CN1954912A - Nano iron oxide catalyst and its synthetic method - Google Patents
Nano iron oxide catalyst and its synthetic method Download PDFInfo
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- CN1954912A CN1954912A CN 200510113970 CN200510113970A CN1954912A CN 1954912 A CN1954912 A CN 1954912A CN 200510113970 CN200510113970 CN 200510113970 CN 200510113970 A CN200510113970 A CN 200510113970A CN 1954912 A CN1954912 A CN 1954912A
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Abstract
A nano-iron oxide catalyst for the catalytic oxidizing of CO with high catalytic activity and thermal stability is prepared through dissolving Fe salt and pyrrolidone in N,N-dimethyl formamide, stirring, reaction, cooling, washing and drying.
Description
Technical field
The present invention relates to CO catalytic oxidation field, especially relate to a kind of synthetic method of nano iron oxide catalyst.
Background technology
Iron oxide is a kind of traditional catalyst and the carrier of loaded catalyst.Since nano-sized iron oxide CO oxidation catalyst came out, improve its catalytic activity and heat endurance was the difficult problem that people pay close attention to always.Holland " applied catalysis B-environment " (Applied Catalysis B:Environmental, 2003, the 43rd volume, the 151st page) to mention, the nano-sized iron oxide beaded catalyst with small size and bigger serface all is being significantly improved aspect CO oxidation catalytic activity and the heat endurance than traditional micron order catalyst; The synthetic hollow tubular structure nano iron oxide catalyst of thermal decomposition method that passes through of U.S.'s " inorganic chemistry " (Inorg.Chem.,, the 43rd volume, the 6540th page in 2004) report is having greatly improved again than preamble aspect catalytic activity and the heat endurance.Yet still there are three big shortcomings in the nano iron oxide catalyst that more than obtains: the one, and the work that rises of catalyst is individual process slowly, the playing activity temperature region scope is greater than 100 ℃; The 2nd, light-off temperature is still too high, more than 300 ℃; The 3rd, heat endurance still is relatively poor, and as the nano iron oxide catalyst to hollow tubular structure, the light-off temperature with CO oxidation catalysis test has for the third time improved 12 ℃ and 28 ℃ respectively than the test of catalysis for the first time for the second time.The existence of these problems has seriously limited the commercial Application of nano iron oxide catalyst.
Summary of the invention
The present invention proposes the method for a kind of synthetic standard cube hexahedron nano iron oxide catalyst, purpose is to prepare Stability Analysis of Structures, have high CO catalytic activity and heat endurance, can develop into the ferric oxide catalyst of the nano catalytic material of new generation that has a extensive future.
The present invention adopts solvent-thermal method synthesis of nano ferric oxide catalyst, detailed process is as follows: molysite and polyvinylpyrrolidone (PVP) surfactant dissolves in N, in dinethylformamide (DMF) solvent, are fully stirred the back and add reactor, be heated to 140-200 ℃, insulation.After the reaction, cool to room temperature, washing, drying.
The catalytic reaction testing arrangement is seen shown in the accompanying drawing 1.Unstripped gas (3.33%CO, 6.67%O
2And 90%N
2) entering reaction unit with the flow velocity of 360ml/min, Range of measuring temp is 150 ℃-300 ℃, the content of product detects by gas-chromatography.
Our yardstick by the preparation of above method is about the nano-sized iron oxide granule novel catalysis material that 30-50nm, appearance are accurate cube hexahedron pattern, have high CO oxidation catalytic activity (light-off temperature is 230 ℃, and the playing activity temperature region scope is less than 5 ℃) and high heat endurance (light-off temperature with CO oxidation catalysis test has for the third time only improved 5 ℃ and 15 ℃ respectively than the test of catalysis for the first time for the second time).
Nano iron oxide catalyst of the present invention is controlled the pattern and the catalytic performance of ferric oxide particles by accurate control preparation condition; With the nano iron oxide catalyst of existing other structure (as the nano particle of no specific morphology, the nano wire of hollow etc.) compare, iron oxide CO oxidation catalytic property of the present invention is obviously superior, and technology of preparing is simple, equipment is less demanding, with low cost, thereby have great application prospect in fields such as gas purification (for example: eliminate automobile CO tail gas and cigarette CO and filter) and gas sensors.
Description of drawings
Fig. 1 is a catalytic activity testing arrangement schematic diagram: 1 is gas flowmeter, and 2 is thermocouple, and 3 is silica wool, and 4 is catalyst.
Transmission electron microscope (a, c) and ESEM (b) photo and the structural model (d) of the nano iron oxide catalyst that Fig. 2 synthesizes for the present invention.
Fig. 3 is the efficiency curve of the nano iron oxide catalyst CO catalytic oxidation that synthesizes of the present invention.
The specific embodiment
Example 1: with analytically pure ferric nitrate and the 0.600g molecular weight with 9 crystallizations water of 0.404g (1mmol) is 30000 polyvinylpyrrolidone surfactant (PVP, Mw=30000) add in the 70ml polytetrafluoroethylene (PTFE) hydro-thermal jar, then accurately measure 36ml N with pipette, dinethylformamide (DMF) fully stirs and obtains transparent dark red solution.Then with steel shell with hydro-thermal jar sealing, change in the resistance furnace heating rate with 5 ℃/min over to and be heated to 160 ℃ and be incubated 10h, then continue heating rate with 5 ℃/min and be warming up to 180 ℃ and be incubated 20h again.After the reaction, the hydro-thermal jar is naturally cooled to room temperature.Last red precipitate is by water and ethanol washing, centrifugal, and after the air dry, obtains bronzing brown iron oxide body catalyst in air.
Example 2: be 30000 polyvinylpyrrolidone surfactant (PVP with 0.270g (1mmol) iron chloride and 0.600g molecular weight, Mw=30000) add in the 70ml polytetrafluoroethylene (PTFE) hydro-thermal jar, then accurately measure 36ml N with pipette, dinethylformamide (DMF) fully stirs and obtains transparent dark red solution.Then with steel shell with hydro-thermal jar sealing, change in the resistance furnace heating rate with 5 ℃/min over to and be heated to 160 ℃ and be incubated 10h, then continue heating rate with 5 ℃/min and be warming up to 180 ℃ and be incubated 20h again.After the reaction, the hydro-thermal jar is naturally cooled to room temperature.Last red precipitate is by water and ethanol washing, centrifugal, and after the air dry, obtains bronzing brown iron oxide body catalyst in air.
Example 3: be 58000 polyvinylpyrrolidone surfactant (PVP with 0.199g (1mmol) frerrous chloride and 1.160g molecular weight, Mw=58000) add in the 70ml polytetrafluoroethylene (PTFE) hydro-thermal jar, then accurately measure 36ml N with pipette, dinethylformamide (DMF) fully stirs and obtains transparent dark red solution.Then with steel shell with hydro-thermal jar sealing, change over to and be warming up to 180 ℃ with 5 ℃/min in the resistance furnace and be incubated 30h again.After the reaction, the hydro-thermal jar is naturally cooled to room temperature.Last red precipitate is by water and ethanol washing, centrifugal, and after the air dry, obtains bronzing brown iron oxide body catalyst in air.
Claims (2)
1, a kind of synthetic method of nano iron oxide catalyst is characterized in that: with molysite and polyvinylpyrrolidone surfactant dissolves in N, in the dinethylformamide solvent, fully stir the back and add reactor, be heated to 140-200 ℃, insulation, after the reaction, cool to room temperature, washing, drying.
2, a kind of method synthesis of nano ferric oxide catalyst that adopts claim 1, this catalyst yardstick are about 30-50nm, appearance is accurate cube hexahedron pattern.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510113970 CN1954912A (en) | 2005-10-24 | 2005-10-24 | Nano iron oxide catalyst and its synthetic method |
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|---|---|---|---|
| CN 200510113970 CN1954912A (en) | 2005-10-24 | 2005-10-24 | Nano iron oxide catalyst and its synthetic method |
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| CN1954912A true CN1954912A (en) | 2007-05-02 |
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| CN 200510113970 Pending CN1954912A (en) | 2005-10-24 | 2005-10-24 | Nano iron oxide catalyst and its synthetic method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108523215A (en) * | 2018-03-21 | 2018-09-14 | 云南中烟工业有限责任公司 | Reduce the modified activated carbon additive and the preparation method and application thereof of CO burst sizes in flue gas |
| CN108685164A (en) * | 2018-03-21 | 2018-10-23 | 云南中烟工业有限责任公司 | Reduce the ferrous coordination compound additive and the preparation method and application thereof of CO burst sizes in flue gas |
-
2005
- 2005-10-24 CN CN 200510113970 patent/CN1954912A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108523215A (en) * | 2018-03-21 | 2018-09-14 | 云南中烟工业有限责任公司 | Reduce the modified activated carbon additive and the preparation method and application thereof of CO burst sizes in flue gas |
| CN108685164A (en) * | 2018-03-21 | 2018-10-23 | 云南中烟工业有限责任公司 | Reduce the ferrous coordination compound additive and the preparation method and application thereof of CO burst sizes in flue gas |
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Open date: 20070502 |