102500298A (en) * | 2011-11-24 | 2012-06-20 | 武汉大学 | Preparation method of metal oxides and composite microspheres of metal oxides |
| CN103768939A (en) * | 2013-12-31 | 2014-05-07 | 杭州天蓝环保设备有限公司 | Denitration synergist and SNCR (selective non-catalytic reduction) denitration synergism method |
| CN104028281A (en) * | 2014-06-27 | 2014-09-10 | 北京林业大学 | Multiphase catalytic ozone oxidation depollution technology based on enhanced ozone adsorption and application thereof |
| CN106076348A (en) * | 2016-06-12 | 2016-11-09 | 常州大学 | A kind of Fe-Al-Ce ternary metal oxide method for preparing catalyst |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115920889A (en) * | 2022-11-07 | 2023-04-07 | 上海交通大学 | Preparation and application of foamed spinel catalyst |
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Application publication date: 20171229 |