CN107010672B - A kind of preparation method of lead tungstate nano tubular crystal - Google Patents
A kind of preparation method of lead tungstate nano tubular crystal Download PDFInfo
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- CN107010672B CN107010672B CN201710309361.8A CN201710309361A CN107010672B CN 107010672 B CN107010672 B CN 107010672B CN 201710309361 A CN201710309361 A CN 201710309361A CN 107010672 B CN107010672 B CN 107010672B
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- C—CHEMISTRY; METALLURGY
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- C01G41/00—Compounds of tungsten
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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Abstract
The invention discloses a kind of preparation methods of lead tungstate nano tubular crystal, first prepare the deionized water solution of sodium tungstate, plumbi nitras, polyethylene glycol (PEG 6000) and potassium acetate, then lead nitrate solution and potassium acetate solution are mixed, obtain acetate lead precipitation solution, sodium tungstate solution and polyglycol solution are mixed again, finally the mixed solution of sodium tungstate and polyethylene glycol is mixed with acetate lead precipitation solution, then mixed solution is put into temperature control microwave hydrothermograph, after carrying out microwave treatment, lead tungstate nano tubular crystal is obtained.The present invention successfully prepares lead tungstate nano tubular crystal for the first time, and because it has unique one-dimensional tubular structure, in luminous, optical fiber, photocatalysis, microwave, scintillator, detector etc., with more excellent performance, method provided by the present invention, there is operation easy, little energy of consumption, mild condition, pollution-free, it is easy to accomplish industrialized production.
Description
Technical field
The invention belongs to technical field of inorganic nonmetallic materials, and in particular to a kind of preparation of lead tungstate nano tubular crystal
Method.
Background technology
Lead tungstate is a kind of important inorganic scintillator material, since its excellent scintillation properties such as die-away time is short, spoke
It is high according to hardness, the advantages that density is high and cheap, shine, optical fiber, photocatalysis, microwave, scintillator, detector etc. are much led
Domain has very extensive purposes, is one of research hotspot in recent years.
It is well known that the nano crystal material with special appearance often shows some excellent performances, and therefore, system
All have in terms of theoretical basis research and practical application for the lead tungstate nano tubular crystal for going out novel in shape very important
Meaning.
The content of the invention
The object of the present invention is to provide a kind of methods for preparing lead tungstate nano tubular crystal at normal temperatures and pressures, have work
Skill is simple, easy to operate, it is of low cost the advantages that, gained lead tungstate nano tubular crystal has unique one-dimensional tubular structure,
In luminous, optical fiber, photocatalysis, microwave, scintillator, detector etc., there is more excellent performance, have more extensive
Application prospect.
The object of the invention to solve the technical problems is realized using following technical scheme.
According to a kind of preparation method of lead tungstate nano tubular crystal proposed by the present invention, comprise the following steps：
(1), the second that the plumbi nitras aqueous solution and concentration that compound concentration is 0.1-1.0mol/L respectively are 0.2-2.0mol/L
Sour aqueous solutions of potassium；
(2), plumbi nitras aqueous solution made from step (1) and potassium acetate solution are mixed, obtained containing acetate lead precipitation
With the mixture A of potassium nitrate solution；The molar ratio of potassium acetate and plumbi nitras is 2 during mixing:1；
(3), the poly- second that the wolframic acid sodium water solution and mass fraction that compound concentration is 0.12-1.2mol/L respectively are 0.5%
Glycol (PEG-6000) aqueous solution, and the two is mixed, 30min is stirred, it is molten to obtain the mixing containing sodium tungstate and polyethylene glycol
Liquid；
(4), mixed solution obtained by mixture A obtained by step (2) and step (3) is mixed, obtains mixture B, then
Container equipped with mixture B is put into temperature control microwave hydrothermograph and carries out microwave treatment, is washed repeatedly with distilled water afterwards anti-
Product is answered, after filtered, drying, obtains lead tungstate nano tubular crystal.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
A kind of preparation method of foregoing lead tungstate nano tubular crystal, wherein, sodium tungstate and acetic acid when step (4) mixes
The molar ratio of lead is 1.2:1.
A kind of preparation method of foregoing lead tungstate nano tubular crystal, wherein, the work(of microwave during step (4) microwave treatment
Rate is 400-1600W, and the microwave time is 10-30min, and the temperature of microwave treatment is 60-90 DEG C.
A kind of preparation method of foregoing lead tungstate nano tubular crystal, wherein, wolframic acid sodium water solution when step (3) mixes
Volume ratio with polyethylene glycol (PEG-6000) aqueous solution is 1:1.
A kind of preparation method of foregoing lead tungstate nano tubular crystal, wherein, the sodium tungstate, potassium acetate, nitric acid
Lead, the purity of polyethylene glycol are pure not less than chemistry.
The key problem in technology point of the present invention is：
(1) first plumbi nitras aqueous solution and potassium acetate solution must be mixed, it is first as reaction that acetate lead precipitation is made
Drive body；
(2) have to mix wolframic acid sodium water solution and polyethylene glycol (PEG-6000) aqueous solution, prepare sodium tungstate
With the mixed solution of polyethylene glycol；
(3) having to will be equipped with mixture B (mixture B contains acetate lead precipitation, potassium nitrate, sodium tungstate, polyethylene glycol)
Container be put into temperature control microwave hydrothermograph and carry out microwave treatment；
(4) it must be provided simultaneously with for 3 points more than, otherwise cannot get lead tungstate nano tubular crystal.And must obtain second
Lead plumbate precipitation is infeasible using other lead-containing compounds as precursor；Must be made with polyethylene glycol (PEG-6000)
It is infeasible using other surfactants for surfactant；Must mixed solution be subjected to microwave treatment, use is other
Processing mode is infeasible.
The beneficial effects of the present invention are：
The present invention has prepared the high lead tungstate nano tubular crystal of good crystallinity, purity, equipment letter at normal temperatures and pressures
Single, easy to operate, mild condition, easy control of process conditions, the little energy of consumption is of low cost, pollution-free, it is easy to accomplish work
Industry metaplasia is produced.Obtained lead tungstate nano tubular crystal has unique one-dimensional tubular structure, lead tungstate nano tubular crystal
Length be about 2-6um, the pipe thickness of nanotube is about 20-100nm, shine, optical fiber, photocatalysis, microwave, scintillator,
The fields such as detector have broad application prospects.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, and in order to allow the above and other objects, features and advantages of the present invention can
It is clearer and more comprehensible, it is special below to lift preferred embodiment, and coordinate attached drawing, detailed description are as follows.
Description of the drawings
Fig. 1 is the XRD spectrum for the lead tungstate nano tubular crystal that the present invention synthesizes；
Fig. 2 is transmission electron microscope (TEM) photo for the lead tungstate nano tubular crystal that the present invention synthesizes.
Specific embodiment
Further to illustrate the present invention to reach the technological means and effect that predetermined goal of the invention is taken, below in conjunction with
Attached drawing and preferred embodiment, to according to a kind of preparation method of lead tungstate nano tubular crystal proposed by the present invention, specific reality
Mode, structure, feature and its effect are applied, is described in detail as after.
Embodiment 1
(1), making solvent compound concentration is 0.10mol/L respectively plumbi nitras aqueous solution and concentration with deionized water is
The potassium acetate solution of 0.2mol/L；
(2), plumbi nitras aqueous solution made from step (1) and potassium acetate solution are mixed, obtained containing acetate lead precipitation
With the mixture A of potassium nitrate solution；The molar ratio of potassium acetate and plumbi nitras is 2 during mixing:1；
(3), making solvent compound concentration is 0.12mol/L respectively wolframic acid sodium water solution and mass fraction with deionized water is
0.5% Aqueous Solutions of Polyethylene Glycol, and the two is mixed in equal volume, it stirs 30 minutes, obtains containing sodium tungstate and polyethylene glycol
Mixed solution；
(4), mixed solution obtained by mixture A obtained by step (2) and step (3) is mixed into (wherein sodium tungstate and acetic acid
The molar ratio of lead is 1.2:1) mixture B, is obtained, then the container equipped with mixture B is put into temperature control microwave hydrothermograph
Microwave treatment, microwave power 400W are carried out, the microwave time is 30 minutes, and microwave temperature is 60 degree.Then with distilled water repeatedly
Washing reaction product after filtering, drying, obtains lead tungstate nano tubular crystal.
The length of gained lead tungstate nano tubular crystal is 2-4um, and the pipe thickness of nanotube is 50-100nm.Its XRD
Collection of illustrative plates is shown in Fig. 1；Transmission electron microscope picture is shown in Fig. 2.As can be seen from Figure 2 products therefrom has apparent nano tubular structure.
Embodiment 2
(1), it is 1mol/ to make solvent compound concentration is 0.5mol/L respectively plumbi nitras aqueous solution and concentration with deionized water
The potassium acetate solution of L；
(2), plumbi nitras aqueous solution made from step (1) and potassium acetate solution are mixed, obtained containing acetate lead precipitation
With the mixture A of potassium nitrate solution；The molar ratio of potassium acetate and plumbi nitras is 2 during mixing:1；
(3), making solvent compound concentration is 0.6mol/L respectively wolframic acid sodium water solution and mass fraction with deionized water is
0.5% Aqueous Solutions of Polyethylene Glycol, and the two is mixed in equal volume, it stirs 30 minutes, obtains containing sodium tungstate and polyethylene glycol
Mixed solution；
(4), mixed solution obtained by mixture A obtained by step (2) and step (3) is mixed into (wherein sodium tungstate and acetic acid
The molar ratio of lead is 1.2:1) mixture B, is obtained, then the container equipped with mixture B is put into temperature control microwave hydrothermograph
Microwave treatment, microwave power 800W are carried out, the microwave time is 20 minutes, and microwave temperature is 70 degree.Then with distilled water repeatedly
Washing reaction product after filtering, drying, obtains lead tungstate nano tubular crystal.
Embodiment 3
(1), making solvent compound concentration is 1.0mol/L respectively plumbi nitras aqueous solution and concentration with deionized water is
The potassium acetate solution of 2.0mol/L；
(2), plumbi nitras aqueous solution made from step (1) and potassium acetate solution are mixed, obtained containing acetate lead precipitation
With the mixture A of potassium nitrate solution；The molar ratio of potassium acetate and plumbi nitras is 2 during mixing:1；
(3), making solvent compound concentration is 1.2mol/L respectively wolframic acid sodium water solution and mass fraction with deionized water is
0.5% Aqueous Solutions of Polyethylene Glycol, and the two is mixed in equal volume, it stirs 30 minutes, obtains containing sodium tungstate and polyethylene glycol
Mixed solution；
(4), mixed solution obtained by mixture A obtained by step (2) and step (3) is mixed into (wherein sodium tungstate and acetic acid
The molar ratio of lead is 1.2:1) mixture B, is obtained, then the container equipped with mixture B is put into temperature control microwave hydrothermograph
Microwave treatment, microwave power 1600W are carried out, the microwave time is 10 minutes, and microwave temperature is 90 degree.Then with distilled water repeatedly
Washing reaction product after filtering, drying, obtains lead tungstate nano tubular crystal.
The above described is only a preferred embodiment of the present invention, not make limitation in any form to the present invention, though
So the present invention is disclosed above with preferred embodiment, however is not limited to the present invention, any to be familiar with this professional technology people
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, technical spirit according to the invention
To any simple modification, equivalent change and modification that above example is made, in the range of still falling within technical solution of the present invention.
Claims (2)
1. a kind of preparation method of lead tungstate nano tubular crystal, it is characterised in that comprise the following steps：
(1), the potassium acetate that the plumbi nitras aqueous solution and concentration that compound concentration is 0.1-1.0mol/L respectively are 0.2-2.0mol/L
Aqueous solution；
(2), plumbi nitras aqueous solution made from step (1) and potassium acetate solution are mixed, obtained containing acetate lead precipitation and nitre
The mixture A of sour potassium solution；The molar ratio of potassium acetate and plumbi nitras is 2 during mixing:1；
(3), the polyethylene glycol that the wolframic acid sodium water solution and mass fraction that compound concentration is 0.12-1.2mol/L respectively are 0.5%
Aqueous solution, and the two is mixed, 30min is stirred, obtains the mixed solution containing sodium tungstate and polyethylene glycol；
(4), mixture A obtained by step (2) and step (3) gained mixed solution are mixed, sodium tungstate and lead acetate during mixing
Molar ratio be 1.2:1, mixture B is obtained, then the container equipped with mixture B is put into temperature control microwave hydrothermograph and is carried out
Microwave treatment, the power of microwave is 400-1600W, and the microwave time is 10-30min, and the temperature of microwave treatment is 60-90 DEG C, it
Afterwards with distilled water washing reaction product repeatedly, after filtered, drying, lead tungstate nano tubular crystal is obtained；
Obtained lead tungstate nano tubular crystal has one-dimensional tubular structure, and the length of lead tungstate nano tubular crystal is 2-
6um, the pipe thickness of nanotube is 20-100nm.
2. the preparation method of lead tungstate nano tubular crystal according to claim 1, it is characterised in that the sodium tungstate,
Potassium acetate, plumbi nitras, the purity of polyethylene glycol are pure not less than chemistry.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502843A (en) * | 2011-11-07 | 2012-06-20 | 河北联合大学 | Method for preparing lanthanum molybdate nanotube material by microwave radiation method |
| CN103526293A (en) * | 2013-10-14 | 2014-01-22 | 洛阳理工学院 | Method of preparing cadmium tungstate nanowire by microwave method |
| CN105967236A (en) * | 2016-05-06 | 2016-09-28 | 洛阳理工学院 | Preparation method of tubular lead molybdate nano-material |
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- 2017-05-04 CN CN201710309361.8A patent/CN107010672B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502843A (en) * | 2011-11-07 | 2012-06-20 | 河北联合大学 | Method for preparing lanthanum molybdate nanotube material by microwave radiation method |
| CN103526293A (en) * | 2013-10-14 | 2014-01-22 | 洛阳理工学院 | Method of preparing cadmium tungstate nanowire by microwave method |
| CN105967236A (en) * | 2016-05-06 | 2016-09-28 | 洛阳理工学院 | Preparation method of tubular lead molybdate nano-material |
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