CN103977805A - Catalyst for removing soot particles in tail gas of diesel vehicle, and preparation method thereof - Google Patents

Catalyst for removing soot particles in tail gas of diesel vehicle, and preparation method thereof Download PDF

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Publication number
CN103977805A
CN103977805A CN201410213870.7A CN201410213870A CN103977805A CN 103977805 A CN103977805 A CN 103977805A CN 201410213870 A CN201410213870 A CN 201410213870A CN 103977805 A CN103977805 A CN 103977805A
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catalyst
titanium sheet
soot particles
preparation
nitrate
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CN201410213870.7A
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Chinese (zh)
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孟明
于一夫
曹春梅
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Tianjin University
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Tianjin University
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Abstract

The invention relates to a catalyst for removing soot particles in the tail gas of a diesel vehicle, and a preparation method of the catalyst. The preparation method comprises the steps of dissolving ferric chloride and sodium sulfate into deionized water according to the molar ratio of 1: 1, putting a cleaned titanium sheet into the mixed solution, and carrying out reaction under the hydrothermal condition to obtain the titanium sheet with Fe2O3 nanorod array growing on the surface; soaking the obtained titanium sheet in different nitrate solutions; carrying out calcination to obtain the catalyst MO/Fe2O3 nanorod, wherein M is Ce, Ni, Co or K. The method takes cheap metal salt as raw material, so that the production cost of the catalyst is low; furthermore, a hydrothermal method and an impregnation method are used for preparing the catalyst, so that the technology is simple, and the reaction process is easy to control; the obtained catalyst has an integral structure, thus being convenient to amplify and apply. The catalyst has good activity in the simulated reaction of removing the soot particles of the tail gas emitted by the diesel vehicle.

Description

Eliminate catalyst and the preparation method of carbon soot particles in exhaust gas from diesel vehicle
Technical field
The present invention relates to a kind of Fe that eliminates carbon soot particles in exhaust gas from diesel vehicle 2o 3nanometer stick array Catalysts and its preparation method, belongs to the technical field of diesel car tail gas refining catalyst.
Background technology
Because diesel engine has higher fuel economy, lower operating cost and good durability, obtained application more and more widely in automobile market.But the carbon soot particles of emission of diesel engine has brought serious infringement to the healthy of the mankind and the environment of depending on for existence.At present, a variety of technology are proposed for the content that reduces carbon soot particles in exhaust gas from diesel vehicle.Wherein, the catalytic combustion technology combining with grain catcher is widely regarded as a kind of elimination soot technology of efficient, low energy consumption, and the key of this technology is exactly to search out that a kind of activity is high, the catalyst of good stability.Although various for eliminating the catalyst type of carbon soot particles, as composite metal oxide, noble metals etc. such as simple metal oxide, perovskite and spinelles, but all there is a general problem in them: the aperture of catalyst is generally below 20nm, oarse-grained soot can not enter the inside in hole, reduce both touch opportunities, made initiation temperature higher.According to this deficiency, the invention provides a kind of preparation method of the nanometer stick array catalyst of eliminating carbon soot particles in exhaust gas from diesel vehicle, and investigated their effect.
Summary of the invention
The object of the present invention is to provide a kind of Catalysts and its preparation method and application of eliminating carbon soot particles, described catalyst is Fe 2o 3nanometer stick array catalyst, its preparation process is simple, for eliminating the effective of carbon soot particles.
The present invention is realized by following technical proposals:
A kind of catalyst of eliminating carbon soot particles in exhaust gas from diesel vehicle of the present invention is Fe 2o 3nanometer stick array, consists of MO/Fe 2o 3nanometer rods, wherein M=Ce, Ni, Co or K.
The preparation method of catalyst of the present invention, its step is as follows:
1) anhydrous ferric trichloride and anhydrous sodium sulfate are dissolved in deionized water 1:1～1.5 in molar ratio, put into the water heating kettle that polytetrafluoro liner is housed, then put into titanium sheet, then at 120～160 DEG C, react respectively 6～10 hours;
2) take out titanium sheet and in baking oven, at 100～140 DEG C, be dried 1～3h;
3) the surface length obtaining in step 1 is had to Fe 2o 3the titanium sheet of nanometer stick array is immersed in 4～6h in nitrate solution after being dried;
4) the titanium sheet in step 3 is dry, dry rear sample is transferred to roasting in Muffle furnace, at 500 DEG C, heats 4～8h, makes final products MO/Fe 2o 3nanometer rods.
Described nitrate is cerous nitrate, nickel nitrate, cobalt nitrate or potassium nitrate.
Catalyst of the present invention is applied to the eradicating efficacy checking of eliminating carbon soot particles in exhaust gas from diesel vehicle:
20mg carbon soot particles is joined in 100ml ethanol, utilize ultrasonic technique to make the suspension of carbon soot particles.The hanging drop of carbon soot particles is added to monoblock type sheet catalyst MO/Fe 2o 3nanorod surfaces, wherein the mass ratio of carbon soot particles and catalyst is between 1:10～1:20.In baking oven, between 100～140 DEG C, dry 0.2～0.4h obtains the mixture of catalyst and soot; Mixture is transferred in thermogravimetric reaction tank, passes into nitrogen oxide atmosphere, it consists of: 500ppm NO, 10vol.%O 2, all the other are N 2, gas flow rate 100mlmin -1, be warming up to 700 DEG C from room temperature with the speed of 10 DEG C/min, in the time that temperature reaches initiation temperature, the carbon soot particles in mixture is burnt.
The present invention adopts hydro-thermal method and infusion process to prepare metal oxide-loaded Fe 2o 3nanometer stick array catalyst, its advantage is: adopting cheap slaine is raw material, and the production cost of catalyst is low; In addition, adopt hydro-thermal method and infusion process preparation, technique is simple, and course of reaction is easily controlled; The catalyst obtaining has all-in-one-piece structure, is convenient to amplify and application.The catalyst of gained of the present invention can, by carbon soot particles completing combustion before 500 DEG C of simulation exhaust gas from diesel vehicle discharge, reach the object of carbon soot particles low temperature elimination in exhaust gas from diesel vehicle.
Brief description of the drawings
Fig. 1 is embodiment 1, embodiment 2, embodiment 3, embodiment 4 and embodiment 5 gained samples, eliminates the curve map of carbon soot particles with the simulation of Re Chong – differential thermal method under nitrogen oxide atmosphere.
Detailed description of the invention
Embodiment 1
1. 0.16g ferric trichloride and 0.14g sodium sulphate are dissolved in deionized water, are made into respectively the solution of 80ml, 100ml or 120ml;
2. above-mentioned gained solution is placed in to 150ml and contains teflon-lined stainless steel still, then add titanium sheet (1cm x1cm);
3. water heating kettle is reacted respectively to 6h, 8h or 10h at 120 DEG C, 140 DEG C or 160 DEG C;
4. reacted titanium sheet is dried respectively at 100 DEG C, 120 DEG C or 140 DEG C to 1h, 2h or 3h;
And then move into Muffle furnace, with 10 DEG C of min -1heating rate be heated to 500 DEG C, after roasting 4h, 6h or 8h, make catalyst, be labeled as Fe.
Embodiment 2
1. 0.16g ferric trichloride and 0.14g sodium sulphate are dissolved in deionized water, are made into respectively the solution of 80ml, 100ml or 120ml;
2. above-mentioned gained solution is placed in to 150ml and contains teflon-lined stainless steel still, then add titanium sheet (1cm x1cm);
3. water heating kettle is reacted respectively to 6h, 8h or 10h at 120 DEG C, 140 DEG C or 160 DEG C;
4. reacted titanium sheet is dried respectively at 100 DEG C, 120 DEG C or 140 DEG C to 1h, 2h or 3h, obtains the long Fe that has 2o 3the titanium sheet of nanometer stick array;
5. titanium sheet obtained above is placed in the cerous nitrate solution of 100ml0.1M and soaks respectively 4h, 5h or 6h, take out dry;
And then move into Muffle furnace, with 10 DEG C of min -1heating rate be heated to 500 DEG C, after roasting 4h, 6h or 8h, make catalyst, be labeled as Ce/Fe.
Embodiment 3
1. 0.16g ferric trichloride and 0.14g sodium sulphate are dissolved in deionized water, are made into respectively the solution of 80ml, 100ml or 120ml;
2. above-mentioned gained solution is placed in to 150ml and contains teflon-lined stainless steel still, then add titanium sheet (1cm x1cm);
3. water heating kettle is reacted respectively to 6h, 8h or 10h at 120 DEG C, 140 DEG C or 160 DEG C;
4. reacted titanium sheet is dried respectively at 100 DEG C, 120 DEG C or 140 DEG C to 1h, 2h or 3h, obtains the long Fe that has 2o 3the titanium sheet of nanometer stick array;
5. titanium sheet obtained above is placed in the nickel nitrate solution of 100ml0.1M and soaks respectively 4h, 5h or 6h, take out dry;
And then move into Muffle furnace, with 10 DEG C of min -1heating rate be heated to 500 DEG C, after roasting 4h, 6h or 8h, make catalyst, be labeled as Ni/Fe.
Embodiment 4
1. 0.16g ferric trichloride and 0.14g sodium sulphate are dissolved in deionized water, are made into respectively the solution of 80ml, 100ml or 120ml;
2. above-mentioned gained solution is placed in to 150ml and contains teflon-lined stainless steel still, then add titanium sheet (1cm x1cm);
3. water heating kettle is reacted respectively to 6h, 8h or 10h at 120 DEG C, 140 DEG C or 160 DEG C;
4. reacted titanium sheet is dried respectively at 100 DEG C, 120 DEG C or 140 DEG C to 1h, 2h or 3h, obtains the long Fe that has 2o 3the titanium sheet of nanometer stick array;
5. titanium sheet obtained above is placed in the cobalt nitrate solution of 100ml0.1M and soaks respectively 4h, 5h or 6h, take out dry;
And then move into Muffle furnace, with 10 DEG C of min -1heating rate be heated to 500 DEG C, after roasting 4h, 6h or 8h, make catalyst, be labeled as Co/Fe.
Embodiment 5
1. 0.16g ferric trichloride and 0.14g sodium sulphate are dissolved in deionized water, are made into respectively the solution of 80ml, 100ml or 120ml;
2. above-mentioned gained solution is placed in to 150ml and contains teflon-lined stainless steel still, then add titanium sheet (1cm x1cm);
3. water heating kettle is reacted respectively to 6h, 8h or 10h at 120 DEG C, 140 DEG C or 160 DEG C;
4. reacted titanium sheet is dried respectively at 100 DEG C, 120 DEG C or 140 DEG C to 1h, 2h or 3h, obtains the long Fe that has 2o 3the titanium sheet of nanometer stick array;
5. titanium sheet obtained above is placed in the potassium nitrate solution of 100ml0.1M and soaks respectively 4h, 5h or 6h, take out dry;
And then move into Muffle furnace, with 10 DEG C of min -1heating rate be heated to 500 DEG C, after roasting 4h, 6h or 8h, make catalyst, be labeled as K/Fe.
The Application Example one of catalyst
Below embodiment 1, embodiment 2, embodiment 3, embodiment 4 and embodiment 5 gained samples are studied the catalytic combustion activity of carbon soot particles in diesel vehicle, concrete research method is as follows:
Carbon soot particles combustion catalysis activity rating carries out on the TG/DTA instrument of Perkin Elmer company, uses the Printex – U Soot (C:92.2wt.% of Degussa company; H:0.6wt.%; Volatiles:6wt.%) be reactant.20mg carbon soot particles is joined in 100ml ethanol, utilize ultrasonic technique to obtain the suspension of carbon soot particles.The hanging drop of carbon soot particles is added to monoblock type sheet catalyst MO/Fe 2o 3nanorod surfaces, wherein the mass ratio of carbon soot particles and catalyst is 1:20, in air, dry 0.2～0.4h at 100～140 DEG C, reaches the contact mode that deposits sedimentation, obtains the mixture of catalyst and soot; Mixture is transferred in thermogravimetric reaction tank, passes into nitrogen oxide atmosphere, in nitrogen oxide atmosphere, be heated to 700 DEG C, 10 DEG C of min of heating rate from 100 DEG C -1, gas flow rate is 100mlmin -1, nitrogen oxide gaseous mixture consists of: 500ppmNO, 10vol.%O 2, N 2for Balance Air.
Experimental result as shown in Figure 1, Fe 2o 3nanometer stick array catalyst cupport metal oxide CeO 2, NiO, Co 3o 4and K 2after O, the ignition temperature of carbon soot particles obviously reduces, and wherein the combustion catalysis activity of the prepared sample soot of embodiment 4 is the highest, with unadulterated sample F e 2o 3nanometer rods catalyst is compared, and the temperature that carbon-smoke combustion maximum rate is corresponding has reduced by 50 DEG C.

Claims (3)

1. eliminate a catalyst for carbon soot particles in exhaust gas from diesel vehicle, it is characterized in that catalyst is Fe 2o 3nanometer stick array, consists of MO/Fe 2o 3nanometer rods, wherein M=Ce, Ni, Co or K.
2. the preparation method of catalyst claimed in claim 1, its characterization step is as follows:
1) anhydrous ferric trichloride and anhydrous sodium sulfate are dissolved in deionized water 1:1～1.5 in molar ratio, put into the water heating kettle that polytetrafluoro liner is housed, then put into titanium sheet, then at 120～160 DEG C, react respectively 6～10 hours;
2) take out titanium sheet and in baking oven, at 100～140 DEG C, be dried 1～3h;
3) the surface length obtaining in step 1 is had to Fe 2o 3the titanium sheet of nanometer stick array is immersed in 4～6h in nitrate solution after being dried;
4) the titanium sheet in step 3 is dry, dry rear sample is transferred to roasting in Muffle furnace, at 500 DEG C, heats 4～8h, makes final products MO/Fe 2o 3nanometer rods.
3. the preparation method of catalyst as claimed in claim 2, is characterized in that described nitrate is cerous nitrate, nickel nitrate, cobalt nitrate or potassium nitrate.
CN201410213870.7A 2014-05-20 2014-05-20 Catalyst for removing soot particles in tail gas of diesel vehicle, and preparation method thereof Pending CN103977805A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105990560A (en) * 2015-02-09 2016-10-05 北京大学 Iron oxide porous nanorod array electrode material and preparation method thereof
CN109499593A (en) * 2018-11-28 2019-03-22 济南大学 The preparation method and products obtained therefrom of a kind of integral catalyzer containing potassium and zinc oxide nano rod and application
CN113649008A (en) * 2021-08-19 2021-11-16 郑州大学 High-activity integral catalyst for eliminating soot particles in tail gas of diesel vehicle and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101767012A (en) * 2009-12-25 2010-07-07 昆明理工大学 Low-temperature combustion catalyst for eliminating diesel engine carbon black
CN103400980A (en) * 2013-07-30 2013-11-20 浙江大学 Iron sesquioxide/nickel oxide core-shell nanorod array film as well as preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101767012A (en) * 2009-12-25 2010-07-07 昆明理工大学 Low-temperature combustion catalyst for eliminating diesel engine carbon black
CN103400980A (en) * 2013-07-30 2013-11-20 浙江大学 Iron sesquioxide/nickel oxide core-shell nanorod array film as well as preparation method and application thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
晏冬霞等: "Ce1-xFexO2复合氧化物的结构及其催化碳烟低温燃烧性能", 《物理化学学报》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105990560A (en) * 2015-02-09 2016-10-05 北京大学 Iron oxide porous nanorod array electrode material and preparation method thereof
CN105990560B (en) * 2015-02-09 2018-04-27 北京大学 Ferric oxide multi-porous nano-bar array electrode material and preparation method thereof
CN109499593A (en) * 2018-11-28 2019-03-22 济南大学 The preparation method and products obtained therefrom of a kind of integral catalyzer containing potassium and zinc oxide nano rod and application
CN113649008A (en) * 2021-08-19 2021-11-16 郑州大学 High-activity integral catalyst for eliminating soot particles in tail gas of diesel vehicle and preparation method thereof

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Application publication date: 20140813