CN106365194A - Preparation method of lanthanum titanate nanometer material - Google Patents
Preparation method of lanthanum titanate nanometer material Download PDFInfo
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- CN106365194A CN106365194A CN201610989919.7A CN201610989919A CN106365194A CN 106365194 A CN106365194 A CN 106365194A CN 201610989919 A CN201610989919 A CN 201610989919A CN 106365194 A CN106365194 A CN 106365194A
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- lanthanium titanate
- lanthanum
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title abstract description 11
- 229910052746 lanthanum Inorganic materials 0.000 title abstract description 7
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 title abstract description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 72
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 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 25
- 238000004132 cross linking Methods 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000002086 nanomaterial Substances 0.000 claims description 39
- GYUPBLLGIHQRGT-UHFFFAOYSA-N pentane-2,4-dione;titanium Chemical compound [Ti].CC(=O)CC(C)=O GYUPBLLGIHQRGT-UHFFFAOYSA-N 0.000 claims description 22
- 238000003837 high-temperature calcination Methods 0.000 claims description 9
- 230000004044 response Effects 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 244000248349 Citrus limon Species 0.000 claims 2
- 235000005979 Citrus limon Nutrition 0.000 claims 2
- -1 acyl acetone titanium Chemical compound 0.000 claims 1
- 239000011541 reaction mixture Substances 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 27
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000001354 calcination Methods 0.000 abstract description 3
- RYSXWUYLAWPLES-MTOQALJVSA-N (Z)-4-hydroxypent-3-en-2-one titanium Chemical compound [Ti].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O RYSXWUYLAWPLES-MTOQALJVSA-N 0.000 abstract 2
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 239000000446 fuel Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 9
- 238000006555 catalytic reaction Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000003801 milling Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- LSYIMYXKHWXNBV-UHFFFAOYSA-N lanthanum(3+) oxygen(2-) titanium(4+) Chemical compound [O-2].[La+3].[Ti+4] LSYIMYXKHWXNBV-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
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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
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to the field of inorganic nonmetallic material preparation, and particularly relates to a preparation method of a lanthanum titanate nanometer material. The preparation method comprises the steps that lanthanum nitrate, titanium acetylacetonate and citric acid are taken as raw materials, the raw materials are stirred to be dissolved in water and then subjected to a cross-linking reaction under the stirring and heating conditions, a reaction product is naturally cooled and then put into a mortar to be ground, a continuous high-temperature calcining reaction is conducted, the temperature is lowered to room temperature, and then the lanthanum titanate nanometer material is obtained, wherein the mole ratio of lanthanum nitrate to titanium acetylacetonate to citric acid is 1:1:(6-60). According to the preparation method, the purity of the target product is high, and the preparation cost is low; the yield of the target product ranges from 99.2% to 99.8%, the size of the target product ranges from 30 nm to 50 nm, and the requirement on the lanthanum titanate nanometer material product in the industrial application field can be met; products made of the material can be applied to the fields of ferroelectric cells, photovoltaic cells, photocatalytic cells, fuel cells and the like.
Description
Technical field
The invention belongs to the preparing technical field of Inorganic Non-metallic Materials, concretely relate to a kind of lanthanium titanate
(la2ti2o7) nano material preparation method.
Background technology
Lanthanium titanate (la2ti2o7, lanthanum titanium oxide), No. cas is [12031-47-9], is a kind of
The function ceramics powder of new synthetic.Can serve as piezoelectric, photoelectric material, ferroelectric material etc..Due to lanthanium titanate
It is typical laminated perovskite (a2b2o7) type rare earth metal composite oxide, there is catalysis activity is high, photo-quantum efficiency is big etc.
Advantage, can efficient utilization luminous energy, thus have quite varied at aspects such as photolysis water hydrogen, Organic substance decomposition, environmental improvements
Purposes.
The conventional synthetic method of lanthanium titanate typically adopts traditional solid phase high temperature process, the method not only high energy consumption, and
Sinter for a long time, the product cut size of synthesis is big and skewness is thus have impact on its serviceability.How using economy
Rational process route, synthesizes the product that purity is high, particle diameter is little and is evenly distributed, and the emphasis having become as researcher grinds
Study carefully problem.
Content of the invention
It is contemplated that providing a kind of process is simple in place of overcoming the deficiencies in the prior art, purpose product high income, system
Standby low cost, operating procedure is simple, the preparation method of the good lanthanium titanate nano material of uniformity.The present invention is by using crosslinking
Agent is it is achieved that the technical process of pure phase lanthanium titanate nano material is produced in Low Temperature Solid-Phase calcining.By multigroup contrast test it was found that
Cross-linking agent plays an important role in the reaction, is successfully generated using its fusing in the reaction and combustion heat release and has well
The lanthanium titanate nano material of degree of crystallinity.Preparation method of the present invention can be applied equally to the other functional materials similar with lanthanium titanate
Chemosynthesis research, and have broad application prospects.
For reaching above-mentioned purpose, the present invention is realized in.
A kind of preparation method of lanthanium titanate nano material, is that Lanthanum (III) nitrate, titanium acetylacetone and citric acid is abundant in water
Dissolving, after in stirring and carrying out cross-linking reaction under heating condition, puts into after natural cooling in mortar and grinds, the high-temperature calcination that continues is anti-
Should, temperature drop to room temperature, that is, obtain lanthanium titanate nano material.
As a kind of preferred version, the mol ratio of Lanthanum (III) nitrate of the present invention, titanium acetylacetone and citric acid is 1: 1: 6
～60.
As another kind of preferred version, the molar concentration of Lanthanum (III) nitrate of the present invention is 0.01～0.5 mol/l；Described
Titanium acetylacetone molar concentration be 0.01～0.5 mol/l；The molar concentration of described citric acid is 0.06～3.0
mol/l.
Further, the time of stirring and dissolving of the present invention is 30～60 minutes.
Further, the mixing speed of cross-linking reaction of the present invention is 100～600 revs/min, cross-linking reaction
Temperature is 150～500 ° of c, and cross-linking reaction time is 1～10 h.
Further, the time ground in described mortar is 1～3 h.
Further, in 600～800 ° of c, heating rate divides the temperature of described high-temperature calcination reaction for 5～20 ° of c/
Clock, the response time is 4～24 h.
Compared with prior art, the present invention has following features.
(1) the preparation technology route of lanthanium titanate nano material is simple, and preparation cost is low, easy to control, has higher
Production efficiency, synthesis lanthanium titanate nanoparticle size be 30 ~ 50 nm.Purpose product high income (99.2%～99.9%), can
Meet the requirement to lanthanium titanate nano material product for the industrial application.
(2) purpose product lanthanium titanate nano material, its purity height (99.92%～99.98%), impurity content is low, uniformly
Property good (by sem figure it can be seen that).
(3) energy gap of the purpose product lanthanium titanate nano material of present invention preparation is 3.0～3.1 ev, can meet work
The requirement to stannic acid yttrium material product for the industry application.
(4) the purpose product lanthanium titanate nano material of present invention preparation is used with photocatalyst, and degradation rate can within 60 minutes
Reach (97.0%～99.8%), there is higher catalysis activity.
Brief description
The invention will be further described with reference to the accompanying drawings and detailed description.Protection scope of the present invention not only office
It is limited to the statement of following content.
Fig. 1 is the X-ray diffraction pattern of the lanthanium titanate nano material prepared by the present invention.
Fig. 2 is the sem figure of the lanthanium titanate nano material prepared by the present invention.
Fig. 3 is the sem figure of the lanthanium titanate nano material prepared by the present invention.
Fig. 4 is the sem figure of the lanthanium titanate nano material prepared by the present invention.
Fig. 5 is the sem figure of the lanthanium titanate nano material prepared by the present invention.
Fig. 6 is the visible-uv absorption spectra of the lanthanium titanate nano material prepared by the present invention.
Fig. 7 is the energy gap figure of the lanthanium titanate nano material prepared by the present invention.
Specific embodiment
The present invention with Lanthanum (III) nitrate, titanium acetylacetone and citric acid as raw material, raw material according to certain mol ratio, in water
Fully dissolve, then in stirring and after cross-linking reaction under heating condition, grind in mortar, the high-temperature calcination that continues is reacted, temperature
Drop to room temperature, that is, obtain tantalic acid lanthanum powder body, its preparation process is.
(1) by Lanthanum (III) nitrate, titanium acetylacetone and citric acid according to certain molar ratio weighing after, be placed in fully molten in water
Solution, the time of stirring and dissolving is 30～60 minutes.
(2) by above-mentioned solution, low whipping speed is 100～600 revs/min, and temperature is 150～500 ° of c, cross-linking reaction
1～10 h.
(3) product after above-mentioned cross-linking reaction is put in mortar and grind, the time of grinding is 1～3 h.
(4) put in chamber type electric resistance furnace after loading product thing after above-mentioned grinding in crucible, calcination reaction, reaction temperature
600～800 ° of c, heating rate is 5～20 ° of c/ minutes, and the response time is 4～24 h, that is, lanthanium titanate nano material is obtained.
(5) by the use of prepared lanthanium titanate nano material as photocatalyst (0.1g/l), the methyl orange of the 10mg/l that degrades
Solution.In photocatalysis experiment, light source used is 500w mercury lamp.Before irradiation, the methyl orange solution containing catalysis material is in the dark
Stirring 30 minutes, carries out illumination after reaching adsorption equilibrium.With spectrophotometric determination methyl orange dye concentration change.
Referring to the x-ray diffraction style figure of lanthanium titanate nano material prepared by the present invention for the Fig. 1, its pdf card number is:
28-0517.Referring to shown in Fig. 2～5, being scanning electron microscope (sem) figure that the lanthanium titanate nano material prepared by the present invention is carried out, institute
Obtain product lanthanium titanate nano material, the uniformity of material is good, the size of nanoparticle is 30 ~ 50 nm.Fig. 6 is that the present invention is made
The visible uv absorption spectra of standby lanthanium titanate nano material, its ABSORPTION EDGE is in 406 nm.Fig. 7 is prepared by the present invention
Lanthanium titanate nano material bandwidth figure, energy gap about 3.05 ev.
Embodiment 1.
It is sufficiently stirred in water dissolving by putting into after Lanthanum (III) nitrate, titanium acetylacetone and citric acid precise, mixing time 30
Minute.The mol ratio of above-mentioned Lanthanum (III) nitrate, titanium acetylacetone and citric acid is 1: 1: 6.The molar concentration of Lanthanum (III) nitrate is 0.01 mol/
l；The molar concentration of titanium acetylacetone is 0.01mol/l；The molar concentration of citric acid is 0.06 mol/l.Then by this solution,
Low whipping speed is 100 revs/min, and the temperature of cross-linking reaction is 150 ° of c, cross-linking reaction 10 h, after reaction, naturally cools to
Room temperature, puts into and grinds careful, milling time 3 h in mortar.Chamber type electric resistance furnace is put into after above-mentioned mixture is loaded in crucible
In, carry out high-temperature calcination, heating rate is 5 ° of c/ minutes, 800 ° of c of reaction temperature, and the response time is 4 h, obtains after cooling
Lanthanium titanate nano material.The size of its nanoparticle is 35 nm, and energy gap is 3.05 ev, and the yield of product is 99.8%, produces
Product purity is 99.95%, impurity content: carbon is less than 0.05%.Evaluate in the experiment of catalysis activity in photocatalysis, the degraded of 60 minutes
Rate is 98.6%.
Embodiment 2.
It is sufficiently stirred in water dissolving by putting into after Lanthanum (III) nitrate, titanium acetylacetone and citric acid precise, mixing time 60
Minute.The mol ratio of above-mentioned Lanthanum (III) nitrate, titanium acetylacetone and citric acid is 1: 1: 60.The molar concentration of Lanthanum (III) nitrate is 0.05
mol/l；The molar concentration of titanium acetylacetone is 0.5 mol/l；The molar concentration of citric acid is 3.0 mol/l.Then this is molten
Liquid, low whipping speed is 600 revs/min, and the temperature of cross-linking reaction is 500 ° of c, cross-linking reaction 10 h, after reaction, naturally cold
But to room temperature, put into and in mortar, grind careful, milling time 3 h.Box electricity is put into after above-mentioned mixture is loaded in crucible
In resistance stove, carry out high-temperature calcination, heating rate is 10 ° of c/ minutes, 800 ° of c of reaction temperature, and the response time is 24 h, after cooling
Obtain lanthanium titanate nano material.The size of its nanoparticle is 50 nm, and energy gap is 3.1 ev, and the yield of product is
99.9%, product purity is 99.93%, impurity content: carbon is less than 0.07%.Evaluate in the experiment of catalysis activity in photocatalysis, 60 points
The degradation rate of clock is 99.1%.
Embodiment 3.
It is sufficiently stirred in water dissolving by putting into after Lanthanum (III) nitrate, titanium acetylacetone and citric acid precise, mixing time 40
Minute.The mol ratio of above-mentioned Lanthanum (III) nitrate, titanium acetylacetone and citric acid is 1: 1: 30.The molar concentration of Lanthanum (III) nitrate is 0.1 mol/
l；The molar concentration of titanium acetylacetone is 0.1 mol/l；The molar concentration of citric acid is 3.0 mol/l.Then by this solution,
Mixing speed is 200 revs/min, and the temperature of cross-linking reaction is 200 ° of c, cross-linking reaction 5 h, after reaction, naturally cools to room
Temperature, puts into and grinds careful, milling time 2 h in mortar.Put in chamber type electric resistance furnace after above-mentioned mixture is loaded in crucible,
Carry out high-temperature calcination, heating rate is 5 ° of c/ minutes, 600 ° of c of reaction temperature, and the response time is 24 h, obtains titanium after cooling
Sour lanthanum nano material.The size of its nanoparticle is 45 nm, and energy gap is 3.0 ev, and the yield of product is 99.6%, product
Purity is 99.96%, impurity content: carbon is less than 0.04%.Evaluate in the experiment of catalysis activity in photocatalysis, the degradation rate of 60 minutes
For 98.5%.
Embodiment 4.
It is sufficiently stirred in water dissolving by putting into after Lanthanum (III) nitrate, titanium acetylacetone and citric acid precise, mixing time 30
Minute.The mol ratio of above-mentioned Lanthanum (III) nitrate, titanium acetylacetone and citric acid is 1: 1: 12.The molar concentration of Lanthanum (III) nitrate is 0.1 mol/
l；The molar concentration of titanium acetylacetone is 0.1 mol/l；The molar concentration of citric acid is 1.2 mol/l.Then by this solution,
Mixing speed is 300 revs/min, and the temperature of cross-linking reaction is 300 ° of c, cross-linking reaction 5 h, after reaction, naturally cools to room
Temperature, puts into and grinds careful, milling time 2 h in mortar.Put in chamber type electric resistance furnace after above-mentioned mixture is loaded in crucible,
Carry out high-temperature calcination, heating rate is 20 ° of c/ minutes, 700 ° of c of reaction temperature, and the response time is 12 h, obtains after cooling
Lanthanium titanate nano material.The size of its nanoparticle is 40 nm, and energy gap is 3.05 ev, and the yield of product is 99.7%, produces
Product purity is 99.92%, impurity content: carbon is less than 0.08%.Evaluate in the experiment of catalysis activity in photocatalysis, the degraded of 60 minutes
Rate is 97.0%.
Embodiment 5.
It is sufficiently stirred in water dissolving by putting into after Lanthanum (III) nitrate, titanium acetylacetone and citric acid precise, mixing time 60
Minute.The mol ratio of above-mentioned Lanthanum (III) nitrate, titanium acetylacetone and citric acid is 1: 1: 12.The molar concentration of Lanthanum (III) nitrate is 0.2 mol/
l；The molar concentration of titanium acetylacetone is 0.2 mol/l；The molar concentration of citric acid is 2.4 mol/l.Then by this solution,
Mixing speed is 300 revs/min, and the temperature of cross-linking reaction is 400 ° of c, cross-linking reaction 10 h, after reaction, naturally cools to room
Temperature, puts into and grinds careful, milling time 3 h in mortar.Put in chamber type electric resistance furnace after above-mentioned mixture is loaded in crucible,
Carry out high-temperature calcination, heating rate is 20 ° of c/ minutes, 800 ° of c of reaction temperature, and the response time is 6 h, obtains titanium after cooling
Sour lanthanum nano material.The size of its nanoparticle is 40 nm, and energy gap is 3.1 ev, and the yield of product is 99.5%, product
Purity is 99.98%, impurity content: carbon is less than 0.02%.Evaluate in the experiment of catalysis activity in photocatalysis, the degradation rate of 60 minutes
For 99.8%.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of preparation method of lanthanium titanate nano material is it is characterised in that by Lanthanum (III) nitrate, titanium acetylacetone and citric acid in water
Middle stirring and dissolving, carries out cross-linking reaction in stirring and under heating condition, puts in mortar and grind after natural cooling, the high temperature that continues is forged
Burn reaction, temperature drop to room temperature, that is, obtain lanthanium titanate nano material.
2. lanthanium titanate nano material according to claim 1 preparation method it is characterised in that: described Lanthanum (III) nitrate, second
The mol ratio of acyl acetone titanium and citric acid is 1: 1: 6～60.
3. lanthanium titanate nano material according to claim 2 preparation method it is characterised in that: the rubbing of described Lanthanum (III) nitrate
Your concentration is 0.01～0.5 mol/l；The molar concentration of described titanium acetylacetone is 0.01～0.5 mol/l；Described lemon
The molar concentration of lemon acid is 0.06～3.0 mol/l.
4. lanthanium titanate nano material according to claim 3 preparation method it is characterised in that: described stirring and dissolving
Time is 30～60 minutes.
5. lanthanium titanate preparation method of nano material according to claim 4 it is characterised in that: the stirring of described cross-linking reaction
Mix speed and be 100～600 revs/min, the temperature of cross-linking reaction is 150～500 ° of c, and cross-linking reaction time is 1～10 h.
6. the arbitrary described lanthanium titanate preparation method of nano material according to Claims 1 to 5 it is characterised in that: described grinds
The time ground in alms bowl is 1～3 h.
7. lanthanium titanate preparation method of nano material according to claim 6 it is characterised in that: described high-temperature calcination reaction
Temperature in 600～800 ° of c, heating rate is 5～20 ° of c/ minutes, and the response time is 4～24 h.
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| CN110745864A (en) * | 2019-12-03 | 2020-02-04 | 中南大学 | Perovskite type lanthanum titanate material and preparation method and application thereof |
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