CN100558645C - Ultra-fine perovskite type LaFeO 3And LaMnO 3A kind of preparation method - Google Patents
Ultra-fine perovskite type LaFeO 3And LaMnO 3A kind of preparation method Download PDFInfo
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- CN100558645C CN100558645C CNB2007101435212A CN200710143521A CN100558645C CN 100558645 C CN100558645 C CN 100558645C CN B2007101435212 A CNB2007101435212 A CN B2007101435212A CN 200710143521 A CN200710143521 A CN 200710143521A CN 100558645 C CN100558645 C CN 100558645C
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- 229910017771 LaFeO Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims description 13
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 50
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 50
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000008117 stearic acid Substances 0.000 claims abstract description 50
- 239000000843 powder Substances 0.000 claims abstract description 33
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 15
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims abstract description 14
- CNFDGXZLMLFIJV-UHFFFAOYSA-L manganese(II) chloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Mn+2] CNFDGXZLMLFIJV-UHFFFAOYSA-L 0.000 claims abstract description 14
- 238000005303 weighing Methods 0.000 claims abstract description 14
- 239000007787 solid Substances 0.000 claims abstract description 13
- 230000004927 fusion Effects 0.000 claims abstract description 12
- 238000009841 combustion method Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 22
- 238000013019 agitation Methods 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000000446 fuel Substances 0.000 claims description 4
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- 238000005049 combustion synthesis Methods 0.000 description 4
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- 239000000376 reactant Substances 0.000 description 4
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
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- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
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- 238000005054 agglomeration Methods 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
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Abstract
A kind ofly prepare ultra-fine perovskite type LaFeO with the gel of stearic acid combustion method
3And LaMnO
3Method, scheme is: (1) 1: 1 in molar ratio: (7-10), respectively weighing lanthanum nitrate, iron nitrate, stearic acid.With lanthanum nitrate, the iron nitrate solid is fused in the fusion stearic acid, and temperature control 114-125 ℃, the above one-tenth of reaction 5h gel.Gel is placed 300-500 ℃ of retort furnace, burn LaFeO
3Powder; (2) 1: 1 in molar ratio: (7-10), difference weighing lanthanum nitrate, Manganous chloride tetrahydrate, stearic acid.With lanthanum nitrate, the Manganous chloride tetrahydrate solid is fused in the fusion stearic acid, and temperature control 104-118 ℃, the above one-tenth of reaction 6h gel.Gel is placed 300-500 ℃ retort furnace, burn LaMnO
3Powder.
Description
Technical field
The invention belongs to perovskite typed superfine powder LaFeO
3And LaMnO
3Preparing technical field specifically is to prepare perovskite typed superfine powder LaFeO with the gel of stearic acid combustion method
3And LaMnO
3
Background technology
LaFeO
3And LaMnO
3Belong to perovskite-type rare-earth composite oxides, it can be used as the catalyzer of environmental pollution treatment, oxygen sensor, solid fuel cell etc.Its most of performances depend on the production method of powder.So a good synthetic method often can greatly change its physical and chemical performance.
Preparation LaFeO
3And LaMnO
3Method adopt high temperature solid-state method, chemical coprecipitation, sol-gel method, hydrothermal synthesis method and low-temperature combustion synthesis usually.The properties of sample of high temperature solid-state method preparation is good, physical strength height, and have preferably active and anti-poisoning capability, but the product cut size and the homogeneity that make with this method are relatively poor, and easily introduce impurity, too high sintering and the reunion that causes product easily of temperature in the calcination process.The prepared perovskite typed powder of chemical coprecipitation has higher specific surface area and reactive behavior, but can't the realization response thing at the homodisperse of molecular level.Sol-gel method prepares perovskite-type rare-earth composite oxides to be had: (1) temperature of reaction is low, and reaction process is easy to control; (2) uniformity coefficient of goods, purity height (homogeneity can reach molecule or atomic level); (3) stoichiometry is accurate, is easy to modification, adulterated wide ranges (comprising adulterated amount and kind).But the preparation required time is longer, is difficult for realizing industrialization.At present in order to the specific surface of the perofskite type oxide that last method synthesized mostly below 10m2/g because specific surface is lower, thereby influence its various physical and chemical performances greatly.
Combustion synthesis method is synthetic and propose with respect to self propagating high temperature.People such as Patil were raw material with the saturated aqueous solution (oxygenant) and the organic-fuel (reductive agent) of metal-salt first in 1988, each raw material is soluble in water, the Pyrex hard glass container that will fill solution then is positioned on the hot plate or in the retort furnace, be heated to 573～773K, solution seethes with excitement, concentrates, smolders, rapid burning on fire then obtains the loose oxide compound ultrafine powder of spumescence.This technology utilization metal and nonmetal, the solid state reaction compound of permutoid reaction can take place, and use one matter or the mixture that redox reaction can take place, under certain temperature trigger redox reaction takes place, utilize its big energy of emitting, finally obtain desired product.The globule size of products obtained therefrom and distribution etc. and fuel used kind, synthesis condition etc. all have much relations.
Gel-burning synthetic method is a kind of low-temperature burning chemical process that sol-gel wet-chemical synthesis method and self-propagating combustion synthesis method are organically combined, and has simply fast, convenient, and easily realizes characteristics such as industrialization.Low-temperature combustion method prepares LaFeO at present
3And LaMnO
3And the employed organic-fuel of hotchpotch is Padil, glycine etc.Because building-up process adopts aqueous solution combustion method synthetic powder, products obtained therefrom reunion degree is bigger, and specific surface area is little.
The stearic acid complex compound gel combustion method that we adopted is based on stearic acid fusing point lower (68-70 ℃), and itself also can be used as the solvent of metal-salt, and stearic acid has the dual function of Synergist S-421 95 and tensio-active agent concurrently, in building-up process, only there is less water to participate in, thereby prevented the hydrolytic precipitation of metal ion, and can reduce the agglomeration of product.The solid particulate that a large amount of gas percussions that produce in the combustion processes in addition form both can make powder granularity diminish, and also can prevent the reunion between the particle.So it is even to make size distribution under suitable condition, the superfine powder that particle diameter is little.Be expected to improve greatly the various physical and chemical performances of product.
Summary of the invention
The present invention has overcome present gel combustion synthesis method synthetic LaFeO
3And LaMnO
3It is big to have granularity, and specific surface area is little, and shortcoming pockety utilizes stearic acid complex compound gel combustion method to prepare the ultra-fine LaFeO of perovskite typed
3And LaMnO
3Provide stearic acid to prepare the ultra-fine LaFeO of perovskite typed
3And LaMnO
3Suitable condition.
The present invention adopts with following scheme to realize, specifically may further comprise the steps: (1) dissolves (2) lanthanum nitrate with stearic acid, iron nitrate under the constant temperature oil bath heating condition; Lanthanum nitrate, two groups of solids of Manganous chloride tetrahydrate are dissolved in respectively in the fusion stearic acid, and under the constant temperature magnetic agitation, the control certain temperature makes reaction system become the complex compound gel behind the reaction certain hour.(3) gel is burnt at a certain temperature, can directly synthesize LaFeO
3And LaMnO
3
In the gel generative process, the mol ratio of reactant, reaction times and temperature all influence granularity, purity and the pattern of last powder.When the stearic acid amount is crossed low owing to lack enough complexing agent molecules, all complexings of nitrate, the powder granularity skewness of preparation, powder reuniting.The stearic acid amount is big more, and the products obtained therefrom particle diameter is more little, and the reason that reduces can think that it is more tiny that this helps powder granularity owing to along with the increasing of stearic acid add-on, generated more gas.But the stearic acid amount is too high, and can make has more organic substance residues in the final product, so should select suitable reactant ratio for use.Reaction times is too short, and reactant can not be completed into complex compound, causes final combustion powder purity low, and uhligite easily is mixed with dephasign in mutually.So it is very important to control the suitable reaction times.Temperature of reaction raises, and speed of response is accelerated, and the gained powder granularity is less, and reaction can be finished with fast speeds, considers the characteristic of each reactant itself, so the preparation of each perovskite composite oxide is all had a suitable reaction temperature.
The preparation condition that present method is suitable is:
LaFeO
3: 1: 1 in molar ratio: (7-10), difference weighing lanthanum nitrate, iron nitrate, stearic acid.Under the oil bath heating condition, with the stearic acid dissolving, under the constant temperature magnetic agitation, with lanthanum nitrate, the solid of iron nitrate is dissolved in the fusion stearic acid earlier, temperature control 114-125 ℃, more than the reaction 5h, makes it generate gel.Gel is placed 300 ℃ of-500 ℃ of retort furnaces, and heating makes its burning.Can directly obtain perovskite typed superfine powder LaFeO
3(coincide with standard card 75-0541, isometric system (cubic), a=b=c=3.926)
LaMnO
3: 1: 1 in molar ratio: (7-10), difference weighing lanthanum nitrate, Manganous chloride tetrahydrate, stearic acid.Under the oil bath heating condition, with the stearic acid dissolving, under the constant temperature magnetic agitation, with lanthanum nitrate, the solid of Manganous chloride tetrahydrate is dissolved in the fusion stearic acid earlier, temperature control 104-118 ℃, more than the reaction 6h, makes it generate gel.Gel is placed 300 ℃-500 ℃ retort furnace, and heating makes its burning.Can directly obtain perovskite typed superfine powder LaMnO
3(coincide with standard card 72-0841, rhombic system (orthorhombic), a=5.742, b=7.668, c=5.532)
Utilize suitable preparation condition, can prepare perofskite type oxide than bigger serface.LaFeO
3And LaMnO
3The specific surface area and the pattern of powder see Table 1
Table 1 LaFeO
3And LaMnO
3The specific surface area of powder and pattern
The present invention has following advantage and effect:
Raw material used in the present invention is easy to get, and nontoxic.The technology that is adopted has fast simple, and is convenient, and easily realize characteristics such as industrialization.Owing to use the stearic acid can produce greater amount gas, and combustion processes only has the participation of less water, makes the specific surface area of products obtained therefrom big, is expected to improve the various physical and chemical performances of product.
Description of drawings
Fig. 1 is 1: 1: 10 in molar ratio, respectively weighing lanthanum nitrate, iron nitrate, stearic acid.Under the oil bath heating condition, wet 116 ℃ of control, reaction 6.0h makes its burning in 300 ℃ of retort furnaces.The direct perovskite typed superfine powder LaFeO of Huo Deing
3X ray diffracting spectrum (XRD).
Fig. 2 is 1: 1: 10 in molar ratio, respectively weighing lanthanum nitrate, iron nitrate, stearic acid.Under the oil bath heating condition, 116 ℃ of temperature controls, reaction 6.0h makes its burning in 300 ℃ of retort furnaces.The direct perovskite typed superfine powder LaFeO of Huo Deing
3Awkward silence at a meeting emission scan Electronic Speculum picture (SEM).
Fig. 31: 1: 10 in molar ratio, weighing lanthanum nitrate, Manganous chloride tetrahydrate, stearic acid respectively.Under the oil bath heating condition, 108 ℃ of temperature controls, reaction 6.0h makes it generate gel.Place 450 ℃ of retort furnaces to make its burning gel.The direct perovskite typed superfine powder LaMnO of Huo Deing
3X ray diffracting spectrum (XRD).
Fig. 41: 1: 10 in molar ratio, weighing lanthanum nitrate, Manganous chloride tetrahydrate, stearic acid respectively.Under the oil bath heating condition, 108 ℃ of temperature controls, reaction 6h makes it generate gel.Place 450 ℃ of retort furnaces to make its burning gel.The direct perovskite typed superfine powder LaMnO of Huo Deing
3Awkward silence at a meeting emission scan Electronic Speculum picture (SEM).
Embodiment
1.LaFeO
3Preparation
Embodiment 1
1: 1: 10 in molar ratio, difference weighing lanthanum nitrate, iron nitrate, stearic acid.Under the oil bath heating condition, with the stearic acid dissolving, under the constant temperature magnetic agitation, with lanthanum nitrate, the solid of iron nitrate is dissolved in the fusion stearic acid earlier, 116 ℃ of temperature controls, and reaction 6.0h makes it generate gel.Gel is placed 300 ℃ of retort furnaces, and heating makes its burning.Can directly obtain perovskite typed superfine powder LaFeO
3The XRD of powder and pattern are seen Fig. 1 and Fig. 2
Embodiment 2
1: 1: 8 in molar ratio, difference weighing lanthanum nitrate, iron nitrate, stearic acid.Under the oil bath heating condition, with the stearic acid dissolving, under the constant temperature magnetic agitation, with lanthanum nitrate, the solid of iron nitrate is dissolved in the fusion stearic acid earlier, 114 ℃ of temperature controls, and reaction 5.0h makes it generate gel.Gel is placed 300 ℃ of retort furnaces, and heating makes its burning.Can directly obtain perovskite typed superfine powder LaFeO
3The long-pending pattern that reaches of specific grain surface sees Table 1
2.LaMnO
3Preparation
Embodiment 1
1: 1: 10 in molar ratio, difference weighing lanthanum nitrate, Manganous chloride tetrahydrate, stearic acid.Under the oil bath heating condition, with the stearic acid dissolving, under the constant temperature magnetic agitation, with lanthanum nitrate, the solid of Manganous chloride tetrahydrate is dissolved in the fusion stearic acid earlier, 108 ℃ of temperature controls, and reaction 6h makes it generate gel.Gel is placed 450 ℃ of retort furnaces, and heating makes its burning.Can directly obtain perovskite typed superfine powder LaMnO
3The XRD of powder and pattern are seen Fig. 3 and Fig. 4
Embodiment 2
1: 1: 8 in molar ratio, difference weighing lanthanum nitrate, Manganous chloride tetrahydrate, stearic acid.Under the oil bath heating condition, with the stearic acid dissolving, under the constant temperature magnetic agitation, with lanthanum nitrate, the solid of Manganous chloride tetrahydrate is dissolved in the fusion stearic acid earlier, 105 ℃ of temperature controls, and reaction 6h makes it generate gel.Gel is placed 450 ℃ of retort furnaces, and heating makes its burning.Can directly obtain perovskite typed superfine powder LaMnO
3The specific surface area and the pattern of powder see Table 1
Claims (1)
1. one kind prepares ultra-fine perovskite type LaFeO
3And LaMnO
3Method, adopt the gel of stearic acid combustion method to prepare perovskite typed LaFeO
3And LaMnO
3, specifically may further comprise the steps: dissolve stearic acid earlier under the constant temperature oil bath heating condition (1); (2) lanthanum nitrate, iron nitrate; Lanthanum nitrate, two groups of solids of Manganous chloride tetrahydrate are dissolved in respectively in the fusion stearic acid, and under the constant temperature magnetic agitation, the temperature control certain temperature makes reaction system become the complex compound gel behind the reaction certain hour; (3) gel is burnt at a certain temperature, can be through the directly synthetic LaFeO of step burning
3And LaMnO
3, it is characterized in that 1. used fuel and complex compound are stearic acid; 2. screened the suitable condition of preparation; The suitable condition of preparation is:
LaFeO
3: 1: 1 in molar ratio: (7-10), difference weighing lanthanum nitrate, iron nitrate, stearic acid were under the oil bath heating condition, earlier stearic acid is dissolved, under the constant temperature magnetic agitation, with lanthanum nitrate, the solid of iron nitrate is dissolved in the fusion stearic acid, temperature control 114-125 ℃, more than the reaction 5h, make it generate gel, gel is placed 300 ℃ of-500 ℃ of horses expense stoves, heating makes its burning, can directly obtain perovskite typed superfine powder LaFeO
3
LaMnO
3: 1: 1 in molar ratio: (7-10), difference weighing lanthanum nitrate, Manganous chloride tetrahydrate, stearic acid were under the oil bath heating condition, earlier stearic acid is dissolved, under the constant temperature magnetic agitation, with lanthanum nitrate, the solid of Manganous chloride tetrahydrate is dissolved in the fusion stearic acid, temperature control 104-118 ℃, more than the reaction 6h, make it generate gel, gel is placed 300 ℃-500 ℃ horse expense stove, heating makes its burning, can directly obtain perovskite typed superfine powder LaMnO
3
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