CN102190671A - 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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- CN102190671A CN102190671A CN2011100650947A CN201110065094A CN102190671A CN 102190671 A CN102190671 A CN 102190671A CN 2011100650947 A CN2011100650947 A CN 2011100650947A CN 201110065094 A CN201110065094 A CN 201110065094A CN 102190671 A CN102190671 A CN 102190671A
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- pyridylazo
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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 owing to its particular structure and good character, at single-electronic transistor, the field ballistic transistor, transmission in the nanoelectronics, laser, 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.].Present most bibliographical information mainly concentrates on the synthetic and property research of inorganic nano material, and less to the preparation and the property research of organic nano material.Organic nano material is subjected to people day by day and payes attention to owing to have excellent photoelectric property.For example, people utilized the micro emulsion method synthesized 2-(anthracene-9-yl)-9,9 '-the 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 non-linear optical fields such as organic light emission switch and optical limiter spare.Along with the development of current nanosecond science and technology, the morphology control of Zn (Pan) 2 nano materials has been become one of research focus.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 do not see the report of Zn (Pan) 2 nano belt as yet.
Summary of the invention
The purpose of this invention is to provide the preparation method of a kind of zinc-1-(2-pyridylazo)-beta naphthal nano belt, it may further comprise the 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 solution B; An amount of Zinc diacetate dihydrate is dissolved in the solvent orange 2 A, obtains solution C; After solution B and solution C mixing, move in the autoclave; Under 120 to 140 ℃ temperature, reacted 12 to 48 hours; After reaction finishes,,, the throw out of gained is placed under the vacuum dry, obtain zinc-1-(2-the pyridylazo)-beta naphthal powder of reddish-brown with distilled water and ethanol washing precipitation successively with the product centrifugation.
Alcohol concn is 25% to 50% (volume ratio) in the described A solvent.
The concentration of 1-in the described B solution (2-pyridylazo)-beta naphthal is 149 mg/ml.
The concentration range of Zinc diacetate dihydrate is 110 mg/ml in the described C solution.
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 the 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 be simple and easy to, weak point consuming time, simple to operate, be suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is infrared spectra (FTIR) figure of zinc-1-(2-the pyridylazo)-beta naphthal of first embodiment of the invention preparation.
Fig. 2 is the stereoscan photograph (SEM) of first embodiment of the invention zinc-1-(2-pyridylazo)-beta naphthal.
Embodiment
The purpose of this invention is to provide the preparation method of 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) with 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 among the A, obtains the solution C that Zinc diacetate dihydrate concentration is 110 mg/ml; (4) with after solution B and the solution C mixing, move in the autoclave; (5) under 120 to 140 ℃ temperature, reacted 12 to 48 hours; (6) after reaction finishes,,, the throw out of gained is placed under the vacuum dry, obtain zinc-1-(2-the pyridylazo)-beta naphthal powder of reddish-brown with distilled water and ethanol washing precipitation successively with the product centrifugation.
Below in conjunction with accompanying drawing the embodiment of the invention is described in further detail.
Embodiment one:
10 milliliters of dehydrated alcohols and 30 ml distilled waters are mixed, obtain 25% alcohol solvent, 0.298 gram 1-(2-pyridylazo)-beta naphthal is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, 0.220 the gram Zinc diacetate dihydrate is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, after above-mentioned two solution mixing, move in the autoclave, be warming up to 120 ℃ and isothermal reaction then 24 hours.After reaction finishes,,, the throw out of gained is placed under the vacuum dry, obtain the reddish-brown powder, promptly obtain zinc-1-(2-pyridylazo)-beta naphthal nano belt with distilled water and ethanol washing precipitation successively with the product centrifugation.See also the Zn (Pan) of Fig. 1 first embodiment preparation
2Infrared spectrogram, by ultimate analysis and Fig. 1 as can be known the prepared product of the inventive method be zinc-1-(2-pyridylazo)-beta naphthal.See also the Zn (Pan) of Fig. 2 first embodiment preparation
2Sem 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 two
20 milliliters of dehydrated alcohols and 20 ml distilled waters are mixed, obtain 50% alcohol solvent, 0.298 gram 1-(2-pyridylazo)-beta naphthal is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, 0.220 the gram Zinc diacetate dihydrate is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, after above-mentioned two solution mixing, move in the autoclave, be warming up to 120 ℃ and isothermal reaction then 24 hours.Other conditions of preparation equally also obtain size and homoeomorphic product with embodiment 1.
Embodiment three
10 milliliters of dehydrated alcohols and 30 ml distilled waters are mixed, obtain 25% alcohol solvent, 0.298 gram 1-(2-pyridylazo)-beta naphthal is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, 0.220 the gram Zinc diacetate dihydrate is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, after above-mentioned two solution mixing, move in the autoclave, be warming up to 120 ℃ and isothermal reaction then 12 hours.Other conditions of preparation equally also obtain size and homoeomorphic product with embodiment 1.
Embodiment four
10 milliliters of dehydrated alcohols and 30 ml distilled waters are mixed, obtain 25% alcohol solvent, 0.298 gram 1-(2-pyridylazo)-beta naphthal is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, 0.220 the gram Zinc diacetate dihydrate is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, after above-mentioned two solution mixing, move in the autoclave, be warming up to 120 ℃ and isothermal reaction then 48 hours.Other conditions of preparation equally also obtain size and homoeomorphic product with embodiment 1.
Embodiment five
20 milliliters of dehydrated alcohols and 20 ml distilled waters are mixed, obtain 50% alcohol solvent, 0.298 8 gram 1-(2-pyridylazo)-beta naphthal is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, 0.220 the gram Zinc diacetate dihydrate is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, after above-mentioned two solution mixing, move in the autoclave, be warming up to 140 ℃ and isothermal reaction then 12 hours.Other conditions of preparation equally also obtain size and homoeomorphic product with embodiment 1.
Embodiment six
10 milliliters of dehydrated alcohols and 30 ml distilled waters are mixed, obtain 25% alcohol solvent, 0.298 gram 1-(2-pyridylazo)-beta naphthal is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, 0.220 the gram Zinc diacetate dihydrate is dissolved in the alcohol solvent of 20 milliliters of above-mentioned configurations, after above-mentioned two solution mixing, move in the autoclave, be warming up to 140 ℃ and isothermal reaction then 24 hours.Other conditions of preparation equally also obtain size and homoeomorphic product with embodiment 1.
Claims (5)
1. the preparation method of a zinc-1-(2-pyridylazo)-beta naphthal nano belt, it may further comprise the steps:
Dehydrated alcohol and water are mixed by certain volume ratio, obtain solvent orange 2 A;
1-(2-pyridylazo)-beta naphthal powder dissolution in solvent orange 2 A, is obtained solution B;
Zinc diacetate dihydrate is dissolved among the A, obtains solution C;
After solution B and solution C mixing, move in the autoclave;
Under 120 to 140 ℃ temperature, reacted 12 to 48 hours;
After reaction finishes,,, the throw out of gained is placed under the vacuum dry, obtain zinc-1-(2-the pyridylazo)-beta naphthal powder of reddish-brown with distilled water and ethanol washing precipitation successively with the product centrifugation.
2. the preparation method of zinc-1-according to claim 1 (2-pyridylazo)-beta naphthal nano belt is characterized in that: the concentration range of alcohol solvent is between 25% to 50% (volume ratio) in the described A solution.
3. the preparation method of zinc-1-according to claim 1 (2-pyridylazo)-beta naphthal nano belt is characterized in that: the concentration of 1-in the described B solution (2-pyridylazo)-beta naphthal is 149 mg/ml.
4. the preparation method of zinc-1-according to claim 1 (2-pyridylazo)-beta naphthal nano belt is characterized in that: the concentration of Zinc diacetate dihydrate is 110 mg/ml in the described C solution.
5. the preparation method of zinc-1-according to claim 1 (2-pyridylazo)-beta naphthal nano belt is characterized in that: it 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.
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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 (1)
| Title |
|---|
| HONG-CHENG PAN: "Sonochemical synthesis and resonance light scattering effect of Zn(II)bis(1-(2-pyridylazo)-2-naphthol) nanorods", 《NANOTECHNOLOGY》, vol. 18, no. 19, 31 December 2007 (2007-12-31), pages 1 - 6, XP020119129, DOI: doi:10.1088/0957-4484/18/19/195606 * |
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