CN102101685B - Aluminium hydroxide nanometer strip and preparation method thereof - Google Patents
Aluminium hydroxide nanometer strip and preparation method thereof Download PDFInfo
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- CN102101685B CN102101685B CN2009102425842A CN200910242584A CN102101685B CN 102101685 B CN102101685 B CN 102101685B CN 2009102425842 A CN2009102425842 A CN 2009102425842A CN 200910242584 A CN200910242584 A CN 200910242584A CN 102101685 B CN102101685 B CN 102101685B
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Abstract
The invention relates to an aluminium hydroxide nanometer strip and a preparation method thereof. The shape structure of the aluminium hydroxide nanometer strip is a three-dimensional radial structure. The preparation method of the aluminium hydroxide nanometer strip comprises the following steps of: dissolving dissoluble aluminium salt and carbamide into an alcohol-water mixed solvent; and then sequentially heating an obtained mixture at the temperature of 340-373 K and 393-573 K for 6-15 hours and 2-10 hours. The aluminium hydroxide nanometer strip as an additive can be used for enhancing the mechanical property of a material, thus, the application range of the aluminium hydroxide nanometer strip is further enlarged.
Description
Technical field
The present invention relates to a kind of aluminium hydrate nano band and preparation method thereof.
Background technology
White lake is because its huge specific surface area and voidage can be used as catalyzer, support of the catalyst and sorbent material use.Yet its specific surface area and voidage are not only depended in the widespread use of white lake, and the appearance structure of white lake also to its application have very important significance (J Mater Sci 38,2673-2678).Bibliographical information is arranged; As precipitation agent, adopt homogeneous precipitation method to prepare white lake [J.Am Chem.Soc, 59 (7) with urea; 1190-1196; (1937)], having document to report for work thereafter again adopts homogeneous precipitation method to prepare aluminium hydrate nano rod fiber [MicroporousMesoporous Mater, 12339-44 (2009)] under the condition that PEG exists.But mostly the white lake for preparing in the prior art is unformed aluminium hydroxide, and its mechanical property is excellent inadequately.
Summary of the invention
The objective of the invention is to overcome the insufficient shortcoming of mechanical property of the white lake of prior art for preparing; Provide a kind of novel appearance structure to be the aluminium hydrate nano band of three-dimensional radial structure; To improve the mechanical property of aluminium hydrate nano band, further enlarge its range of application.
The invention provides a kind of aluminium hydrate nano band, wherein, the appearance structure of this aluminium hydrate nano band is three-dimensional radial structure.
The present invention also provides a kind of preparation method of aluminium hydrate nano band; Wherein, This preparation method comprises aluminum soluble salt and urea is dissolved in the pure water mixed solvent, then with the gained mixture successively temperature be under 340-373K and the 393-573K heating 6-15 hour with 2-10 hour.
Aluminium hydrate nano band of the present invention has the appearance structure of three-dimensional radial structure, uses aluminium hydrate nano band of the present invention as additive, can improve the mechanical property of material, thereby further enlarge the range of application of nano-aluminum hydroxide.The result of embodiment and Comparative Examples shows that the modulus of adding the Z 150PH of aluminium hydrate nano band of the present invention is 5GPa, and intensity is 150MPa, and mechanical property is superior to the not Z 150PH and the Z 150PH that adds unformed aluminium hydroxide of adding aluminum hydroxide nano belt.
Description of drawings
The XRD figure of the aluminium hydrate nano band that Fig. 1 makes for embodiment 1;
The TEM figure of the aluminium hydrate nano band that Fig. 2 makes for embodiment 1;
The TEM figure of the aluminium hydrate nano band that Fig. 3 makes for embodiment 2.
Embodiment
One side of the present invention provides a kind of aluminium hydrate nano band, and wherein, the appearance structure of this aluminium hydrate nano band is three-dimensional radial structure, shown in Fig. 2 and 3.
In the present invention, the length of said aluminium hydrate nano band can be 0.2-2 μ m, is preferably 0.5-1.5 μ m; Width can be 90-250nm, is preferably 100-200nm; Thickness can be 10-30nm, is preferably 15-25nm.
Another aspect of the present invention also provides a kind of preparation method of aluminium hydrate nano band; Wherein, This preparation method comprises aluminum soluble salt and urea is dissolved in the pure water mixed solvent, then with the gained mixture successively temperature be under 340-373K and the 393-573K heating 6-15 hour with 2-10 hour.The preparation method of aluminium hydrate nano band of the present invention carries out on the basis of reacting by heating through the popular response temperature 340K-373K at aluminum soluble salt and urea reaction; Further improve temperature of reaction to 393K-573K; And further reacting by heating 2-10 hour; Preferred 3-8 hour, under this kind reaction conditions, can generate the aluminium hydrate nano band that appearance structure is three-dimensional radial structure.
In preparation method of the present invention, can carry out quickly and efficiently in order to make reaction, to produce required aluminium hydrate nano band, the mol ratio of said aluminum soluble salt and said urea is preferably 1: 3-10, more preferably 1: 6-9.Under the preferable case, said aluminum soluble salt can be in aluminum chloride, Tai-Ace S 150 and the aluminum nitrate one or more.
In preparation method of the present invention, in the process of aluminum soluble salt and urea reaction, the reaction solvent of use is preferably pure water mixed solvent.For this reaction is more effectively carried out, the gross weight of said aluminum soluble salt and urea and the weight ratio of said pure water mixed solvent are preferably 0.005-0.1: 1, and 0.01-0.08 more preferably: 1.And in the said pure water mixed solvent, the volume ratio of alcohol and water is preferably 1: 9-9: 1, more preferably 1: 6-6: 1.The alcohol of said alcohol for dissolving each other with water, for example one or more in methyl alcohol, ethanol, Virahol, pinakon and the glycol ether.
The preparing method's of aluminium hydrate nano band of the present invention concrete steps are following:
(1) according to the above ratio a certain amount of aluminum soluble salt and urea are dissolved in the pure water mixed solvent, at room temperature stir to clarify;
(2) solution that step (1) is obtained is poured reaction kettle into and is carried out heat treated, and Heating temperature is 340K～373K, and be 6～15 hours heat-up time;
(3) mixture that step (2) is obtained is warming up to 393K～573K again, and the intensification post-heating time is 2-10 hour;
(4) mixture that step (3) is obtained is through centrifugal (1000rpm; 5min) separation or suction filtration; Obtain deposition; And with the redistilled water washing precipitation removing impurity, with the deposition of centrifugal back gained or the solid that filters the back gained with freeze drier-25 ℃ of dryings 12 hours down, obtain the aluminium hydrate nano band.
The appearance structure of aluminium hydrate nano band of the present invention is three-dimensional radial structure, uses aluminium hydrate nano band of the present invention can improve the mechanical property of material as additive, further enlarges its range of application.The result of embodiment and Comparative Examples shows; (modulus is 5GPa to add the mechanical property of the Z 150PH of aluminium hydrate nano band of the present invention; Intensity is 150MPa) (modulus is 3GPa all to be superior to not the Z 150PH of adding aluminum hydroxide nano belt; Intensity is 100MPa) and add the Z 150PH (modulus is 3.5GPa, and intensity is 102MPa) of unformed aluminium hydroxide.
Embodiment 1
Take by weighing 0.96g AlCl
36H
2O and 1.8g urea add the mixed solvent (pure water ratio is 1: 1) of 40ml second alcohol and water, and at room temperature stirring obtains settled solution, the solution of configuration is poured in the reaction kettle, and carried out heat treated, and temperature of reaction is 355K.React and again temperature is risen to 440K after 10 hours, intensification continued reaction 6 hours.Take out sample centrifugal (1000rpm, 5min) precipitation separation.To precipitate with freeze drier to descend dry 12 hours, obtain white powder at-25 ℃.
Embodiment 2
Take by weighing 1.36g Al
2(SO
4)
3Add in the mixed solvent of 40ml ethanol, pinakon and water (pure water ratio is 9: 1) with 2.4g urea; At room temperature stir and obtain settled solution; The solution of configuration is poured in the reaction kettle, and carried out heat treated, temperature of reaction is 340K; React and again temperature is risen to 393K after 15 hours, intensification continued reaction 10 hours.Take out sample from the suction filtration precipitation separation.To precipitate with freeze drier to descend dry 12 hours, obtain white powder at-25 ℃.
Embodiment 3
Take by weighing 0.12g AlCl
36H
2In the mixed solvent of O and 0.09g urea adding 40ml glycol ether and water (pure water ratio is 1: 9); At room temperature stir and obtain settled solution; The solution of configuration is poured in the reaction kettle, and carried out heat treated, temperature of reaction is 373K; React and again temperature is risen to 573K after 6 hours, intensification continued heating 2 hours.Take out sample centrifugal (1000rpm, 5min) precipitation separation.To precipitate with freeze drier to descend dry 12 hours, obtain white powder at-25 ℃.
Comparative Examples 1
Take by weighing 0.96g AlCl
36H
2O and 1.8g urea add the mixed solvent (pure water ratio is 1: 1) of 40ml second alcohol and water, and at room temperature stirring obtains settled solution, the solution of configuration is poured in the reaction kettle, and carried out heat treated, and temperature of reaction is 355K, reacts 10 hours.Take out sample centrifugal (1000rpm, 5min) precipitation separation.To precipitate with freeze drier to descend dry 12 hours, obtain white powder at-25 ℃.
Comparative Examples 2
Take by weighing 0.96g AlCl
36H
2O and 1.8g urea add the mixed solvent (pure water ratio is 1: 1) of 40ml second alcohol and water; At room temperature stirring obtains settled solution, the solution of configuration is poured in the reaction kettle, and carried out heat treated; Temperature of reaction is 355K, reacts 16 hours (being the summation of twice heat-up time among the embodiment 1).Take out sample centrifugal (1000rpm, 5min) precipitation separation.To precipitate with freeze drier to descend dry 12 hours, obtain white powder at-25 ℃.
Performance test
1, the appearance structure of aluminium hydrate nano band, size and crystalline phase
Embodiment 1-3 and the prepared white powder of Comparative Examples 1-2 are used the XRD determining crystalline phase, utilize TEM to show appearance structure, mean length, width and thickness.The result sees table 1.The XRD of embodiment 1 and TEM also like Fig. 1, shown in 2, the TEM of embodiment 2 is also as shown in Figure 3.TEM result shows that the prepared aluminium hydrate nano band of embodiment 1-3 begins growth from any and is three-dimensional radial distribution.
Table 1
| Sample | Appearance structure | Length (μ m) | Thickness (nm) | Width (nm) | Crystalline phase |
| Embodiment 1 | Three-dimensional radial | 0.6-1.2 | 17-30 | 100-150 | γ-AlOOH |
| Embodiment 2 | Three-dimensional radial | 0.22-0.5 | 21-31 | 168-248 | γ-AlOOH |
| Embodiment 3 | Three-dimensional radial | 0.553-1.97 | 10-16 | 90-163 | γ-AlOOH |
| Comparative Examples 1 | Nano particle | - | - | - | Unformed |
| Comparative Examples 2 | Nano particle | - | - | - | Unformed |
2, the aluminium hydrate nano band is to the influence of Z 150PH film dynamic performance
Take by weighing 2g Z 150PH (number-average molecular weight is 73000, alcoholysis degree be 98%) and be dissolved in the 10ml redistilled water, stir at 353K and obtain transparent settled solution.In this solution, add the prepared white lake of 0.16g embodiment 1 or Comparative Examples 2, stir it is uniformly dispersed, obtain dispersion liquid.Pour the transparent settled solution of Z 150PH of above-mentioned dispersion liquid and above-mentioned not aluminium hydroxide into film that petridish forms thickness 0.4-0.6mm respectively.(method of pressing GB2918 is regulated sample state and experimental standard environment respectively prepared film to be carried out the detection of mechanical property; Method by GB6672 is carried out thickness measurement and mechanical measurement, uses the omnipotent stretching experiment machine of CMT4104 type microcomputer control electronics to measure modulus and intensity).The result sees table 2.The modulus of adding the Z 150PH of aluminium hydrate nano band of the present invention is 5GPa, and intensity is 150MPa, is higher than the modulus and the intensity of Z 150PH with the Z 150PH that adds unformed aluminium hydroxide of adding aluminum hydroxide nano belt not respectively.
Table 2
| The white lake that adds | Modulus (GPa) | Intensity (MPa) |
| Do not have | ?3 | ?100 |
| Embodiment 1 | ?5 | ?150 |
| Comparative Examples 2 | ?3.5 | ?102 |
Claims (6)
1. an aluminium hydrate nano band is characterized in that, the appearance structure of this aluminium hydrate nano band is three-dimensional radial structure, and the length of said aluminium hydrate nano band is 0.2-2 μ m, and width is 90-250nm, and thickness is 10-30nm.
2. the preparation method of an aluminium hydrate nano band; It is characterized in that; This preparation method comprises aluminum soluble salt and urea is dissolved in the pure water mixed solvent; Be to heat under 340-373K and the 393-573K 6-15 hour and 2-10 hour in temperature successively with the gained mixture then, the gross weight of said aluminum soluble salt and urea and the weight ratio of said pure water mixed solvent are 0.005-0.1:1, and the mol ratio of said aluminum soluble salt and said urea is 1:3-10.
3. preparation method according to claim 2, wherein, said aluminum soluble salt is one or more in aluminum chloride, Tai-Ace S 150 and the aluminum nitrate.
4. preparation method according to claim 2, wherein, in the said pure water mixed solvent, the volume ratio of alcohol and water is 1:9-9:1.
5. preparation method according to claim 4, wherein, the alcohol of said alcohol for dissolving each other with water.
6. preparation method according to claim 5, wherein, said alcohol is one or more in methyl alcohol, ethanol, Virahol, pinakon and the glycol ether.
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| CN102101685B true CN102101685B (en) | 2012-11-28 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1608997A (en) * | 2004-10-27 | 2005-04-27 | 上海大学 | Prepn process of nano aluminium hydroxide |
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|---|---|---|---|---|
| CN1608997A (en) * | 2004-10-27 | 2005-04-27 | 上海大学 | Prepn process of nano aluminium hydroxide |
Non-Patent Citations (1)
| Title |
|---|
| J.L. SHI et al..FORMATION OF MONOSIZED SPHERICAL ALUMINUM HYDROXIDE PARTICLES BY UREA METHOD.《Solid State Ionics》.1989,第32/33卷第537-543页. * |
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