CN101323442A - Solvent-thermal synthesis of lanthanum phosphate nanorod - Google Patents
Solvent-thermal synthesis of lanthanum phosphate nanorod Download PDFInfo
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- CN101323442A CN101323442A CNA2008100295021A CN200810029502A CN101323442A CN 101323442 A CN101323442 A CN 101323442A CN A2008100295021 A CNA2008100295021 A CN A2008100295021A CN 200810029502 A CN200810029502 A CN 200810029502A CN 101323442 A CN101323442 A CN 101323442A
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- LQFNMFDUAPEJRY-UHFFFAOYSA-K lanthanum(3+);phosphate Chemical compound [La+3].[O-]P([O-])([O-])=O LQFNMFDUAPEJRY-UHFFFAOYSA-K 0.000 title claims abstract description 47
- 239000002073 nanorod Substances 0.000 title claims abstract description 39
- 238000003786 synthesis reaction Methods 0.000 title description 2
- 230000015572 biosynthetic process Effects 0.000 title 1
- 239000000243 solution Substances 0.000 claims abstract description 26
- 239000002904 solvent Substances 0.000 claims abstract description 22
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 12
- 229910000162 sodium phosphate Inorganic materials 0.000 claims abstract description 12
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000007864 aqueous solution Substances 0.000 claims description 9
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical group [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 abstract description 11
- 239000013078 crystal Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 2
- 238000001354 calcination Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 238000010189 synthetic method Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000012761 high-performance material Substances 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 238000003836 solid-state method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- -1 rare earth ion Chemical class 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000004304 visual acuity Effects 0.000 description 1
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Abstract
The invention discloses a method for using a solvent to carry out thermosynthesis so as to obtain nanorods of lanthanum phosphate; the method comprises the following steps of: mixing a lanthanum chloride solution with the concentration of 1.0-2.0mol/L and a sodium phosphate solution with the concentration of 1.0-2.0mol/L, wherein, the sodium phosphate and the lanthanum chloride have equal molar ratio; adding an n-butanol solvent and leading the volume ratio of water and the n-butanol to be 0.5 to 2 : 1 with the molar concentration of the lanthanum chloride in the mixed solution being 0.2 to 0.5mol/L; stirring the mixture till the mixture is even; adjusting the PH value of the solution to be 3 to 6 by phosphoric acid and hot reaction is carried out for 6.0 to 48 hours under the condition that the temperature is 140 to 220 DEG C. The synthetic method of the invention is simple, environment-friendly, green and economical, low-temperature, without needing calcination, and can obtain products directly in the solution; the obtained lanthanum phosphate has high purity, belongs to the monoclinic crystal system and is the nano rod with monazite structure; the nano rod has the diameter of less than 10nm, even fineness, single appearance and good dispersity.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, be specifically related to the method for the synthetic lanthanum phosphate nano rod of a kind of solvent thermal.
Background technology
RE phosphate has fabulous photoluminescent property, high quantum yield, it is the good luminescent material of a class, be applicable to that high-density excites the environment that excites with the high-energy quantum, can be used for special glass, laser technology, compact fluorescent lamp, plasma flat demonstration.Since the chemico-physical properties of RE phosphate self, lanthanum orthophosphate (LaPO
4) be often used as a kind of good substrate material of other rare earth ion that mixes, in optical material, occupy critical role.Simultaneously, RE phosphate LaPO
4The fusing point height is to be fit to the oxide fibre coated material that high temperature uses, with Al
2O
3The combined high temperature good stability can prepare Al
2O
3/ LaPO
4High temperature can be processed composite ceramics, has advantages such as high temperature resistant, corrosion-resistant, oxidation-resistance, electrical insulating property be good, is widely used in the engineering field.On the other hand, since the singularity of rare earth element structure, LaPO
4Can be used for that molecular sieve is carried out modification and regulate its surface acid alkalescence, thereby make it aspect catalytic chemistry, also have unique effect.
Relevant in recent years nano materials research finds, the microstructure of material such as size, granule-morphology, special surface property, degree of crystallinity and size distribution, particles dispersed etc. have very large influence to the machining property and the catalytic property of the luminous efficiency of device and resolving power, material.Synthetic particle is tiny, good dispersity, be evenly distributed, the nano-powder of pattern homogeneous, be the prerequisite of preparation high performance material.In order to satisfy people to the high performance material demand, preparation LaPO
4The novel process of ultrafine powder continues to bring out.At present, preparation LaPO
4Method mainly contain high temperature solid-state method, the precipitator method, hydrothermal method etc.The common long-time heating of high temperature solid-state method is ground the powder obtain single phase at last, good crystalline but the powder reuniting phenomenon is serious, and grain diameter is bigger; And ball milling has destroyed surface tissue, and it is big to influence its performance and energy consumption.The precipitator method can add the crystal shape that low quantity of surfactant is improved the sedimentation and filtration performance and changed deposit seeds, have controlled subsidence rate, and sintering temperature decreases, can obtain fine, uniform powder, but the necessary ageing of precipitation and mother liquor, the phase purity that obtains is not high, and degree of crystallinity is bad.Hydrothermal method is carried out under lower temperature, can prepare high purity thing phase, crystallization perfection, dispersed better, the nano particle of even particle size distribution, simple to operate, environmental pollution is little, the product for preparing does not need ball milling, but currently only in the aqueous solution, carry out with the synthetic lanthanum phosphate nano rod of hydrothermal method is general, the big or small heterogeneity of lanthanum phosphate nano rod that obtains, dispersed bad.
Summary of the invention
Main purpose of the present invention is to overcome the shortcoming of existing synthetic technology, the method of the synthetic lanthanum phosphate nano rod of a kind of solvent thermal is provided, the gained lanthanum orthophosphate belongs to oblique system, be the monazite structure nano rod, the diameter of rod is less than 10nm, even thickness, pattern are single, and its size can be controlled by reaction conditions.
The present invention is on the hydrothermal method basis, add organic solvent, n-butanol or n-propyl alcohol, adopt solvent-thermal method to synthesize lanthanum orthophosphate, obtained mutually pure monazite structure nano rod, the diameter of rod is less than 10nm, even thickness, pattern are single, are the thinnest and dispersed best lanthanum phosphate nano rods of present synthetic.Performance based on material generally can be optimized with the minimizing of particle diameter, therefore, the lanthanum phosphate nano rod of our resulting tiny and good dispersity is expected to improve the physico-chemical properties such as stability, optics and catalysis of lanthanum orthophosphate, thereby strengthens it in the engineering Application for Field.
Purpose of the present invention is achieved through the following technical solutions:
The method of the synthetic lanthanum phosphate nano rod of a kind of solvent thermal: with concentration is that 1.0～2.0mol/L lanthanum chloride solution and concentration are that 1.0～2.0mol/L sodium phosphate aqueous solution mixes, wherein mol ratio such as sodium phosphate and Lanthanum trichloride; Add the propyl carbinol solvent, making water and propyl carbinol volume ratio is 0.5～2: 1, and the volumetric molar concentration of Lanthanum trichloride in mixing solutions is 0.2～0.5mol/L, be stirred to mix after, with phosphoric acid regulator solution pH=3～6, in temperature is solvent thermal reaction 6.0～48h under 140～220 ℃ of conditions, gets the lanthanum phosphate nano rod.
For further realizing purpose of the present invention, described solvent thermal reaction is to carry out in having the teflon-lined autoclave.
Preferred 180～220 ℃ of the temperature of described solvent thermal reaction.
The concentration of described Lanthanum trichloride in mixing solutions is 0.3～0.4mol/L.
The pH of described reaction soln is preferably 4～6.
With respect to existing synthetic technology, the present invention has following advantage and beneficial effect:
(1) the present invention adopts solvent-thermal method to synthesize the lanthanum phosphate nano rod, compares with other chemical synthesis process to have environmental friendliness, green economy, low temperature, need not calcine can directly obtain advantages such as product, good reproducibility in solution.
(2) gained lanthanum orthophosphate purity height of the present invention belongs to oblique system, is the monazite structure nano rod, the rod diameter less than 10nm, even thickness, pattern is single, good dispersity.
Description of drawings
Fig. 1 is the XRD figure of the prepared lanthanum phosphate nano rod of experimental example of the present invention 1～6.
Fig. 2 be the prepared lanthanum phosphate nano rod of the embodiment of the invention 2 transmission electron microscope photo (JEOL2010 type high-resolution-ration transmission electric-lens scanner, 100kV).
Embodiment
For better understanding the present invention, below in conjunction with embodiment the present invention is done detailed description further, but the scope of protection of present invention is not limited to the scope that embodiment represents.
With 10ml1.0mol/L lanthanum chloride solution and 10ml1.0mol/L sodium phosphate aqueous solution, join in the 30ml propyl carbinol, the volumetric molar concentration of Lanthanum trichloride in mixing solutions is 0.2mol/L, be stirred to mix after, with phosphoric acid regulator solution pH=4, transfer to and have in the teflon-lined autoclave, solvent thermal reaction 4h under 220 ℃ of conditions makes the lanthanum phosphate nano rod in the thermostat container.Shown in curve among Fig. 11, all diffraction peaks can both be corresponding with the base peak of the oblique system lanthanum orthophosphate of bottom, and hence one can see that, and gained lanthanum phosphate nano rod is the monazite structure of pure phase, belongs to oblique system, the monazite structure.According to Scherrer formula D=κ λ/β cos θ, κ is the Scherrer constant, general value 0.89; λ is the X ray wavelength, value 0.154056nm in the present embodiment; β is the diffraction peak halfwidth, and promptly summit is converted into radian again to the width in the place of the mid-height of peak base after measuring; θ is a diffraction angle.Can estimate that grain-size D is about 8nm.Because the particle diameter of material is more little generally speaking, specific surface area is big more, can make its physical and chemical performance optimization, so institute's synthetic lanthanum phosphate nano rod can be applicable to optics or catalytic performance reinforcement aspect in this patent.
With 1.0mol/L lanthanum chloride solution and 1.0mol/L sodium phosphate aqueous solution, join in the 30ml n-propyl alcohol, other experimental implementation is identical with enforcement 1 with reagent dosage, makes the lanthanum phosphate nano rod.Shown in curve among Fig. 12, all diffraction peaks can both be corresponding with the base peak of the oblique system lanthanum orthophosphate of bottom, hence one can see that, and gained lanthanum phosphate nano rod is the monazite structure of pure phase, by the halfwidth of broadening, can estimate that with the Scherrer formula grain-size is about 7nm.
With 10ml1.5mol/L lanthanum chloride solution and 15ml1.0mol/L sodium phosphate aqueous solution, join in the 25ml propyl carbinol, the volumetric molar concentration of Lanthanum trichloride in mixing solutions is 0.3mol/L, be stirred to mix after, with phosphoric acid regulator solution pH=5, transfer to and have in the teflon-lined autoclave, solvent thermal reaction 24h under 180 ℃ of conditions makes the lanthanum phosphate nano rod in the thermostat container.Shown in curve among Fig. 13, all diffraction peaks can both be corresponding with the base peak of the oblique system lanthanum orthophosphate of bottom, hence one can see that, and gained lanthanum phosphate nano rod is the monazite structure of pure phase, by the halfwidth of broadening, can estimate that with the Scherrer formula grain-size is about 9nm.
With 10ml1.5mol/L lanthanum chloride solution and 15ml1.0mol/L sodium phosphate aqueous solution, join in the 25ml n-propyl alcohol, other experimental implementation is identical with enforcement 1 with reagent dosage, makes the lanthanum phosphate nano rod.Shown in curve among Fig. 14, all diffraction peaks can both be corresponding with the base peak of the oblique system lanthanum orthophosphate of bottom, hence one can see that, and gained lanthanum phosphate nano rod is the monazite structure of pure phase, by the halfwidth of broadening, can estimate that with the Scherrer formula grain-size is about 8nm.Fig. 2 is the transmission electron microscope photo of the lanthanum phosphate nano rod of preparation.As shown in Figure 2, present embodiment gained lanthanum phosphate nano clavate looks are single, even thickness, the diameter of rod substantially all below 10nm, good dispersity.
With 10ml2.0mol/L lanthanum chloride solution and 20ml1.0mol/L sodium phosphate aqueous solution, join in the 20ml propyl carbinol, adding the volumetric molar concentration of Lanthanum trichloride in mixing solutions again is 0.4mol/L, be stirred to mix after, with phosphoric acid regulator solution pH=6, transfer to and have in the teflon-lined autoclave, solvent thermal reaction 48h under 140 ℃ of conditions makes the lanthanum phosphate nano rod in the thermostat container.Shown in curve among Fig. 15, all diffraction peaks can both be corresponding with the base peak of the oblique system lanthanum orthophosphate of bottom, hence one can see that, and gained lanthanum phosphate nano rod is the monazite structure of pure phase, by the halfwidth of broadening, can estimate that with the Scherrer formula grain-size is about 10nm.
With 10ml2.0mol/L lanthanum chloride solution and 20ml1.0mol/L sodium phosphate aqueous solution, join in the 20ml n-propyl alcohol, other experimental implementation is identical with enforcement 5 with reagent dosage, makes the lanthanum phosphate nano rod.Shown in curve among Fig. 16, all diffraction peaks can both be corresponding with the base peak of the oblique system lanthanum orthophosphate of bottom, hence one can see that, and gained lanthanum phosphate nano rod is the monazite structure of pure phase, by the halfwidth of broadening, can estimate that with the Scherrer formula grain-size is about 8nm.
Claims (5)
1, the method for the synthetic lanthanum phosphate nano rod of a kind of solvent thermal is characterized in that: with concentration is that 1.0～2.0mol/L lanthanum chloride solution and concentration are that 1.0～2.0mol/L sodium phosphate aqueous solution mixes, wherein mol ratio such as sodium phosphate and Lanthanum trichloride; Add the propyl carbinol solvent, making water and propyl carbinol volume ratio is 0.5～2: 1, and the volumetric molar concentration of Lanthanum trichloride in mixing solutions is 0.2～0.5mol/L, be stirred to mix after, with phosphoric acid regulator solution pH=3～6, in temperature is solvent thermal reaction 6.0～48h under 140～220 ℃ of conditions, gets the lanthanum phosphate nano rod.
2, the method for the synthetic lanthanum phosphate nano rod of a kind of solvent thermal according to claim 1 is characterized in that described solvent thermal reaction is to carry out in having the teflon-lined autoclave.
3, the method for the synthetic lanthanum phosphate nano rod of a kind of solvent thermal according to claim 1 and 2 is characterized in that the concentration of Lanthanum trichloride in mixing solutions is 0.3～0.4mol/L.
4, the method for the synthetic lanthanum phosphate nano rod of a kind of solvent thermal according to claim 1 and 2 is characterized in that the temperature of described solvent thermal reaction is 180～220 ℃.
5, the method for the synthetic lanthanum phosphate nano rod of a kind of solvent thermal according to claim 1 and 2 is characterized in that the pH=4 of reaction soln～6.
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| CN2008100295021A CN101323442B (en) | 2008-07-16 | 2008-07-16 | Solvent-thermal synthesis of lanthanum phosphate nanorod |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071460A (en) * | 2010-11-19 | 2011-05-25 | 长春理工大学 | Method for preparing europium-doped lanthanum phosphate porous nanorods on basis of herring sperm DNA template |
| CN111747392A (en) * | 2020-07-17 | 2020-10-09 | 南昌航空大学 | Method for preparing semi-hydrated samarium phosphate rodlike nanocrystalline |
| CN115340077A (en) * | 2022-07-22 | 2022-11-15 | 承德莹科精细化工股份有限公司 | Preparation method of high-purity lanthanum phosphate |
-
2008
- 2008-07-16 CN CN2008100295021A patent/CN101323442B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071460A (en) * | 2010-11-19 | 2011-05-25 | 长春理工大学 | Method for preparing europium-doped lanthanum phosphate porous nanorods on basis of herring sperm DNA template |
| CN102071460B (en) * | 2010-11-19 | 2012-10-31 | 长春理工大学 | Method for preparing europium-doped lanthanum phosphate porous nanorods on basis of herring sperm DNA template |
| CN111747392A (en) * | 2020-07-17 | 2020-10-09 | 南昌航空大学 | Method for preparing semi-hydrated samarium phosphate rodlike nanocrystalline |
| CN111747392B (en) * | 2020-07-17 | 2023-03-14 | 南昌航空大学 | Method for preparing semi-hydrated samarium phosphate rod-shaped nanocrystalline |
| CN115340077A (en) * | 2022-07-22 | 2022-11-15 | 承德莹科精细化工股份有限公司 | Preparation method of high-purity lanthanum phosphate |
| CN115340077B (en) * | 2022-07-22 | 2024-05-03 | 承德莹科精细化工股份有限公司 | Preparation method of high-purity lanthanum phosphate |
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