CN104528753B - A kind of method that antifungin lanthanum powder is prepared with combustion method - Google Patents
A kind of method that antifungin lanthanum powder is prepared with combustion method Download PDFInfo
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- CN104528753B CN104528753B CN201510042711.XA CN201510042711A CN104528753B CN 104528753 B CN104528753 B CN 104528753B CN 201510042711 A CN201510042711 A CN 201510042711A CN 104528753 B CN104528753 B CN 104528753B
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- combustion
- antifungin
- lanthanum
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- mixed solution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/12—Borates
- C01B35/128—Borates containing plural metal or metal and ammonium
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- 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
Abstract
The present invention relates to a kind of method that boron magnesium lanthanum powder is prepared with combustion method.By controlling raw material proportioning, solution ph, with reference to setting from sintering temperature after climing combustion and calcining at constant temperature time, bulk powdered antifungin lanthanum can be made（LaMgB5O10）Powder.It is 1 by mol ratio：1：5：La (the NO of (2.5~3.2)3)3·6H2O、Mg(NO3)2·6H2O、H3BO3And C2H5NO2It is mixed in corundum crucible, add appropriate distilled water, after mixed solution is heated to 70 DEG C and stirred with the magnetic stirring apparatus with heating, the pH value of ammoniacal liquor regulation mixed solution is slowly added dropwise between 2~4, it is placed in Muffle furnace and is heated to occurring self-propagating combustion and is calcined 2~6h at 900 DEG C, because the reaction time is short, combustion-gas flow severe impact, be conducive to the reunion degree between the refinement of particle, reduction powder product particles.
Description
Technical field
The present invention relates to a kind of method that antifungin lanthanum powder is prepared with combustion method, belong to the technology of preparing of antifungin lanthanum powder
Field.
Background technology
Borate due to the diversity of its matrix structure, as luminescent material host material by domestic and foreign scholars depth
Enter research.Early in the beginning of the eighties, antifungin is regarded as a kind of photoluminescent host material, with correlative study not
It is broken into ripe, host material has turned to polycation borate by single cation borate, and alkaline earth metal borate M3La3
(BO3)5（M=Mg2+、Ca2+、Sr2+、Ba2+) due to its unique structure, it is rare earth doped after have preferable luminescent properties.At present, have
Close into rare earth doped antifungin lanthanum（LaMgB5O10）The report of fluorescent material is more and more, and LaMgB5O10It is used as preferable hair
One of host material of luminescent material, pure phase LaMgB5O10Synthesis also by appearing in the newspapers.Saubat B etc. use high temperature process heat
Method successfully synthesizes pure phase LaMgB5O10, and combustion method is easy to operate, technique is easy, and principle is simple, passes through oxidant（Nitric acid
Salt）And reducing agent（Incendiary agent）The amount of heat of violent redox reaction release is spontaneous to be spread, and rapid reaction is prepared thin
The antifungin lanthanum of pine（LaMgB5O10）Product.It is with soluble metallic salt to use combustion synthesis method（Nitrate）And organic-fuel
（Such as glycine, urea, citric acid）As reactant, metal nitrate serves as oxidant in the reaction, and organic-fuel is anti-
Reducing agent is served as in answering, reaction system is lighted at a certain temperature triggers violent redox reaction, with pushing away for combustion wave
Dynamic, reactant is changed into rapidly final product, and this greatly shortens experimental period.And resulting product is evenly distributed,
Purity is high, and its lytic activity is high.This method technique is simple, and the energy expenditure of equipment when the addition of incendiary agent can reduce roasting can
Antifungin lanthanum is prepared with the roaster of lower-wattage, but the selection of incendiary agent is most important, and the species and addition of incendiary agent will
Directly affect the purity of powder.
The present invention uses lanthanum nitrate hexahydrate（La(NO3)3·6H2O）, magnesium nitrate hexahydrate（Mg(NO3)2·6H2O）And boric acid
（H3BO3）For oxidant, glycine（C2H5NO2）As incendiary agent and reducing agent, the technical problems to be solved by the invention are fast
Speed efficiently production particle refinement, reunion degree is low, and size is small, even-grained fluffy powder shape antifungin lanthanum powder, it is determined that
Prepare antifungin lanthanum（LaMgB5O10）The optimum process condition of powder.
The content of the invention
Antifungin lanthanum is prepared with combustion method it is an object of the invention to provide one kind（LaMgB5O10）The method of powder, uses the party
Antifungin lanthanum powder made from method, because the reaction time is short, combustion-gas flow severe impact, is conducive to the refinement of particle, reduction
Interparticle reunion degree, by controlling raw material proportioning, solution ph, with reference to setting from sintering temperature and roasting time after climing combustion
The antifungin lanthanum powder of bulk shape can be prepared.
To achieve the above object, the present invention uses following technical scheme：Raw material is La (NO3)3×6H2O、Mg(NO3)2·
6H2O、H3BO3And C2H5NO2.In combustion reaction, La (NO3)3·6H2O、Mg(NO3)2·6H2O、H3BO3And C2H5NO2Mole match somebody with somebody
Than the purity for directly affecting powder, the thermochemical theory in propellant chemistry calculates fuel（Reducing agent）With nitrate（Oxygen
Agent）Mol ratio.By calculating the total reducing agent and oxidant of raw material, using the two data as fuel and nitrate
Stoichiometric coefficient, it is assumed that comburant burns completely, then product is CO2、N2And H2O, Elements C, H chemical valence be respectively+
4 valencys and+1 valency, element O chemical valences are-divalents, and N is the neutral element of 0 valency.Calculate and understand that its theoretical molar ratio is：
La(NO3)3·6H2O：Mg(NO3)2·6H2O：H3BO3：C2H5NO2=1：1：5：2.778
It is 1 by mol ratio：1：5：（2.5~3.2）La (NO3)3·6H2O、Mg(NO3)2·6H2O、H3BO3And C2H5NO2
It is mixed in corundum crucible, adds appropriate distilled water, mixed solution is heated to 70 DEG C with the magnetic stirring apparatus with heating and stirred
After mixing uniformly, the pH value of ammoniacal liquor regulation mixed solution is slowly added dropwise between 2~4, resulting solution is precursor liquid.Crucible is put
Enter in Muffle furnace and heat, when temperature is sufficiently high, solvent is gradually evaporated as gel in precursor liquid, is reaching its ignition temperature
When, self-propagating combustion reaction occurs in Muffle furnace, combustion reaction process terminated in more than ten seconds, continue 900 DEG C of roastings 2~
After 6h, fully reaction, bulk sprills product, i.e. antifungin lanthanum powder are obtained in crucible, X-ray diffraction analysis (XRD) show
Its characteristic spectral line and antifungin lanthanum standard spectrum JCPDS (35-0120）Unanimously.
It is of the invention that there is advantages below compared with existing preparation technology：
1st, simple with technique, short preparation period, equipment requirement is low, and yield is high, the characteristics of distribution of reaction products is uniform, holds
Easily realize industrialized production.
2nd, the present invention is by controlling raw material proportioning, solution ph, with reference to setting from sintering temperature and constant temperature calcining after climing combustion
Time can prepare bulk powdered antifungin lanthanum powder, because the reaction time is short, combustion-gas flow severe impact, be conducive to grain
The refinement of son, reduces interparticle reunion degree, and control process is easily operated.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrogram of the antifungin lanthanum powder prepared under the present embodiment.
Embodiment
Embodiment 1
A certain amount of La (NO are weighed respectively3)3·6H2O、Mg(NO3)2·6H2O、H3BO3And C2H5NO2, their mol ratio
For 1：1：5：2.5, it is mixed in corundum crucible, adds appropriate distilled water, magnetic agitation of the mixed solution with heating
After device is heated to 70 DEG C and stirred, the pH value that ammoniacal liquor regulation mixed solution is slowly added dropwise is 4, and resulting solution is forerunner
Liquid.Crucible is put into Muffle furnace and is heated to occurring to continue after self-propagating combustion reaction being calcined 5h at 900 DEG C, bulk shape powder is obtained
Last product, XRD spectra analysis result shows that product is antifungin lanthanum.
Embodiment 2
A certain amount of La (NO are weighed respectively3)3·6H2O、Mg(NO3)2·6H2O、H3BO3And C2H5NO2, their mol ratio
For 1：1：5：2.7, it is mixed in corundum crucible, adds appropriate distilled water, magnetic agitation of the mixed solution with heating
After device is heated to 70 DEG C and stirred, the pH value that ammoniacal liquor regulation mixed solution is slowly added dropwise is 4, and resulting solution is forerunner
Liquid.Crucible is put into Muffle furnace and is heated to occurring to continue after self-propagating combustion reaction being calcined 4h at 900 DEG C, bulk shape powder is obtained
Last product, XRD spectra analysis result shows that product is antifungin lanthanum.
Embodiment 3
A certain amount of La (NO are weighed respectively3)3·6H2O、Mg(NO3)2·6H2O、H3BO3And C2H5NO2, their mol ratio
For 1：1：5：2.8, it is mixed in corundum crucible, adds appropriate distilled water, magnetic agitation of the mixed solution with heating
After device is heated to 70 DEG C and stirred, the pH value that ammoniacal liquor regulation mixed solution is slowly added dropwise is 3, and resulting solution is forerunner
Liquid.Crucible is put into Muffle furnace and is heated to occurring to continue after self-propagating combustion reaction being calcined 4h at 900 DEG C, bulk shape is obtained
Powdered product, XRD spectra analysis result shows that product is antifungin lanthanum.
Embodiment 4
A certain amount of La (NO are weighed respectively3)3·6H2O、Mg(NO3)2·6H2O、H3BO3And C2H5NO2, their mol ratio
For 1：1：5：3, it is mixed in corundum crucible, adds appropriate distilled water, magnetic stirring apparatus of the mixed solution with heating
After being heated to 70 DEG C and stirring, the pH value that ammoniacal liquor regulation mixed solution is slowly added dropwise is 3, and resulting solution is precursor liquid.
Crucible is put into Muffle furnace and is heated to occurring to continue after self-propagating combustion reaction being calcined 6h at 900 DEG C, bulk sprills are obtained
Product, XRD spectra analysis result shows that product is antifungin lanthanum.
Embodiment 5
A certain amount of La (NO are weighed respectively3)3·6H2O、Mg(NO3)2·6H2O、H3BO3And C2H5NO2, their mol ratio
For 1：1：5：3, it is mixed in corundum crucible, adds appropriate distilled water, magnetic stirring apparatus of the mixed solution with heating
After being heated to 70 DEG C and stirring, the pH value that ammoniacal liquor regulation mixed solution is slowly added dropwise is 3, and resulting solution is precursor liquid.
Crucible is put into Muffle furnace and is heated to occurring to continue after self-propagating combustion reaction being calcined 2h at 900 DEG C, bulk sprills are obtained
Product, XRD spectra analysis result shows that product is antifungin lanthanum.
Embodiment 6
A certain amount of La (NO are weighed respectively3)3·6H2O、Mg(NO3)2·6H2O、H3BO3And C2H5NO2, their mol ratio
For 1：1：5：3.2, it is mixed in corundum crucible, adds appropriate distilled water, magnetic agitation of the mixed solution with heating
After device is heated to 70 DEG C and stirred, the pH value that ammoniacal liquor regulation mixed solution is slowly added dropwise is 2, and resulting solution is forerunner
Liquid.Crucible is put into Muffle furnace and is heated to occurring to continue after self-propagating combustion reaction being calcined 3h at 900 DEG C, bulk shape powder is obtained
Last product, XRD spectra analysis result shows that product is antifungin lanthanum.
Claims (1)
1. one kind prepares antifungin lanthanum LaMgB with combustion method5O10The method of powder, it is characterised in that raw material is La (NO3)3·
6H2O、Mg(NO3)2·6H2O、H3BO3With glycine C2H5NO2, by the La (NO of appropriate mol ratio3)3·6H2O、Mg(NO3)2·
6H2O、H3BO3And C2H5NO2It is mixed in corundum crucible, adds appropriate distilled water, magnetic agitation of the mixed solution with heating
After device is heated to proper temperature and stirred, the pH value that ammoniacal liquor adjusts mixed solution is slowly added dropwise, is placed in Muffle furnace
It is heated to occurring self-propagating combustion and is calcined a few houres at a certain temperature, obtains bulk powdered antifungin lanthanum product；
La(NO3)3·6H2O、Mg(NO3)2·6H2O、H3BO3And C2H5NO2Mol ratio be 1：1：5：(2.5~3.2)；Mixing
After solution is heated to 70 DEG C and stirred with the magnetic stirring apparatus with heating, by the way that ammoniacal liquor is added dropwise, the pH of mixed solution is adjusted
Value is between 2~4；The sintering temperature is 900 DEG C, 2~6h of roasting time.
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| CN201510042711.XA CN104528753B (en) | 2015-01-10 | 2015-01-28 | A kind of method that antifungin lanthanum powder is prepared with combustion method |
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| CN2015100110167 | 2015-01-10 | ||
| CN201510042711.XA CN104528753B (en) | 2015-01-10 | 2015-01-28 | A kind of method that antifungin lanthanum powder is prepared with combustion method |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874860A (en) * | 2012-09-08 | 2013-01-16 | 辽宁石油化工大学 | Method for preparing magnesium aluminate lanthanum powder through combustion method |
| CN103866387A (en) * | 2014-04-01 | 2014-06-18 | 中国科学院福建物质结构研究所 | (Yb<3+>: LaMgB5O10) doped laser crystal and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874860A (en) * | 2012-09-08 | 2013-01-16 | 辽宁石油化工大学 | Method for preparing magnesium aluminate lanthanum powder through combustion method |
| CN103866387A (en) * | 2014-04-01 | 2014-06-18 | 中国科学院福建物质结构研究所 | (Yb<3+>: LaMgB5O10) doped laser crystal and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Synthesis and Structural Study of the New Rare Earth Magnesium Borates LnMgB5010 (Ln= La,... , Er);Bernadette Saubat et al.;《Journal of Solid State Chemistry》;19801231;第34卷;271-277 * |
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