CN106542579A - A kind of preparation method of flower ball-shaped calcium molybdate - Google Patents
A kind of preparation method of flower ball-shaped calcium molybdate Download PDFInfo
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- CN106542579A CN106542579A CN201510603430.7A CN201510603430A CN106542579A CN 106542579 A CN106542579 A CN 106542579A CN 201510603430 A CN201510603430 A CN 201510603430A CN 106542579 A CN106542579 A CN 106542579A
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- molybdate
- flower ball
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- calcium chloride
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Abstract
The present invention discloses a kind of by chelating agen ethylenediaminetetraacetic acid (EDTA) chelating Ca2+The method for preparing flower ball-shaped calcium molybdate, the method are completed by following steps：With calcium chloride, sodium molybdate as raw material, a certain amount of distilled water is separately added into, magnetic agitation makes its mix homogeneously, is poured sodium molybdate in calcium chloride solution in stirring, ultrasonic reaction half an hour after continuing to stir 15 minutes, by pelleting centrifugation, wash, be dried to obtain flower ball-shaped calcium molybdate.Calcium chloride used in the present invention, sodium molybdate, EDTA etc. are cheap and easy to get, nontoxic, and ultrasound is easily operated, and reaction unit are required low.Flower ball-shaped calcium molybdate obtained in the present invention has larger specific surface area simultaneously, with preferable photoluminescence performance.
Description
Technical field
The invention belongs to micro Nano material synthesis technical field, and in particular to a kind of flower ball-shaped calcium molybdate and preparation method thereof.
Background technology
Since new century, people are paid close attention to further and are paid attention to functional material.From from the perspective of inorganic nano material synthesis, and
The physical property and chemical property of the non-fundamental particle for simply forming material decides material function, and more determinative is this
A little fundamental particles are in which way building material.The material that same molecule is built in a different manner, its crystallization degree,
The Nomenclature Composition and Structure of Complexes on geometric shape, size, inside and surface etc. is likely to present very big difference, so as to cause material
The performance of material also presents very big difference.Therefore, it can be synthesized using existing element under various conditions,
The distinct inorganic nano material of various yardsticks, pattern, crystallinity, microstructure is prepared, day is met with this increasingly
The different demands of the industrial and agricultural production, national defence and science and technology of exhibition.
In past several years, scheelite type metal molybdate enjoys the concern of researcher, extensive in every field mainly due to which
Application, such as photo luminescent devices, solid state optics Amplifier Based On Stimulated Emission Of Radiation, optical fiber, scintillation detector, humidity sensor, catalyst etc..
In numerous scheelite type molybdates, calcium molybdate (CaMoO4) due to being furtherd investigate with excellent luminescent properties.Research
As a result show：CaMoO4The luminescent properties of powder are affected by its granular size and pattern, therefore study CaMoO4Crystal shape
The controlledly synthesis of looks is significant.Although someone has synthesized difference by hydro-thermal method, microwave method, microemulsion method etc.
The CaMoO of pattern4, but there is special appearance and homogeneous CaMoO by easy method synthesis4Nano material is remained
One great challenge.
The content of the invention
To overcome the deficiencies in the prior art, it is an object of the invention to provide one kind is in the presence of ultrasonic wave added, with calcium chloride and molybdenum
Method of the sour sodium for Material synthesis flower ball-shaped calcium molybdate.
The object of the present invention is achieved like this, chelates the Ca in calcium chloride by adding ethylenediaminetetraacetic acid (EDTA)2+, control
System produces the speed of precipitation, prevents from generating the reunion of too fast generation due to precipitation, obtains the homogeneous flower ball-shaped calcium molybdate of pattern.
The present invention prepares comprising the following steps that for flower ball-shaped calcium molybdate：
(1) a certain amount of calcium chloride and EDTA are weighed in beaker, appropriate distilled water, abundant magnetic agitation is added；
(2) a certain amount of sodium molybdate is weighed in beaker, add appropriate distilled water, abundant magnetic agitation；
(3) sodium molybdate solution is poured in the beaker for filling calcium chloride solution；
(4) solution is continued into magnetic agitation 15 minutes, is moved in ultrasonic cleaner afterwards, ultrasonic half an hour；
(5) by respectively washing three times of the precipitation distilled water for obtaining and ethanol, be placed in and 6h be dried in 60 DEG C of baking ovens and obtain flower ball-shaped
Calcium molybdate.
Further, the addition of described EDTA is respectively 0g, 0.003g and 0.0006g.
The present invention utilizes calcium chloride and sodium molybdate is raw material, chelates the Ca in calcium chloride using chelating agen EDTA2+, control generation
The speed of precipitation, adjusts the pattern of product, is easy to get with raw material, nontoxic, the features such as easy to operate, is conducive to obtaining homogeneous
Product.More importantly the present invention obtains flower ball-shaped calcium molybdate, has excellent performance in terms of luminescence generated by light.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) photo prepared by example 1.
Fig. 2 is scanning electron microscope (SEM) photo prepared by example 2.
Fig. 3 is scanning electron microscope (SEM) photo prepared by example 3.
Fig. 4 is the X ray diffracting spectrum (being scheelite phase) prepared by example 1-3.
Specific embodiment
Below by way of specific embodiment be used for further illustrate the present invention description method, it is not intended that the present invention is limited to these
Embodiment.
Embodiment 1：
A kind of preparation method of flower ball-shaped calcium molybdate, comprises the steps：
(1) a certain amount of calcium chloride and 0.006g EDTA are weighed in beaker, adds appropriate distilled water, abundant magnetic force to stir
Mix；
(2) a certain amount of sodium molybdate is weighed in beaker, add appropriate distilled water, abundant magnetic agitation；
(3) sodium molybdate solution is poured in the beaker for filling calcium chloride solution；
(4) solution is continued into magnetic agitation 15 minutes, is moved in ultrasonic cleaner afterwards, ultrasonic half an hour；
(5) by respectively washing three times of the precipitation distilled water for obtaining and ethanol, be placed in and 6h be dried in 60 DEG C of baking ovens and obtain flower ball-shaped
Calcium molybdate.
Product obtained by preparing is scanned through electron microscope observation, and as seen from Figure 1, the calcium molybdate for obtaining is flower ball-shaped.
By X-ray diffraction analysis, according to JCPDS-ICDD 7-212, it is pure scheelite knot to obtain which to calcium molybdate obtained by preparing
Structure.
Embodiment 2：
A kind of preparation method of flower ball-shaped calcium molybdate, comprises the steps：
(1) a certain amount of calcium chloride and 0g EDTA are weighed in beaker, appropriate distilled water, abundant magnetic agitation is added；
(2) a certain amount of sodium molybdate is weighed in beaker, add appropriate distilled water, abundant magnetic agitation；
(3) sodium molybdate solution is poured in the beaker for filling calcium chloride solution；
(4) solution is continued into magnetic agitation 15 minutes, is moved in ultrasonic cleaner afterwards, ultrasonic half an hour；
(5) by respectively washing three times of the precipitation distilled water for obtaining and ethanol, be placed in and 6h be dried in 60 DEG C of baking ovens and obtain flower ball-shaped
Calcium molybdate.
Embodiment 3：
A kind of preparation method of flower ball-shaped calcium molybdate, comprises the steps：
(1) a certain amount of calcium chloride and 0.012g EDTA are weighed in beaker, adds appropriate distilled water, abundant magnetic force to stir
Mix；
(2) a certain amount of sodium molybdate is weighed in beaker, add appropriate distilled water, abundant magnetic agitation；
(3) sodium molybdate solution is poured in the beaker for filling calcium chloride solution；
(4) solution is continued into magnetic agitation 15 minutes, is moved in ultrasonic cleaner afterwards, ultrasonic half an hour；
(5) by respectively washing three times of the precipitation distilled water for obtaining and ethanol, be placed in and 6h be dried in 60 DEG C of baking ovens and obtain flower ball-shaped
Calcium molybdate.
Claims (3)
1. a kind of preparation method of flower ball-shaped calcium molybdate, which comprises the steps：
(1) a certain amount of calcium chloride and EDTA are weighed in beaker, appropriate distilled water, abundant magnetic agitation is added；
(2) a certain amount of sodium molybdate is weighed in beaker, add appropriate distilled water, abundant magnetic agitation；
(3) sodium molybdate solution is poured in the beaker for filling calcium chloride solution；
(4) solution is continued into magnetic agitation 15 minutes, is moved in ultrasonic cleaner afterwards, ultrasonic half an hour；
(5) by respectively washing three times of the precipitation distilled water for obtaining and ethanol, be placed in and 6h be dried in 60 DEG C of baking ovens and spent
Spherical calcium molybdate.
2. the method for preparing flower ball-shaped calcium molybdate according to claim 1, it is characterised in that EDTA used is respectively
0g, 0.006g and 0.012g.
3. it is pure scheelite-type structure calcium molybdate by the product obtained by claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510603430.7A CN106542579A (en) | 2015-09-17 | 2015-09-17 | A kind of preparation method of flower ball-shaped calcium molybdate |
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| CN201510603430.7A CN106542579A (en) | 2015-09-17 | 2015-09-17 | A kind of preparation method of flower ball-shaped calcium molybdate |
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| CN106542579A true CN106542579A (en) | 2017-03-29 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106915774A (en) * | 2017-05-04 | 2017-07-04 | 洛阳理工学院 | A kind of preparation method of barium molybdate nano piece self assembly ball |
| CN109663590A (en) * | 2018-12-29 | 2019-04-23 | 泉州师范学院 | It is a kind of using egg shell as catalysis material of reactor and the preparation method and application thereof |
| CN109810706A (en) * | 2019-01-15 | 2019-05-28 | 河北大学 | One type laurustinus shape mixes europium calcium molybdate raw powder's production technology |
| CN110040779A (en) * | 2019-05-05 | 2019-07-23 | 河南师范大学 | A kind of preparation method of calcium molybdate luminescent material |
| CN111704164A (en) * | 2020-07-01 | 2020-09-25 | 洛阳理工学院 | Preparation method of barium molybdate flower-like crystal |
| CN114632528A (en) * | 2022-03-30 | 2022-06-17 | 青岛科技大学 | Cadmium selenide/calcium molybdate photocatalyst and preparation method and application thereof |
-
2015
- 2015-09-17 CN CN201510603430.7A patent/CN106542579A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106915774A (en) * | 2017-05-04 | 2017-07-04 | 洛阳理工学院 | A kind of preparation method of barium molybdate nano piece self assembly ball |
| CN106915774B (en) * | 2017-05-04 | 2018-05-22 | 洛阳理工学院 | A kind of preparation method of barium molybdate nano piece self assembly ball |
| CN109663590A (en) * | 2018-12-29 | 2019-04-23 | 泉州师范学院 | It is a kind of using egg shell as catalysis material of reactor and the preparation method and application thereof |
| CN109810706A (en) * | 2019-01-15 | 2019-05-28 | 河北大学 | One type laurustinus shape mixes europium calcium molybdate raw powder's production technology |
| CN110040779A (en) * | 2019-05-05 | 2019-07-23 | 河南师范大学 | A kind of preparation method of calcium molybdate luminescent material |
| CN110040779B (en) * | 2019-05-05 | 2021-07-13 | 河南师范大学 | Preparation method of calcium molybdate luminescent material |
| CN111704164A (en) * | 2020-07-01 | 2020-09-25 | 洛阳理工学院 | Preparation method of barium molybdate flower-like crystal |
| CN111704164B (en) * | 2020-07-01 | 2023-01-24 | 洛阳理工学院 | Preparation method of barium molybdate flower-like crystal |
| CN114632528A (en) * | 2022-03-30 | 2022-06-17 | 青岛科技大学 | Cadmium selenide/calcium molybdate photocatalyst and preparation method and application thereof |
| CN114632528B (en) * | 2022-03-30 | 2023-07-25 | 青岛科技大学 | Cadmium selenide/calcium molybdate photocatalyst and preparation method and application thereof |
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