CN115650190A - Method for synthesizing bismuth phosphate powder by room-temperature solid-phase method - Google Patents
Method for synthesizing bismuth phosphate powder by room-temperature solid-phase method Download PDFInfo
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Abstract
The invention discloses a method for synthesizing bismuth phosphate powder by a room-temperature solid-phase method, and relates to the technical field of preparation of bismuth phosphate. The invention comprises the following steps: s1: weighing Bi (NO) 3 ) 3 ·5H 2 2 to 5g of O (pentahydrate bismuth nitrate) powder 2 PO 4 ·12H 2 2.5-5.5 g of O (disodium hydrogen phosphate dodecahydrate); s2: mixing the above Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 Grinding the O in a mortar respectively; s3: grinding the Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 O, mixing and uniformly stirring to obtain mixed powder; s4: placing the mixed powder inGrinding in a mortar; s5: washing the ground mixed powder with pure water, and performing centrifugal separation; s6: and (3) drying the mixed powder after centrifugal separation in a drying box to obtain powder, namely the bismuth phosphate nano powder. The method does not need complex and expensive equipment, and has the advantages of simple operation, low cost and high yield.
Description
Technical Field
The invention relates to the technical field of preparation of bismuth phosphate, in particular to a method for synthesizing bismuth phosphate powder by a room-temperature solid-phase method.
Background
Bismuth phosphate is used as a novel bismuth-based photocatalytic material, the band gap width at room temperature is 3.85eV, the bismuth phosphate has excellent conductivity, and the transfer of photogenerated carriers is promoted 4 (bismuth phosphate) nanorods having higher catalytic activity than commercial titanium dioxide (P-25); by changing the solvent of room temperature coprecipitation method, eu (europium element, lanthanide series element, no. 63) with controllable phase and different Eu content can be successfully prepared 3+ (europium ion) -doped bismuth phosphate nanocrystals; the temperature and the pH value of a hydrothermal method are adjusted to controllably prepare hexagonal phase, low-temperature monoclinic phase and high-temperature monoclinic phase bismuth phosphate; the methods can enable the bismuth phosphate nanostructure to have the characteristics of high purity, controllable morphology and the like, but all the methods need relatively complicated equipment, have long synthesis time and low yield, and are not beneficial to large-scale industrial production, so that a method for synthesizing bismuth phosphate powder by a room-temperature solid-phase method is urgently needed to solve the problems.
Disclosure of Invention
The invention aims to solve the technical problems and provides a method for synthesizing bismuth phosphate powder by a room-temperature solid-phase method, which does not need complex and expensive equipment, and has the advantages of simple operation, low cost and high yield.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a room temperature solid phase method for synthesizing bismuth phosphate powder comprises the following steps:
s1: weighing Bi (NO) 3 ) 3 ·5H 2 O (Mirabilitum pentahydrate)Bismuth acid) powder 2 to 5g, naH 2 PO 4 ·12H 2 2.5-5.5 g of O (disodium hydrogen phosphate dodecahydrate) powder;
s2: mixing the above Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 Grinding the O in a mortar respectively;
s3: grinding the Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 O, mixing and uniformly stirring to obtain mixed powder;
s4: putting the mixed powder into a mortar for grinding;
s5: washing the ground mixed powder with pure water, and performing centrifugal separation;
s6: and (3) drying the mixed powder after centrifugal separation in a drying box to obtain powder, namely the bismuth phosphate nano powder.
As a modification, the chemicals used in S1 are all analytically pure.
As a modification, the grinding time in S2 is 2 to 5 minutes.
As an improvement, the mortar in the S2 is an agate mortar, the agate mortar is suitable for advanced grinding of laboratories, pharmaceutical factories and chemical laboratories, has high compressive strength and acid and alkali resistance, and no mortar body substance is mixed into ground materials after grinding.
As an improvement, the mortar in the S4 is an agate mortar, and the grinding time is 3-8 minutes.
As a modification, the purity of the pure water in S5 is analytical purity.
As an improvement, the drying temperature in the S6 is 50-70 ℃.
After adopting the structure, the invention has the following advantages:
1. the method does not need complex and expensive equipment, has simple equipment and preparation process, simple and convenient operation, capability of preparing a large amount of materials, low cost, high yield, contribution to industrial production, high purity of the prepared materials and small particles;
2. the invention can prepare the nanometer material in shorter reaction time, and the dispersion material and the control agent do not participate in the reaction process, are both easy to dissolve in water and clean, and the whole process has simple and easy method, low operation cost, suitability for flow process, no impurity, recyclable reaction waste treatment, small environmental pollution and wide application range.
The foregoing summary is provided for the purpose of description only and is not intended to be limiting in any way. In addition to the illustrative aspects, embodiments, and features described above, further aspects, embodiments, and features of the present invention will be readily apparent by reference to the drawings and following detailed description.
Drawings
Fig. 1 is an X-ray diffraction (XRD) structure spectrum of bismuth phosphate nano-powder prepared in the first embodiment of a method for synthesizing bismuth phosphate powder by a room temperature solid phase method according to the present invention.
FIG. 2 shows BiPO in the first embodiment of the method for synthesizing bismuth phosphate powder by room temperature solid phase method 4 Scanning electron microscope photographs of the nanocrystals at low magnification (a) and at high magnification (b).
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the embodiments or technical descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Detailed Description
In the following, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature, and not as restrictive.
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
With reference to fig. 1-2, a room temperature solid phase method for synthesizing bismuth phosphate powder comprises the following steps:
s1: weighing proper amount of Bi (NO) 3 ) 3 ·5H 2 O (bismuth nitrate pentahydrate) powder and NaH 2 PO 4 ·12H 2 O (disodium hydrogen phosphate dodecahydrate) powder;
s2: mixing the above Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 Grinding the O in a mortar respectively;
s3: grinding the Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 Mixing and uniformly stirring O to obtain mixed powder;
s4: putting the mixed powder into a mortar for grinding;
s5: washing the ground mixed powder with pure water, and performing centrifugal separation;
s6: and (3) drying the mixed powder after centrifugal separation in a drying box to obtain powder, namely the bismuth phosphate nano powder.
Example one
Weighing Bi (NO) 3 ) 3 ·5H 2 3g of O (bismuth nitrate pentahydrate) powder 2 PO 4 ·12H 2 O (disodium hydrogen phosphate dodecahydrate) powder 3.7g, bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 The purity of O is analytically pure;
mixing the above Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 Grinding the O in agate mortars for 3 minutes respectively;
grinding the Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 Mixing and uniformly stirring O to obtain mixed powder;
grinding the mixed powder in an agate mortar for 5 minutes;
washing the ground mixed powder with pure water, wherein the purity of the pure water is analytically pure, and performing centrifugal separation;
and (3) drying the centrifugally separated mixed powder in a drying oven at 60 ℃, wherein the obtained powder is the bismuth phosphate nano powder.
Prepared BiPO 4 The mass of the nanocrystal was 1.782g, calculated as BiPO synthesized by room temperature solid phase reaction 4 The yield of the nano-crystal is 92%, and it can be seen from fig. 1 that the purity of the bismuth phosphate powder is very high, and no other impurity peak is found, and the comparison with the XRD standard card library proves that the prepared bismuth phosphate nano-powder is hexagonal BiPO 4 (JCPDS card file No. 45-1370), four main peaks (2 θ =20.1 °, 29.0 °, 31.3 °, and 41.8 °) respectively correspond to hexagonal-phase BiPO 4 The (101), (111), (102) and (211) planes of (a), thus indicating that the bismuth phosphate powder is of the allite type; FIG. 2 shows that the prepared bismuth phosphate nanopowder is mainly irregular particles with a diameter within 100 nm.
Example two
Weighing Bi (NO) 3 ) 3 ·5H 2 2g of O (bismuth nitrate pentahydrate) powder 2 PO 4 ·12H 2 O (disodium hydrogen phosphate dodecahydrate) powder 2.5g 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 The purity of O is analytically pure;
mixing the above Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 Grinding O in agate mortars for 2 minutes;
grinding the Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 O, mixing and uniformly stirring to obtain mixed powder;
grinding the mixed powder in an agate mortar for 3 minutes;
washing the ground mixed powder with pure water, wherein the purity of the pure water is analytically pure, and performing centrifugal separation;
and (3) drying the centrifugally separated mixed powder in a drying oven at 50 ℃, wherein the obtained powder is the bismuth phosphate nano powder.
EXAMPLE III
Weighing Bi (NO) 3 ) 3 ·5H 2 O (bismuth nitrate pentahydrate) powder 5g 2 PO 4 ·12H 2 O (disodium hydrogen phosphate dodecahydrate) powder 5.5g 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 The purity of O is analytically pure;
mixing the above Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 Grinding the O in agate mortars for 5 minutes respectively;
grinding the Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 Mixing and uniformly stirring O to obtain mixed powder;
grinding the mixed powder in an agate mortar for 8 minutes;
washing the ground mixed powder with pure water, wherein the purity of the pure water is analytically pure, and performing centrifugal separation;
and (3) drying the centrifugally separated mixed powder in a drying oven at 70 ℃, wherein the obtained powder is the bismuth phosphate nano powder.
The present invention and its embodiments have been described above, and the description is not intended to be limiting, and the drawings are only one embodiment of the present invention, and the actual structure is not limited thereto. In summary, those skilled in the art should be able to conceive of the present invention without creative design of the similar structural modes and embodiments without departing from the spirit of the present invention, and all of them should fall into the protection scope of the present invention.
Claims (7)
1. A room temperature solid phase method for synthesizing bismuth phosphate powder is characterized in that: the method comprises the following steps:
s1: weighing Bi (NO) 3 ) 3 ·5H 2 2 to 5g of O (bismuth nitrate pentahydrate) powder 2 PO 4 ·12H 2 2.5-5.5 g of O (disodium hydrogen phosphate dodecahydrate) powder;
s2: mixing the above Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 Grinding the O in a mortar respectively;
s3: grinding the Bi (NO) 3 ) 3 ·5H 2 O and NaH 2 PO 4 ·12H 2 Mixing and uniformly stirring O to obtain mixed powder;
s4: grinding the mixed powder in a mortar;
s5: washing the ground mixed powder with pure water, and performing centrifugal separation;
s6: and (3) drying the centrifugally separated mixed powder in a drying box to obtain powder, namely the bismuth phosphate nano powder.
2. The room-temperature solid-phase method for synthesizing bismuth phosphate powder according to claim 1, wherein the method comprises the following steps: the purity of the chemicals used in S1 is analytical grade.
3. The room-temperature solid-phase method for synthesizing bismuth phosphate powder according to claim 1, wherein the method comprises the following steps: the grinding time in the step S2 is 2-5 minutes.
4. The room-temperature solid-phase method for synthesizing bismuth phosphate powder according to claim 1, wherein the method comprises the following steps: and the mortar in the S2 is an agate mortar.
5. The room-temperature solid-phase method for synthesizing bismuth phosphate powder according to claim 1, wherein the method comprises the following steps: and in the S4, the mortar is an agate mortar, and the grinding time is 3-8 minutes.
6. The room-temperature solid-phase method for synthesizing bismuth phosphate powder according to claim 1, wherein the method comprises the following steps: the purity of the pure water in the S5 is analytical purity.
7. The room-temperature solid-phase method for synthesizing bismuth phosphate powder according to claim 1, wherein the method comprises the following steps: and the drying temperature in the S6 is 50-70 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103111315A (en) * | 2013-03-15 | 2013-05-22 | 南开大学 | Preparation method of bismuth phosphate (BiPO4) photocatalysts differing in structure |
| EP2796531A1 (en) * | 2011-12-22 | 2014-10-29 | GC Corporation | Agent for imparting fluorescence to ceramic |
| CN104477869A (en) * | 2014-12-31 | 2015-04-01 | 新疆大学 | Method for synthesizing bismuth phosphate nano particles by room-temperature solid-phase chemical method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2796531A1 (en) * | 2011-12-22 | 2014-10-29 | GC Corporation | Agent for imparting fluorescence to ceramic |
| CN103111315A (en) * | 2013-03-15 | 2013-05-22 | 南开大学 | Preparation method of bismuth phosphate (BiPO4) photocatalysts differing in structure |
| CN104477869A (en) * | 2014-12-31 | 2015-04-01 | 新疆大学 | Method for synthesizing bismuth phosphate nano particles by room-temperature solid-phase chemical method |
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