CN103754935B - Method for synthesizing lead molybdate tower crystal at room temperature - Google Patents
Method for synthesizing lead molybdate tower crystal at room temperature Download PDFInfo
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- CN103754935B CN103754935B CN201410006307.2A CN201410006307A CN103754935B CN 103754935 B CN103754935 B CN 103754935B CN 201410006307 A CN201410006307 A CN 201410006307A CN 103754935 B CN103754935 B CN 103754935B
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Abstract
The invention discloses a method for synthesizing lead molybdate tower crystal at room temperature. The method comprises the following steps: mixing a sodium molybdate solution with a lead nitrate solution according to the ratio of 1:1, so as to obtain a sediment solution; adjusting the PH value of the obtained sediment solution to 3-6 by using a dilute nitric acid solution; repeatedly washing a reaction product by using deionized water and absolute ethyl alcohol; filtering and baking, so as to obtain the lead molybdate tower crystal. The lead molybdate tower crystal structure is simple in technology, low in cost, and high in purity, and has a special morphology.
Description
Technical field
The present invention relates to a kind of method of synthesizing Crystals of Lead Molybdate, under particularly relating to a kind of room temperature, synthesize lead molybdate tower
The method of shape crystal.
Background technology
Crystals of Lead Molybdate belongs to tetragonal system, without symmetry centre, without opticity, owing to having high acousto-optic quality factor, it 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 a kind of 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 Coke Powder prepared is low, easily reunite, be difficult to the size and the pattern that control crystal grain.In addition, hydrothermal method is also prepare the common method of lead molybdate, but needs special conversion unit---hydrothermal reaction kettle, operation more complicated, and temperature of reaction is higher than 100 degree, and cost is higher, be difficult to realize industrialization, and the Crystals of Lead Molybdate pattern formed is single.But the nano crystal material in production practice with special appearance just can show the use properties of some excellences, and therefore, the lead molybdate nanocrystal preparing novel in shape all has very important significance in theoretical basis research and practical application.But preparation method now used at present cannot meet this requirement.
Summary of the invention
The object of the invention is the deficiency in order to solve the problems of the technologies described above existence, providing one at normal temperatures and pressures, preparation technology is simple, with low cost, purity is high and have the tower-like crystal preparation method of lead molybdate of the nanocrystalline structure of special appearance.
The preparation method of the tower-like crystal of lead molybdate of the present invention, concrete steps are as follows:
Step one, Sodium orthomolybdate is dissolved in deionized water, forms sodium molybdate aqueous solution, the MoO in regulator solution
4 2-the concentration of ion is 0.2-2.5mol/L;
Step 2, lead nitrate is dissolved in deionized water, forms the lead nitrate aqueous solution, the Pb in regulator solution
2+the concentration of ion is 0.2-2.5mol/L;
The lead nitrate aqueous solution that step 3, sodium molybdate aqueous solution step one obtained and step 2 obtain mixes in the ratio of 1:1, thus is precipitated solution;
Step 4, the pH value of precipitation solution obtained with dilute nitric acid solution regulating step three are 3-6, then precipitation solution are left standstill 1-8 hour;
Step 5, use deionized water and dehydrated alcohol repetitive scrubbing 3-5 secondary response product, filter, dry, namely obtain the tower-like crystal of lead molybdate.
In preparation process of the present invention, at normal temperatures and pressures, the pH value of mixing solutions must be adjusted to 3-6, otherwise can not get the tower-like crystal of lead molybdate, this is because in acid condition, the H in reaction system
+the growth of ion pair lead molybdate nanocrystal has guide effect, and lead molybdate nanocrystal is only at H
+under the guide effect of ion, just can obtain the tower-like crystal of lead molybdate, and when pH value is adjusted to 4, the use properties of the Crystals of Lead Molybdate obtained is best.
In preparation process of the present invention, the purity of said Sodium orthomolybdate, lead nitrate and dehydrated alcohol is all not less than chemical pure.
In step 4, precipitation solution leaves standstill 1-8 hour, is to allow lead molybdate nanocrystal crystalline growth fully.
By deionized water and dehydrated alcohol repetitive scrubbing reaction product 3-5 times in step 5, be the Na in order to wash off in solution
+ion and NO
3 -ion, makes the Crystals of Lead Molybdate purity that obtains higher.
Filtering in step 5, dry, is the Na in order to wash off in solution
+ion and NO
3 -ion, thus form the tower-like crystal powder of lead molybdate.
Beneficial effect of the present invention is:
The present invention has prepared good crystallinity, the tower-like crystal of lead molybdate that purity is high at normal temperatures and pressures, and has unique one dimension tower structure and higher length-to-diameter ratio, and length-to-diameter ratio is generally at about 15-18.At present, other preparation method also not yet prepares the tower-like crystal of the lead molybdate like this with one-dimentional structure.The synthetic method of the tower-like crystal of lead molybdate of the present invention, have that equipment is simple, easy control of process conditions, preparation the advantage such as with low cost, be easy to suitability for industrialized production.The tower-like crystal of lead molybdate of the present invention has broad application prospects in fields such as lidar, acousto-optical device, optical fiber, luminescent material, photocatalysts.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the tower-like crystal of lead molybdate that the present invention synthesizes;
Fig. 2 is transmission electron microscope (TEM) photo of the tower-like crystal of lead molybdate that the present invention synthesizes.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1
Step one, Sodium orthomolybdate is dissolved in deionized water, forms sodium molybdate aqueous solution, the MoO in regulator solution
4 2-the concentration of ion is 0.2mol/L;
Step 2, lead nitrate is dissolved in deionized water, forms the lead nitrate aqueous solution, the Pb in regulator solution
2+the concentration of ion is 0.2mol/L;
Step 3, the water-soluble liquid-phase mixing of lead nitrate that sodium molybdate aqueous solution obtained for step one and step 2 are obtained, the precipitation solution obtained;
Step 4, the pH value of precipitation solution obtained with dilute nitric acid solution regulating step three are 3, then precipitation solution are left standstill 2 hours;
Step 5, use deionized water and dehydrated alcohol repetitive scrubbing reaction product, filter, dry, namely obtain the tower-like crystal of lead molybdate.Its XRD figure spectrum is shown in Fig. 1; Transmission electron microscope picture is shown in Fig. 2.
Fig. 1 illustrates that the tower-like crystal of lead molybdate of the present invention does not have dephasign, and purity is very high, and diffraction peak is very sharp-pointed, and thus the tower-like crystal structure of lead molybdate is good; Fig. 2 illustrates the tower-like crystal of lead molybdate of the present invention, and the two ends diameter of the tower-like crystal of the lead molybdate obtained is about 100-150nm, and length is 1-2um.
Embodiment 2
Step one, Sodium orthomolybdate is dissolved in deionized water, forms sodium molybdate aqueous solution, the MoO in regulator solution
4 2-the concentration of ion is 1.5mol/L;
Step 2, lead nitrate is dissolved in deionized water, forms the lead nitrate aqueous solution, the Pb in regulator solution
2+the concentration of ion is 1.5mol/L;
Step 3, the water-soluble liquid-phase mixing of lead nitrate that sodium molybdate aqueous solution obtained for step one and step 2 are obtained, the precipitation solution obtained;
Step 4, the pH value of precipitation solution obtained with dilute nitric acid solution regulating step three are 4, then precipitation solution are left standstill 5 hours;
Step 5, use deionized water and dehydrated alcohol repetitive scrubbing reaction product, filter, dry, namely obtain the tower-like crystal of lead molybdate.
Embodiment 3
Step one, Sodium orthomolybdate is dissolved in deionized water, forms sodium molybdate aqueous solution, the MoO in regulator solution
4 2-the concentration of ion is 2.5mol/L;
Step 2, lead nitrate is dissolved in deionized water, forms the lead nitrate aqueous solution, the Pb in regulator solution
2+the concentration of ion is 2.5mol/L;
Step 3, the water-soluble liquid-phase mixing of lead nitrate that sodium molybdate aqueous solution obtained for step one and step 2 are obtained, the precipitation solution obtained;
Step 4, the pH value of precipitation solution obtained with dilute nitric acid solution regulating step three are 6, then precipitation solution are left standstill 8 hours;
Step 5, use deionized water and dehydrated alcohol repetitive scrubbing reaction product, filter, dry, namely obtain the tower-like crystal of lead molybdate.
Claims (2)
1. synthesize a method for the tower-like crystal of lead molybdate under room temperature, it is characterized in that: step one, Sodium orthomolybdate is dissolved in deionized water, form sodium molybdate aqueous solution, the MoO in regulator solution
4 2-the concentration of ion is 0.2-2.5mol/L; Step 2, lead nitrate is dissolved in deionized water, forms the lead nitrate aqueous solution, the Pb in regulator solution
2+the concentration of ion is 0.2-2.5mol/L; The lead nitrate aqueous solution that step 3, sodium molybdate aqueous solution step one obtained and step 2 obtain mixes in the ratio of 1:1, thus is precipitated solution; Step 4, the pH value of precipitation solution obtained with dilute nitric acid solution regulating step three are 3-6, then precipitation solution are left standstill 2-8 hour; Step 5, use deionized water and absolute ethanol washing 3-5 secondary response product, filter, dry, namely obtain the tower-like crystal of lead molybdate.
2. synthesize the method for the tower-like crystal of lead molybdate under a kind of room temperature according to claim 1, it is characterized in that: the MoO in sodium molybdate solution
4 2-the concentration of ion is 0.2mol/L, the Pb in lead nitrate solution
2+the concentration of ion is 0.2 mol/L.
3, synthesize the method for the tower-like crystal of lead molybdate under a kind of room temperature according to claim 1, it is characterized in that: the MoO in sodium molybdate solution
4 2-the concentration of ion is 1.5mol/L, the Pb in lead nitrate solution
2+the concentration of ion is 1.5 mol/L.
4, synthesize the method for the tower-like crystal of lead molybdate under a kind of room temperature according to claim 1, it is characterized in that: step 4, the pH value of precipitation solution obtained with dilute nitric acid solution regulating step three are 4.
5, synthesize the method for the tower-like crystal of lead molybdate under a kind of room temperature according to claim 1, it is characterized in that: step 5, use deionized water and absolute ethanol washing 5 secondary response product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| RU2643546C2 (en) * | 2016-02-24 | 2018-02-02 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Кабардино-Балкарский государственный университет им. Х.М. Бербекова" (КБГУ) | Method of producing lead tungsten from water solutions |
| 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 |
| CN109231270B (en) * | 2018-12-06 | 2020-10-16 | 洛阳理工学院 | Preparation method of lead molybdate dendritic crystal |
| CN110937633B (en) * | 2019-12-09 | 2022-04-12 | 天津科技大学 | Preparation method of needle-shaped sodium molybdate dihydrate crystal |
Citations (1)
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| CN103387263A (en) * | 2013-07-11 | 2013-11-13 | 洛阳理工学院 | Lead molybdate nano crystal material and preparation method thereof |
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| CN103387263A (en) * | 2013-07-11 | 2013-11-13 | 洛阳理工学院 | Lead molybdate nano crystal material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Effect of high pressure on the Raman and electronic absorption spectra of PbMo04 and PbWO4;A. Jayaraman, et al.;《PHYSICAL REVIEW B》;19850415;第31卷;第5423-5427页 * |
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