CN102173446A - Method for preparing nanometer lanthana ultrasonic microemulsion - Google Patents
Method for preparing nanometer lanthana ultrasonic microemulsion Download PDFInfo
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- CN102173446A CN102173446A CN 201010612576 CN201010612576A CN102173446A CN 102173446 A CN102173446 A CN 102173446A CN 201010612576 CN201010612576 CN 201010612576 CN 201010612576 A CN201010612576 A CN 201010612576A CN 102173446 A CN102173446 A CN 102173446A
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Abstract
The invention discloses a method for preparing nanometer lanthana ultrasonic microemulsion, which comprises the following steps of: putting a certain mass of 2-ethylhexyl sodium sulfosuccinate and octane into a reactor, and dripping a certain amount of ammonia water slowly at normal temperature, under normal pressure and under the condition of ultrasonic oscillation to form 2-ethylhexyl sodium sulfosuccinate-octane-ammonia water microemulsion; putting a certain mass of 2-ethylhexyl sodium sulfosuccinate and octane into the reactor, and dripping a certain amount of lanthanum nitrate slowly under the condition of the ultrasonic oscillation to form 2-ethylhexyl sodium sulfosuccinate-octane-lanthanum nitrate microemulsion; and mixing the two kinds of microemulsion slowly under the condition of the ultrasonic oscillation, performing centrifugal separation, eluting, drying under vacuum, and calcining at a controlled temperature to obtain nanometer La2O3. The nanometer lanthana ultrasonic microemulsion forms uniform, transparent and stable W/O microemulsion at normal temperature, under normal pressure and under the action of the ultrasonic oscillation; and the obtained nanometer lanthana has high dispersion, uniform size distribution and controllable grain sizes.
Description
Technical field
The present invention relates to a kind of nano material preparation technology, the ultrasonic micro emulsion preparation method of particularly a kind of nano lanthanum oxide.
Background technology
The nano lanthanum oxide crystal has also that specific surface area is big, many excellent characteristic such as chemistry and optical activity height, adsorption selectivity are strong, mobility of lattice oxygen except that the advantage that possesses general nano material.La
2O
3Be a kind of broad-spectrum rare earth material, be with a wide range of applications aspect catalystic material, electronic emission material, stupalith, luminescent material, the hydrogen storage material.Because the nanocrystalline particle diameter of lanthanum trioxide all will influence the character of relevant material greatly with purity, so high purity, suitably the research and development of grain diameter nano lanthanum trioxide are very important.
The method for preparing at present nano lanthanum oxide has: sol-gel method, hydrogen-carbonate are by the precipitator method, polymer microgel template, ultrasonic degradation method, solid-phase synthesis etc.The process control complexity of these methods, operation of equipment expense height, the products obtained therefrom uniform particles is poor, and particle easily bonds or reunion etc.Microemulsion technology is the preparation nano material novel method that has grown up since the eighties in 20th century.Distinctive microtexture of microemulsion and the characteristic that is presented make it show obvious superiority aspect preparation of nanoparticle, this method not only can prepare the uniform nanoparticle of size distribution, can also regulate and control crystalline state, pattern, particle diameter and the size distribution etc. of nanoparticle by each structural parameter that changes microemulsion, thus the nano lanthanum oxide of preparation desired properties.
And the formation of microemulsion is the key of micro-emulsion technology.Common microemulsion system mainly forms by oil phase, water, tensio-active agent and four kinds of components of cosurfactant are spontaneous under proper condition, and appearance transparent, low viscosity are thermodynamic stable system.Can be that oil content is dispersed in (O/W type) in the water, also can be water-dispersion (w/o type) in oil.In the W/O microemulsion, surround the aqueous solution and the micro emulsion particle that forms has constituted small " pond " by unimolecular layer that tensio-active agent and cosurfactant constituted, the size of its water nuclear several between tens nanometers, these small " ponds " are separated from one another, be exactly " microreactor ", or be called nano-reactor.This microreactor has very big interface, helps chemical reaction and carries out.Two kinds of reactants are dissolved in respectively in two parts of microemulsions, then these two parts of microemulsions are mixed under certain condition, two kinds of reactants that are in the different water nuclears mix mutually by the internuclear exchange of substance of water, react then.When the microemulsion boundary strength was enough big, because of reaction is subjected to the big or small restriction of water nuclear (i.e. reaction is limited in the water nuclear), the growth of reaction product also just was under control like this, will be dispersed in the microemulsion with the form of nano particle.
The content of water, tensio-active agent, cosurfactant and oil phase has direct relation in the water nuclear radius of reactor and the system, also select to have direct relation with tensio-active agent, cosurfactant and oil phase kind, therefore, it is even that microemulsion technology obtains particle diameter, and the key of the nano lanthanum oxide of controllable granularity is to determine relevant microemulsion parameter and form the stable microemulsion liquid system.But there is the problem of three aspects in present microemulsion technology: the one, and the formation complexity of microemulsion system; Usually microemulsion system mainly is made of oil phase, water, tensio-active agent and four kinds of components of cosurfactant, employed as previous experiments is in the microemulsion system of tensio-active agent with CTAB, and the alcohol that must add as cosurfactant could form microemulsion.The 2nd, difficult parameters control.The common microemulsion that constitutes by four kinds of components, must reasonable disposition oil phase, tensio-active agent and help the ratio of the three kinds of components in surface to form to have good molten water effect and stable microemulsion liquid system, dispose of the parameter more difficult control of the ratio of three components with respect to the microemulsion that only disposes oil phase, tensio-active agent two component ratios.The 3rd, microemulsion system is stable inadequately.The three component microemulsion systems that the do not contain cosurfactant shape that is translucent is usually placed and will be occurred precipitation in several days.These factors will have influence on nanocrystalline particle diameter of lanthanum trioxide and purity, thereby influence the performance of relevant lanthanum trioxide nanocrystalline material.
Summary of the invention
Purpose of the present invention just is to provide a kind of nano lanthanum oxide ultrasonic micro emulsion preparation method, and this method is easy to operate, and synthesis technique is simple, and it is even to access particle diameter, the nano lanthanum oxide of controllable granularity.
To achieve these goals, the technical solution used in the present invention is such: the ultrasonic micro emulsion preparation method of a kind of nano lanthanum oxide, the 2-ethylhexyl sodium sulfosuccinate and the octane of certain mass are placed reactor, under normal temperature, normal pressure and sonic oscillation condition, slowly drip certain amount of ammonia water, form 2-ethylhexyl sodium sulfosuccinate-octane-ammonia microemulsion, comprise NH in this microemulsion droplets water nuclear
3.H
2The O molecule; The 2-ethylhexyl sodium sulfosuccinate and the octane of certain mass are placed reactor, under the sonic oscillation condition, slowly drip a certain amount of lanthanum nitrate, form 2-ethylhexyl sodium sulfosuccinate-octane-lanthanum nitrate microemulsion, comprise La (NO in the drop water nuclear of this microemulsion
3)
3Particulate. The material transfer and the chemical reaction of material got white precipitate through centrifugation then in two kinds of slow hybrid concurrency unboiled water of microemulsion were examined under the sonic oscillation condition, obtained cubic crystal structure nanometer La through drip washing, vacuum-drying, temperature control calcining again
2O
3Sonic oscillation has effects such as intensive dispersion, stirring and emulsification, can promote the dispersion of material in emulsion system, and the microemulsion that generates is had certain stabilization.Under the effect of ultra-sonic oscillation, drop between 2-ethylhexyl sodium sulfosuccinate-octane-ammonia microemulsion and 2-ethylhexyl sodium sulfosuccinate-octane-lanthanum nitrate microemulsion system will bump, merge and separate, and the material that drop water comprises in examining exchanges mutually and reacts: La (NO
3)
3+ 3NH
3.H
2O=3NH
4NO
3+ La (OH)
3, the particle of formation product:
Because the water nuclear radius is a fixed, the growth of particle is subjected to the restriction of water nuclear radius, and the size of particles of Sheng Chenging also just is under control therein.
As preferably, described 2-ethylhexyl sodium sulfosuccinate is 1: 1～9 with the ratio of the quality of octane.
As preferably, described hyperacoustic oscillation frequency is 2 * 10
4Hz.
Because too high lanthanum nitrate concentration will cause microemulsion to become translucent, low excessively concentration will reduce the product amount.As preferably, the concentration of described lanthanum nitrate is 0.5molL
-1
Separate fully in order to be of value to above-mentioned two kinds of microemulsions, get in the white precipitate process in above-mentioned two kinds of microemulsion centrifugations, add ethanol and carry out breakdown of emulsion, centrifugal rotational speed is 2000r/min, more than the centrifugation 30min.
As preferably, the gained white precipitate at 80 ℃ of vacuum-drying 20h, obtains nanometer La then with acetone-dehydrated alcohol drip washing three times
2O
3Precursor.
As preferably, in the temperature control calcination process, temperature is set to 800 ℃, and calcination time is more than the 3h.Can be of value to the tensio-active agent that is attracted to the nano lanthanum oxide surface is like this removed fully.
As preferably, be that 2-ethylhexyl sodium sulfosuccinate-octane-ammonia microemulsion slowly is added drop-wise in 2-ethylhexyl sodium sulfosuccinate-octane-lanthanum nitrate microemulsion under normal temperature, normal pressure and action of ultrasonic waves in described two kinds of slow mixing processes of microemulsion.
Compared with prior art, the invention has the advantages that:
1, the present invention combines the ultrasonic wave radiation method with the micro emulsion method, for microemulsion technology finds new research direction in the development of field of nano material preparation; Microemulsion among the present invention under the sonic oscillation effect, forms the stable w/o type microemulsion of homogeneous transparent without cosurfactant under normal temperature, condition of normal pressure; Sonic oscillation has effects such as intensive dispersion, stirring and emulsification, can promote the dispersion of material in emulsion system, and the microemulsion that generates is had stabilization.
2, the nano lanthanum oxide high dispersing that forms among the present invention; The nano lanthanum oxide size distribution is even, and particle diameter is controlled.
Description of drawings
Fig. 1 is the prepared nanometer La of the present invention for the present invention
2O
3Size distribution figure;
Fig. 2 is the prepared nanometer La of the present invention
2O
3Transmission electron microscope (TEM) figure;
Fig. 3 is the prepared nanometer La of the present invention
2O
3X-ray diffraction (XRD) figure;
Fig. 4 is the structure iron of preparation facilities of the present invention.
Embodiment
The invention will be further described with concrete enforcement below in conjunction with accompanying drawing;
Embodiment 1
The ultrasonic micro emulsion preparation method of a kind of nano lanthanum oxide, its experimental procedure is:
(1) referring to Fig. 4, under normal temperature, normal pressure, 2-ethylhexyl sodium sulfosuccinate 4g, octane 4g are placed Erlenmeyer flask 3, Erlenmeyer flask 3 is placed in the ultrasonoscope 4, ultrasonoscope 4 is placed on the worktable 5, and two iron clamps are set on worktable 5, on the iron clamp respectively clamping one drop-burette 1 is arranged and connects the electrode 2 of conductivitimeter, fill 4ml ammoniacal liquor in the drop-burette 1, the lower end of described drop-burette 1 and electrode 2 is all stretched in the Erlenmeyer flask 3; The oscillation frequency of setting ultrasonoscope is 2 * 10
4Hz slowly drips w/o type 2-ethylhexyl sodium sulfosuccinate-octane-ammonia microemulsion that 4ml ammoniacal liquor forms homogeneous transparent under hyperacoustic oscillating condition;
(2) referring to Fig. 4, according to the method identical with 1, referring to Fig. 4, under normal temperature, normal pressure, 2-ethylhexyl sodium sulfosuccinate 4g, octane 4g are placed Erlenmeyer flask 3, Erlenmeyer flask 3 is placed in the ultrasonoscope 4, ultrasonoscope 4 is placed on the worktable 5, two iron clamps are set on worktable 5, on the iron clamp respectively clamping one drop-burette 1 is arranged and connects the electrode 2 of conductivitimeter, fill 4ml0.5molL in the drop-burette 1
-1Lanthanum nitrate, the described lower end that connects drop-burette 1 and electrode 2 is all stretched in the Erlenmeyer flask 3; The oscillation frequency of setting ultrasonoscope is 2 * 10
4Hz is 2 * 10 in oscillation frequency
4Hyperacoustic oscillating condition of Hz slowly drips 4ml0.5molL down
-1Lanthanum nitrate form the w/o type 2-ethylhexyl sodium sulfosuccinate-octane-lanthanum nitrate microemulsion of homogeneous transparent;
(3) be 2 * 10 in normal temperature, normal pressure and oscillation frequency
4Under the ultrasonic wave of Hz 2-ethylhexyl sodium sulfosuccinate-octane-ammonia microemulsion slowly is added drop-wise in 2-ethylhexyl sodium sulfosuccinate-octane-lanthanum nitrate microemulsion, forms mixed solution, sonic oscillation 0.5h then.
(4) add the 40ml dehydrated alcohol to reacted mixed solution, and centrifugation gets white precipitate under the 2000r/min rotating speed, more than the centrifugation 30min.
(5) gained white precipitate volume ratio is 1: 1 a acetone-dehydrated alcohol drip washing three times, at 80 ℃ of vacuum-drying 20h, obtains nanometer La then
2O
3Precursor.
(6) with nanometer La
2O
3Precursor obtains nanometer La more than the calcining 3h down for 800 ℃ at temperature control
2O
3
Embodiment 2:
The ultrasonic micro emulsion preparation method of a kind of nano lanthanum oxide, its experimental procedure is:
(1) referring to Fig. 4, under normal temperature, normal pressure, 2-ethylhexyl sodium sulfosuccinate 4g, octane 36g are placed Erlenmeyer flask 3, Erlenmeyer flask 3 is placed in the ultrasonoscope 4, ultrasonoscope 4 is placed on the worktable 5, and two iron clamps are set on worktable 5, on the iron clamp respectively clamping one drop-burette 1 is arranged and connects the electrode 2 of conductivitimeter, fill 4ml ammoniacal liquor in the drop-burette 1, the lower end of described drop-burette 1 and electrode 2 is all stretched in the Erlenmeyer flask 3; The oscillation frequency of setting ultrasonoscope is 2 * 10
4Hz slowly drips w/o type 2-ethylhexyl sodium sulfosuccinate-octane-ammonia microemulsion that 4ml ammoniacal liquor forms homogeneous transparent under hyperacoustic oscillating condition;
(2) referring to Fig. 4, according to the method identical with 1, under normal temperature, normal pressure, 2-ethylhexyl sodium sulfosuccinate 4g, octane 36g are placed Erlenmeyer flask 3, Erlenmeyer flask 3 is placed in the ultrasonoscope 4, and ultrasonoscope 4 is placed on the worktable 5, and two iron clamps are set on worktable 5, on the iron clamp respectively clamping one drop-burette 1 is arranged and connects the electrode 2 of conductivitimeter, fill 4ml0.5molL in the drop-burette 1
-1Lanthanum nitrate, the lower end of described drop-burette 1 and electrode 2 is all stretched in the Erlenmeyer flask 3; The oscillation frequency of setting ultrasonoscope is 2 * 10
4Hz is 2 * 10 in oscillation frequency
4Hyperacoustic oscillating condition of Hz slowly drips 4ml0.5molL down
-1Lanthanum nitrate form the w/o type 2-ethylhexyl sodium sulfosuccinate-octane-lanthanum nitrate microemulsion of homogeneous transparent;
(3) be 2 * 10 in normal temperature, normal pressure and oscillation frequency
4Under the ultrasonic wave of Hz 2-ethylhexyl sodium sulfosuccinate-octane-ammonia microemulsion slowly is added drop-wise in 2-ethylhexyl sodium sulfosuccinate-octane-lanthanum nitrate microemulsion, forms mixed solution, sonic oscillation 0.5h then.
(4) add the 40ml dehydrated alcohol to reacted mixed solution, and centrifugation gets white precipitate under the 2000r/min rotating speed, more than the centrifugation 30min.
(5) gained white precipitate volume ratio is 1: 1 a acetone-dehydrated alcohol drip washing three times, at 80 ℃ of vacuum-drying 20h, obtains nanometer La then
2O
3Precursor.
(6) with nanometer La
2O
3Precursor obtains nanometer La more than the calcining 3h down for 800 ℃ at temperature control
2O
3
Embodiment 3:
The ultrasonic micro emulsion preparation method of a kind of nano lanthanum oxide, its experimental procedure is:
(1) referring to Fig. 4, under normal temperature, normal pressure, 2-ethylhexyl sodium sulfosuccinate 4g, octane 20g are placed Erlenmeyer flask 3, Erlenmeyer flask 3 is placed in the ultrasonoscope 4, ultrasonoscope 4 is placed on the worktable 5, and two iron clamps are set on worktable 5, on the iron clamp respectively clamping one drop-burette 1 is arranged and connects the electrode 2 of conductivitimeter, fill 4ml ammoniacal liquor in the drop-burette 1, the described lower end that connects drop-burette 1 and electrode 2 is all stretched in the Erlenmeyer flask 3; The oscillation frequency of setting ultrasonoscope is 2 * 10
4Hz slowly drips w/o type 2-ethylhexyl sodium sulfosuccinate-octane-ammonia microemulsion that 4ml ammoniacal liquor forms homogeneous transparent under hyperacoustic oscillating condition;
(2) referring to Fig. 4, according to the method identical with 1, under normal temperature, normal pressure, 2-ethylhexyl sodium sulfosuccinate 4g, octane 20g are placed Erlenmeyer flask 3, Erlenmeyer flask 3 is placed in the ultrasonoscope 4, and ultrasonoscope 4 is placed on the worktable 5, and two iron clamps are set on worktable 5, on the iron clamp respectively clamping one drop-burette 1 is arranged and connects the electrode 2 of conductivitimeter, fill 4ml0.5molL in the drop-burette 1
-1Lanthanum nitrate, the lower end of described drop-burette 1 and electrode 2 is all stretched in the Erlenmeyer flask 3; The oscillation frequency of setting ultrasonoscope is 2 * 10
4Hz is 2 * 10 in oscillation frequency
4Hyperacoustic oscillating condition of Hz slowly drips 4ml0.5molL down
-1Lanthanum nitrate form the w/o type 2-ethylhexyl sodium sulfosuccinate-octane-lanthanum nitrate microemulsion of homogeneous transparent;
(3) be 2 * 10 in normal temperature, normal pressure and oscillation frequency
4Under the ultrasonic wave of Hz 2-ethylhexyl sodium sulfosuccinate-octane-ammonia microemulsion slowly is added drop-wise in 2-ethylhexyl sodium sulfosuccinate-octane-lanthanum nitrate microemulsion, forms mixed solution, sonic oscillation 0.5h then.
(4) add the 40ml dehydrated alcohol to reacted mixed solution, and centrifugation gets white precipitate under the 2000r/min rotating speed, more than the centrifugation 30min.
(5) gained white precipitate volume ratio is 1: 1 a acetone-dehydrated alcohol drip washing three times, at 80 ℃ of vacuum-drying 20h, obtains nanometer La then
2O
3Precursor.
(6) with nanometer La
2O
3Precursor obtains nanometer La more than the calcining 3h down for 800 ℃ at temperature control
2O
3
Detected result: referring to Fig. 1, the nano lanthanum oxide size distribution is 20～30nm; Referring to Fig. 2, the good dispersity of nano lanthanum oxide particulate; Referring to Fig. 3, nanometer La
2O
3The XRD curve respectively in 2 θ=25.18,27.93,28.92,38.76,45.02,51.34, characteristic peak appearred in 54.76 places, by reference standard collection of illustrative plates, nanometer La
2O
3XRD curvilinear characteristic peak and pdf card 24-0554 basically identical, the nano lanthanum oxide crystalline form is a cubic crystal structure.
Sonic oscillation has effects such as intensive dispersion, stirring and emulsification, can promote the dispersion of material in emulsion system, and the microemulsion that generates had stabilization, the microemulsion system that the present invention forms under sonic oscillation is transparence, and places after 30 days and do not produce deposited phenomenon.The above only is a preferred implementation of the present invention, and protection scope of the present invention also not only is confined to the foregoing description, and all technical schemes that belongs under the thinking of the present invention all belong to protection scope of the present invention.Should be pointed out that for those skilled in the art the some improvements and modifications not breaking away under the principle of the invention prerequisite also should be considered as protection scope of the present invention.
Claims (8)
1. ultrasonic micro emulsion preparation method of nano lanthanum oxide, it is characterized in that: the 2-ethylhexyl sodium sulfosuccinate and the octane of certain mass are placed reactor, under normal temperature, normal pressure and sonic oscillation condition, slowly drip certain amount of ammonia water, form 2-ethylhexyl sodium sulfosuccinate-octane-ammonia microemulsion; The 2-ethylhexyl sodium sulfosuccinate and the octane of certain mass are placed reactor, under the sonic oscillation condition, slowly drip a certain amount of lanthanum nitrate, form 2-ethylhexyl sodium sulfosuccinate-octane-lanthanum nitrate microemulsion; The material transfer and the chemical reaction of material got white precipitate through centrifugation then in two kinds of slow hybrid concurrency unboiled water of microemulsion were examined under the sonic oscillation condition, obtained cubic crystal structure nanometer La through drip washing, vacuum-drying, temperature control calcining again
2O
3
2. the ultrasonic micro emulsion preparation method of a kind of nano lanthanum oxide according to claim 1 is characterized in that: described 2-ethylhexyl sodium sulfosuccinate is 1: 1～9 with the ratio of the quality of octane.
3. the ultrasonic micro emulsion preparation method of a kind of nano lanthanum oxide according to claim 1 is characterized in that: described hyperacoustic oscillation frequency is 2 * 10
4Hz.
4. the ultrasonic micro emulsion preparation method of a kind of nano lanthanum oxide according to claim 1 is characterized in that: the concentration of described lanthanum nitrate is 0.5molL
-1
5. the ultrasonic micro emulsion preparation method of a kind of nano lanthanum oxide according to claim 1, it is characterized in that: get in the white precipitate process in above-mentioned two kinds of microemulsion centrifugations, add ethanol and carry out breakdown of emulsion, centrifugal rotational speed is 2000r/min, more than the centrifugation 30min.
6. the ultrasonic micro emulsion preparation method of a kind of nano lanthanum oxide according to claim 1 is characterized in that: the gained white precipitate at 80 ℃ of vacuum-drying 20h, obtains nanometer La then with acetone-dehydrated alcohol drip washing three times
2O
3Precursor.
7. the ultrasonic micro emulsion preparation method of a kind of nano lanthanum oxide according to claim 1 is characterized in that: in the temperature control calcination process, temperature is set to 800 ℃, and calcination time is more than the 3h.
8. the ultrasonic micro emulsion preparation method of a kind of nano lanthanum oxide according to claim 1 is characterized in that: in described two kinds of slow mixing processes of microemulsion is under normal temperature, normal pressure and action of ultrasonic waves 2-ethylhexyl sodium sulfosuccinate-octane-ammonia microemulsion slowly to be added drop-wise in 2-ethylhexyl sodium sulfosuccinate-octane-lanthanum nitrate microemulsion.
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|---|---|---|---|---|
| CN102504604A (en) * | 2011-10-17 | 2012-06-20 | 南京航空航天大学 | Ultrasonic ball-milling compound preparation method of high dispersion nano lanthanum oxide slurry |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1733611A (en) * | 2005-08-12 | 2006-02-15 | 安泰科技股份有限公司 | Zirconium dioxide nano powder material preparation method |
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| CN1733611A (en) * | 2005-08-12 | 2006-02-15 | 安泰科技股份有限公司 | Zirconium dioxide nano powder material preparation method |
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| Title |
|---|
| 《后勤工程学院学报》 20080131 赵光哲等 微乳体系中纳米La2O3的制备 29-32 1-8 第24卷, 第1期 * |
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|---|---|---|---|---|
| CN102504604A (en) * | 2011-10-17 | 2012-06-20 | 南京航空航天大学 | Ultrasonic ball-milling compound preparation method of high dispersion nano lanthanum oxide slurry |
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