CN100339305C - Microwave synthesis preparation method for praseodymium hydroxide nanometer rod - Google Patents
Microwave synthesis preparation method for praseodymium hydroxide nanometer rod Download PDFInfo
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- CN100339305C CN100339305C CNB2005100621760A CN200510062176A CN100339305C CN 100339305 C CN100339305 C CN 100339305C CN B2005100621760 A CNB2005100621760 A CN B2005100621760A CN 200510062176 A CN200510062176 A CN 200510062176A CN 100339305 C CN100339305 C CN 100339305C
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- praseodymium
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- nanometer rod
- potassium hydroxide
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Abstract
The present invention discloses a preparation method of a praseodymium oxide (Pr (OH) 3) nanometer rod by microwave synthesis, which comprises the following steps: (1) dissolving praseodymium oxide powder in an HNO3 solution with a concentration of 10 to 20% to form a solution, or dissolving praseodymium salt in water to form a solution; (2) then, dripping a potassium hydroxide solution in the solution, controlling the pH value between 11 and 13, and producing gelatinous materials; (3) mixing the gelatinous materials with the potassium hydroxide solution during stirring so that the concentration of praseodymium in the final mixture is from 0.01 to 0.05 mol/L and the concentration of potassium hydroxide is from 1 to 11 mol/l; (4)finally, heating the mixture in a microwave oven for 10 to 60 minutes under a reflux condition, and cooling, separating, cleaning and drying the mixture to obtain the Pr (OH) 3 nanometer rod. The average diameter of the nanometer rod is from 7 to 14 nanometers, and the average length is from 26 to 83 nanometers. The microwave radiation heating technique has the advantages of high speed, uniformity, energy saving and high efficiency; reaction speed and synthesis efficiency can be increased.
Description
Technical field
The present invention relates to the preparation of nano material, relate in particular to the method for the synthetic praseodymium hydroxide nanometer rod of a kind of microwave, belong to technical field of inorganic chemical industry.
Background technology
Rare-earth compound has many special physics, chemistry, electronics, magnetics and optical property, it is had in fields such as magneticsubstance, energy-accumulating material, catalysis, indicating meter and tribology widely use.Compare with body phase material, nano level rare earth compound will make it be further enhanced at aspect of performance, have better catalytic performance, hydrogen storage performance, electricity and optical property and nanometer size effect.China has abundant rare earth resources, and the nano material of research and preparation rare earth compound has important scientific meaning and using value to the in-depth utilization of rare earth resources.
Since 1991 found carbon nanotube, monodimension nanometer material such as nanotube, nano wire, nanometer rod and nanofiber etc. were because its character such as light, electricity, magnetic and potential application prospect thereof with uniqueness causes global extensive concern.As a kind of important wet chemical synthesis, the hydro-thermal synthetic technology is widely used in the synthetic of multiple nano material, comprising nano materials such as synthesis of nano line and nanometer rod. Li Yadongs etc. [1] have been reported the method with hydrothermal technique synthesizing rare-earth hydroxide nanorod and nano wire, and disclose a kind of method [2] of synthesizing rare-earth hydroxide nano line.The method characteristics that they proposed are to carry out hydro-thermal reaction in airtight container, and temperature is at 100～250 ℃, and the time was at 7～24 hours.But this long-time heating to hydrothermal reaction kettle need consume more electric energy, has not only wasted the energy, has also reduced combined coefficient.
The carry out microwave radiation heating technology has advantage quick, even, energy-conservation and that efficient is high.It can make speed of response improve 10～100 times.Therefore, synthetic and nano material has obtained using widely in synthetic microwave heating technique at organic chemistry.Microwave heating technique successfully has been applied to the synthetic of metal nano material, metal oxide nano-material and nano metal sulfide material.But up to the present, the document and the patent of synthetic praseodymium hydroxide nanometer rod yet there are no open report fast with the carry out microwave radiation heating technology.
The main reference document:
[1]Xun?Wang，Yadong?Li.Fullerene-Like?Rare-Earth?Nanoparticles.Angew.Chem.Int.Ed.2003，42，3497-3500
[2] Li Yadong, king's instruction, the method for synthesizing rare-earth oxyhydroxide or oxide nano thread and powder thereof, CN1182038C
Summary of the invention
The object of the present invention is to provide the method for the synthetic praseodymium hydroxide nanometer rod of a kind of microwave.
The step of method is as follows:
1) with the Praseodymium trioxide powder dissolution at 10～20%HNO
3In the solution, form solution; Perhaps the salt of praseodymium is dissolved in and forms solution in the water;
2) drip potassium hydroxide solution then in above-mentioned solution, control pH value generates jelly between 11～13;
3) under agitation condition, above-mentioned jelly is mixed with potassium hydroxide solution, in the end the concentration in the mixture is at 0.01～0.05mol/L to make praseodymium, and the concentration of potassium hydroxide is at 1～11mol/L;
4) at last with said mixture microwave heating 10～60 minutes in microwave oven under refluxad, cooling, separation, washing, drying obtain the nanometer rod of praseodymium hydroxide.Its mean diameter is between 7～14 nanometers, and mean length is between 26～83 nanometers.
The salt of described praseodymium is praseodymium nitrate or praseodymium chloride.
Method of the present invention compared with the prior art has following advantage:
The method of prior art synthesizing rare-earth hydroxide nanorod or nano wire mainly adopts solvent thermal process, this method need be carried out heating and the insulation of long period to airtight hydrothermal reaction kettle, generally need 7～24 hours, consumed more electric energy, so not only waste the energy, and reduced combined coefficient.
Employing carry out microwave radiation heating technology of the present invention has fast, evenly, save energy and efficient high advantage, fast reaction speed improves combined coefficient greatly.
Description of drawings
Accompanying drawing is the transmission electron microscope photo of the synthetic praseodymium hydroxide nanometer rod of microwave.
Embodiment
The present invention is at 10～20%HNO with the Praseodymium trioxide powder dissolution
3Form solution in the solution; Perhaps the salt of praseodymium is dissolved in and forms solution in the water, in above-mentioned solution, drip potassium hydroxide solution then, adjust pH value between 11～13, the precipitation of generation jelly.Under agitation condition, the potassium hydroxide solution of resulting jelly and different concns is mixed, in the end the concentration in the mixture is at 0.01～0.05mol/L to make praseodymium, and the concentration of potassium hydroxide is at 1～11mol/L.At last with the microwave heating 10～60 minutes in microwave oven under refluxad of this mixture, naturally cooling then is with collecting behind centrifugation and the deionized water thorough washing and drying can obtain praseodymium hydroxide nanometer rod.The salt of the praseodymium that the present invention adopts is praseodymium nitrate and praseodymium chloride.
The reaction process of the synthetic praseodymium hydroxide nanometer rod of the present invention can be expressed as follows:
Pr
2O
3+6HNO
3＝2Pr
3++6NO
3 -+3H
2O
Pr
3++ 3OH
-=Pr (OH)
3(gelatinous precipitate) (the pH value is between 11～13)
Pr (OH)
3(gelatinous precipitate)=Pr (OH)
3(nanometer rod) (through after the microwave treatment)
Embodiment 1:
The 0.82g Praseodymium trioxide is dissolved in the HNO of 30mL 20%
3In the solution, form clear soln.The KOH solution of dropping 10% transfers to the pH value about 13 in this solution, generates gelationus throw out.Under agitation jelly and dense potassium hydroxide solution are mixed, the volume of final mixture is 100 mL, and the concentration of praseodymium wherein is 0.05mol/L, and the concentration of potassium hydroxide is 11mol/L.Last mixture is transferred in the 250ml round-bottomed flask, under refluxad heated 60min in the microwave oven, behind the naturally cooling, drying obtains praseodymium hydroxide nanometer rod with collecting also behind centrifugation and the deionized water thorough washing.Transmission electron microscope observing shows that praseodymium hydroxide nanometer rod has uniform diameter, and mean diameter is 14 nanometers, and mean length is 83 nanometers.The transmission electron microscope photo of the synthetic praseodymium hydroxide nanometer rod of microwave is seen Fig. 1.
Embodiment 2:
The 0.82g Praseodymium trioxide is dissolved in the HNO of 30mL 20%
3In the solution, form clear soln.The KOH solution of dropping 10% transfers to the pH value about 12 in this solution, generates gelationus throw out.Under agitation jelly and dense potassium hydroxide solution are mixed, the volume of final mixture is 100mL, and the concentration of praseodymium wherein is 0.05mol/L, and the concentration of potassium hydroxide is 11mol/L.Last mixture is transferred in the 250ml round-bottomed flask, under refluxad heated 10min in the microwave oven, behind the naturally cooling, drying obtains praseodymium hydroxide nanometer rod with collecting also behind centrifugation and the deionized water thorough washing.Transmission electron microscope observing shows that the praseodymium hydroxide nanometer rod mean diameter is 9 nanometers, and mean length is 43 nanometers.
Embodiment 3:
The 0.50g Praseodymium trioxide is dissolved in the HNO of 30mL20%
3In the solution, form clear soln.The KOH solution of dropping 10% transfers to the pH value about 12 in this solution, generates gelationus throw out.Under agitation jelly and dense potassium hydroxide solution are mixed, the volume of final mixture is 100mL, and the concentration of praseodymium wherein is 0.03mol/L, and the concentration of potassium hydroxide is 5mol/L.Last mixture is transferred in the 250ml round-bottomed flask, under refluxad heated 40min in the microwave oven, behind the naturally cooling, drying obtains praseodymium hydroxide nanometer rod with collecting also behind centrifugation and the deionized water thorough washing.Transmission electron microscope observing shows that the praseodymium hydroxide nanometer rod mean diameter is 11 nanometers, and mean length is 32 nanometers.
Embodiment 4
The 0.164g Praseodymium trioxide is dissolved in the HNO3 solution of 30mL 10%, forms clear soln.The KOH solution of dropping 10% transfers to the pH value about 11 in this solution, generates gelationus throw out.Under agitation jelly and dense potassium hydroxide solution are mixed, the volume of final mixture is 100mL, and the concentration of praseodymium wherein is 0.01mol/L, and the concentration of potassium hydroxide is 1mol/L.Last mixture is transferred in the 250ml round-bottomed flask, under refluxad heated 20min in the microwave oven, behind the naturally cooling, drying obtains praseodymium hydroxide nanometer rod with collecting also behind centrifugation and the deionized water thorough washing.Transmission electron microscope observing shows that the praseodymium hydroxide nanometer rod mean diameter is 7 nanometers, and mean length is 26 nanometers.
Embodiment 5:
0.003 molar nitric acid praseodymium is dissolved in the 30mL water, forms clear soln.The KOH solution of dropping 10% transfers to the pH value about 12 in this solution, generates gelationus throw out.Under agitation jelly and dense potassium hydroxide solution are mixed, the volume of final mixture is 100mL, and the concentration of praseodymium wherein is 0.03mol/L, and the concentration of potassium hydroxide is 9mol/L.Last mixture is transferred in the 250ml round-bottomed flask, under refluxad heated 50min in the microwave oven, behind the naturally cooling, drying obtains praseodymium hydroxide nanometer rod with collecting also behind centrifugation and the deionized water thorough washing.Transmission electron microscope observing shows that the praseodymium hydroxide nanometer rod mean diameter is 12 nanometers, and mean length is 53 nanometers.
Embodiment 6:
0.002 mole of praseodymium chloride is dissolved in the 30mL water, forms clear soln.The KOH solution of dropping 10% transfers to the pH value about 13 in this solution, generates gelationus throw out.Under agitation jelly and dense potassium hydroxide solution are mixed, the volume of final mixture is 100mL, and the concentration of praseodymium wherein is 0.02mol/L, and the concentration of potassium hydroxide is 2mol/L.Last mixture is transferred in the 250ml round-bottomed flask, under refluxad heated 60min in the microwave oven, behind the naturally cooling, drying obtains praseodymium hydroxide nanometer rod with collecting also behind centrifugation and the deionized water thorough washing.Transmission electron microscope observing shows that the praseodymium hydroxide nanometer rod mean diameter is 10 nanometers, and mean length is 29 nanometers.
Claims (2)
1. the method for the synthetic praseodymium hydroxide nanometer rod of a microwave is characterized in that the step of method is as follows:
1) with the Praseodymium trioxide powder dissolution at 10～20%HNO
3In the solution, form solution; Perhaps the salt of praseodymium is dissolved in and forms solution in the water;
2) drip potassium hydroxide solution then in above-mentioned solution, control pH value generates jelly between 11～13;
3) under agitation condition, above-mentioned jelly is mixed with potassium hydroxide solution, in the end the concentration in the mixture is at 0.01～0.05mol/L to make praseodymium, and the concentration of potassium hydroxide is at 1～11mol/L;
4) at last with said mixture microwave heating 10～60 minutes in microwave oven under refluxad, cooling, separation, washing, drying obtain the nanometer rod of praseodymium hydroxide.
2. the method for the synthetic praseodymium hydroxide nanometer rod of a kind of microwave according to claim 1, the salt that it is characterized in that described praseodymium is praseodymium nitrate or praseodymium chloride.
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|---|---|---|---|
| CNB2005100621760A CN100339305C (en) | 2005-12-23 | 2005-12-23 | Microwave synthesis preparation method for praseodymium hydroxide nanometer rod |
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| CN100339305C true CN100339305C (en) | 2007-09-26 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010501002A (en) * | 2006-08-14 | 2010-01-14 | マヨ ファウンデイション フォア メディカル エデュケイション アンド リサーチ | Rare earth nanoparticles |
| CN102942203B (en) * | 2012-11-14 | 2014-04-16 | 陕西科技大学 | Preparation method of bar-shaped lanthanum hydroxide nanocrystal |
| CN106241852A (en) * | 2016-06-22 | 2016-12-21 | 中山大学 | A kind of Pr (OH)3the preparation method of monodimension nano stick |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62132731A (en) * | 1985-12-03 | 1987-06-16 | Seitetsu Kagaku Co Ltd | Production of rare earth metal oxide |
| CN1403375A (en) * | 2002-10-11 | 2003-03-19 | 清华大学 | Synthesis process of nanostring and nanopowder of RE hydroxide or oxide |
| CN1424257A (en) * | 2003-01-10 | 2003-06-18 | 清华大学 | Rare earth hydroxide nano tubes and synthesis of serial rare earth compounds nano tubes |
-
2005
- 2005-12-23 CN CNB2005100621760A patent/CN100339305C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62132731A (en) * | 1985-12-03 | 1987-06-16 | Seitetsu Kagaku Co Ltd | Production of rare earth metal oxide |
| CN1403375A (en) * | 2002-10-11 | 2003-03-19 | 清华大学 | Synthesis process of nanostring and nanopowder of RE hydroxide or oxide |
| CN1424257A (en) * | 2003-01-10 | 2003-06-18 | 清华大学 | Rare earth hydroxide nano tubes and synthesis of serial rare earth compounds nano tubes |
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