CN102502558A - Synthetic method of CePO4 nano material with hexagonal structures - Google Patents

Synthetic method of CePO4 nano material with hexagonal structures Download PDF

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Publication number
CN102502558A
CN102502558A CN2011103547257A CN201110354725A CN102502558A CN 102502558 A CN102502558 A CN 102502558A CN 2011103547257 A CN2011103547257 A CN 2011103547257A CN 201110354725 A CN201110354725 A CN 201110354725A CN 102502558 A CN102502558 A CN 102502558A
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reaction system
mixed liquor
synthetic method
reaction
temperature
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CN2011103547257A
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Chinese (zh)
Inventor
吴锦绣
李梅
任海仙
柳召刚
胡艳红
王觅堂
张燕云
金佳鹏
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Inner Mongolia University of Science and Technology
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Inner Mongolia University of Science and Technology
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Abstract

The invention relates to a synthetic method of CePO4 nano material with hexagonal structures, and belongs to the nano material field of rare earth phosphate. The synthetic method comprises the steps as follows: CeO2 is taken as Cerium sources and is dissolved in hydrochloric acid; mixed liquor is heated, H2O2 is added in the mixed liquor, the mixed liquor is stirred so as to lead H2O2 to be is dissolved in the mixed liquor completely, and then CeCl3 is obtained; H3PO4 is added in the mixed liquor, and then the pH value of a reaction system is regulated through NaOH so as to range from 1 to 1.5; in addition, the mixed liquor is stirred for 20 to 30 minutes to achieve thorough mixing and then is put in an ultrasonic reactor, the temperature ranges from 20 to 60 DEG C, the ultrasonic reaction time ranges from 0.5 to 3 hours, the ordinary temperature ageing time ranges from 12 to 48 hours, and then products are obtained. The synthetic method has the advantages as follows: the material preparation method is simple, and the synthesis temperature is low; the material of H3PO4 can be utilized repeatedly, the cost of the material is low, and expensive surface-active agents are not needed to be used as templates; the synthetic method is characterized by no utilization of organic solvent, no environment pollution, energy conservation, high conversion rate and the like, and is easy for industrialized production; in addition, synthesis temperature can be reduced effectively, the advantages of good repeatability and the like can be achieved, and the synthetic method is an ideal green technology.

Description

A kind of CePO of hexagonal structure 4The compound method of nano material
Technical field
The present invention relates to a kind of hexagonal structure CePO 4The compound method of nano material belongs to the rare earth phosphate nano field of materials.
Background technology
Because REE has particular configurations of electronic shell, rare earth compound shows light, electricity, the magnetic function of many excellences.RE phosphate is owing to have good chemicalstability and thermostability; So its purposes is very extensive; The electricity, the luminescent material that are mainly used in high performance optical device, stupalith, catalysis, transmitter, hot-pressed material, biological spike mark and cause, for example neutron conductor, photon converting material, laserable material etc. with 4f electronic shell electronics; The CePO of while one dimension Nano structure 4Have high-specific surface area, can greatly widen
CePO 4Application Areas, visible nano level CePO 4Has very big application potential.At present synthetic CePO 4Traditional method mainly contain coprecipitation method, high temperature hydrothermal method, solid phase method, spray heating decomposition, concrete building-up process is seen bibliographical information (Wu Xueyan, Hong Peng etc.; SCI, 2003,1 (24): 1-4; Ruigang W, Pan W, Jian C.et al.; Luminous journal, 2001,22 (4): 412-415; Yang Dingming, Zhu Dachuan, Dai Yatang etc.; Rare Metals Materials and engineering, 2005,34 (3): 436-435; ) Chinese invention patent (publication number: CN 101318640A, application number: 200810106379.9), disclose a kind of CePO of monocline 4The compound method of nano material mainly is synthetic with the high temperature hydrothermal method.And the synthetic CePO of ultrasonic method also of no use up to now 4Bibliographical information.
These traditional methods have that synthesis temperature height or raw material can not reuse, cost of material is high, transformation efficiency is low, percent crystallinity is low, and shortcomings such as the difficult control of pattern are unfavorable for large-scale production and application.Therefore develop low temperature, low cost, the synthetic CePO of simple method with one dimension Nano structure 4Method significant.
Summary of the invention
The object of the present invention is to provide a kind of can be at low temperature, simple and easy process obtains the CePO of appearance homogeneous, handling strong a kind of hexagonal structure cheaply 4The compound method of nano material
Technical solution:
The present invention is with CeO 2Being dissolved in volumetric molar concentration as the cerium source is in 3.0～12.0mol/L hydrochloric acid, under 60～100 ℃ of temperature, adds H 2O 2Stirring is dissolved it fully, and obtaining volumetric molar concentration is 0.05～0.5mol/L CeCl 3Solution A adds H then in solution A 3PO 4Obtain reaction system B, make the PO among the reaction system B 4 3-/ Ce 3+Mol ratio be 2.5～50, using the pH value of NaOH conditioned reaction system B again is 1～1.5, and stirs and made its thorough mixing in 20～30 minutes; Obtain reaction system C, C puts into ultrasonic reactor with reaction system, in 20～60 ℃ TR; Ultrasonic reaction 0.5～3h, normal temperature ageing 12～48h, suction filtration, washing then; Products obtained therefrom is dried 6～10h in 60～80 ℃ TR, obtain the CePO of hexagonal structure 4Powder.
Ce among the said reaction system C 3+Volumetric molar concentration be 0.1～0.005mol/L, H 3PO 4Volumetric molar concentration be 0.0125～5.0mol/L, PO 4 3-/ Ce 3+Mol ratio be 2.5～50, temperature of reaction is 20～60 ℃, reaction times 0.5～3h, normal temperature ageing 12～48h.
Saidly in reaction system B, regulate the pH value with aqueous ammonia to replace NaOH.
Beneficial effect of the present invention is:
Material preparation method of the present invention is simple and easy, and synthesis temperature is low; Raw material H 3PO 4Can reuse, cost of material is cheap, need not expensive tensio-active agent and makes masterplate; Have not with an organic solvent, free from environmental pollution, save energy, transformation efficiency are high, be easy to characteristics such as suitability for industrialized production; Can reduce advantages such as synthesis temperature, good reproducibility effectively, be a kind of ideal green technology.
Description of drawings:
Fig. 1 is hexagonal structure CePO of the present invention 4XRD figure;
Wherein: a is PO among the reaction system C 4 3-/ Ce 3+Mol ratio be 5, temperature of reaction is 60 ℃, the XRD of ultrasonic reaction 1h detects figure;
B. be PO among the reaction system C 4 3-/ Ce 3+Mol ratio be 5, temperature of reaction is 20 ℃, the XRD of ultrasonic reaction 1h detects figure;
C. be PO among the reaction system C 4 3-/ Ce 3+Mol ratio be 2.5, temperature of reaction is 40 ℃, the XRD of ultrasonic reaction 1.5h detects figure;
D. be PO among the reaction system C 4 3-/ Ce 3+Mol ratio be 10, temperature of reaction is 40 ℃, the XRD of ultrasonic reaction 1.5h detects figure;
E. be PO among the reaction system C 4 3-/ Ce 3+Mol ratio be 50, temperature of reaction is 20 ℃, the XRD of ultrasonic reaction 3h detects figure.
Fig. 2 is PO among the reaction system C of the present invention 4 3-/ Ce 3+Mol ratio be 5, temperature of reaction is 60 ℃, the TEM Electronic Speculum of ultrasonic reaction 1h detects figure.
Fig. 3 is PO among the reaction system C of the present invention 4 3-/ Ce 3+Mol ratio be 10, temperature of reaction is 40 ℃, the TEM Electronic Speculum of ultrasonic reaction 1.5h detects figure.
Fig. 4 is PO among the reaction system C of the present invention 4 3-/ Ce 3+Mol ratio be 10, temperature of reaction is 40 ℃, the diffraction spot of ultrasonic reaction 1.5h detects figure; Synthetic CePO is described 4Powder is a polycrystalline state.
Fig. 5 is PO among the reaction system C of the present invention 4 3-/ Ce 3+Mol ratio be 50, temperature of reaction is 20 ℃, the TEM Electronic Speculum of ultrasonic reaction 3h detects figure.
Embodiment
Precursor CeCl 3The preparation method of solution: take by weighing 8.606gCeO 2, add zero(ppm) water then, ydrogen peroxide 50 and 6mol/L hydrochloric acid, heated and stirred is dissolved it fully under 80 ℃ of temperature, is settled in the 500mL volumetric flask with zero(ppm) water, gets 0.1mol/LCeCl 3Solution A.
Embodiment 1:
Take by weighing the 40mL solution A and put into beaker, add the 1.4mL SPA, obtain reaction system B, make H among the reaction system B 3PO 4Concentration be 0.25mol/L, using the NaOH adjust pH is 1, uses the zero(ppm) water constant volume at last, making reaction system B is 80mL; And after magnetic agitation made its thorough mixing in 30 minutes, obtain reaction system C, will obtain reaction system C and put into ultrasonic reactor; Under 60 ℃ temperature, ultrasonic reaction 1h, normal temperature ageing 24h; Suction filtration, respectively wash three times, product is put into 60 ℃ the dry 6h of vacuum drying oven, obtain white CePO with zero(ppm) water and absolute ethyl alcohol 4Powder.
Embodiment 2:
Take by weighing the 40mL solution A and put into beaker, add the 0.7mL SPA, obtain reaction system B, make H among the reaction system B 3PO 4Concentration be 0.125mol/L, using the NaOH adjust pH is 1.5, uses the zero(ppm) water constant volume at last, making reaction system B is 80mL; And magnetic agitation made its thorough mixing in 30 minutes, obtained reaction system C, and C puts into ultrasonic reactor with reaction system; Under 40 ℃ temperature, ultrasonic reaction 1.5h, normal temperature ageing 24h; Suction filtration, respectively wash three times, product is put into 60 ℃ the dry 6h of vacuum drying oven, obtain white CePO with zero(ppm) water and absolute ethyl alcohol 4Powder.
Embodiment 3:
Take by weighing the 20mL solution A and put into beaker, add the 14mL SPA, obtain reaction system B, make H among the reaction system B 3PO 4Concentration be 2.5mol/L, using the NaOH adjust pH is 1, uses the zero(ppm) water constant volume at last, making reaction system B is 80mL; And magnetic agitation made its thorough mixing in 30 minutes, obtained reaction system C, and C puts into ultrasonic reactor with reaction system; Under 20 ℃ temperature, ultrasonic reaction 3h, normal temperature ageing 24h; Suction filtration, respectively wash three times, product is put into 80 ℃ the dry 8h of vacuum drying oven, obtain white CePO with zero(ppm) water and absolute ethyl alcohol 4Powder.
Embodiment 4:
Take by weighing the 20mL solution A and put into beaker, add the 1.4mL SPA, obtain reaction system B, make H among the reaction system B 3PO 4Concentration be 0.25mol/L, using the ammoniacal liquor adjust pH is 1, uses the zero(ppm) water constant volume at last, making reaction system B is 80mL; And magnetic agitation made its thorough mixing in 30 minutes, obtained reaction system C, and C puts into ultrasonic reactor with reaction system; Under 60 ℃ temperature, ultrasonic reaction 0.5h, normal temperature ageing 24h; Suction filtration, respectively wash three times, product is put into 80 ℃ the dry 6h of vacuum drying oven, obtain white CePO with zero(ppm) water and absolute ethyl alcohol 4Powder.
Embodiment 5:
Take by weighing the 10mL solution A and put into beaker, add the 1.4mL SPA, obtain reaction system B, make H among the reaction system B 3PO 4Concentration be 0.25mol/L, using the ammoniacal liquor adjust pH is 1.5, uses the zero(ppm) water constant volume at last, making reaction system B is 80mL; And magnetic agitation made its thorough mixing in 30 minutes, obtained reaction system C, and C puts into ultrasonic reactor with reaction system; Under 40 ℃ temperature, ultrasonic reaction 0.5h, normal temperature ageing 24h; Suction filtration, respectively wash three times, product is put into 80 ℃ the dry 10h of vacuum drying oven, obtain white CePO with zero(ppm) water and absolute ethyl alcohol 4Powder.

Claims (3)

1. the CePO of a hexagonal structure 4The compound method of nano material is characterized in that, with CeO 2Being dissolved in volumetric molar concentration as the cerium source is in 3.0～12.0mol/L hydrochloric acid, under 60～100 ℃ of temperature, adds H 2O 2Stirring is dissolved it fully, and obtaining volumetric molar concentration is 0.05～0.5mol/L CeCl 3Solution A adds H then in solution A 3PO 4Obtain reaction system B, make the PO among the reaction system B 4 3-/ Ce 3+Mol ratio be 2.5～50, using the pH value of NaOH conditioned reaction system B again is 1～1.5, and stirs and made its thorough mixing in 20～30 minutes; Obtain reaction system C, C puts into ultrasonic reactor with reaction system, in 20～60 ℃ TR; Ultrasonic reaction 0.5～3h, normal temperature ageing 12～48h, suction filtration, washing then; Products obtained therefrom is dried 6～10h in 60～80 ℃ TR, obtain the CePO of hexagonal structure 4Powder.
2. the CePO of a kind of hexagonal structure according to claim 1 4The compound method of nano material is characterized in that, Ce among the reaction system C 3+Volumetric molar concentration be 0.1～0.005mol/L, H 3PO 4Volumetric molar concentration be 0.0125～5.0mol/L, PO 4 3-/ Ce 3+Mol ratio be 2.5～50, temperature of reaction is 20～60 ℃, reaction times 0.5～3h, normal temperature ageing 12～48h.
3. the CePO of a kind of hexagonal structure according to claim 1 4The compound method of nano material, compound method, it is characterized in that, in reaction system B, regulate the pH value with aqueous ammonia to replace NaOH.
CN2011103547257A 2011-10-25 2011-10-25 Synthetic method of CePO4 nano material with hexagonal structures Pending CN102502558A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112551499A (en) * 2020-12-24 2021-03-26 益阳鸿源稀土有限责任公司 Preparation method of high-purity nano cerium phosphate powder

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101318640A (en) * 2008-05-13 2008-12-10 北京科技大学 Process for synthesizing CePO4 nano-material with monocline structure
CN101704543A (en) * 2009-11-25 2010-05-12 深圳大学 Method for preparing cerous phosphate nano wire

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101318640A (en) * 2008-05-13 2008-12-10 北京科技大学 Process for synthesizing CePO4 nano-material with monocline structure
CN101704543A (en) * 2009-11-25 2010-05-12 深圳大学 Method for preparing cerous phosphate nano wire

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
CUICUI YU ETAL: "Facile sonochemical synthesis and photoluminescent properties of lanthanide orthophosphate nanoparticles", 《JOURNAL OF SOLID STATE CHEMISTRY》, 5 November 2008 (2008-11-05), pages 339 - 347 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112551499A (en) * 2020-12-24 2021-03-26 益阳鸿源稀土有限责任公司 Preparation method of high-purity nano cerium phosphate powder
CN112551499B (en) * 2020-12-24 2023-05-26 益阳鸿源稀土有限责任公司 Preparation method of high-purity nano cerium phosphate powder

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Application publication date: 20120620