CN107362795A - A kind of preparation method of three layers of Ca-Ti ore type wind resource assessment gas combustion catalyst of high temperature resistant support type - Google Patents
A kind of preparation method of three layers of Ca-Ti ore type wind resource assessment gas combustion catalyst of high temperature resistant support type Download PDFInfo
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- CN107362795A CN107362795A CN201710664284.8A CN201710664284A CN107362795A CN 107362795 A CN107362795 A CN 107362795A CN 201710664284 A CN201710664284 A CN 201710664284A CN 107362795 A CN107362795 A CN 107362795A
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Abstract
The invention discloses a kind of preparation method of three layers of Ca-Ti ore type wind resource assessment gas combustion catalyst of high temperature resistant support type, and the catalyst is applied to wind resource assessment gas catalyst combustion reaction.The preparation of the catalyst is to react the nitrate solution of La, Mn element matched containing certain metallic atom, citric acid solution, parachloroanilinum solution, ammonium bicarbonate soln and support powder, reacted 11 hours in 115 DEG C of autoclave, 3h is finally calcined under conditions of 1100 DEG C, forms three layers of perovskite type catalyst La of high temperature resistant support type3Mn2O7/MgAl2O4.The preparation method of the catalyst is environmentally safe, can realize wind resource assessment gas completely burned at a lower temperature, has excellent catalytic activity and good resistance to elevated temperatures.
Description
Technical field
The present invention relates to a kind of preparation method of three layers of Ca-Ti ore type wind resource assessment gas combustion catalyst of high temperature resistant support type,
Particularly relate to a kind of preparation method of three layers of Ca-Ti ore type wind resource assessment gas combustion catalyst of high temperature resistant support type.
Background technology
Methane-air mixed gas of the methane content less than 3% is generally called wind resource assessment gas.Coal, natural gas and
Substantial amounts of wind resource assessment gas can be produced during shale gas exploitation, and methane concentration is too low in wind resource assessment gas, recycles first
Alkane technical difficulty is big, cost is high.The current enterprise of most of coal minings etc. now is in coal mining often all by caused wind
Gas-removing gas is directly discharged in air, not only causes the waste of the energy and resource, also as a huge greenhouse gases
Emission source.Therefore, how effectively, it is friendly using wind resource assessment gas be an important technology that the enterprises such as current coal mining face
Problem.One's early years American scientist proposes carries out catalysis burning by wind resource assessment gas, is generated electricity etc. with obtaining energy, so as to real
Show effective utilization of wind resource assessment gas, this method obtains the accreditation of scientist at present, has become the common recognition of people.It is but real
Existing wind resource assessment gas catalysis burning carries out this process that generates electricity, it is important to develops a kind of efficient, high temperature resistant, low cost wind row
Device in Gas combustion catalyst.
At present, noble metal catalyst is a kind of effective wind resource assessment combustion catalyst, can make wind resource assessment gas 200~
Burnt between 400 DEG C complete, but due to noble metal price, resistance to elevated temperatures difference and easy-sintering, therefore be not appropriate for extensive
Applied in wind resource assessment gas catalyst combustion reaction.Therefore, people expand the support type mistake stronger to cheap and easy to get, oxygen storage capacity
Cross the research of metal oxide catalyst, such as Fe2O3/Al2O3Catalyst etc., but these oxides burn in wind resource assessment gas
In course of reaction, high temperature caused by the burning of wind resource assessment gas can often can make to occur between the active component and carrier of catalyst
React to each other, reduce the catalytic activity of catalyst, therefore these oxides are as wind resource assessment gas combustion catalyst, heat-resisting quantity
It can not still meet commercial Application, so people turn one's attention to property stabilization and not the base metal combined oxidation of easy-sintering again
Thing catalyst, such as hexa-aluminate composite oxides, perovskite composite oxide, spinel complex oxide etc..Wherein calcium
Titanium ore type oxide has single perovskite (ABO3), double-perovskite (ABB ' O6), laminated perovskite (An+1BnO3n+1) etc., wherein single calcium
Titanium ore and double-perovskite type metal composite catalyst are in the existing numerous studies of wind resource assessment gas catalysis combustion field, but support type
Three layers of perovskite type metal composite oxide catalysts are relatively fewer as the research of wind resource assessment gas combustion catalyst.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of three layers of Ca-Ti ore type wind resource assessment gas combustion of high temperature resistant support type
The preparation method of catalyst is burnt, is that a kind of three layers of Ca-Ti ore type wind row of high temperature resistant support type have been prepared in 1100 DEG C of roastings in temperature
Device in Gas combustion catalyst La3Mn2O7/MgAl2O4, the catalyst is used in wind resource assessment gas catalyst combustion reaction, Neng Goushi
Wind resource assessment gas completely burned under present lower temperature, has excellent catalytic activity and good resistance to elevated temperatures.
A kind of preparation side of three layers of Ca-Ti ore type wind resource assessment gas combustion catalyst of high temperature resistant support type of the present invention
Method, implementation are as follows：Take Mg (NO3)2·6H2O (analysis is pure) 2.5659g, Al (NO3)3·9H2O (analysis is pure) 7.5026g,
Citric acid (C6H8O7·H2O) magnetic agitation is completely dissolved in 6.3042g, 110ml deionized water addition 1000ml beaker, its
The amount of middle magnesium atom and the material of aluminium atom ratio is 1: 2, the material of citric acid and metallic atom (magnesium, the amount of aluminium atom total material)
Ratio be 1: 1；Transfer it in 75 DEG C of water-bath and heat, and be 7 with the pH value of 20% concentrated ammonia liquor regulation solution,
And form wet colloidal sol in 75 DEG C of water bath with thermostatic control agitating and heating 7h；Obtained wet colloidal sol is transferred in 95 DEG C of baking oven, heated
17h, obtain xerogel；Obtained xerogel is transferred in agate mortar after the finely ground mesh to 40-60 and is put into Muffle furnace, 500
DEG C roasting 3.5h；The sample obtained after roasting is transferred in high temperature furnace, 1100 DEG C of roasting 3h obtain catalyst carrier MgAl2O4；
Take La (NO3)3·6H2O (analysis is pure) 1.3875g, 50%Mn (NO3)20.7948g、NH4HCO3(analysis is pure) 0.5625g, lemon
Acid (C6H8O7·H2O) 1.5825g adds 110ml deionized waters, and the wherein amount ratio of the material of lanthanum atom and manganese atom is 3: 2, lemon
The ratio of the material of lemon acid and metallic atom (lanthanum, the amount of manganese atom total material) is 1: 1.37, makes it completely molten in the case where being stirred continuously
Solution, 0.1595g parachloroanilinum (analysis is pure) and the above-mentioned MgAl prepared of 2.3946g are added into solution2O4Carrier, Ran Houfang
Heated into 75 DEG C of water-baths, and wet colloidal sol is formed after water bath with thermostatic control agitating and heating 7h；Obtained wet colloidal sol is transferred to
27h is heated in 115 DEG C of baking oven, obtains xerogel；Obtained xerogel is transferred to it is finely ground to 40-60 mesh in agate mortar,
After be put into Muffle furnace, 700 DEG C roasting 3.8h；The sample 0.85g after 700 DEG C of roastings is taken to be transferred in 100ml polytetrafluoroethylene (PTFE)
In the high-pressure hydrothermal reaction kettle of courage, and 0.09mol/L ammonium bicarbonate soln 58ml are added into reactor, reactor is transferred to
11h is heated in 115 DEG C of baking oven, it is to be heated to finish, it is cooled to room temperature suction filtration；The solid sample that will be obtained, under the conditions of 95 DEG C
Heating, drying 10h, after be transferred in high temperature furnace, 1100 DEG C roasting 3h obtain three layers of Ca-Ti ore type wind resource assessment of high temperature resistant support type
Gas combustion catalyst La3Mn2O7/MgAl2O4。
The catalyst of the present invention has excellent catalytic activity in wind resource assessment gas combustion reaction, and specific experiment operation is
Using volume fraction be 2% methane gas (be equipped with 18% oxygen and 80% nitrogen as Balance Air) as simulate wind resource assessment
Gas, it is passed into the quartz ampoule fixed bed reactors equipped with 40-60 mesh, the caliber of reactor is 10mm, air speed 48000h-1,
Temperature programming speed is 5 DEG C/min, is tested using the FQ-B types infrared gas analyser of Foshan Analytical Instrument Co., Ltd production,
And it is recorded under different reaction temperatures, the conversion ratio of methane in wind resource assessment gas.In addition, produced using German Bruker companies
D8ADVANCE types Powder X-ray Diffractometer test catalyst thing phase composition, the running parameter of the instrument is as follows：Radiation source
For CuK α (λ=0.15406nm), operating voltage 36kV, electric current 20mA, 10 °~80 ° of scanning range, 2 ° of sweep speed/
min。
The present invention is with three layers of perovskite type catalyst La of high temperature resistant support type3Mn2O7/MgAl2O4Fired as wind resource assessment gas
Burn catalyst, and with perovskite type catalyst La3Mn2O7Contrasted, find three layers of perovskite catalyst La of support type3Mn2O7/
MgAl2O4There is preferable wind resource assessment gas combustion catalysis activity；Obtained La is had found by XRD tests3Mn2O7/MgAl2O4Urge
Agent sample is typical three layers of Ca-Ti ore type La3Mn2O7Diffraction maximum and spinelle MgAl2O4Diffraction maximum, do not occur any miscellaneous
Peak.
It is an advantage of the invention that：Three layers of perovskite type catalyst La of the high temperature resistant support type prepared3Mn2O7/MgAl2O4With
In wind resource assessment gas catalyst combustion reaction, the results showed that have preferable catalytic activity and excellent resistance to elevated temperatures, prepared
Journey is environmentally safe.
The present invention essential characteristics be：
1st, three layers of perovskite type catalyst La of the high temperature resistant support type prepared3Mn2O7/MgAl2O4For wind resource assessment gas
Catalyst combustion reaction, initiation temperature T10=423.4 DEG C and complete conversion temperature T90=626.8 DEG C be much better than it is unsupported compound
Metal oxide catalyst；
2nd, three layers of perovskite type catalyst La of the high temperature resistant support type prepared3Mn2O7/MgAl2O4For wind resource assessment gas
Catalyst combustion reaction, possess good resistance to elevated temperatures, still there is good methyl hydride combustion catalyst performance after 1100 DEG C of roastings.
Brief description of the drawings
Fig. 1 is that (1) catalyst A is La3Mn2O7/MgAl2O4Support type perovskite catalyst active testing figure；(2) catalyst
B is La3Mn2O7Perovskite type catalyst active testing figure；
Fig. 2 is that (1) A is La3Mn2O7/MgAl2O4The X ray diffracting spectrum of support type perovskite catalyst；(2) B is
La3Mn2O7The X ray diffracting spectrum of perovskite type catalyst.
It is anti-corresponding to the conversion ratio (10%, 90%) of methane in the wind resource assessment gas combustion reaction of the different catalysts of table 1
Answer temperature (T10、T90)。
Embodiment：
Embodiment 1：Take Mg (NO3)2·6H2O (analysis is pure) 2.5659g, Al (NO3)3·9H2O (analysis is pure) 7.5026g,
Citric acid (C6H8O7·H2O) magnetic agitation is completely dissolved in 6.3042g, 110ml deionized water addition 1000ml beaker；Its
The amount of middle magnesium atom and the material of aluminium atom ratio is 1: 2, the material of citric acid and metallic atom (magnesium, the amount of aluminium atom total material)
Ratio be 1: 1；It is transferred into 75 DEG C of water-bath and heats afterwards, and is 7 with the pH value of 20% concentrated ammonia liquor regulation solution, and
Wet colloidal sol is formed in 75 DEG C of water bath with thermostatic control agitating and heating 7h；Obtained wet colloidal sol is transferred in 95 DEG C of baking oven, heats 17h,
Obtain xerogel；Obtained xerogel is transferred in agate mortar after the finely ground mesh to 40-60 and is put into Muffle furnace, 500 DEG C of roastings
Burn 3.5h；The sample obtained after roasting is transferred in high temperature furnace, 1100 DEG C of roasting 3h obtain catalyst carrier MgAl2O4；Take La
(NO3)3·6H2O (analysis is pure) 1.3875g, 50%Mn (NO3)20.7948g、NH4HCO3(analysis is pure) 0.5625g, citric acid
(C6H8O7·H2O) 1.5825g adds 110ml deionized waters, is completely dissolved it in the case where being stirred continuously, is added into solution
0.1595g parachloroanilinum (analysis is pure) and the above-mentioned MgAl prepared of 2.3946g2O4Carrier, the wherein thing of lanthanum atom and manganese atom
The amount ratio of matter is 3: 2, and the ratio of the material of citric acid and metallic atom (lanthanum, the amount of manganese atom total material) is 1: 1.37, Ran Houfang
Heated into 75 DEG C of water-baths, and wet colloidal sol is formed after 75 DEG C of water bath with thermostatic control agitating and heating 7h；Obtained wet colloidal sol is turned
Move on in 115 DEG C of baking oven and heat 27h, obtain xerogel；Obtained xerogel is transferred to finely ground to 40-60 in agate mortar
Mesh, after be put into Muffle furnace, 700 DEG C roasting 3.8h；The sample 0.85g after 700 DEG C of roastings is taken to be transferred to 100ml polytetrafluoroethylene (PTFE)
In the high-pressure hydrothermal reaction kettle of inner bag, and 0.09mol/L ammonium bicarbonate soln 58ml are added into reactor, reactor is shifted
11h is heated into 115 DEG C of baking ovens, it is to be heated to finish, it is cooled to room temperature suction filtration；The solid sample that will be obtained, in 85 DEG C of conditions
Lower heating, drying 10h, after be transferred in high temperature furnace, 1100 DEG C of roasting 3h obtain three layers of Ca-Ti ore type wind of high temperature resistant support type row watt
This gas combustion catalyst La3Mn2O7/MgAl2O4。
Comparative example 1：Take La (NO3)3·6H2O 4.1625g, 50%Mn (NO3)22.6844g, citric acid (C6H8O7·H2O)
5.3875g, which is put into 1000ml beakers to add under 110ml deionized water magnetic agitations, is completely dissolved it, wherein lanthanum atom and manganese
The amount ratio of the material of atom is 3: 2, and the ratio of the material of citric acid and metallic atom (lanthanum, the amount of manganese atom total material) is 1: 1.5,
Then it is put into 75 DEG C of water-bath；And wet colloidal sol is formed after 75 DEG C of water bath with thermostatic control agitating and heating 7h, the wet gel that will be obtained
27h in 115 DEG C of baking oven is put into be dried to form xerogel；Obtained xerogel mortar is finely ground to 40-60 mesh, after be put into
700 DEG C of Muffle kiln roasting 3.8h；By the sample after roasting, 1100 DEG C of high temperature kiln roasting 3h is transferred to；Finally give
La3Mn2O7Catalyst sample.
Obtained catalyst carries out the test of catalytic activity according to the methods below：
40-60 mesh catalyst 200mg made from Example 1 and comparative example 1, it is placed in diameter 10mm fixed bed quartz
In reactor, FQ-B types infrared gas analyser preheating 1-2h is opened, then nitrogen is passed through in analyzer with emptying reactor
In foreign gas, it is 30L/h to control the flow velocity of nitrogen with flowmeter, treats infrared spectrum analyser pointer nulling and stable 10-
15min, nitrogen is closed, then be passed through wind resource assessment gas, it is 25-30L/h to control flowmeter gas flow rate, when infrared spectrum analyser pointer
100 stable 10-15min are pointed to, are started to warm up, temperature programming speed is 5 DEG C/min.Record and calculate reaction at different temperatures
CH in corresponding wind resource assessment gas after reaching stable4Conversion ratio.
2 high temperature resistant support type of table, three layers of perovskite type catalyst La3Mn2O7/MgAl2O4Wind resource assessment gas combustion reaction in
Reaction temperature corresponding to the conversion ratio of methane.
Claims (1)
- A kind of 1. preparation method of three layers of Ca-Ti ore type wind resource assessment gas combustion catalyst of high temperature resistant support type, it is characterised in that： Take Mg (NO3)2·6H2O 2.5659g、Al(NO3)3·9H2O 7.5026g, citric acid (C6H8O7·H2O) 6.3042g, add 110ml deionized waters, are completely dissolved it in the case where being stirred continuously, and are then put into 75 DEG C of water-bath and heat, and with 25% ammoniacal liquor The pH value for adjusting solution is 7, forms gel after heating response stirring 7h in 75 DEG C of water-bath, the wet gel that will be obtained, 95 17h is dried under the conditions of DEG C and forms xerogel；Obtained xerogel is finely ground to 40-60 mesh, 500 DEG C of roasting 3.5h；After being calcined Sample again 1100 DEG C be calcined 3h；Finally give carrier MgAl2O4.Take La (NO3)3·6H2O (analysis is pure) 1.3875g, 50% Mn(NO3)20.7948g、NH4HCO3(analysis is pure) 0.5625g, citric acid (C6H8O7·H2O) 1.5825g adds 110ml deionizations The amount ratio of water, the wherein material of lanthanum atom and manganese atom is 3: 2, citric acid and metallic atom (lanthanum, the amount of manganese atom total material) The ratio of material be 1: 1.37, be completely dissolved it in the case where being stirred continuously, (the analysis of 0.1595g parachloroanilinum added into solution It is pure) and the above-mentioned MgAl prepared of 2.3946g2O4Carrier, after be put into 75 DEG C of water-bath, formed after heating stirring reaction 7h solidifying Glue；The wet gel that will be obtained, 27h formation xerogel is dried under conditions of 115 DEG C；Obtained xerogel is finely ground to 40-60 Mesh, then 700 DEG C of roasting 3.8h；The sample 0.85g after 700 DEG C of roastings is taken to be transferred to the water under high pressure of 100ml polytetrafluoroethylliner liners In thermal response kettle, and 0.09mol/L ammonium bicarbonate solns 58ml is added into reactor；Reactor is transferred to 115 DEG C of baking 11h is heated in case, to be heated finish is cooled to room temperature, filters；The solid sample that will be obtained, the heating, drying under the conditions of 95 DEG C 10h, then be calcined 3h at 1100 DEG C and finally give three layers of Ca-Ti ore type wind resource assessment gas combustion catalyst of high temperature resistant support type La3Mn2O7/MgAl2O4, and the catalyst is applied to wind resource assessment gas catalyst combustion reaction.
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| CN111740015A (en) * | 2020-06-27 | 2020-10-02 | 苏州大学 | Perovskite precursor solution for improving stability of perovskite solar cell |
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| CN111740015B (en) * | 2020-06-27 | 2022-08-12 | 苏州大学 | Perovskite precursor solution for improving stability of perovskite solar cell |
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