CN102557140B - Preparation method of porous fusiform barium tungstate - Google Patents

Abstract

The invention provides a preparation method of porous fusiform barium tungstate. Sodium tungstate and barium nitrate are adopted as starting reactants, citric acid is adopted as metal ion complexing agent and material growth directing agent, distilled water is adopted as solvent, and the microwave radiation technology is adopted. The obtained barium tungstate material is of a nano-sheet-assembledporous fusiform structure, and has the characteristics of uniform size, regular morphology, porous structure, good symmetry and the like, and a single porous fusiform barium tungstate material is 4.5to 6.0 micrometers in size, 1.1 to 2.3 micrometers in thickness and 2.2 to 2.9 micrometers in side length. The citric acid-assisted microwave radiation method has the technical advantages of mild reaction, easy-to-control process, simplicity, high efficiency, good selectivity, high product purity, safety, environment-friendliness and the like, and accords with the new concept of green and friendly chemistry, and the technique provides necessary technical support and practical support for broadening the high-efficiency, controllable and low-cost synthesis of barium tungstate materials.

Description

A kind of preparation of porous fusiformis barium wolframate

[technical field]: the invention belongs to inorganic micro Nano material preparation field, particularly relate to a kind of preparation of porous fusiformis barium wolframate.

[background technology]: in recent years, thereby the synthetic micro Nano material with novel pattern of the efficient control of material introducing material preparation process that will have special construction and function becomes one of research focus of micro-nano technical field gradually.Especially, citric acid is as the surfactant of a quasi-representative, can water-soluble and multiple organic solvent, and because its structural performance can significantly be regulated and control crystal nucleation and growth velocity in liquid phase environment, and induce crystal to realize the directional preponderance growth, opened up brand-new route (K.Zhang, J.Liang for realizing micro-nano the melting of scantling, S.Wang, J.Liu, K.X.Ren, X Zheng, H.Luo, Y.J.Peng, X.Zou, X.Bo, J.H.Li, X.B.Yu, Cryst.Growth Des., 2012,12,793-803.).

The crystalline structure of barium wolframate self uniqueness gives material superior luminous and stimulated Raman scattering characteristic, therefore can be used as good optical material or laser donor material, have important use in fields such as photoelectronics, medicine and pharmacology, laser sensings and be worth and DEVELOPMENT PROSPECT.At present, the main method of preparation barium tungstate nanometer material has solid reaction process, hydrothermal method, microemulsion method, microwave method and the precipitator method etc., mostly be pattern (Y.H.Shen such as nano particle, nano wire, nanometer rod, micron ball and micron block and make product, W.Li, T.H.Li, Mater.Lett., 2011,65,2956-2958; S.Y.Hou, Y.Xing, H.Ding, X.C.Liu, B.Liu, X.J.Sun, Mater.Lett., 2011,29,623-627; CN 101805022A).Chinese invention patent CN 1923706A discloses a kind of method that adopts microemulsion method to prepare dendroid barium tungstate nano crystal, form microemulsion system by adding a certain proportion of octane, propyl carbinol and cetyl trimethylammonium bromide and water in this technology, stirring under temperature range is 20～35 ℃ and made dendroid barium tungstate nanometer material in 1 minute, be the shortcoming of emulsifying agent but this method existence needs the multiple organic solvent of interpolation.A.Phuruangrat seminar is raw material with nitrate of baryta and sodium wolframate, has successfully prepared barium tungstate nanometer particle (A.Phuruangrat, the T.Thongtem of pattern homogeneous by microwave irradiation, S.Thongtem, J.Phys.Chem.Solids, 2009,70,955-959.).But still there is certain technical deficiency in other barium wolframate micro Nano materials with special appearance to existing preparation method to efficient controlledly synthesis, and are reducing reaction cost, improve product purity and efficiently regulating and control the necessity that aspect such as product pattern still has further investigation research.Particularly less bibliographical information adopts the auxiliary microwave irradiation of citric acid to prepare the barium wolframate micro Nano material of pattern homogeneous.Therefore, at above-mentioned key issue, patent of the present invention provides a kind of preparation method of porous barium wolframate, be complexing of metal ion agent and material structure directed agents with the citric acid in the building-up process, the applied microwave radiation method is prepared the porous shuttle type barium wolframate material of the regular nanometer sheet assembling of pattern, and the efficient controlled low cost of barium wolframate material is synthetic to provide necessary technology guarantee and practice to support to this technology in order to widen.

[summary of the invention]: the summary of the invention of this patent is to provide a kind of preparation of porous fusiformis barium wolframate, its characteristics are that it is complexing of metal ion agent and material growth directed agents that initial reaction stage is introduced citric acid, it is controlled material nucleation and growth velocity significantly, and induces the crystal orientation dominant growth to become the three-dimensional shuttle type barium wolframate material of the regular nanometer sheet assembling of pattern; This synthetic method have reaction temperature and, easily control of process, simple and effective, selectivity is good, product purity is high and technical superiority such as safety and environmental protection, meets green friendly chemical new concept.

[technical scheme of the present invention]: patent of the present invention provides a kind of preparation of porous fusiformis barium wolframate, be initial reactant with sodium wolframate and nitrate of baryta, citric acid is complexing of metal ion agent and directed agents, and distilled water is solvent, adopt the microwave radiation Technology, the concrete operations scheme is as follows:

The first, at room temperature, accurately weighing 0.1649 restrains sodium wolframate (NaWO ₄2H ₂O) solid adds 10 ml distilled waters, thus the sodium tungstate solution of preparation certain concentration;

The second, weighing 0.1307 gram nitrate of baryta (Ba (NO ₃) ₂) and 0.0105 gram citric acid, add 10 ml waters, high-speed stirring 5 minutes, preparation mixing solutions;

Three, the described solution of step 1 is transferred in the step 2 solution, continues to stir 10 minutes;

Four, this mixing solutions is placed the microwave reactor sustained reaction stopped in 30 minutes;

Five, wash respectively 3～5 times with distilled water and dehydrated alcohol behind the products therefrom naturally cooling, 60 ℃ of vacuum-drying 48 hours can obtain porous shuttle type barium wolframate material.

Described barium wolframate material shows that through X-ray diffraction analysis the thing of products therefrom is BaWO mutually ₄It is the porous shuttle type structured material by nanometer sheet assembling, feature such as have that size is even, pattern is regular, structure porous and symmetry are good, and single barium wolframate porous shuttle section bar material is of a size of 4.5～6.0 microns, thickness is 1.1～2.3 microns, and the length of side is 2.2～2.9 microns.

[advantage of the present invention and effect]: patent of the present invention relates to a kind of preparation of porous fusiformis barium wolframate, and have the following advantages and beneficial effect: 1, raw material is cheap and easy to get; 2, citric acid is the agent of system complexing of metal ion and structure directing agent, and it can significantly control material nucleation and growth velocity in liquid phase environment, and the guiding crystal is grown along particular crystal orientation; 3, the microwave building-up process have reaction temperature and, easily control of process, simple and effective, selectivity is good, product purity is high and technical superiority such as safety and environmental protection, meets green friendly chemical new concept; 4, the efficient controlled low cost of barium wolframate material is synthetic to provide necessary technology guarantee and practice to support to this technology in order to widen.

[description of drawings]:

Fig. 1 is the X-ray diffraction analysis figure of synthetic sample

Fig. 2 is low power scanning electronic microscope (SEM) figure of porous fusiformis barium wolframate

Fig. 3 is the high power SEM figure of porous fusiformis barium wolframate

Fig. 4 is the SEM figure that porous fusiformis barium wolframate further amplifies

[embodiment]:

Embodiment: preparation method and the structural characterization of porous fusiformis barium wolframate

At room temperature, accurately weighing 0.1649 restrains sodium wolframate (NaWO ₄2H ₂O) solid adds 10 ml distilled waters, the sodium tungstate solution of preparation certain concentration; Secondly, weighing 0.1307 gram nitrate of baryta (Ba (NO ₃) ₂) and 0.0105 gram citric acid, adding 10 ml waters, high-speed stirring 5 minutes is prepared the two mixing solutions; Then, sodium tungstate solution is transferred in the solution that contains nitrate of baryta and citric acid, continues to stir 10 minutes; This mixing solutions was placed the microwave reactor sustained reaction 30 minutes; After question response stopped, products therefrom was through naturally cooling, and washed respectively 4 times with distilled water and dehydrated alcohol, and 60 ℃ of vacuum-drying 48 hours can obtain porous shuttle type barium wolframate material.The thing that shows products therefrom through X-ray diffraction analysis is BaWO mutually ₄, corresponding standard card number: 8-457, spacer: I41/a (no.88),

(Fig. 1).Product low power SEM test (as Fig. 2) shows that product main body pattern is porous shuttle type structure, characteristics such as have that size is even, pattern is regular, structure porous and symmetry are good; High power SEM test (as Fig. 3) shows that single porous shuttle type barium wolframate scantling is 4.5～6.0 microns, and thickness is 1.1～2.3 microns, and the length of side is 2.2～2.9 microns; The SEM test (Fig. 4) of further amplifying shows that these porous barium tungstate micron shuttle type structures are assembled by a large amount of ultrathin nanometer sheets.

Claims (1)

1. the preparation of a porous fusiformis barium wolframate is initial reactant with sodium wolframate and nitrate of baryta, and citric acid is complexing of metal ion agent and directed agents, and distilled water is solvent, adopts the microwave radiation Technology, and the concrete operations scheme is as follows:

The first, at room temperature, accurately weighing 0.1649 restrains sodium wolframate Na ₂WO ₄2H ₂The O solid adds 10 ml distilled waters, thus the sodium tungstate solution of preparation certain concentration;

The second, weighing 0.1307 gram nitrate of baryta Ba (NO ₃) ₂With 0.0105 gram citric acid, add 10 ml waters, high-speed stirring 5 minutes, preparation mixing solutions;

Three, the described solution of step 1 is transferred in the step 2 solution, continues to stir 10 minutes;

Four, this mixing solutions is placed the microwave reactor sustained reaction stopped in 30 minutes;

Five, wash respectively 3～5 times with distilled water and dehydrated alcohol behind the products therefrom naturally cooling, 60 ℃ of vacuum-drying 48 hours can obtain porous shuttle type barium wolframate material.

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