CN101624211B - Method for preparing lead hydroxide nano-rod based on liquid-phase chemical reaction - Google Patents
Method for preparing lead hydroxide nano-rod based on liquid-phase chemical reaction Download PDFInfo
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- CN101624211B CN101624211B CN2009101360658A CN200910136065A CN101624211B CN 101624211 B CN101624211 B CN 101624211B CN 2009101360658 A CN2009101360658 A CN 2009101360658A CN 200910136065 A CN200910136065 A CN 200910136065A CN 101624211 B CN101624211 B CN 101624211B
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Abstract
The invention discloses a method for preparing a lead hydroxide nano-rod, belonging to the technical field of nanometer material preparation. The method is characterized in that lead nitrate and soluble chloride are dissolved in de-ionized water according to a mol proportion of 1:1-1:10 to prepare a solution; the solution is heated to 50-90 DEG C; alkali is added into the solution according to the mol proportion of the lead nitrate and the alkali substance of 1:3; the solution is stirred to obtain white participate; the white participate is filtered, washed and dried to obtain the lead hydroxide nano-rod. The lead hydroxide nano-rod is a hexagon structure with the length of about 50 micrometers and the diameter of 20-500 nanometers. The method has simple and convenient operation, high yield and no pollution to the environment.
Description
Technical field
The present invention relates to a kind of method for preparing nanometer rod, particularly a kind of method of utilizing preparing lead hydroxide nano-rod based on liquid-phase chemical reaction.
Background technology
Quasi-one-dimensional nanometer material as nanofiber, nanometer rod etc., is nanoscale on two-dimensional direction, and its major diameter is big.With three-dimensional all is that the block materials of macro-scale is compared, have unique physical and chemical properties, as have small-size effect, and quantum effect, surface effectss etc. can demonstrate unique optical characteristics, electrology characteristic, catalysis characteristics etc.
The method for preparing at present quasi-one-dimensional nanometer material is many, as chemical Vapor deposition process, and physical evaporation method, template, electrochemical deposition method, solid phase method, hydrothermal method etc.
Lead hydroxide has a wide range of applications, as is cell dyeing, work and absorption agent etc.Yet the preparation method about lead hydroxide nano-rod based does not see bibliographical information yet.
Summary of the invention
Order of the present invention is to provide a kind of method of preparing lead hydroxide nano-rod based on liquid-phase chemical reaction, and it comprises the following steps: that (1) is dissolved into lead nitrate in the deionized water wiring solution-forming; (2) be 1 in lead nitrate and soluble chloride amount of substance ratio in the solution in step (1): 1-1: 10 add soluble chlorides; (3) solution in the step (2) is heated to 50-80 degree centigrade; (4) the amount ratio in lead nitrate and alkaloid substance is 1: 3 adding alkali in the solution in step (3), stirs, and obtains white depositions, and filtration, washing, drying promptly get lead hydroxide nano-rod based; Further, described soluble chloride comprises sodium-chlor or Repone K; Further, described alkali comprises sodium hydroxide or potassium hydroxide.In addition, the present invention also provides the lead hydroxide nano-rod based by method for preparing, and the length of lead hydroxide nano-rod based is the 10-100 micron, and diameter is the 20-500 nanometer, and purity is up to 99%, and crystalline structure is a hexagonal structure.This method is easy and simple to handle, the productive rate height, and the reaction times is short, and environment is not polluted.The inventor finds that when adding sodium-chlor in first liquid solution, because the effect of the inhibition hydrolysis of chlorion, the gained throw out is a lead hydroxide nano-rod based when research lead nitrate and the reaction of alkali lye phase chemistry.The method that the present invention prepares lead hydroxide nano-rod based is that lead nitrate and sodium-chlor are dissolved into deionized water formation solution by a certain percentage, and be heated to certain temperature, in solution, add a certain amount of potassium hydroxide again, stir, obtain white depositions, filtration, washing, drying promptly get lead hydroxide nano-rod based.
Description of drawings
Fig. 1 is the XRD spectral line of the lead hydroxide nano-rod based of liquid phase chemical reaction method preparation of the present invention.
Fig. 2 is the stereoscan photograph of the lead hydroxide nano-rod based of liquid phase chemical reaction method preparation of the present invention.
Fig. 3 is the transmission electron microscope photo of the lead hydroxide nano-rod based of liquid phase chemical reaction method preparation of the present invention.
Fig. 4 is the high-resolution-ration transmission electric-lens photo of the lead hydroxide nano-rod based of liquid phase chemical reaction method preparation of the present invention.
Fig. 5 is the selected area electron diffraction spectrum of the lead hydroxide nano-rod based of liquid phase chemical reaction method preparation of the present invention.
Embodiment
With lead nitrate and sodium-chlor be dissolved into dried up in, wiring solution-forming, the concentration of lead nitrate is 0.01mol/l, and the concentration of sodium-chlor is 0.01-0.10mol/l, and heated solution is to 50-80 degree centigrade, add the potassium hydroxide solid again, the concentration of potassium hydroxide is 0.03mol/l, stirs, and obtains white depositions, filtration, washing, drying promptly get lead hydroxide nano-rod based.
Embodiment 1
Get 0.166g lead nitrate and 0.06g sodium-chlor and be dissolved in the 50ml deionized water, solution is heated to 80 degrees centigrade, then, get 0.084g potassium hydroxide solid and be added in the solution, stir, obtain white depositions, filtration, washing, drying promptly get lead hydroxide nano-rod based.As shown in Figure 1, product is accredited as lead hydroxide through X-ray powder diffraction; With scanning electronic microscope product is carried out morphology analysis, as can be seen from Figure 2 its pattern is a rod, and the length of rod is about 50 microns, and the diameter of rod is between the 100-500 nanometer, and length-to-diameter ratio is up to more than 100; It also is bar-shaped that Fig. 3 is presented at the pattern of seeing under the transmission electron microscope; Fig. 4 is presented at the lattice fringe of seeing clearly (002) crystal face under the high resolution transmission electron microscopy, and the interplanar distance of (002) crystal face is about 6.43
Fig. 5 has shown the selected area electron diffraction spectrum of lead hydroxide nano-rod based, through demarcating, confirms that its crystalline structure is a hexagonal structure.
Get 0.662g lead nitrate and 0.117g sodium-chlor and be dissolved in the 200ml deionized water, solution is heated to 90 degrees centigrade, then, get 0.336g potassium hydroxide solid and be added in the solution, stir, obtain white depositions, filtration, washing, drying promptly get lead hydroxide nano-rod based.
Embodiment 3
Get 0.662g lead nitrate and 0.234g sodium-chlor and be dissolved in the 200ml deionized water, solution is heated to 90 degrees centigrade, then, get 0.084g potassium hydroxide solid and be added in the solution, stir, obtain white depositions, filtration, washing, drying promptly get lead hydroxide nano-rod based.
Get 0.662g lead nitrate and 0.351g sodium-chlor and be dissolved in the 200ml deionized water, solution is heated to 90 degrees centigrade, then, get 0.084g potassium hydroxide solid and be added in the solution, stir, obtain white depositions, filtration, washing, drying promptly get lead hydroxide nano-rod based.
Embodiment 5
Get 0.662g lead nitrate and 0.468g sodium-chlor and be dissolved in the 200ml deionized water, solution is heated to 90 degrees centigrade, then, get 0.084g potassium hydroxide solid and be added in the solution, stir, obtain white depositions, filtration, washing, drying promptly get lead hydroxide nano-rod based.
Embodiment 3
Get 0.662g lead nitrate and 0.585g sodium-chlor and be dissolved in the 200ml deionized water, solution is heated to 90 degrees centigrade, then, get 0.084g potassium hydroxide solid and be added in the solution, stir, obtain white depositions, filtration, washing, drying promptly get lead hydroxide nano-rod based.
Claims (4)
1. the method for a preparing lead hydroxide nano-rod based on liquid-phase chemical reaction is characterized in that comprising the following steps:
(1) lead nitrate is dissolved in the deionized water wiring solution-forming;
(2) be 1 in lead nitrate and soluble chloride amount of substance ratio in the solution in step (1): 1-1: 10 add soluble chlorides;
(3) solution in the step (2) is heated to 50-80 degree centigrade;
(4) the amount ratio in lead nitrate and alkaloid substance is 1: 3 adding alkali in the solution in step (3), stirs, and obtains white depositions, and filtration, washing, drying promptly get lead hydroxide nano-rod based.
2. by the described method of claim 1, it is characterized in that: described soluble chloride comprises sodium-chlor or Repone K.
3. by the described method of claim 1, it is characterized in that: described alkali comprises sodium hydroxide or potassium hydroxide.
4. lead hydroxide nano-rod based by the preparation of the described method of claim 1, it is characterized in that: the length of lead hydroxide nano-rod based is the 10-100 micron, and diameter is the 20-500 nanometer, and purity is up to 99%, and crystalline structure is a hexagonal structure.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101360658A CN101624211B (en) | 2009-04-27 | 2009-04-27 | Method for preparing lead hydroxide nano-rod based on liquid-phase chemical reaction |
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| CN2009101360658A CN101624211B (en) | 2009-04-27 | 2009-04-27 | Method for preparing lead hydroxide nano-rod based on liquid-phase chemical reaction |
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| CN101624211A CN101624211A (en) | 2010-01-13 |
| CN101624211B true CN101624211B (en) | 2011-03-16 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102747227B (en) * | 2012-06-18 | 2014-02-05 | 东南大学 | Method for preparing superfine lead oxide by using electrode active materials of wasted lead acid batteries |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1491896A (en) * | 2002-10-23 | 2004-04-28 | 新疆大学 | Process for preparing lead oxide nano stick by solid phase chemical reaction |
| CN101348277A (en) * | 2007-07-18 | 2009-01-21 | 北京化工大学 | Synthetic method of nano lead hydrate |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1491896A (en) * | 2002-10-23 | 2004-04-28 | 新疆大学 | Process for preparing lead oxide nano stick by solid phase chemical reaction |
| CN101348277A (en) * | 2007-07-18 | 2009-01-21 | 北京化工大学 | Synthetic method of nano lead hydrate |
Non-Patent Citations (1)
| Title |
|---|
| 杜江燕等.铅(II)化合物与NaOH室温条件下的固相化学反应研究.《无机化学学报》.1999,第15卷(第3期),383-387. * |
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