CN103387263B - Lead molybdate nano crystal material and preparation method thereof - Google Patents
Lead molybdate nano crystal material and preparation method thereof Download PDFInfo
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- CN103387263B CN103387263B CN201310290718.4A CN201310290718A CN103387263B CN 103387263 B CN103387263 B CN 103387263B CN 201310290718 A CN201310290718 A CN 201310290718A CN 103387263 B CN103387263 B CN 103387263B
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- sodium
- molybdate
- chromate
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Abstract
A lead molybdate nano crystal material and a preparation method thereof are disclosed. The preparation method comprises following steps: respectively dissolving sodium chromate, lead nitrate and sodium molybdate in deionized water to prepare a sodium chromate solution, a lead nitrate solution and a sodium molybdate solution, mixing the sodium chromate solution with the lead nitrate solution according to the mole ratio of CrO4<2-> to Pb<2+> of 1:1, obtaining a solution containing the lead chromate precipitation, then mixing the sodium molybdate solution with the solution containing the lead chromate precipitation according to the mole ration of MoO4<2-> to Pb<2+> of 1:1, standing for 3 to 10 hours, filtering to obtain the precipitation generated by the reactions, repeatedly washing the precipitation with deionized water and absolute ethanol, and then drying the precipitation so as to obtain the product. The preparation method produces a lead molybdate nano crystal material, which has good crystallinity, high purity and a high length-diameter ratio. The material has vast application prospects in the fields of acousto-optic devices, optical fibers, optical materials and photocatalyst.
Description
Technical field
The present invention relates to a kind of nano crystal material of inorganic non-metallic, specifically a kind of Lead molybdate nano crystal material and preparation method thereof.
Background technology
Lead molybdate is a kind of type material with scheelite-type structure, in the scanning of lidar, TV and large screen display, the optical memory of photonic computer and laser communication and nuclear equipment etc., there is higher practical value, simultaneously as a kind of photocatalyst, luminescent material and optical fiber, also there is boundless application prospect.
Traditional method preparing lead molybdate is solid reaction process, although this method technique is simple, often need high-temperature heat treatment in this way, energy consumption is higher, and the purity of preparation low, easily reunite, be difficult to the size and the pattern that control crystal grain.
Summary of the invention
For solving low, the easy reunion of purity of Lead molybdate nano crystal material existence prepared by existing method and being difficult to control the problem such as grain-size and pattern, the invention provides a kind of Lead molybdate nano crystal material and preparation method thereof.
The present invention is the technical scheme solving the problems of the technologies described above employing: a kind of Lead molybdate nano crystal material, and the crystal grain of this nano crystal material is bar-shaped.
Prepare the method for this Lead molybdate nano crystal material, comprise the following steps:
1) Sodium chromate, lead nitrate and Sodium orthomolybdate are dissolved in deionized water prepare chromium acid sodium solution, lead nitrate solution and sodium molybdate solution respectively, for subsequent use;
2) step 1 is got) obtained chromium acid sodium solution and lead nitrate solution be according to CrO
4 2-and Pb
2+mol ratio is the ratio mixing of 1:1, obtains the solution left standstill 1-3 hour containing precipitation of lead chromate;
3) step 1 is got) obtained sodium molybdate solution and step 2) solution containing precipitation of lead chromate that obtains is according to MoO
4 2-and Pb
2+mol ratio is standing 3-10 hour after the ratio mixing of 1:1, filters and obtains reacting the throw out generated, then with deionized water and dehydrated alcohol repetitive scrubbing, oven dry throw out, i.e. obtained product.
CrO in described chromium acid sodium solution
4 2-concentration be 0.1 ~ 1.5mol/L, Pb in lead nitrate solution
2+concentration be 0.1 ~ 1.5mol/L, MoO in sodium molybdate solution
4 2-concentration be 0.1 ~ 1.5mol/L.
Bar-shaped lead molybdate prepared by the present invention is compared to spherical lead molybdate prepared by prior art and has larger length-to-diameter ratio, thus there is larger specific surface area, and the specific surface area of nano material is larger, its performance is better, and thus bar-shaped lead molybdate can significantly improve it in very many-sided performance such as photochemical catalysis and luminescent properties.
The precipitation of lead chromate that the present invention first adopts chromium acid sodium solution and lead nitrate solution to be obtained by reacting, and then prepare lead molybdate with precipitation of lead chromate and sodium molybdate solution reaction, during owing to adopting sodium molybdate solution as reaction system, even if lead molybdate also has very strong nucleation capability at normal temperatures, and the grain shape of lead chromate is bar-shaped, therefore lead chromate reacts the lead molybdate crystal grain generated and also according to bar-shaped growth, thus can prepare bar-shaped Lead molybdate nano crystal material in sodium molybdate solution system with Sodium orthomolybdate.Prepare lead molybdate in prior art to need through high-temperature roasting, although also can Crystals of Lead Molybdate be obtained, in roasting process, the growth of Crystals of Lead Molybdate will be promoted further, be thus difficult to obtain the little lead molybdate nanocrystal of size, and be difficult to obtain bar-shaped Crystals of Lead Molybdate such as one dimension such as grade.
Beneficial effect: the present invention compared with prior art, has the following advantages:
1) crystal grain of Crystals of Lead Molybdate of the present invention is bar-shaped, spherical Crystals of Lead Molybdate prepared by prior art of comparing, there is higher length-to-diameter ratio, therefore, have broad application prospects in fields such as acousto-optical device, optical fiber, luminescent material, photocatalysts;
2) the present invention adopts normal temperature and pressure to obtain product, and prior art of comparing needs roasting to obtain product, and equipment used is simple, and reaction conditions is gentle, saves the energy and production time, reduces cost.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the lead molybdate nanometer rod that the present invention synthesizes;
Fig. 2 is transmission electron microscope (TEM) photo of the lead molybdate nanometer rod that the present invention synthesizes.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, and the purity of Sodium orthomolybdate, Sodium chromate, lead nitrate and dehydrated alcohol selected in following embodiment is all not less than chemical pure.
For the ease of operation, the concentration of the chromium acid sodium solution prepared in the same embodiment, lead nitrate solution and sodium molybdate solution is equal, only needs to add equal-volume like this when operating, can certainly be unequal, a demand fulfillment CrO
4 2-, Pb
2+and MoO
4 2-mol ratio be 1:1:1.
Embodiment 1
Prepare the method for bar-shaped Lead molybdate nano crystal material, comprise the following steps:
1) respectively Sodium chromate, lead nitrate and Sodium orthomolybdate are dissolved in deionized water prepare chromium acid sodium solution that concentration is 0.1mol/L, lead nitrate solution that concentration is 0.1mol/L and concentration is the sodium molybdate solution of 0.1mol/L, for subsequent use;
2) step 1 is got) obtained chromium acid sodium solution and lead nitrate solution be according to CrO
4 2-and Pb
2+mol ratio is the ratio mixing of 1:1, obtains solution left standstill containing precipitation of lead chromate 1 hour;
3) step 1 is got) obtained sodium molybdate solution and step 2) solution containing precipitation of lead chromate that obtains is according to MoO
4 2-and Pb
2+mol ratio is that the ratio of 1:1 mixes latter standing 3 hours, filters the throw out obtaining reacting generation, and then use deionized water and dehydrated alcohol repetitive scrubbing, oven dry throw out, namely obtained grain shape is bar-shaped Lead molybdate nano crystal material.
After measured, the diameter of this Lead molybdate nano crystal material is 20-40nm, and length is 300-400nm, and as shown in Figure 1, transmission electron microscope picture as shown in Figure 2 for its XRD figure spectrum.
Embodiment 2
Prepare the method for bar-shaped Lead molybdate nano crystal material, comprise the following steps:
1) respectively Sodium chromate, lead nitrate and Sodium orthomolybdate are dissolved in deionized water prepare chromium acid sodium solution that concentration is 0.5mol/L, lead nitrate solution that concentration is 0.5mol/L and concentration is the sodium molybdate solution of 0.5mol/L, for subsequent use;
2) step 1 is got) obtained chromium acid sodium solution and lead nitrate solution be according to CrO
4 2-and Pb
2+mol ratio is the ratio mixing of 1:1, obtains solution left standstill containing precipitation of lead chromate 2 hours;
3) step 1 is got) obtained sodium molybdate solution and step 2) solution containing precipitation of lead chromate that obtains is according to MoO
4 2-and Pb
2+mol ratio is that the ratio of 1:1 mixes latter standing 5 hours, filters the throw out obtaining reacting generation, and then use deionized water and dehydrated alcohol repetitive scrubbing, oven dry throw out, namely obtained grain shape is bar-shaped Lead molybdate nano crystal material.
After measured, the diameter of this Lead molybdate nano crystal material is 20-40nm, and length is 300-400nm.
Embodiment 3
Prepare the method for bar-shaped Lead molybdate nano crystal material, comprise the following steps:
1) respectively Sodium chromate, lead nitrate and Sodium orthomolybdate are dissolved in deionized water prepare chromium acid sodium solution that concentration is 1.5mol/L, lead nitrate solution that concentration is 1.5mol/L and concentration is the sodium molybdate solution of 1.5mol/L, for subsequent use;
2) step 1 is got) obtained chromium acid sodium solution and lead nitrate solution be according to CrO
4 2-and Pb
2+mol ratio is the ratio mixing of 1:1, obtains solution left standstill containing precipitation of lead chromate 3 hours;
3) step 1 is got) obtained sodium molybdate solution and step 2) solution containing precipitation of lead chromate that obtains is according to MoO
4 2-and Pb
2+mol ratio is that the ratio of 1:1 mixes latter standing 10 hours, filters the throw out obtaining reacting generation, and then use deionized water and dehydrated alcohol repetitive scrubbing, oven dry throw out, namely obtained grain shape is bar-shaped Lead molybdate nano crystal material.
After measured, the diameter of this Lead molybdate nano crystal material is 30-40nm, and length is 400-500nm.
Embodiment 4
Prepare the method for bar-shaped Lead molybdate nano crystal material, comprise the following steps:
1) respectively Sodium chromate, lead nitrate and Sodium orthomolybdate are dissolved in deionized water prepare chromium acid sodium solution that concentration is 0.8mol/L, lead nitrate solution that concentration is 0.8mol/L and concentration is the sodium molybdate solution of 0.8mol/L, for subsequent use;
2) step 1 is got) obtained chromium acid sodium solution and lead nitrate solution be according to CrO
4 2-and Pb
2+mol ratio is the ratio mixing of 1:1, obtains solution left standstill containing precipitation of lead chromate 2 hours;
3) step 1 is got) obtained sodium molybdate solution and step 2) solution containing precipitation of lead chromate that obtains is according to MoO
4 2-and Pb
2+mol ratio is that the ratio of 1:1 mixes latter standing 7 hours, filters the throw out obtaining reacting generation, and then use deionized water and dehydrated alcohol repetitive scrubbing, oven dry throw out, namely obtained grain shape is bar-shaped Lead molybdate nano crystal material.
After measured, the diameter of this Lead molybdate nano crystal material is 30-40nm, and length is 300-400nm.
Claims (2)
1. a preparation method for Lead molybdate nano crystal material, the crystal grain of this nano crystal material is bar-shaped, it is characterized in that, comprises the following steps:
1) Sodium chromate, lead nitrate and Sodium orthomolybdate are dissolved in deionized water prepare chromium acid sodium solution, lead nitrate solution and sodium molybdate solution respectively, for subsequent use;
2) step 1 is got) obtained chromium acid sodium solution and lead nitrate solution be according to CrO
4 2-and Pb
2+mol ratio is the ratio mixing of 1:1, obtains the solution left standstill 1-3 hour containing precipitation of lead chromate;
3) step 1 is got) obtained sodium molybdate solution and step 2) solution containing precipitation of lead chromate that obtains is according to MoO
4 2-and Pb
2+mol ratio is standing 3-10 hour after the ratio mixing of 1:1, filters and obtains reacting the throw out generated, then with deionized water and dehydrated alcohol repetitive scrubbing, oven dry throw out, i.e. obtained product.
2. the preparation method of Lead molybdate nano crystal material according to claim 1, is characterized in that: CrO in described chromium acid sodium solution
4 2-concentration be 0.1 ~ 1.5mol/L, Pb in lead nitrate solution
2+concentration be 0.1 ~ 1.5mol/L, MoO in sodium molybdate solution
4 2-concentration be 0.1 ~ 1.5mol/L.
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| CN103754935B (en) * | 2014-01-07 | 2015-04-08 | 洛阳理工学院 | Method for synthesizing lead molybdate tower crystal at room temperature |
| CN105016389B (en) * | 2015-07-14 | 2016-10-19 | 首都师范大学 | A kind of lead molybdate nanocrystal of carbon shell cladding and preparation method thereof |
| CN105967236B (en) * | 2016-05-06 | 2017-07-07 | 洛阳理工学院 | A kind of preparation method of tubulose lead molybdate nano material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU510493A1 (en) * | 1974-05-12 | 1976-04-15 | Предприятие П/Я Г-4392 | The method of obtaining lead-molybdate crop |
| CN1635194A (en) * | 2003-12-30 | 2005-07-06 | 宁波大学 | Falling crucible method growth process for lead molybdate single crystal |
| CN102071466A (en) * | 2010-12-24 | 2011-05-25 | 金堆城钼业股份有限公司 | Method for preparing lead molybdate polycrystalline material |
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2013
- 2013-07-11 CN CN201310290718.4A patent/CN103387263B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU510493A1 (en) * | 1974-05-12 | 1976-04-15 | Предприятие П/Я Г-4392 | The method of obtaining lead-molybdate crop |
| CN1635194A (en) * | 2003-12-30 | 2005-07-06 | 宁波大学 | Falling crucible method growth process for lead molybdate single crystal |
| CN102071466A (en) * | 2010-12-24 | 2011-05-25 | 金堆城钼业股份有限公司 | Method for preparing lead molybdate polycrystalline material |
Non-Patent Citations (1)
| Title |
|---|
| Synthesis of homogeneous bunched lead molybdate nanobelts in large scale via vertical SLM system at room temperature;Feng Qiangdong etc.;《Applied Physics A》;20080125;第91卷(第1期);第161-165页 * |
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