CN106365194B - A kind of preparation method of lanthanium titanate nano material - Google Patents
A kind of preparation method of lanthanium titanate nano material Download PDFInfo
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- CN106365194B CN106365194B CN201610989919.7A CN201610989919A CN106365194B CN 106365194 B CN106365194 B CN 106365194B CN 201610989919 A CN201610989919 A CN 201610989919A CN 106365194 B CN106365194 B CN 106365194B
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 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 111
- 238000006243 chemical reaction Methods 0.000 claims abstract description 53
- 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 37
- GYUPBLLGIHQRGT-UHFFFAOYSA-N pentane-2,4-dione;titanium Chemical compound [Ti].CC(=O)CC(C)=O GYUPBLLGIHQRGT-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000004132 cross linking Methods 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000007146 photocatalysis Methods 0.000 claims abstract description 10
- 230000001699 photocatalysis Effects 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims description 15
- 230000003197 catalytic effect Effects 0.000 claims description 13
- 230000035484 reaction time Effects 0.000 claims description 13
- 239000002105 nanoparticle Substances 0.000 claims description 12
- 238000002474 experimental method Methods 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 238000003801 milling Methods 0.000 claims description 10
- 230000015556 catabolic process Effects 0.000 claims description 9
- 238000006731 degradation reaction Methods 0.000 claims description 9
- 238000011156 evaluation Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims 2
- 238000003756 stirring Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000007769 metal material Substances 0.000 abstract description 2
- 230000005621 ferroelectricity Effects 0.000 abstract 1
- 239000000446 fuel Substances 0.000 abstract 1
- 230000005622 photoelectricity Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 229910052746 lanthanum Inorganic materials 0.000 description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229910017582 La2Ti2O7 Inorganic materials 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000000227 grinding Methods 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
- 239000000843 powder Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 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
- 238000005516 engineering process 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
- DRIUWMIAOYIBGN-UHFFFAOYSA-N lanthanum titanium Chemical compound [Ti][La] DRIUWMIAOYIBGN-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 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
- 238000011017 operating method Methods 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 230000002035 prolonged effect 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
- 238000011160 research Methods 0.000 description 1
- 238000005245 sintering 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
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 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
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- 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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- 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 preparation field of inorganic non-metallic material, a kind of more particularly to preparation method of lanthanium titanate nano material, it is using lanthanum nitrate, titanium acetylacetone and citric acid as raw material, first stirring and dissolving in water, then cross-linking reaction is carried out under stirring and heating condition, is put into mortar and grinds after natural cooling, the high-temperature calcination that continues reaction, temperature drops to room temperature, that is, obtains lanthanium titanate nano material.The molar ratio of lanthanum nitrate, titanium acetylacetone and citric acid is 1: 1: 6~60.The object of the invention product purity is high, and manufacturing cost is low.Purpose product yield is 99.2%~99.8%, and size is 30 ~ 50 nm, can meet requirement of the industrial application to lanthanium titanate nano material product.Prepared product can be used for the fields such as ferroelectricity, photoelectricity, photocatalysis and fuel cell.
Description
Technical field
The invention belongs to the preparing technical field of inorganic non-metallic material, concretely relates to a kind of lanthanium titanate
（La2Ti2O7）The preparation method of nano material.
Background technology
Lanthanium titanate（La2Ti2O7,Lanthanum Titanium Oxide）, No. CAS is [12031-47-9], is a kind of
New artificial synthesized function ceramics powder.It may be used 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 catalytic activity is high, photo-quantum efficiency is big etc.
Advantage, can efficiently utilize luminous energy, thus in photolysis water hydrogen, organic matter decomposition, environmental improvement etc. with quite varied
Purposes.
The conventional synthetic method of lanthanium titanate generally uses traditional solid phase high temperature process, this method not only high energy consumption, but also
Prolonged sintering, the product cut size of synthesis is big and skewness is so as to have impact on its performance.How using economy
Rational process route, synthesizes the product that purity is high, particle diameter is small and is evenly distributed, and the emphasis for having become researcher is ground
Study carefully problem.
The content of the invention
It is contemplated that being provided in place of overcome the deficiencies in the prior art, a kind of technique is simple, and purpose product high income, makes
Standby cost is low, and operating procedure is simple, the preparation method of the good lanthanium titanate nano material of uniformity.The present invention is by using crosslinking
Agent, realizes the technical process that pure phase lanthanium titanate nano material is produced in Low Temperature Solid-Phase calcining.Pass through multigroup contrast test, it was found that
Crosslinking agent plays an important role in the reaction, is successfully generated with good using its fusing in the reaction and combustion heat release
The lanthanium titanate nano material of crystallinity.Preparation method of the present invention can be applied equally to the other functional materials similar with lanthanium titanate
Chemical synthesis research, and have broad application prospects.
To reach above-mentioned purpose, what the present invention was realized in.
A kind of preparation method of lanthanium titanate nano material, is that lanthanum nitrate, titanium acetylacetone and citric acid is abundant in water
Dissolving, after carrying out cross-linking reaction under stirring and heating condition, is put into mortar after natural cooling and grinds, the high-temperature calcination that continues is anti-
Should, temperature drops to room temperature, that is, obtains lanthanium titanate nano material.
As a preferred embodiment, the molar ratio of lanthanum nitrate of the present invention, titanium acetylacetone and citric acid is 1: 1: 6
~60.
As another preferred solution, the molar concentration of lanthanum nitrate of the present invention is 0.01~0.5 mol/L；It is described
The molar concentration of titanium acetylacetone be 0.01~0.5 mol/L；The molar concentration of the 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 °C, and cross-linking reaction time is 1~10 h.
Further, the time ground in the mortar is 1~3 h.
Further, for the temperature of high-temperature calcination reaction at 600~800 °C, heating rate is 5~20 °C/point
Clock, reaction time are 4~24 h.
Compared with prior art, the present invention has following features.
（1）The preparation process route of lanthanium titanate nano material is simple, and manufacturing cost is low, easy to control, has higher
Production efficiency, synthesis lanthanium titanate nano-particle size be 30 ~ 50 nm.Purpose product high income（99.2%~99.9%）, can
Meet requirement of the industrial application to lanthanium titanate nano material product.
（2）Purpose product lanthanium titanate nano material, its purity are high（99.92%~99.98%）, impurity content is low, uniformly
Property is good（It can be seen that by SEM figures）.
（3）The energy gap of purpose product lanthanium titanate nano material prepared by the present invention is 3.0~3.1 eV, can meet work
Requirement of the industry application field to stannic acid yttrium material product.
（4）Purpose product lanthanium titanate nano material prepared by the present invention is used with photocatalyst, and degradation rate can within 60 minutes
Reach（97.0%~99.8%）, there is higher catalytic activity.
Brief description of the drawings
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 diffractogram of the lanthanium titanate nano material prepared by the present invention.
Fig. 2 is the SEM figures of the lanthanium titanate nano material prepared by the present invention.
Fig. 3 is the SEM figures of the lanthanium titanate nano material prepared by the present invention.
Fig. 4 is the SEM figures of the lanthanium titanate nano material prepared by the present invention.
Fig. 5 is the SEM figures of the lanthanium titanate nano material prepared by the present invention.
Fig. 6 is 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.
Embodiment
The present invention is using lanthanum nitrate, titanium acetylacetone and citric acid as raw material, and raw material is according to certain mol ratio, in water
Fully dissolving, then grinds under stirring and heating condition after cross-linking reaction in mortar, the high-temperature calcination that continues reaction, temperature
Room temperature is dropped to, that is, obtains tantalic acid lanthanum powder, its preparation process is.
（1）By lanthanum nitrate, titanium acetylacetone and citric acid according to certain molar ratio weighing after, be put into water fully it is molten
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 °C, cross-linking reaction
1~10 h.
（3）Product after above-mentioned cross-linking reaction is put into mortar and is ground, the time of grinding is 1~3 h.
（4）It is put into after product thing after above-mentioned grinding is fitted into crucible in chamber type electric resistance furnace, calcination reaction, reaction temperature
600~800 °C, heating rate is 5~20 °C/minute, and the reaction time is 4~24 h, that is, lanthanium titanate nano material is made.
（5）Photochemical catalyst is used as by the use of prepared lanthanium titanate nano material（0.1g/L）, the methyl orange for the 10mg/L that degrades
Solution.Light source used is 500W mercury lamps in photocatalysis experiment.Before irradiation, the methyl orange solution containing catalysis material is in the dark
Stirring 30 minutes, illumination is carried out after reaching adsorption equilibrium.Changed with spectrophotometric determination methyl orange dye concentration.
Referring to the X-ray diffraction pattern figure that Fig. 1 is the lanthanium titanate nano material prepared by the present invention, its PDF card number is：
28-0517.Referring to the scanning electron microscope shown in Fig. 2~5, carried out for the lanthanium titanate nano material prepared by the present invention（SEM）Figure, institute
Product lanthanium titanate nano material is obtained, the uniformity of material is good, and the size of nano-particle is 30 ~ 50 nm.Fig. 6 is made for the present invention
The visible uv absorption spectra of standby lanthanium titanate nano material, its ABSORPTION EDGE is in 406 nm or so.Fig. 7 is prepared by the present invention
Lanthanium titanate nano material bandwidth figure, about 3.05 eV of energy gap.
Embodiment 1.
Dissolving, mixing time 30 will be sufficiently stirred into the water after lanthanum nitrate, titanium acetylacetone and citric acid precise
Minute.The molar ratio of above-mentioned lanthanum nitrate, titanium acetylacetone and citric acid is 1: 1: 6.The molar concentration of lanthanum 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 the solution,
Low whipping speed is 100 revs/min, and the temperature of cross-linking reaction is 150 °C, and 10 h of cross-linking reaction, after reaction, naturally cools to
Room temperature, is put into mortar and grinds careful, 3 h of milling time.Chamber type electric resistance furnace is put into after above-mentioned mixture is fitted into crucible
In, high-temperature calcination is carried out, heating rate is 5 °C/minute, and 800 °C of reaction temperature, the reaction time is 4 h, is obtained after cooling
Lanthanium titanate nano material.The size of its nano-particle is 35 nm, and energy gap is 3.05 eV, and the yield of product is 99.8%, production
Product purity is 99.95%, impurity content：Carbon is less than 0.05%.In the experiment of photocatalysis evaluation catalytic activity, the degraded of 60 minutes
Rate is 98.6%.
Embodiment 2.
Dissolving, mixing time 60 will be sufficiently stirred into the water after lanthanum nitrate, titanium acetylacetone and citric acid precise
Minute.The molar ratio of above-mentioned lanthanum nitrate, titanium acetylacetone and citric acid is 1: 1: 60.The molar concentration of lanthanum 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 it is this is molten
Liquid, low whipping speed are 600 revs/min, and the temperature of cross-linking reaction is 500 °C, cross-linking reaction 10 h, naturally cold after reaction
But to room temperature, it is put into mortar and grinds careful, 3 h of milling time.Box electricity is put into after above-mentioned mixture is fitted into crucible
Hinder in stove, carry out high-temperature calcination, heating rate is 10 °C/minute, and 800 °C of reaction temperature, the reaction time is 24 h, after cooling
Obtain lanthanium titanate nano material.The size of its nano-particle is 50 nm, and energy gap is 3.1 eV, and the yield of product is
99.9%, product purity 99.93%, impurity content：Carbon is less than 0.07%.In the experiment of photocatalysis evaluation catalytic activity, 60 points
The degradation rate of clock is 99.1%.
Embodiment 3.
Dissolving, mixing time 40 will be sufficiently stirred into the water after lanthanum nitrate, titanium acetylacetone and citric acid precise
Minute.The molar ratio of above-mentioned lanthanum nitrate, titanium acetylacetone and citric acid is 1: 1: 30.The molar concentration of lanthanum 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 the solution,
Mixing speed is 200 revs/min, and the temperature of cross-linking reaction is 200 °C, and 5 h of cross-linking reaction, after reaction, naturally cools to room
Temperature, is put into mortar and grinds careful, 2 h of milling time.It is put into after above-mentioned mixture is fitted into crucible in chamber type electric resistance furnace,
High-temperature calcination is carried out, heating rate is 5 °C/minute, and 600 °C of reaction temperature, the reaction time is 24 h, and titanium is obtained after cooling
Sour lanthanum nano material.The size of its nano-particle 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%.In the experiment of photocatalysis evaluation catalytic activity, the degradation rate of 60 minutes
For 98.5%.
Embodiment 4.
Dissolving, mixing time 30 will be sufficiently stirred into the water after lanthanum nitrate, titanium acetylacetone and citric acid precise
Minute.The molar ratio of above-mentioned lanthanum nitrate, titanium acetylacetone and citric acid is 1: 1: 12.The molar concentration of lanthanum 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 the solution,
Mixing speed is 300 revs/min, and the temperature of cross-linking reaction is 300 °C, and 5 h of cross-linking reaction, after reaction, naturally cools to room
Temperature, is put into mortar and grinds careful, 2 h of milling time.It is put into after above-mentioned mixture is fitted into crucible in chamber type electric resistance furnace,
High-temperature calcination is carried out, heating rate is 20 °C/minute, and 700 °C of reaction temperature, the reaction time is 12 h, is obtained after cooling
Lanthanium titanate nano material.The size of its nano-particle is 40 nm, and energy gap is 3.05 eV, and the yield of product is 99.7%, production
Product purity is 99.92%, impurity content：Carbon is less than 0.08%.In the experiment of photocatalysis evaluation catalytic activity, the degraded of 60 minutes
Rate is 97.0%.
Embodiment 5.
Dissolving, mixing time 60 will be sufficiently stirred into the water after lanthanum nitrate, titanium acetylacetone and citric acid precise
Minute.The molar ratio of above-mentioned lanthanum nitrate, titanium acetylacetone and citric acid is 1: 1: 12.The molar concentration of lanthanum 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 the solution,
Mixing speed is 300 revs/min, and the temperature of cross-linking reaction is 400 °C, and 10 h of cross-linking reaction, after reaction, naturally cools to room
Temperature, is put into mortar and grinds careful, 3 h of milling time.It is put into after above-mentioned mixture is fitted into crucible in chamber type electric resistance furnace,
High-temperature calcination is carried out, heating rate is 20 °C/minute, and 800 °C of reaction temperature, the reaction time is 6 h, and titanium is obtained after cooling
Sour lanthanum nano material.The size of its nano-particle 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%.In the experiment of photocatalysis evaluation catalytic activity, the degradation rate of 60 minutes
For 99.8%.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the invention, for the skill of this area
For art personnel, the invention may be variously modified and varied.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of preparation method of lanthanium titanate nano material, it is characterised in that lanthanum nitrate, titanium acetylacetone and citric acid is accurate
Dissolving, mixing time 30 minutes are sufficiently stirred after weighing into the water；Mole of above-mentioned lanthanum nitrate, titanium acetylacetone and citric acid
Than for 1: 1: 6；The molar concentration of lanthanum nitrate is 0.01mol/L；The molar concentration of titanium acetylacetone is 0.01mol/L；Citric acid
Molar concentration be 0.06mol/L；Then it is 100 revs/min by the solution, low whipping speed, the temperature of cross-linking reaction is
150 DEG C, cross-linking reaction 10h, after reaction, cooled to room temperature, is put into mortar and grinds careful, milling time 3h；Will be above-mentioned
Mixture be fitted into crucible after be put into chamber type electric resistance furnace, carry out high-temperature calcination, heating rate be 5 DEG C/min, reaction
800 DEG C, reaction time 4h of temperature, lanthanium titanate nano material is obtained after cooling；The size of its nano-particle is 35nm, is prohibited
Bandwidth is 3.05eV, and the yield of product is 99.8%, product purity 99.95%, impurity content：Carbon is less than 0.05%；Urged in light
In the experiment for changing evaluation catalytic activity, the degradation rate of 60 minutes is 98.6%.
2. a kind of preparation method of lanthanium titanate nano material, it is characterised in that lanthanum nitrate, titanium acetylacetone and citric acid is accurate
Dissolving, mixing time 60 minutes are sufficiently stirred after weighing into the water；Mole of above-mentioned lanthanum nitrate, titanium acetylacetone and citric acid
Than for 1: 1: 60；The molar concentration of lanthanum nitrate is 0.05 mol/L；The molar concentration of titanium acetylacetone is 0.5mol/L；Citric acid
Molar concentration be 3.0 mol/L；Then it is 600 revs/min by the solution, low whipping speed, the temperature of cross-linking reaction is
500 DEG C, cross-linking reaction 10h, after reaction, cooled to room temperature, is put into mortar and grinds careful, milling time 3h；Will be above-mentioned
Mixture be fitted into crucible after be put into chamber type electric resistance furnace, carry out high-temperature calcination, heating rate be 10 DEG C/min, instead
800 DEG C, reaction time 24h of temperature is answered, lanthanium titanate nano material is obtained after cooling；The size of its nano-particle is 50nm,
Energy gap is 3.1eV, and the yield of product is 99.9%, product purity 99.93%, impurity content：Carbon is less than 0.07%；In light
In the experiment of catalytic evaluation catalytic activity, the degradation rate of 60 minutes is 99.1%.
3. a kind of preparation method of lanthanium titanate nano material, it is characterised in that lanthanum nitrate, titanium acetylacetone and citric acid is accurate
Dissolving, mixing time 40 minutes are sufficiently stirred after weighing into the water；Mole of above-mentioned lanthanum nitrate, titanium acetylacetone and citric acid
Than for 1: 1: 30；The molar concentration of lanthanum nitrate is 0.1mol/L；The molar concentration of titanium acetylacetone is 0.1mol/L；Citric acid
Molar concentration is 3.0mol/L；Then by the solution, low whipping speed is 200 revs/min, and the temperature of cross-linking reaction is 200 DEG C
, cross-linking reaction 5h, after reaction, cooled to room temperature, is put into mortar and grinds careful, milling time 2h；By above-mentioned mixing
Thing is put into chamber type electric resistance furnace after being fitted into crucible, carries out high-temperature calcination, and heating rate is 5 DEG C/min, reaction temperature 600
DEG C, reaction time 24h, lanthanium titanate nano material is obtained after cooling；The size of its nano-particle is 45 nm, energy gap
For 3.0 eV, the yield of product is 99.6%, product purity 99.96%, impurity content：Carbon is less than 0.04%；Evaluated in photocatalysis
In the experiment of catalytic activity, the degradation rate of 60 minutes is 98.5%.
4. a kind of preparation method of lanthanium titanate nano material, it is characterised in that lanthanum nitrate, titanium acetylacetone and citric acid is accurate
Dissolving, mixing time 30 minutes are sufficiently stirred after weighing into the water；Mole of above-mentioned lanthanum nitrate, titanium acetylacetone and citric acid
Than for 1: 1: 12；The molar concentration of lanthanum nitrate is 0.1mol/ L；The molar concentration of titanium acetylacetone is 0.1mol/L；Citric acid
Molar concentration be 1.2 mol/L；Then by the solution, low whipping speed is 300 revs/min, and the temperature of cross-linking reaction is 300
DEG C, cross-linking reaction 5h, after reaction, cooled to room temperature, is put into mortar and grinds careful, milling time 2h；Above-mentioned is mixed
Compound is put into chamber type electric resistance furnace after being fitted into crucible, carries out high-temperature calcination, and heating rate is 20 DEG C/min, reaction temperature
700 DEG C, reaction time 12h, lanthanium titanate nano material is obtained after cooling；The size of its nano-particle is 40 nm, forbidden band
Width is 3.05eV, and the yield of product is 99.7%, product purity 99.92%, impurity content：Carbon is less than 0.08%；In photocatalysis
In the experiment for evaluating catalytic activity, the degradation rate of 60 minutes is 97.0%.
5. a kind of preparation method of lanthanium titanate nano material, it is characterised in that lanthanum nitrate, titanium acetylacetone and citric acid is accurate
Dissolving, mixing time 60 minutes are sufficiently stirred after weighing into the water；Mole of above-mentioned lanthanum nitrate, titanium acetylacetone and citric acid
Than for 1: 1: 12；The molar concentration of lanthanum nitrate is 0.2mol/L；The molar concentration of titanium acetylacetone is 0.2mol/L；Citric acid
Molar concentration is 2.4mol/L；Then by the solution, low whipping speed is 300 revs/min, and the temperature of cross-linking reaction is 400 DEG C
, cross-linking reaction 10h, after reaction, cooled to room temperature, is put into mortar and grinds careful, 3 h of milling time；Above-mentioned is mixed
Compound is put into chamber type electric resistance furnace after being fitted into crucible, carries out high-temperature calcination, and heating rate is 20 DEG C/min, reaction temperature
800 DEG C, reaction time 6h, lanthanium titanate nano material is obtained after cooling；The size of its nano-particle is 40nm, and forbidden band is wide
Spend for 3.1eV, the yield of product is 99.5%, product purity 99.98%, impurity content：Carbon is less than 0.02%；Commented in photocatalysis
In the experiment of valency catalytic activity, the degradation rate of 60 minutes is 99.8%.
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