CN103922409A - Preparation method of ellipsoidal SmW2O6(OH)3 microcrystal - Google Patents

Preparation method of ellipsoidal SmW2O6(OH)3 microcrystal Download PDF

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CN103922409A
CN103922409A CN201410155072.3A CN201410155072A CN103922409A CN 103922409 A CN103922409 A CN 103922409A CN 201410155072 A CN201410155072 A CN 201410155072A CN 103922409 A CN103922409 A CN 103922409A
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smw
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crystallite
smw2o6
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CN103922409B (en
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黄剑锋
李颖慧
李嘉胤
卢靖
曹丽云
欧阳海波
吴建鹏
孔新刚
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Yancheng julonghu Business Cluster Development Co.,Ltd.
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Shaanxi University of Science and Technology
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Abstract

The invention provides a preparation method of ellipsoidal SmW2O6(OH)3 microcrystal. The preparation method comprises the following steps: dropwise adding Na2WO4 liquor into Sm(NO3)3 liquor, then continuously stirring to obtain white turbid liquid, regulating pH to 2-5 to obtain hydrothermal precursor liquor, reacting at 100 DEG C-160 DEG C in a homogeneous-phase reaction instrument for 18-48 hours, separating products in a centrifugal manner, washing and drying to obtain the ellipsoidal SmW2O6(OH)3 microcrystal. The preparation method disclosed by the invention adopts a wet chemical method to prepare the ellipsoidal SmW2O6(OH)3; the hydrothermal technique is simple in process, lower in reaction temperature, short in time, easy in controlling process parameters, does not need high temperature reaction or atmosphere protection, does not need subsequent processing, and can be used for quickly preparing high-purity ellipsoidal SmW2O6(OH)3.

Description

A kind of ellipsoid shape SmW 2o 6(OH) 3the preparation method of crystallite
Technical field
The present invention relates to a kind of SmW 2o 6(OH) 3preparation method, particularly a kind of employing hydrothermal method is prepared ellipsoid shape SmW 2o 6(OH) 3the method of crystallite.
Background technology
Wolframic acid samarium is a kind of water-fast typical rare earth metal tungstate material, may there is the properties such as paramagnetism, ferroelectric, piezoelectricity, pyroelectricity, non-linear electric susceptibility, negative expansion, can be used as photocatalyst material, permanent magnet material, Solid Oxide Fuel Cells, ceramic capacitor material etc., be with a wide range of applications.
The preparation method of rare earth metal tungstate is mainly solid reaction process at present.E.Tomaszewicz is by solid reaction process, with Sm 2o 3and WO 3for raw material has been prepared Sm 2wO 6crystal [E.Tomaszewicz.Reactivity in the solid state between CoWO 4and RE 2wO 6where RE=Sm, Eu, Gd.Thermochimica Acta, 447 (2006) 69-74].The people such as Qin Li have also synthesized Sm with solid reaction process 2wO 6crystal [Qin Li, Venkataraman Thangadurai.Novel Nd 2wo 6-type Sm 2-xa xm 1-yb yo 6-δ(A=Ca, Sr; M=Mo, W; B=Ce, Ni) mixed conductors.Journal of Power Sources, 196 (2011) 169-178].Solid reaction process is prepared wolframic acid samarium, need to be by raw material Sm 2o 3and WO 3evenly mix in proportion, be then heated to comparatively high temps (800 ℃～1200 ℃), the insulation long period (12～24h), obtain product.This method has the advantages such as high yield, technique are simple, however reaction need at high temperature be carried out, preparation cycle compared with long, energy consumption is large, does not meet current pursuit green, environmental protection, energy-conservation, efficient trend.
About in the having been reported of tungstate, wet chemistry method becomes main flow preparation method, and as liquid phase reaction method, microemulsion method, solvent-thermal method, hydrothermal method etc., wherein solvent-thermal method and hydrothermal method are the methods that report is maximum.Chen Lei etc. are by Bi (NO 3) 3, Na 2wO 4in alcohol water mixed solvent, make suspension respectively, after mixing, under solvent thermal condition, surface reaction occurs and formed Bi 2wO 6hollow nano-sphere [Chen Lei, Wu great Xiong etc. in alcohol water mixed solvent, prepare bismuth tungstate hollow nanostructures [J]. Qingdao University of Science and Technology's journal, 2012,33 (1): 9-12]; Xu Chun Song etc. have prepared molybdenum doping Bi by hydrothermal method 2wO 6three-dimensional layering microballoon [Song C X, Zheng Y F.Photocatalytic activities of Mo-doped Bi 2wO 6three-dimensional hierarchical microspheres[J] .J ournal of Hazardous Materials, 2011,192:186-191].That hydrothermal method has is with short production cycle, technique is simple, parameter is easy to control, be convenient to the advantages such as doping vario-property.
Summary of the invention
The object of the present invention is to provide a kind of ellipsoid shape SmW 2o 6(OH) 3the preparation method of crystallite, the method technological process is simple, and parameter is easy to control, and temperature is low, and the production time is short, can prepare highly purified ellipsoid shape SmW 2o 6(OH) 3.
For achieving the above object, the present invention has adopted following technical scheme:
Step 1: by Sm (NO 3) 36H 2o and Na 2wO 42H 2o adds respectively in deionized water, then stirs 5～15min and obtains Sm (NO 3) 3solution and Na 2wO 4solution;
Step 2: by Na 2wO 4solution drops to Sm (NO 3) 3in solution, then constantly stir (5～10 minutes) and obtain white suspension liquid, control mol ratio=0.5～2:1 of Sm:W, and W 6+concentration be 0.02～0.1mol/L;
Step 3: regulate pH to 2～5 of white suspension liquid with the HCl aqueous solution, and continue to stir 30～60min, obtain hydro-thermal precursor liquid;
Step 4: hydro-thermal precursor liquid is packed in hydrothermal reaction kettle, then will put into homogeneous reaction instrument after hydrothermal reaction kettle sealing, and react 18～48h at 100～160 ℃, naturally cool to room temperature after reaction finishes;
Step 5: after step 4, open hydrothermal reaction kettle, the product centrifugation that reaction is obtained is precipitated, successively with putting into vacuum drying oven after deionized water and absolute ethanol washing and drying at 40～60 ℃, can obtain ellipsoid shape SmW by precipitation 2o 6(OH) 3crystallite.
The packing ratio of described hydro-thermal precursor liquid in hydrothermal reaction kettle is 30～60%.
The concentration of the described HCl aqueous solution is 0.5～1.5mol/L.
Beneficial effect of the present invention:
The present invention adopts wet chemistry method to prepare ellipsoid shape SmW 2o 6(OH) 3, hydrothermal method technological process is simple, and temperature of reaction is lower, and the time is short, and processing parameter is easy to control, without pyroreaction or atmosphere protection, without subsequent disposal, can prepare fast highly purified ellipsoid shape SmW 2o 6(OH) 3.The ellipsoid shape SmW that the inventive method makes 2o 6(OH) 3crystallite has larger specific surface area, in fields such as photochemical catalysis and photolysis water hydrogens, has wide research and using value.
Accompanying drawing explanation
Fig. 1 is the SmW of the embodiment of the present invention 1 preparation 2o 6(OH) 3the X-ray diffraction of crystallite (XRD) collection of illustrative plates.
Fig. 2 is the SmW of the embodiment of the present invention 1 preparation 2o 6(OH) 3the scanning electron microscope of crystallite (SEM) photo.
Fig. 3 is degradation rate-time diagram of photocatalytic degradation Rh-B.
Embodiment
Below in conjunction with drawings and Examples, the present invention is elaborated.
Embodiment 1:
Step 1: by analytical pure Sm (NO 3) 36H 2o and Na 2wO 42H 2o adds respectively in a certain amount of deionized water, stirs 15min and obtain clear solution A(Sm (NO on magnetic stirring apparatus 3) 3solution) and clear solution B(Na 2wO 4solution);
Step 2: clear solution B is slowly dropped in clear solution A, constantly stir and obtain white suspension liquid, control Sm:W=2:1(mol ratio), W 6+concentration be 0.05mol/L;
Step 3: the HCl aqueous solution that is 1.0mol/L by concentration regulates the pH=3 of white suspension liquid, and continue to stir 30min, hydro-thermal precursor liquid obtained;
Step 4: hydro-thermal precursor liquid is packed in hydrothermal reaction kettle, and packing ratio is 40%, sealing hydrothermal reaction kettle, puts into homogeneous reaction instrument, at 160 ℃, reacts 24h, after reaction finishes, naturally cools to room temperature;
Step 5: open hydrothermal reaction kettle, the product centrifugation that reaction is obtained is precipitated, by deionized water and absolute ethanol washing precipitation, puts into vacuum drying oven by the precipitation after washing and dries at 60 ℃ successively, can obtain ellipsoid shape SmW 2o 6(OH) 3crystallite.
Referring to Fig. 1, the X-ray diffraction of the present embodiment products therefrom (XRD) collection of illustrative plates shows that product is pure phase monocline SmW 2o 6(OH) 3, and crystallinity is good.Referring to Fig. 2, scanning electron microscope (SEM) photo shows that product has the ellipsoid shape pattern being assembled by nanoplatelet.
Embodiment 2:
Step 1: by analytical pure Sm (NO 3) 36H 2o and Na 2wO 42H 2o adds respectively in a certain amount of deionized water, stirs 10min and obtain clear solution A(Sm (NO on magnetic stirring apparatus 3) 3solution) and clear solution B(Na 2wO 4solution);
Step 2: clear solution B is slowly dropped in clear solution A, constantly stir and obtain white suspension liquid, control Sm:W=1.5:1(mol ratio), W 6+concentration be 0.1mol/L;
Step 3: the HCl aqueous solution that is 1.5mol/L by concentration regulates the pH=4 of white suspension liquid, and continue to stir 60min, hydro-thermal precursor liquid obtained;
Step 4: hydro-thermal precursor liquid is packed in hydrothermal reaction kettle, and packing ratio is 50%, sealing hydrothermal reaction kettle, puts into homogeneous reaction instrument, at 160 ℃, reacts 18h, after reaction finishes, naturally cools to room temperature;
Step 5: open hydrothermal reaction kettle, the product centrifugation that reaction is obtained is precipitated, by deionized water and absolute ethanol washing precipitation, puts into vacuum drying oven by the precipitation after washing and dries at 40 ℃ successively, can obtain ellipsoid shape SmW 2o 6(OH) 3crystallite.
Embodiment 3:
Step 1: by analytical pure Sm (NO 3) 36H 2o and Na 2wO 42H 2o adds respectively in a certain amount of deionized water, stirs 5min and obtain clear solution A(Sm (NO on magnetic stirring apparatus 3) 3solution) and clear solution B(Na 2wO 4solution);
Step 2: clear solution B is slowly dropped in clear solution A, constantly stir and obtain white suspension liquid, control Sm:W=0.5:1(mol ratio), W 6+concentration is 0.0625mol/L;
Step 3: the HCl aqueous solution that is 0.5mol/L by concentration regulates the pH=5 of white suspension liquid, and continue to stir 30min, hydro-thermal precursor liquid obtained;
Step 4: hydro-thermal precursor liquid is packed in hydrothermal reaction kettle, and packing ratio is 60%, sealing hydrothermal reaction kettle, puts into homogeneous reaction instrument, at 140 ℃, reacts 30h, after reaction finishes, naturally cools to room temperature;
Step 5: open hydrothermal reaction kettle, the product centrifugation that reaction is obtained is precipitated, by deionized water and absolute ethanol washing precipitation, puts into vacuum drying oven by the precipitation after washing and dries at 50 ℃ successively, can obtain ellipsoid shape SmW 2o 6(OH) 3crystallite.
Embodiment 4:
Step 1: by analytical pure Sm (NO 3) 36H 2o and Na 2wO 42H 2o adds respectively in a certain amount of deionized water, stirs 10min and obtain clear solution A(Sm (NO on magnetic stirring apparatus 3) 3solution) and clear solution B(Na 2wO 4solution);
Step 2: clear solution B is slowly dropped in clear solution A, constantly stir and obtain white suspension liquid, control Sm:W=1:1(mol ratio), W 6+concentration is 0.021mol/L;
Step 3: the HCl aqueous solution that is 1.5mol/L by concentration regulates the pH=2 of white suspension liquid, and continue to stir 40min, hydro-thermal precursor liquid obtained;
Step 4: hydro-thermal precursor liquid is packed in hydrothermal reaction kettle, and packing ratio is 30%, sealing hydrothermal reaction kettle, puts into homogeneous reaction instrument, at 100 ℃, reacts 48h, after reaction finishes, naturally cools to room temperature;
Step 5: open hydrothermal reaction kettle, the product centrifugation that reaction is obtained is precipitated, by deionized water and absolute ethanol washing precipitation, puts into vacuum drying oven by the precipitation after washing and dries at 60 ℃ successively, can obtain ellipsoid shape SmW 2o 6(OH) 3crystallite.
The present invention adopts hydrothermal method to prepare ellipsoid shape SmW innovatively 2o 6(OH) 3, equipment is simple, easily controls, and temperature is low, and the cycle is short, can prepare easily pure phase ellipsoid shape SmW 2o 6(OH) 3.The prepared ellipsoid shape SmW of embodiment 1-embodiment 4 after testing 2o 6(OH) 3there is obvious photocatalytic activity.Fig. 3 is degradation rate-time diagram of photocatalytic degradation Rh-B, and S1-S4 represents respectively the ellipsoid shape SmW that embodiment 1-embodiment 4 is prepared 2o 6(OH) 3.Visible under UV-irradiation, detect and compare with blank, the prepared ellipsoid shape SmW of embodiment 1-embodiment 4 2o 6(OH) 3rh-B is had to obvious Photocatalytic activity.

Claims (3)

1. an ellipsoid shape SmW 2o 6(OH) 3the preparation method of crystallite, is characterized in that: comprise the following steps:
Step 1: by Sm (NO 3) 36H 2o and Na 2wO 42H 2o adds respectively and in deionized water, obtains Sm (NO 3) 3solution and Na 2wO 4solution;
Step 2: by Na 2wO 4solution drops to Sm (NO 3) 3in solution, then constantly stir and obtain white suspension liquid, control mol ratio=0.5～2:1 of Sm:W, and W 6+concentration be 0.02～0.1mol/L;
Step 3: regulate pH to 2～5 of white suspension liquid with the HCl aqueous solution, and continue to stir 30～60min, obtain hydro-thermal precursor liquid;
Step 4: hydro-thermal precursor liquid is packed in hydrothermal reaction kettle, then will put into homogeneous reaction instrument after hydrothermal reaction kettle sealing, and react 18～48h at 100～160 ℃, naturally cool to room temperature after reaction finishes;
Step 5: after step 4, open hydrothermal reaction kettle, the product centrifugation that reaction is obtained is precipitated, successively with putting into vacuum drying oven after deionized water and absolute ethanol washing and drying at 40～60 ℃, can obtain ellipsoid shape SmW by precipitation 2o 6(OH) 3crystallite.
2. a kind of ellipsoid shape SmW according to claim 1 2o 6(OH) 3the preparation method of crystallite, is characterized in that: the packing ratio of described hydro-thermal precursor liquid in hydrothermal reaction kettle is 30～60%.
3. a kind of ellipsoid shape SmW according to claim 1 2o 6(OH) 3the preparation method of crystallite, is characterized in that: the concentration of the described HCl aqueous solution is 0.5～1.5mol/L.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106587152A (en) * 2016-12-12 2017-04-26 南京工业大学 Rare-earth two-dimensional material EuMoO4(OH) nanosheet as well as preparation method and application thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
JIAO WANG等: ""Luminescent metastable Y2WO6: Ln3+ (Ln = Eu, Er, Sm, andDy)microspheres with controllable morphology via self-assembly"", 《JOURNAL OF MATERIALS CHEMISTRY》, vol. 20, 18 October 2010 (2010-10-18), pages 10894 - 10900 *
曹丽云等: ""NdWO4(OH)粉体的微波水热合成及其光催化性能"", 《陕西科技大学学报》, vol. 31, no. 6, 31 December 2013 (2013-12-31), pages 54 - 57 *
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106587152A (en) * 2016-12-12 2017-04-26 南京工业大学 Rare-earth two-dimensional material EuMoO4(OH) nanosheet as well as preparation method and application thereof

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