CN108658132B - Nitrate assists citric acid complex method low temperature to synthesize Ca-Ti ore type LaCoO3 - Google Patents
Nitrate assists citric acid complex method low temperature to synthesize Ca-Ti ore type LaCoO3 Download PDFInfo
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- CN108658132B CN108658132B CN201810752019.XA CN201810752019A CN108658132B CN 108658132 B CN108658132 B CN 108658132B CN 201810752019 A CN201810752019 A CN 201810752019A CN 108658132 B CN108658132 B CN 108658132B
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- nitrate
- citric acid
- lacoo
- acid complex
- ore type
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 238000000034 method Methods 0.000 title claims abstract description 33
- 229910002254 LaCoO3 Inorganic materials 0.000 title claims abstract description 21
- 229910002651 NO3 Inorganic materials 0.000 title claims abstract description 13
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 10
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000010941 cobalt Substances 0.000 claims abstract description 6
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical class O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 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 description 4
- 238000002156 mixing Methods 0.000 claims description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims 1
- -1 lanthanum acetate cobalt Chemical compound 0.000 claims 1
- 229910000473 manganese(VI) oxide Inorganic materials 0.000 claims 1
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 abstract description 14
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 abstract description 14
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 abstract description 14
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 abstract description 11
- 238000002360 preparation method Methods 0.000 abstract description 8
- 239000004317 sodium nitrate Substances 0.000 abstract description 7
- 235000010344 sodium nitrate Nutrition 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 235000010333 potassium nitrate Nutrition 0.000 abstract description 6
- 239000004323 potassium nitrate Substances 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 238000001354 calcination Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 239000012752 auxiliary agent Substances 0.000 description 8
- 239000011777 magnesium Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000011575 calcium Substances 0.000 description 7
- 239000008364 bulk solution Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 238000001308 synthesis method Methods 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 244000261559 Smilax china Species 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910001963 alkali metal nitrate Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 229910001964 alkaline earth metal nitrate Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000001465 calcium Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- JLRJWBUSTKIQQH-UHFFFAOYSA-K lanthanum(3+);triacetate Chemical compound [La+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JLRJWBUSTKIQQH-UHFFFAOYSA-K 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000011833 salt mixture Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/70—Cobaltates containing rare earth, e.g. LaCoO3
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
- C01P2002/34—Three-dimensional structures perovskite-type (ABO3)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention discloses a kind of low temperature synthesis Ca-Ti ore type LaCoO3Method --- nitrate assist citric acid complex method.The method of the present invention includes the following steps: the presoma of lanthanum and cobalt, citric acid and deionized water being mixed to get solution first, then nitric acid salt assitant (sodium nitrate, potassium nitrate, calcium nitrate or magnesium nitrate) is added into solution, Ca-Ti ore type LaCoO is made after last agitated, dry and low-temperature bake3.Compared with traditional citric acid complex method, the dosage of citric acid is not only can be significantly reduced in nitrate auxiliary citric acid complex method, moreover it is possible to which (500 DEG C) obtain the Ca-Ti ore type LaCoO of pure phase under lower calcination temperature3, while having that preparation process is simple, the advantages such as easy to operate, be conducive to the industrialized production of perofskite type oxide.
Description
Technical field
The present invention relates to a kind of Ca-Ti ore type LaCoO3Preparation method, it is especially a kind of with alkali or alkaline earth metal
Nitrate is adjuvant, prepares LaCoO at lower calcining temperatures by complexing agent of citric acid3Method.
Background technique
Ca-Ti ore type LaCoO3With many special properties, the functional material in many fields has been used as it, such as fuel electricity
Pond, catalyst, gas separator, especially big magneto-resistor and various gas sensors etc. become most attraction and interesting
One of composite oxides.Therefore Ca-Ti ore type LaCoO3Efficiently prepare it is most important.
LaCoO at present3Common synthetic method has: solid reaction process, hydro-thermal method, solution combustion method, sol-gel method,
Coprecipitation, reverse micelle method etc..In these traditional synthetic methods, sol-gel method craft is the simplest, has preferable
Industrial prospect, but the method generally requires the LaCoO that pure phase can be just obtained under 700 DEG C of calcination condition3, high temperature is not only
The waste of the energy is caused, is also easy to cause material that serious agglomeration occurs, makes LaCoO3Application be restricted.Separately
On the one hand, from the point of view of existing report, complexing agent used in sol-gel method preparation process (citric acid) dosage is generally all needed
Will excessively (0.5 times or more of the amount of lanthanum element substance), the consumption of citric acid is bigger.
Need high temperature that could prepare pure phase LaCoO for sol-gal process3Deficiency, have relevant patent report and exist
Pure phase LaCoO is obtained under lower temperature (500 DEG C)3Method, as patent (ZL 201610545762.9) discloses a kind of Portugal
Grape sugar auxiliary electrostatic spin processes low temperature synthesizes Ca-Ti ore type LaCoO3, but that there are still efficiency at present is lower, is difficult to for method of electrostatic spinning
Realize industrialized problem.There is this seminar to disclose a kind of method (CN of green syt lanthanum based perovskite again
201711366602.9) LaCoO of pure phase, has been synthesized under the conditions of low temperature (500 DEG C) using phyteral extracting solution3, but U.S.-China
Unfortunately, in actual application the type and freshness of phyteral raw material to LaCoO3Low temperature synthesis influence compared with
Greatly, so that low temperature preparation pure phase LaCoO3There are certain unstability, therefore its industrial applications also receives certain restrictions.
Therefore it develops and a kind of can be simple at a lower temperature and stably synthesizes pure phase LaCoO3Method, to Ca-Ti ore type
The theoretical research of oxide and industrial application have great importance.
Summary of the invention
In view of the above problems, the purpose of the present invention is to provide a kind of (500 DEG C) synthesis perofskite type oxides of low temperature
LaCoO3Method --- nitrate assist citric acid complex method.
To achieve the purpose of the present invention the technical solution adopted is as follows:
(1) by the presoma of lanthanum, the presoma of cobalt, citric acid and nitric acid salt assitant (MNO3, M=Mg, Ca, Na+K, Na+
Mg, Na+Mg+Ca, Na+K+Mg+Ca) mixing, deionized water is added, stirring and dissolving obtains solution；
(2) solution that (1) obtains is dried, roasts and obtains perofskite type oxide LaCoO3。
Preferably, the presoma of lanthanum used in step (1) is lanthanum nitrate or lanthanum acetate, and the presoma of cobalt used is nitre
Sour cobalt or cobalt acetate, the ratio between amount of substance of lanthanum element and cobalt element is 1:1 in preparation process.
Preferably, auxiliary agent MNO used in step (1)3It is magnesium nitrate or nitre for alkali metal or the nitrate of alkaline-earth metal
One of sour calcium or sodium nitrate, potassium nitrate, magnesium nitrate, in calcium nitrate any several (two kinds, three kinds or four kinds) with
The salt-mixture of arbitrary proportion.The elemental mole ratios of M and lanthanum are 0.008~0.8:1 in preparation process.
Preferably, the dry temperature of step (2) is 75~95 DEG C, and the dry time is 18~50 h, the heating speed of roasting
Rate is 2~8 DEG C/min, and final temperature is 500~600 DEG C, and constant temperature time is 2~5 h.
It can be seen from the above technical scheme that the invention has the following beneficial effects:
(1) this method can obtain the purer Ca-Ti ore type of crystal phase using a small amount of auxiliary agent under 500 DEG C of roasting condition
LaCoO3；
(2) Citric Acid Dosage is fewer than traditional citric acid complex method during the preparation process for this method, can obviously save raw material；
(3) preparation process of this method is simple, easy to operate, mass production easy to accomplish.
Detailed description of the invention
Fig. 1 is the XRD spectra of sample prepared by embodiment 1.
Fig. 2 is the XRD spectra of sample prepared by embodiment 2.
Fig. 3 is the XRD spectra of sample prepared by embodiment 3.
Fig. 4 is the XRD spectra of sample prepared by embodiment 4.
Fig. 5 is the LaCoO that different nitric acid salt assitants assist citric acid complex method to synthesize under the conditions of 500 DEG C3XRD spectrum
Figure.
Specific embodiment
To be best understood from the present invention, the present invention is described further below with reference to embodiment, but the present invention claims
The range of protection is not limited to the range of embodiment expression.
Embodiment 1 (identical Citric Acid Dosage, different assistant concentrations)
Ca-Ti ore type LaCoO is synthesized using nitrate auxiliary citric acid complex method low temperature3:
1) certain density lanthanum nitrate, cobalt nitrate, citric acid, sodium nitrate, potassium nitrate, magnesium nitrate and calcium nitrate are configured first
Mother liquor；Then controlled concentration ratio La3+:Co2+: it is female to pipette suitable lanthanum nitrate, cobalt nitrate and citric acid for citric acid=1:1:0.4
Liquid, magnetic agitation mixing, obtains bulk solution (10 mL)；Then controlled concentration ratio Na+:K+:Mg2+:Ca2+=1:17.12:
1.83:13, pipettes suitable sodium nitrate, potassium nitrate, magnesium nitrate and nitric acid mother liquor of calcium, and magnetic agitation mixing obtains compounding agent solution
(MNO3), MNO is then added into bulk solution3, control the MNO of different samples3Dosage be 1,2,3,4 mL, will finally contain
There is the bulk solution of auxiliary agent to complement to 20 mL, stirring and dissolving obtains reaction solution (La3+Ultimate density be 46.19 mM/
L)；
2) different solution is then transferred in Muffle furnace in 80 DEG C of 24 h of drying in oven, with 5 DEG C/min's
Heating rate rises to 500 DEG C and 4 h of constant temperature from room temperature, obtains LaCoO3Sample, be denoted as respectively 500CA0.4M1,
500CA0.4M2,500CA0.4M3 and 500CA0.4M4.
Fig. 1 is the XRD spectra of sample prepared by embodiment 1, from the figure, it can be seen that different assistant concentrations are at 500 DEG C
Under conditions of citric acid complex method can be assisted to obtain the LaCoO of pure phase3。
Embodiment 2 (identical Citric Acid Dosage, different auxiliary agent compositions)
Ca-Ti ore type LaCoO is synthesized using with nitrate auxiliary citric acid complex method low temperature in embodiment 13Consistent synthesis
Method, respectively with different auxiliary agents: sodium nitrate (being denoted as Na, final concentration of: 8.26 mM/L), calcium nitrate (are denoted as Ca, final concentration
Are as follows: 0.62 mM/L), sodium nitrate+potassium nitrate (being denoted as Na+K, 3.75 mL of dosage), calcium nitrate+magnesium nitrate (be denoted as Ca+Mg, use
Measure 0.5 mL) and sodium nitrate+potassium nitrate+magnesium nitrate (being denoted as Na+K+Mg, 10 mL of dosage) synthesis LaCoO3, mixed aid it is each
Ratio in component ratio and embodiment 1 is consistent, and different samples is respectively labeled as: 500CA0.4Na, 500CA0.4Ca,
500CA0.4Na+K、500CA0.4Ca+Mg、500CA0.4Na+K+Mg。
Fig. 2 is the XRD spectra of sample prepared by embodiment 2, it can be seen from the figure that different auxiliary agents is formed 500
Citric acid complex method can be assisted to obtain the LaCoO of pure phase under conditions of DEG C3。
Embodiment 3 (same auxiliary agent composition, different Citric Acid Dosages)
Ca-Ti ore type LaCoO is synthesized using with nitrate auxiliary citric acid complex method low temperature in embodiment 13Consistent synthesis
Method,
Respectively with different Citric Acid Dosages: CA0.6 (La3+: citric acid=1:0.6, auxiliary dosage: 20 mL) and CA1.0
(La3+: citric acid=1:1.0, auxiliary dosage: 4.2 mL) synthesis LaCoO3, different samples be respectively labeled as 500CA0.6M20,
500CA1.0M4.2。
Fig. 3 is the XRD spectra of sample prepared by embodiment 3, it can be seen from the figure that leading under different Citric Acid Dosages
Peroxy-nitrate auxiliary citric acid complex method can obtain the LaCoO of pure phase under conditions of 500 DEG C3。
Embodiment 4 (same auxiliary agent composition, same Citric Acid Dosage, different calcination temperatures)
Ca-Ti ore type LaCoO is synthesized using with nitrate auxiliary citric acid complex method low temperature in embodiment 13Consistent synthesis
Method, respectively with 600,700,800 DEG C of synthesis LaCoO3, different samples be denoted as respectively 600CA0.4M1,700CA0.4M1,
And 800CA0.4M1.
Fig. 4 is the XRD spectra of sample prepared by embodiment 4, it can be seen from the figure that with the raising of calcination temperature,
The XRD appearance of sample is more sharp, and no miscellaneous peak occurs.
For the ordinary skill in the art, specific embodiment is only exemplarily described the present invention,
Obviously the present invention specific implementation is not subject to the restrictions described above, as long as use the inventive concept and technical scheme of the present invention into
The improvement of capable various unsubstantialities, or not improved the conception and technical scheme of the invention are directly applied to other occasions
, it is within the scope of the present invention.
Claims (2)
1. nitrate assists citric acid complex method low temperature to synthesize Ca-Ti ore type LaCoO3, which comprises the steps of:
(1) by the presoma of lanthanum, the presoma of cobalt, citric acid and nitric acid salt assitant (MNO3) mixing, deionized water, stirring is added
Dissolution, obtains solution, wherein M=Mg, Ca, Na+K or Na+K+Mg+Ca, and the molar ratio of M and lanthanum element is 0.008:1；
(2) solution that (1) obtains is dried, roasts and obtains perofskite type oxide LaCoO3, the temperature of drying therein is
75~95 DEG C, the dry time is 18~50 h, and the heating rate of roasting is 2~8 DEG C/min, and final temperature is 500~600
DEG C, constant temperature time is 2~5 h.
2. nitrate auxiliary citric acid complex method low temperature as described in claim 1 synthesizes Ca-Ti ore type LaCoO3, feature exists
In the presoma that: the presoma of the lanthanum is the lanthanum nitrate perhaps lanthanum acetate cobalt be cobalt nitrate or cobalt acetate.
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| CN111468131B (en) * | 2020-05-28 | 2022-05-24 | 福建师范大学 | LaCoO with high catalytic oxidation activity3Method for synthesizing catalyst |
| CN112717943A (en) * | 2020-12-10 | 2021-04-30 | 昆明理工大学 | Nitric oxide oxidation catalyst and preparation method thereof |
| CN115155603A (en) * | 2022-08-04 | 2022-10-11 | 中国石油大学(北京) | Bimetallic element co-doped lanthanum-based perovskite oxide catalyst and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6017504A (en) * | 1998-07-16 | 2000-01-25 | Universite Laval | Process for synthesizing perovskites using high energy milling |
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| CN101269839A (en) * | 2007-03-22 | 2008-09-24 | 天津市环科机动车尾气催化净化技术有限公司 | Preparation technique for perovskite type rare earth manganate with lemon acid method |
| CN102626632A (en) * | 2012-03-19 | 2012-08-08 | 天津大学 | Perovskite catalyst capable of removing nitrogen oxides and soot in diesel exhaust simultaneously and its preparation method and use |
| CN106186084B (en) * | 2016-07-12 | 2017-11-28 | 福建师范大学 | Glucose auxiliary electrostatic spinning low-temperature bake method prepares Ca-Ti ore type LaCoO3 |
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| US6017504A (en) * | 1998-07-16 | 2000-01-25 | Universite Laval | Process for synthesizing perovskites using high energy milling |
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