CN101445274A - Method for preparing octahedral barium molybdate - Google Patents
Method for preparing octahedral barium molybdate Download PDFInfo
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- CN101445274A CN101445274A CNA200810107412XA CN200810107412A CN101445274A CN 101445274 A CN101445274 A CN 101445274A CN A200810107412X A CNA200810107412X A CN A200810107412XA CN 200810107412 A CN200810107412 A CN 200810107412A CN 101445274 A CN101445274 A CN 101445274A
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Abstract
The invention provides a method for preparing a barium molybdate octahedron. In the method, quaternionic micro-emulsion which comprises nonionic surfactants of alkyl polyoxyethylene (10), ether (OP-10), cyclohexane, n-octanol and water phase is selected to be used and sodium molybdate and barium chloride are used as reactants. After being mixed, components for composing reverse micro-emulsion are stirred strongly in a magnetic stirrer to prepare the uniform and transparent reverse micro-emulsion with stable property. Then, the micro-emulsion of barium chloride is dropped into the micro-emulsion of sodium molybdate. After reaction, aging and centrifugal separation, anhydrous alcohol and secondary water are used for repeated washing to obtain the barium molybdate octahedron with uniform morphology, size and height. The technical proposal which utilizes template action of reverse micelle micro-emulsion for preparing the octahedral barium molybdate solves the hard problems that by the existing barium molybdate octahedron preparing method, the particle size and the morphology of products cannot be controlled conveniently and preparation conditions are harsh. The method for preparing the octahedral barium molybdate has the characteristics of simple production process, safe production process and uneasy agglomeration of products and can be widely applied to the preparation of inorganic functional materials.
Description
Technical field
The present invention relates to a kind of preparation of inorganic functional material, the octahedral method of particularly a kind of uniform barium molybdate of the big low height of employing prepared by reverse microemulsion method pattern.
Background technology
Barium molybdate is the cubic phase alkaline-earth metal molybdate of scheelite-type structure, because special photoelectric properties that itself had, scintillator performance, humidity sensor performance etc. make it become a kind of material that receives much concern of inorganic functional material domain class.Barium molybdate is not only a kind of good photoelectric functional material, and also has potential to use at aspects such as humidity sensor, laser hosts.The property that the nanoscale novel structure is given it will make barium molybdate be applied in field widely.
At present synthetic barium molybdate nano crystal mainly contains following method: high-temperature fusion crystallization method [P.Afanasiev, Mater.Lett.2007,61,4622], crystal pulling method [T.T.Basiev, A.A.Sobol, Y.U.K.Voronko, P.G.Zverev, Opt.Mater.2000,15,205], spontaneous crystallization [D.A.Spassky, S.N.Ivanov, V.N.Kolobanov, V.V.Mikhailin, V.N.Zemskov, B.I.Zadneprovski, LI.Potkin, Radiat.Meas.2004,38,607], polymerization complexometry [A.P.A.Marques.D.M.A.deMelo, C.A.Paskocimas, PS.Pizani, M.R.Joya, E.R.Leite, E.Longo, J.Solid.State.Chem.2006,179,671], citric acid complex method [J.H.Ryu, J.-W.Yoon, C.J.Lim, K.B.Shim, Mater.Res.Bull.2005,40,1468], electrochemical process [C.H.Cui, J.Bi, C.Y.Wu, S.Zhang, D.J.Gao, Mater.Res.Bull.2008,43,1160], hydrothermal synthesis method [C.Zhang, E.Shen, E.Wang, Z.Kang, L.Gao, C.Hu, L.Xu, Mater.Chem.Phys.2006,96,240.], microwave irradiation [L.S.Cavalcante, J.C.Sczancoski, R.LTranquilin, M.R.Joya, P.S.Pizani, J.A.Varela, E.Longo, J.Phys.Chem.Sol.2008,69,2674] etc.There is deficiency to a certain extent in these methods, such as experiment condition harshness, preparation process complexity, cost are higher relatively; Product size, pattern are restive etc.And microemulsion synthesis method [M.P.Pileni, Nature.Mater.2003,2,145] utilize inverse micelles as " microreactor ", can reach the purpose of regulating and control granular size and pattern easily, thereby adopt reverse micro emulsion to prepare different-shape and material with property comes into one's own day by day.At present, the research of employing prepared by reverse microemulsion method barium molybdate inorganic nano structure also seldom.Octahedral barium molybdate yet there are no bibliographical information uniformly.
Summary of the invention
The objective of the invention is to provide that a kind of production technique is simple, safety in order to overcome the defective that above-mentioned prior art exists, product particle size, pattern (shape) are controlled, be uniformly dispersed, the preparation method of the octahedra Sodium orthomolybdate that product performance are good, this method is at room temperature to carry out simultaneously, the reaction conditions gentleness does not need to get final product with the direct centrifugation of emulsion splitter.
Purpose of the present invention can be achieved through the following technical solutions: a kind of preparation method of octahedral barium molybdate is characterized in that this preparation method selects raw material nonionogenic tenside alkyl polyoxyethylene (10) ether (OP-10), hexanaphthene, n-Octanol and water [BaCl for use
2Or Na
2MoO
4] the formation microemulsion, BaCl
2And Na
2MoO
4React, after each component of forming microemulsion is mixed, be prepared into the reverse micro emulsion of homogeneous transparent, with BaCl
2Microemulsion dropwise add Na
2MoO
4Microemulsion in, after the reaction, make the barium molybdate octahedron through ageing, centrifugation, washing, concrete preparation process is as follows:
1), gets raw material alkyl polyoxyethylene (10) ether (OP-10), hexanaphthene, n-Octanol and water [BaCl
2Solution] put into beaker, select alkyl polyoxyethylene (10) ether (OP-10) tensio-active agent and pure blended quality percentage composition, water [BaCl
2Solution] in the ratio ω of amount of substance of the amount of substance of water and alkyl polyoxyethylene (10) ether (OP-10) be 5～20, BaCl
2The concentration of solution is 0.01～0.2mol/L, and behind each component thorough mixing of said mixture, violent stirring is 30 minutes on constant temperature blender with magnetic force, is mixed with uniform microemulsion A;
2), get raw material alkyl polyoxyethylene (10) ether (OP-10), hexanaphthene, n-Octanol and water [Na
2MoO
4Solution] put into beaker, select alkyl polyoxyethylene (10) ether (OP-10) tensio-active agent and pure blended quality percentage composition, water [Na
2MoO
4Solution] in the ratio ω of amount of substance of the amount of substance of water and alkyl polyoxyethylene (10) ether (OP-10) be 5～20, Na
2MoO
4The concentration of solution is 0.01～0.2mol/L, and behind each component thorough mixing of said mixture, violent stirring is 30 minutes on constant temperature blender with magnetic force, is mixed with uniform microemulsion B;
3), microemulsion B is placed on the constant temperature blender with magnetic force, at room temperature slowly drip microemulsion A, along with the adding of microemulsion A, microemulsion becomes white gradually, dropwises the back and continues to stir 30 minutes;
4), the sealed beaker mouth, ageing at room temperature 1～72 hour;
5), reaction solution centrifugation that step 4) is obtained, go unnecessary tensio-active agent and water to obtain the octahedra product of barium molybdate with dehydrated alcohol and secondary water washing.
The ratio P of the amount of substance of the amount of substance of described n-Octanol and alkyl polyoxyethylene (10) ether (OP-10) is 0.5～1.5.
Described step 1), 2) the mol ratio ω of water and tensio-active agent is 10～20 in, can guarantee that the prerequisite that forms microemulsion makes the output of product high as much as possible like this.
The preparation method of octahedral barium molybdate according to claim 1 is characterized in that, Ba in the described step 3)
2+With MoO
4 2-Mol ratio be 1:1.
The preparation method of octahedral barium molybdate according to claim 1 is characterized in that, the reaction times in the described step 4) is 24～48 hours.Reaction times is too short, and crystallinity is relatively poor, and the reaction times is long, and pattern there is no too big variation, considers that preferred reaction time production cycle is 24 hours, and the octahedral barium molybdate pattern size that obtains is consistent.
Compared with prior art, the present invention has following characteristics:
1, being formed in the microemulsion water nuclear of the barium molybdate among the present invention by the content of adjusting water, and then controlled microemulsion water nuclear structure, obtains the barium molybdate nano crystal of desired pattern.
2, come controls reaction speed by rate of addition among the present invention, and then the pattern and the size of control product.
3, the present invention at room temperature carries out, mild condition and easily control, and noenergy consumption, cost is low.
4, the present invention can be widely used in the preparation of inorganic functional material.
Description of drawings
Fig. 1 is the particulate state BaMoO of the embodiment of the invention 1 preparation
4SEM figure;
Fig. 2 is the octahedra BaMoO of the embodiment of the invention 3 preparations
4SEM figure;
Fig. 3 is the octahedra BaMoO of the embodiment of the invention 4 preparations
4SEM figure;
The octahedra BaMoO that Fig. 4 makes for the inventive method
4X-ray diffractogram (XRD).
Embodiment
The invention will be further described below in conjunction with specific embodiment, and the description of embodiment is only for ease of understanding the present invention, but not to the restriction of the present invention's protection.
Embodiment 1
Preparation comprises 0.2mol/LBa
2+Microemulsion A, wherein tensio-active agent (alkyl polyoxyethylene (10) ether (OP-10)) and alcohol mixing quality content be 34%, the mol ratio ω of water and tensio-active agent is 5, all the other are oil phase content; Make corresponding each component concentration MoO consistent with microemulsion A
4 2-Microemulsion B.Under the stirring at room condition, microemulsion A is dropwise added among the microemulsion B, dropwise the back and continue to stir 30 minutes, stop to stir the back sealing, under room temperature still aging 24 hours again.Centrifugation, washing obtain particulate state barium molybdate nano crystal, as Fig. 1.Under this condition, also do not obtain the barium molybdate of octahedral structure owing to the restriction of microemulsion water nuclear structure.
Embodiment 2
Preparation comprises 0.05mol/LBa
2+Microemulsion A, wherein tensio-active agent (alkyl polyoxyethylene (10) ether (OP-10)) and alcohol mixing quality content be 34%, the mol ratio ω of water and tensio-active agent is 10, all the other are oil phase content; Make corresponding each component concentration MoO consistent with microemulsion A
4 2-Microemulsion B.Under the stirring at room condition, microemulsion A is dropwise added among the microemulsion B, dropwise the back and continue to stir 30 minutes, stop to stir the back sealing, under room temperature still aging 4 hours again.Centrifugation, washing obtain the octahedral barium molybdate nanocrystal.The rising of water-content has changed the structure of microemulsion, and then image product pattern, but because the time is shorter, crystallinity is bad.
Embodiment 3
Preparation comprises 0.05mol/LBa
2+Microemulsion A, wherein tensio-active agent (alkyl polyoxyethylene (10) ether (OP-10)) and alcohol mixing quality content be 34%, the mol ratio ω of water and tensio-active agent is 20, all the other are oil phase content; Make corresponding each component concentration MoO consistent with microemulsion A
4 2-Microemulsion B.Under the stirring at room condition, microemulsion A is dropwise added among the microemulsion B, dropwise the back and continue to stir 30 minutes, stop to stir the back sealing, under room temperature still aging 48 hours again.Centrifugation, washing obtain the octahedral barium molybdate nanocrystal, as Fig. 2.As seen during the digestion time sufficiently long, crystallinity is intact.
Embodiment 4
Preparation comprises 0.01mol/LBa
2+Microemulsion A, wherein tensio-active agent (alkyl polyoxyethylene (10) ether (OP-10)) and alcohol mixing quality content be 42%, the mol ratio ω of water and tensio-active agent is 20, all the other are oil phase content; Make corresponding each component concentration MoO consistent with microemulsion A
4 2-Microemulsion B.Under the stirring at room condition, microemulsion A is dropwise added among the microemulsion B, dropwise the back and continue to stir 30 minutes, stop to stir the back sealing, under room temperature still aging 24 hours again.Centrifugation, washing obtain the octahedral barium molybdate nanocrystal, as Fig. 3.The linking group of tensio-active agent increases the pattern that does not influence product a little, and only the product size reduces.
Embodiment 5
Preparation comprises 0.1mol/LBa
2+Microemulsion A, wherein tensio-active agent (alkyl polyoxyethylene (10) ether (OP-10)) and alcohol mixing quality content be 34%, the mol ratio ω of water and tensio-active agent is 20, all the other are oil phase content; Make corresponding each component concentration MoO consistent with microemulsion A
4 2-Microemulsion B.Under the stirring at room condition, microemulsion A is dropwise added among the microemulsion B, dropwise the back and continue to stir 30 minutes, stop to stir the back sealing, under room temperature still aging 72 hours again.Centrifugation, washing obtain the octahedral barium molybdate nanocrystal.Too big variation does not take place in the prolongation along with the time behind the octahedral barium molybdate complete crystallization, illustrates that the microemulsion system selected for use has the better controlled effect to the pattern and the size of product.
Claims (5)
1, the octahedral preparation method of a kind of barium molybdate is characterized in that this preparation method selects raw material nonionogenic tenside alkyl polyoxyethylene (10) ether (OP-10), hexanaphthene, n-Octanol and water [BaCl for use
2Or Na
2MoO
4] the formation microemulsion, BaCl
2And Na
2MoO
4Reaction after forming each component mixing of microemulsion, is prepared into the reverse micro emulsion of homogeneous transparent, again with BaCl
2Microemulsion dropwise add Na
2MoO
4Microemulsion in, after the reaction, make the barium molybdate octahedron through ageing, centrifugation, washing, concrete preparation process is as follows:
1), gets raw material alkyl polyoxyethylene (10) ether (OP-10), hexanaphthene, n-Octanol and water [BaCl
2Solution] put into beaker, select alkyl polyoxyethylene (10) ether (OP-10) tensio-active agent and pure blended quality percentage composition, water [BaCl
2Solution] in the ratio ω of amount of substance of the amount of substance of water and alkyl polyoxyethylene (10) ether (OP-10) be 5～20, BaCl
2The concentration of solution is 0.01～0.2mol/L, and after above-mentioned each component was mixed, violent stirring was 30 minutes on constant temperature blender with magnetic force, is mixed with uniform microemulsion A;
2), get raw material alkyl polyoxyethylene (10) ether (OP-10), hexanaphthene, n-Octanol and water [Na
2MoO
4Solution] put into beaker, select alkyl polyoxyethylene (10) ether (OP-10) tensio-active agent and pure blended quality percentage composition, water [Na
2MoO
4Solution] in the ratio ω of amount of substance of the amount of substance of water and alkyl polyoxyethylene (10) ether (OP-10) be 5～20, Na
2MoO
4The concentration of solution is 0.01～0.2mol/L, and behind each component thorough mixing of said mixture, violent stirring is 30 minutes on constant temperature blender with magnetic force, is mixed with uniform microemulsion B;
3), microemulsion B is placed on the constant temperature blender with magnetic force, at room temperature slowly drip microemulsion A, along with the adding of microemulsion A, microemulsion becomes white gradually, dropwises the back and continues to stir 30 minutes;
4), the sealed beaker mouth, ageing at room temperature 1～72 hour;
5), reaction solution centrifugation that step 4) is obtained, go unnecessary tensio-active agent and water to obtain the octahedra product of barium molybdate with dehydrated alcohol and secondary water washing.
2, the preparation method of octahedral barium molybdate according to claim 1 is characterized in that, the ratio P of the amount of substance of the amount of substance of described n-Octanol and alkyl polyoxyethylene (10) ether (OP-10) is 0.5～1.5.
3, the preparation method of octahedral barium molybdate according to claim 1 is characterized in that, described step 1), 2) in the mol ratio ω of water and tensio-active agent be 10～20.
4, the preparation method of octahedral barium molybdate according to claim 1 is characterized in that, Ba in the described step 3)
2+With MoO
4 2-Mol ratio be 1:1.
5, the preparation method of octahedral barium molybdate according to claim 1 is characterized in that, the reaction times in the described step 4) is 24～48 hours.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051667A (en) * | 2010-12-23 | 2011-05-11 | 广西民族大学 | Method for studying in-situ growing process of MnMo04.H20 nanorod |
| CN103342656A (en) * | 2013-07-04 | 2013-10-09 | 苏州永健生物医药有限公司 | Synthesis method of Telaprevir intermediate |
| CN108622937A (en) * | 2018-05-25 | 2018-10-09 | 山东师范大学 | A method of utilizing surfactant-free microemulsion reaction methods barium molybdate micron and/or nano material |
| CN109761278A (en) * | 2019-02-15 | 2019-05-17 | 山东师范大学 | Using surfactant-free microemulsion as the method for templated synthesis barium chromate nano material |
| CN110015691A (en) * | 2019-05-27 | 2019-07-16 | 山东师范大学 | A method of preparing nanoscale molybdic acid titanate particle |
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2008
- 2008-12-25 CN CN 200810107412 patent/CN101445274B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051667A (en) * | 2010-12-23 | 2011-05-11 | 广西民族大学 | Method for studying in-situ growing process of MnMo04.H20 nanorod |
| CN103342656A (en) * | 2013-07-04 | 2013-10-09 | 苏州永健生物医药有限公司 | Synthesis method of Telaprevir intermediate |
| CN108622937A (en) * | 2018-05-25 | 2018-10-09 | 山东师范大学 | A method of utilizing surfactant-free microemulsion reaction methods barium molybdate micron and/or nano material |
| CN109761278A (en) * | 2019-02-15 | 2019-05-17 | 山东师范大学 | Using surfactant-free microemulsion as the method for templated synthesis barium chromate nano material |
| CN109761278B (en) * | 2019-02-15 | 2021-10-19 | 山东师范大学 | Method for synthesizing barium chromate nano material by taking surfactant-free microemulsion as template |
| CN110015691A (en) * | 2019-05-27 | 2019-07-16 | 山东师范大学 | A method of preparing nanoscale molybdic acid titanate particle |
| CN110015691B (en) * | 2019-05-27 | 2021-10-01 | 山东师范大学 | Method for preparing nano-scale barium molybdate particles |
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