CN103833073B - The preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere - Google Patents
The preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere Download PDFInfo
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- CN103833073B CN103833073B CN201210475687.5A CN201210475687A CN103833073B CN 103833073 B CN103833073 B CN 103833073B CN 201210475687 A CN201210475687 A CN 201210475687A CN 103833073 B CN103833073 B CN 103833073B
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Abstract
The invention discloses a kind of preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere.It adopts solution method, and its step is first by rear stirring soluble in water for nitride powder, obtains the titanium nitride aqueous solution, then in the titanium nitride aqueous solution, adds hydrogen peroxide and ammoniacal liquor successively, and stir at least 1h, obtain precursor solution; Then, first precursor solution is mixed rear stirring mutually with ethanol, obtain microemulsion solution, then heat at least 12h at microemulsion solution is placed in 60 ~ 80 DEG C, obtain white depositions; Subsequently, first washing with alcohol is used to white depositions, then drying at least 24h at being placed on 55 ~ 65 DEG C, obtained diameter is the single dispersing smooth surface amorphous titanium dioxide nano-sphere of 150 ~ 800nm.It is that a kind of need uses any template to make the microemulsion solution method of structure directing agent, the mild condition of not only synthesizing, nontoxic, pollution-free, and cheap, belong to the low-temperature synthetic method of environmental protection, pole is beneficial to the commercial applications of industrialized production and obtained target product.
Description
Technical field
The present invention relates to a kind of preparation method of titanium dioxide nano-sphere, especially a kind of preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere.
Background technology
Titanium dioxide is a kind of widely used wide bandgap semiconductor materials, its good stability, to human non-toxic, and there is wet sensitive, pressure-sensitive and air-sensitive and good photochemical catalysis and opto-electronic conversion performance and be widely applied to the fields such as sensor, photocatalyst, electronic material, paint and other industrial chemicals, and be expected to utilize sun power to demonstrate wide application prospect in organic synthesis, photocatalytic water and environmental improvement etc.At present, people, in order to obtain nanometer titanic oxide material, have made unremitting effort, as the one " preparation method of titanium dioxide nano mesoporous balls " disclosed in Chinese invention patent application prospectus CN 1749172 A that announces on March 22nd, 2006.The preparation method mentioned in this specification sheets is sol-gel method, its concrete steps are first be dissolved in by citric acid in the mixed solution of ammoniacal liquor, water, ethanol, again butyl (tetra) titanate to be added in mixed solution and to stir, or first butyl (tetra) titanate is dissolved in ethanol, citric acid, ammoniacal liquor, water is added successively again in mixed solution, and be stirred to and dissolve completely, afterwards, first the throw out solution of mixed solution after leaving standstill is cleaned, again by drying precipitate, calcining, obtained spherical diameter is the titanium dioxide nano mesoporous hollow or solid sphere of 200 ~ 300nm.But this preparation method also exists shortcoming part, first, as the liquid titanium acid butyl ester of one of raw material except on the high side, also have and be unfavorable for the industrialized deficiency using and transport; Secondly, the acquisition of product needs the technique going through calcining, not only consumes energy but also time-consuming; Secondary again, the particle size range of obtained product is partially narrow, constrains occasion and the field of application; Finally, though obtained product has numerous purposes, be difficult to it can be used as matting agent and for sun-proof field.
Summary of the invention
The technical problem to be solved in the present invention, for overcoming shortcoming part of the prior art, provides that a kind of cost of manufacture is low, the particle diameter variable range of target product is large and has the preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere of eliminate optical property.
For solving technical problem of the present invention, the technical scheme adopted is: the preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere adopts solution method, and particularly completing steps is as follows:
Step 1, first is the ratio of 0.4 ~ 0.6:110 ~ 130 according to weight ratio, by rear stirring soluble in water for nitride powder at least 0.5h, obtain the titanium nitride aqueous solution, add in the titanium nitride aqueous solution successively again concentration be 25 ~ 35% hydrogen peroxide and concentration be the ammoniacal liquor of 25 ~ 28%, and stir at least 1h, wherein, the volume ratio of the titanium nitride aqueous solution, hydrogen peroxide and ammoniacal liquor is 110.4 ~ 130.6:14 ~ 18:14 ~ 18, obtains precursor solution;
Step 2, stirs at least 0.5h after first being mixed mutually according to the ratio that volume ratio is 2 ~ 5:5 ~ 8 with ethanol by precursor solution, obtains microemulsion solution, then heat at least 12h at microemulsion solution is placed in 60 ~ 80 DEG C, obtain white depositions;
Step 3, first uses washing with alcohol to white depositions, then drying at least 24h at being placed on 55 ~ 65 DEG C, and obtained diameter is the single dispersing smooth surface amorphous titanium dioxide nano-sphere of 150 ~ 800nm.
As the further improvement of the preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere, described water is deionized water, or distilled water; Described is 0.5 ~ 1h by the time of rear stirring soluble in water for nitride powder; The described churning time after hydrogen peroxide and ammoniacal liquor that adds successively in the titanium nitride aqueous solution is 1 ~ 3h; Described time precursor solution and ethanol being mixed mutually rear stirring is 0.5 ~ 1h; Described time microemulsion solution being placed in heating at 60 ~ 80 DEG C is 12 ~ 20h; The described time washed white depositions being placed in drying at 55 ~ 65 DEG C is 24 ~ 28h; Described single dispersing smooth surface amorphous titanium dioxide nano-sphere is placed in 400 ~ 500 DEG C at annealing 1 ~ 3h, obtain the anatase crystal titania mesoporous ball that diameter is the single dispersing uneven surface of 150 ~ 800nm.
Relative to the beneficial effect of prior art be, one, scanning electron microscope, X-ray diffractometer and ultraviolet-visual spectrometer is used to characterize respectively to the target product using preparation method to obtain, from its result, obtained target product is numerous, monodispersed, ganoid, diameter is the globe of 150 ~ 800nm; This globe is amorphous titanium dioxide; Along with the increase of amorphous titanium dioxide nanometer ball diameter, the delustring peak generation red shift of obtained target product and occur broadening.Its two, preparation method's science, effectively: both obtained single dispersing smooth surface amorphous titanium dioxide nano-sphere; By the ratio changed between precursor solution and ethanol, the diameter of the target product obtained can artificially be regulated on a large scale again; Also make the target product obtained be provided with eliminate optical property, make it can be used as sun-screening agent, be widely used for the field such as makeup, paint; The cost of preparation is more greatly reduced because of the process choosing and avoid calcining of inexpensive raw material.This need uses any template to make the microemulsion solution method of structure directing agent, the mild condition of not only synthesizing, nontoxic, pollution-free, and cheap, belong to the low-temperature synthetic method of environmental protection, pole is beneficial to the commercial applications of industrialized production and obtained target product.
As the further embodiment of beneficial effect, one is that water is preferably deionized water, or distilled water, avoids the introducing of impurity.Two is that the time of rear stirring soluble in water for nitride powder is preferably 0.5 ~ 1h, churning time add hydrogen peroxide and ammoniacal liquor successively in the titanium nitride aqueous solution after is preferably 1 ~ 3h, the time that precursor solution and ethanol mix rear stirring is mutually preferably 0.5 ~ 1h, time microemulsion solution being placed in heating at 60 ~ 80 DEG C is preferably 12 ~ 20h, the time washed white depositions being placed in drying at 55 ~ 65 DEG C is preferably 24 ~ 28h, when only needing the less time, ensure that the quality of obtained target product.Three is annealing 1 ~ 3h at preferably single dispersing smooth surface amorphous titanium dioxide nano-sphere being placed in 400 ~ 500 DEG C, obtain the anatase crystal titania mesoporous ball that diameter is the single dispersing uneven surface of 150 ~ 800nm, expand the purposes scope of the target product obtained.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, optimal way of the present invention is described in further detail.
Fig. 1 is to one of result that obtained target product uses scanning electron microscope (SEM) to characterize.Can be found out by SEM image, obtained target product is the globe of numerous single dispersing smooth surfaces; Wherein, in Fig. 1 a, the diameter of the diameter of globe to be the diameter of globe in 200nm, Fig. 1 b be globe in 300nm, Fig. 1 c is the diameter of globe in 5200nm, Fig. 1 d is 800nm.Scale length in SEM image as illustrated in fig 1d, is 100nm.
Fig. 2 is respectively to one of result that obtained target product and the products that obtain after target product being carried out 500 DEG C of annealing use X-ray diffraction (XRD) instrument to characterize.Curve 1 in XRD spectra is the spectral line of target product, and from it, target product is non-crystal titanium dioxide; Curve 2 is the spectral line of the product obtained after annealing, and from it, product is anatase crystal titanium dioxide.
Fig. 3 is to one of result that obtained target product uses uv-vis spectra (UV-Vis) instrument to characterize.The delustring spectral line that curve 1 in UV-Vis spectrogram is the spherical diameter of target product when being 200nm, the delustring spectral line that curve 2 is the spherical diameter of target product when being 300nm, the delustring spectral line that curve 3 is the spherical diameter of target product when being 500nm, the delustring spectral line that curve 4 is the spherical diameter of target product when being 800nm.
Fig. 4 is to one of result that the products obtained target product being carried out 500 DEG C of rear acquisitions of annealing use scanning electron microscope to characterize.Can be found out by SEM image, the product obtained after annealing is the globe of uneven surface.
Embodiment
First buy from market or obtain by ordinary method:
Nitride powder; As deionized water or the distilled water of water; Hydrogen peroxide; Ammoniacal liquor; Ethanol.
Then,
Embodiment 1
The concrete steps of preparation are:
Step 1, first is the ratio of 0.4:130 according to weight ratio, by rear stirring 0.5h soluble in water for nitride powder; Wherein, water is deionized water, obtains the titanium nitride aqueous solution.Add in the titanium nitride aqueous solution successively again concentration be 25% hydrogen peroxide and concentration be the ammoniacal liquor of 28%, and stir 1h; Wherein, the volume ratio of the titanium nitride aqueous solution, hydrogen peroxide and ammoniacal liquor is 110.4:18:14, obtains precursor solution.
Step 2, stirs 0.5h after first being mixed mutually according to the ratio that volume ratio is 2:8 with ethanol by precursor solution, obtains microemulsion solution.Heat 20h at again microemulsion solution being placed in 60 DEG C, obtain white depositions.
Step 3, first uses washing with alcohol to white depositions, drier 28h at being placed on 55 DEG C, obtains as shown in Figure 1 d, and the single dispersing smooth surface amorphous titanium dioxide nano-sphere as shown in the curve in Fig. 2 and Fig. 3.
Embodiment 2
The concrete steps of preparation are:
Step 1, first is the ratio of 0.45:125 according to weight ratio, by rear stirring 0.6h soluble in water for nitride powder; Wherein, water is distilled water, obtains the titanium nitride aqueous solution.Add in the titanium nitride aqueous solution successively again concentration be 28% hydrogen peroxide and concentration be the ammoniacal liquor of 27%, and stir 1.5h; Wherein, the volume ratio of the titanium nitride aqueous solution, hydrogen peroxide and ammoniacal liquor is 115:17:15, obtains precursor solution.
Step 2, stirs 0.6h after first being mixed mutually according to the ratio that volume ratio is 3:7 with ethanol by precursor solution, obtains microemulsion solution.Heat 16h at again microemulsion solution being placed in 65 DEG C, obtain white depositions.
Step 3, first uses washing with alcohol to white depositions, drier 27h at being placed on 58 DEG C, obtains as illustrated in figure 1 c, and the single dispersing smooth surface amorphous titanium dioxide nano-sphere as shown in the curve in Fig. 2 and Fig. 3.
Embodiment 3
The concrete steps of preparation are:
Step 1, first is the ratio of 0.5:120 according to weight ratio, by rear stirring 0.7h soluble in water for nitride powder; Wherein, water is deionized water, obtains the titanium nitride aqueous solution.Add in the titanium nitride aqueous solution successively again concentration be 30% hydrogen peroxide and concentration be the ammoniacal liquor of 27%, and stir 2h; Wherein, the volume ratio of the titanium nitride aqueous solution, hydrogen peroxide and ammoniacal liquor is 120:16:16, obtains precursor solution.
Step 2, stirs 0.7h after first being mixed mutually according to the ratio that volume ratio is 4:6 with ethanol by precursor solution, obtains microemulsion solution.Heat 16h at again microemulsion solution being placed in 70 DEG C, obtain white depositions.
Step 3, first uses washing with alcohol to white depositions, drier 26h at being placed on 60 DEG C, obtains as shown in Figure 1 b, and the single dispersing smooth surface amorphous titanium dioxide nano-sphere as shown in the curve in Fig. 2 and Fig. 3.
Embodiment 4
The concrete steps of preparation are:
Step 1, first is the ratio of 0.55:115 according to weight ratio, by rear stirring 0.9h soluble in water for nitride powder; Wherein, water is deionized water (or distilled water), obtains the titanium nitride aqueous solution.Add in the titanium nitride aqueous solution successively again concentration be 33% hydrogen peroxide and concentration be the ammoniacal liquor of 26%, and stir 2.5h; Wherein, the volume ratio of the titanium nitride aqueous solution, hydrogen peroxide and ammoniacal liquor is 125:15:17, obtains precursor solution.
Step 2, stirs 0.8h after first being mixed mutually according to the ratio that volume ratio is 4:6 with ethanol by precursor solution, obtains microemulsion solution.Heat 14h at again microemulsion solution being placed in 75 DEG C, obtain white depositions.
Step 3, first uses washing with alcohol to white depositions, drier 25h at being placed on 63 DEG C, obtains as shown in Figure 1 b, and the single dispersing smooth surface amorphous titanium dioxide nano-sphere as shown in the curve in Fig. 2 and Fig. 3.
Embodiment 5
The concrete steps of preparation are:
Step 1, first is the ratio of 0.6:110 according to weight ratio, by rear stirring 1h soluble in water for nitride powder; Wherein, water is deionized water (or distilled water), obtains the titanium nitride aqueous solution.Add in the titanium nitride aqueous solution successively again concentration be 35% hydrogen peroxide and concentration be the ammoniacal liquor of 25%, and stir 3h; Wherein, the volume ratio of the titanium nitride aqueous solution, hydrogen peroxide and ammoniacal liquor is 130.6:14:18, obtains precursor solution.
Step 2, stirs 1h after first being mixed mutually according to the ratio that volume ratio is 5:5 with ethanol by precursor solution, obtains microemulsion solution.Heat 12h at again microemulsion solution being placed in 80 DEG C, obtain white depositions.
Step 3, first uses washing with alcohol to white depositions, drier 24h at being placed on 65 DEG C, obtains as shown in Figure 1a, and the single dispersing smooth surface amorphous titanium dioxide nano-sphere as shown in the curve in Fig. 2 and Fig. 3.
If expand the purposes scope of obtained target product further, anneal at more obtained single dispersing smooth surface amorphous titanium dioxide nano-sphere can being placed in 400 ~ 500 DEG C 1 ~ 3h, obtains as or be similar to the anatase crystal titania mesoporous ball that the diameter shown in Fig. 4 is the single dispersing uneven surface of 150 ~ 800nm.
Obviously, those skilled in the art can carry out various change and modification to the preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere of the present invention and not depart from the spirit and scope of the present invention.Like this, if belong within the scope of the claims in the present invention and equivalent technologies thereof to these amendments of the present invention and modification, then the present invention is also intended to comprise these change and modification.
Claims (7)
1. a preparation method for single dispersing smooth surface amorphous titanium dioxide nano-sphere, adopts solution method, it is characterized in that completing steps is as follows:
Step 1, first is the ratio of 0.4 ~ 0.6:110 ~ 130 according to weight ratio, by rear stirring soluble in water for nitride powder at least 0.5h, obtain the titanium nitride aqueous solution, add in the titanium nitride aqueous solution successively again concentration be 25 ~ 35% hydrogen peroxide and concentration be the ammoniacal liquor of 25 ~ 28%, and stir at least 1h, wherein, the volume ratio of the titanium nitride aqueous solution, hydrogen peroxide and ammoniacal liquor is 110.4 ~ 130.6:14 ~ 18:14 ~ 18, obtains precursor solution;
Step 2, stirs at least 0.5h after first being mixed mutually according to the ratio that volume ratio is 2 ~ 5:5 ~ 8 with ethanol by precursor solution, obtains microemulsion solution, then heat at least 12h at microemulsion solution is placed in 60 ~ 80 DEG C, obtain white depositions;
Step 3, first uses washing with alcohol to white depositions, then drying at least 24h at being placed on 55 ~ 65 DEG C, and obtained diameter is the single dispersing smooth surface amorphous titanium dioxide nano-sphere of 150 ~ 800nm.
2. the preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere according to claim 1, is characterized in that water is deionized water, or distilled water.
3. the preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere according to claim 1, is characterized in that by the time of rear stirring soluble in water for nitride powder be 0.5 ~ 1h.
4. the preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere according to claim 1, is characterized in that the churning time add hydrogen peroxide and ammoniacal liquor successively in the titanium nitride aqueous solution after is 1 ~ 3h.
5. the preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere according to claim 1, is characterized in that time precursor solution and ethanol being mixed mutually rear stirring is 0.5 ~ 1h.
6. the preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere according to claim 1, the time that it is characterized in that microemulsion solution to be placed in heating at 60 ~ 80 DEG C is 12 ~ 20h.
7. the preparation method of single dispersing smooth surface amorphous titanium dioxide nano-sphere according to claim 1, it is characterized in that washed white depositions to be placed in the time dry at 55 ~ 65 DEG C is 24 ~ 28h.
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| US4999181A (en) * | 1987-11-25 | 1991-03-12 | U.S. Philips Corporation | Method of manufacturing titanium dioxide powder |
| CN1749172A (en) * | 2004-09-15 | 2006-03-22 | 中国科学院合肥物质科学研究院 | The preparation method of titanium dioxide nano mesoporous balls |
| CN1935669A (en) * | 2005-09-22 | 2007-03-28 | 中国科学院理化技术研究所 | Low temperature crystallized nano titanium dioxide powder and sol synthesizing method |
| CN101074113A (en) * | 2007-05-16 | 2007-11-21 | 浙江大学 | Production and use for non-metallic doped nano-TiO |
| CN101973581A (en) * | 2010-09-27 | 2011-02-16 | 彩虹集团公司 | Preparation method of titanium dioxide powder with big particle diameter |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4999181A (en) * | 1987-11-25 | 1991-03-12 | U.S. Philips Corporation | Method of manufacturing titanium dioxide powder |
| CN1749172A (en) * | 2004-09-15 | 2006-03-22 | 中国科学院合肥物质科学研究院 | The preparation method of titanium dioxide nano mesoporous balls |
| CN1935669A (en) * | 2005-09-22 | 2007-03-28 | 中国科学院理化技术研究所 | Low temperature crystallized nano titanium dioxide powder and sol synthesizing method |
| CN101074113A (en) * | 2007-05-16 | 2007-11-21 | 浙江大学 | Production and use for non-metallic doped nano-TiO |
| CN101973581A (en) * | 2010-09-27 | 2011-02-16 | 彩虹集团公司 | Preparation method of titanium dioxide powder with big particle diameter |
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