CN102190671B - Method for preparing zinc-1-(2-pyridylazo)-2-naphthol nano-belts - Google Patents
Method for preparing zinc-1-(2-pyridylazo)-2-naphthol nano-belts Download PDFInfo
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- CN102190671B CN102190671B CN201110065094.7A CN201110065094A CN102190671B CN 102190671 B CN102190671 B CN 102190671B CN 201110065094 A CN201110065094 A CN 201110065094A CN 102190671 B CN102190671 B CN 102190671B
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- beta naphthal
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Abstract
The invention aims to provide a method for preparing zinc-1-(2-pyridylazo)-2-naphthol nano-belts, which comprises the following steps of: mixing absolute ethanol with water in a certain volume ratio to obtain a solvent A; dissolving 1-(2-pyridylazo)-2-naphtho powder in the solvent A to obtain solution B; dissolving a proper amount of zinc acetate dehydrate in the solvent A to obtain solution C; mixing the solution B and the solution C, and transferring to a high pressure reaction kettle; reacting at the temperature of between 120 and 140DEG C for 12 to 48 hours; and after the reaction is finished, performing centrifugal separation on products, washing a precipitate by using distilled water and ethanol in turn, and drying the obtained precipitate in vacuum to obtain reddish brown zinc-1-(2-pyridylazo)-2-naphthol powder. The preparation method is easy to implement and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of zinc-1-(2-pyridylazo)-beta naphthal (Zn (Pan)
2) preparation method of nano belt.Specifically, be to utilize solvent-thermal method to prepare zinc-1-(2-pyridylazo)-beta naphthal nano belt.
Background technology
Monodimension nanometer material is due to its unique structure and good character, at single-electronic transistor, field ballistic transistor, transmission in nanoelectronics, laser, the aspects such as detection have a wide range of applications [referring to (a) S.J.Tans, M.H.Devoret, H.Dai, A.Thess, R.E.Smalley, L.J.Geerligs, C.Dekker, Nature, 1997, 386, 474. (b) J.Hu, T.W.Odom, C.M.Lieber, Acc.Chem.Res.1999, 32, 435. (c) M.Morales, C.M.Lieber, Science, 1998, 279, 208. (d) J.Kong, N.R.Franklin, C.Zhou, M.G.Chapline, S.Peng, K.J.Cho, H.Dai, Science 2000, 287, 622.].Current most bibliographical information mainly concentrates on the synthetic and property research of inorganic nano material, and less to the preparation of organic nano material and property research.Organic nano material is day by day subject to people and payes attention to owing to having excellent photoelectric property.For example, people have utilized a microemulsion method to synthesize 2-(anthracene-9-yl)-9,9 '-dioctyl fluorene nanoparticle, and can be used as the luminous ink [L.Zhao of spray ink Printing, Z.Lei, X.Li, S.Li, J.Xu, B.Peng and W.Huang, Chem.Phys.Lett.2006,420,480.].Therefore, the preparation of organic nano material has become the focus that people pay close attention to.
Zinc-1-(2-pyridylazo)-beta naphthal (Zn (Pan) 2) is a kind of organic coordination compound material, and it has the π-electron coupling of high degree of polarization, has been used to the non-linear optical fields such as organic light emission switch and optical limiter part.Along with the development of current nanosecond science and technology, the morphology control of Zn (Pan) 2 nano materials has been become to one of study hotspot.At present, utilized sonochemical method to prepare Zn (Pan) 2 nanometer rod [referring to (a) H.C.Pan, F.P.Liang, C.J.Mao, J.J.Zhu, H.Y.Chen, Nanotechnology 2007,18,195606.], still there is not yet the report of Zn (Pan) 2 nano belt.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of zinc-1-(2-pyridylazo)-beta naphthal nano belt, it comprises the following steps, and dehydrated alcohol and water are mixed by certain volume ratio, obtains solvent orange 2 A; 1-(2-pyridylazo)-beta naphthal powder dissolution, in solvent orange 2 A, is obtained to solution B; Appropriate Zinc diacetate dihydrate is dissolved in solvent orange 2 A, obtains solution C; By after solution B and solution C mixing, move in autoclave; At the temperature of 120 to 140 ℃, react 12 to 48 hours; After reaction finishes, by product centrifugation, with distilled water and ethanol washing precipitation successively, the throw out of gained is placed under vacuum and is dried, obtain zinc-1-(2-the pyridylazo)-beta naphthal powder of reddish-brown.
In described A solvent, alcohol concn is 25% to 50% (volume ratio).
The concentration of 1-in described B solution (2-pyridylazo)-beta naphthal is 149 mg/ml.
In described C solution, the concentration range of Zinc diacetate dihydrate is 110 mg/ml.
Described autoclave is band teflon-lined stainless steel autogenous pressure reactor.
Zinc-1-of the present invention (2-pyridylazo)-beta naphthal is through ultimate analysis and infrared measurement, and result shows that it is zinc-1-(2-pyridylazo)-beta naphthal.By stereoscan photograph, observing the prepared zinc-1-of the inventive method (2-pyridylazo)-beta naphthal nano belt is that thickness is 10 nanometer to 30 nanometers, and width is 50 nanometer to 200 nanometers, and length is 500 nanometers to 1 micron.
Preparation method's raw material of zinc-1-of the present invention (2-pyridylazo)-beta naphthal nano belt is simple and easy to get, consuming time short, simple to operate, is suitable for suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is infrared spectra (FTIR) figure of zinc-1-(2-pyridylazo)-beta naphthal of preparing of first embodiment of the invention.
Fig. 2 is the stereoscan photograph (SEM) of first embodiment of the invention zinc-1-(2-pyridylazo)-beta naphthal.
Embodiment
The preparation method who the object of this invention is to provide a kind of zinc-1-(2-pyridylazo)-beta naphthal nano belt, its concrete steps comprise: mix dehydrated alcohol and water (1) by certain volume ratio, obtain solvent orange 2 A; (2) by 1-(2-pyridylazo)-beta naphthal powder dissolution in solvent orange 2 A, obtaining 1-(2-pyridylazo)-beta naphthal concentration is the solution B of 149 mg/ml; (3) Zinc diacetate dihydrate is dissolved in A, obtains the solution C that Zinc diacetate dihydrate concentration is 110 mg/ml; (4) by after solution B and solution C mixing, move in autoclave; (5), at the temperature of 120 to 140 ℃, react 12 to 48 hours; (6) after reaction finishes, by product centrifugation, with distilled water and ethanol washing precipitation successively, the throw out of gained is placed under vacuum and is dried, obtain zinc-1-(2-the pyridylazo)-beta naphthal powder of reddish-brown.
Below in conjunction with accompanying drawing, the embodiment of the present invention is described in further detail.
Embodiment mono-:
10 milliliters of dehydrated alcohols and 30 ml distilled waters are mixed, obtain 25% alcohol solvent, 0.298 gram of 1-(2-pyridylazo)-beta naphthal is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, 0.220 gram of Zinc diacetate dihydrate is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, after above-mentioned two solution are mixed, move in autoclave, be then warming up to 120 ℃ and isothermal reaction 24 hours.After reaction finishes, by product centrifugation, with distilled water and ethanol washing precipitation successively, the throw out of gained is placed under vacuum and is dried, obtain reddish-brown powder, obtain zinc-1-(2-pyridylazo)-beta naphthal nano belt.Refer to Zn (Pan) prepared by Fig. 1 the first embodiment
2infrared spectrogram, by ultimate analysis and the prepared product of the known the inventive method of Fig. 1, be zinc-1-(2-pyridylazo)-beta naphthal.Refer to Zn (Pan) prepared by Fig. 2 the first embodiment
2scanning electron microscope (SEM) photograph.Observing the prepared zinc-1-of the inventive method (2-pyridylazo)-beta naphthal nano belt is that thickness is 10 nanometer to 30 nanometers, and width is 50 nanometer to 200 nanometers, and length is 500 nanometers to 1 micron.
Embodiment bis-
20 milliliters of dehydrated alcohols and 20 ml distilled waters are mixed, obtain 50% alcohol solvent, 0.298 gram of 1-(2-pyridylazo)-beta naphthal is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, 0.220 gram of Zinc diacetate dihydrate is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, after above-mentioned two solution are mixed, move in autoclave, be then warming up to 120 ℃ and isothermal reaction 24 hours.Other conditions of preparation, with embodiment 1, equally also obtain size and homoeomorphic product.
Embodiment tri-
10 milliliters of dehydrated alcohols and 30 ml distilled waters are mixed, obtain 25% alcohol solvent, 0.298 gram of 1-(2-pyridylazo)-beta naphthal is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, 0.220 gram of Zinc diacetate dihydrate is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, after above-mentioned two solution are mixed, move in autoclave, be then warming up to 120 ℃ and isothermal reaction 12 hours.Other conditions of preparation, with embodiment 1, equally also obtain size and homoeomorphic product.
Embodiment tetra-
10 milliliters of dehydrated alcohols and 30 ml distilled waters are mixed, obtain 25% alcohol solvent, 0.298 gram of 1-(2-pyridylazo)-beta naphthal is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, 0.220 gram of Zinc diacetate dihydrate is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, after above-mentioned two solution are mixed, move in autoclave, be then warming up to 120 ℃ and isothermal reaction 48 hours.Other conditions of preparation, with embodiment 1, equally also obtain size and homoeomorphic product.
Embodiment five
20 milliliters of dehydrated alcohols and 20 ml distilled waters are mixed, obtain 50% alcohol solvent, 0.298 8 gram of 1-(2-pyridylazo)-beta naphthal is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, 0.220 gram of Zinc diacetate dihydrate is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, after above-mentioned two solution are mixed, move in autoclave, be then warming up to 140 ℃ and isothermal reaction 12 hours.Other conditions of preparation, with embodiment 1, equally also obtain size and homoeomorphic product.
Embodiment six
10 milliliters of dehydrated alcohols and 30 ml distilled waters are mixed, obtain 25% alcohol solvent, 0.298 gram of 1-(2-pyridylazo)-beta naphthal is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, 0.220 gram of Zinc diacetate dihydrate is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, after above-mentioned two solution are mixed, move in autoclave, be then warming up to 140 ℃ and isothermal reaction 24 hours.Other conditions of preparation, with embodiment 1, equally also obtain size and homoeomorphic product.
Claims (2)
1. a preparation method for zinc-1-(2-pyridylazo)-beta naphthal nano belt, it comprises the following steps:
Dehydrated alcohol and water are mixed by certain volume ratio, the concentration range of dehydrated alcohol is counted between 25% to 50% with volume ratio, obtain solvent orange 2 A;
By 1-(2-pyridylazo)-beta naphthal powder dissolution, in solvent orange 2 A, making the concentration of 1-(2-pyridylazo)-beta naphthal is 149 mg/ml, obtains solution B;
Zinc diacetate dihydrate is dissolved in solvent orange 2 A, and making the concentration of Zinc diacetate dihydrate is 110 mg/ml, obtains solution C;
By after solution B and solution C mixing, move in autoclave, at the temperature of 120 to 140 ℃, react 12 to 48 hours, after reaction finishes, by product centrifugation, with distilled water and ethanol washing precipitation successively, the throw out of gained is placed under vacuum and is dried, obtain zinc-1-(2-the pyridylazo)-beta naphthal nano belt of reddish-brown.
2. the preparation method of zinc-1-according to claim 1 (2-pyridylazo)-beta naphthal nano belt, it is characterized in that: the thickness of described zinc-1-(2-pyridylazo)-beta naphthal nano belt is 10 nanometer to 30 nanometers, width is 50 nanometer to 200 nanometers, and length is 500 nanometers to 1 micron.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1743274A (en) * | 2005-07-18 | 2006-03-08 | 南京大学 | Ag2V4011 nano band and its preparing method |
| CN101844808A (en) * | 2010-06-03 | 2010-09-29 | 安徽大学 | Method for preparing bismuthyl chloride nano-flower |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1743274A (en) * | 2005-07-18 | 2006-03-08 | 南京大学 | Ag2V4011 nano band and its preparing method |
| CN101844808A (en) * | 2010-06-03 | 2010-09-29 | 安徽大学 | Method for preparing bismuthyl chloride nano-flower |
Non-Patent Citations (2)
| Title |
|---|
| Hong-Cheng Pan.Sonochemical synthesis and resonance light scattering effect of Zn(II)bis(1-(2-pyridylazo)-2-naphthol) nanorods.《Nanotechnology》.2007,第18卷(第19期),第1-6页. |
| Sonochemical synthesis and resonance light scattering effect of Zn(II)bis(1-(2-pyridylazo)-2-naphthol) nanorods;Hong-Cheng Pan;《Nanotechnology》;20071231;第18卷(第19期);第1-6页 * |
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