CN114105196A - Method for preparing bismuth vanadate superfine powder by gel combustion method and bismuth vanadate powder prepared by method - Google Patents
Method for preparing bismuth vanadate superfine powder by gel combustion method and bismuth vanadate powder prepared by method Download PDFInfo
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- CN114105196A CN114105196A CN202111338782.6A CN202111338782A CN114105196A CN 114105196 A CN114105196 A CN 114105196A CN 202111338782 A CN202111338782 A CN 202111338782A CN 114105196 A CN114105196 A CN 114105196A
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Abstract
The invention relates to the technical field of inorganic substance powder preparation, and discloses a method for preparing bismuth vanadate superfine powder by a gel combustion method and bismuth vanadate powder prepared by the method. The method comprises the following steps: (1) gel formation: dissolving bismuth nitrate, vanadyl nitrate and citric acid in absolute ethyl alcohol and deionized water, stirring and mixing, and heating and evaporating the obtained mixed solution to obtain transparent gel; (2) and (3) combustion reaction: heating the transparent gel obtained in the step (1) to enable the transparent gel to be self-ignited, so as to obtain loose orange-red precursor powder; (3) and (3) calcining: and (3) calcining the precursor powder obtained in the step (2) to obtain bright yellow bismuth vanadate powder. The bismuth vanadate powder prepared by the method has superfine particle size (average particle size is less than 100nm), does not agglomerate and has wider practicability.
Description
Technical Field
The invention relates to the technical field of preparation of inorganic substance powder, in particular to a method for preparing bismuth vanadate superfine powder by a gel combustion method and bismuth vanadate powder prepared by the method.
Background
The bismuth vanadate pigment has no toxicity and colorHigh saturation, etc., and has gradually become a substitute for chrome yellow and cadmium yellow pigments. At the same time, BiVO4As a non-toxic and harmless photocatalyst with high activity and good stability, the photocatalyst can absorb visible light to decompose water to prepare oxygen, can degrade organic matters, wastewater and the like, and has extremely important application value. Bismuth vanadate has 3 crystal structures of monoclinic scheelite, tetragonal scheelite and tetragonal zircon types, wherein the monoclinic scheelite type has a narrower band gap (EV ═ 2.34eV) and exhibits better photocatalytic capability. The nanometer material can produce small scale effect, quantum effect and surface effect owing to its special structure, so that it is different from traditional material in light, electricity, heat and other aspects, and has the characteristics of absorption, catalysis, adsorption, etc.
In the prior art, the preparation method of bismuth vanadate powder mainly comprises a high-temperature solid phase method, a chemical precipitation method and the like. CN107629482B provides a method for preparing bismuth vanadate orange pigment by a coprecipitation method, which comprises the steps of uniformly mixing a dilute nitric acid solution of a vanadium compound, a bismuth compound, aluminum nitrate, cerium nitrate and zinc nitrate with a molybdenum compound aqueous solution, adding ammonia water as a precipitator to obtain a bismuth vanadate precursor, and calcining at high temperature to obtain nano bismuth vanadate powder. CN109110811A reports that bismuth vanadate yellow powder is prepared by taking bismuth oxide and vanadium oxide as reaction raw materials and performing ball milling at high temperature by adopting a solid-phase sintering method. However, the existing chemical precipitation method and the high-temperature solid phase method respectively have the problems of easy product agglomeration, poor product quality controllability and the like, and restrict the mass production of the bismuth vanadate.
Disclosure of Invention
The invention aims to overcome the defects of easy agglomeration of bismuth vanadate powder products and poor product quality controllability existing in the existing method for preparing bismuth vanadate powder, and provides a method for preparing bismuth vanadate superfine powder by a gel combustion method and the bismuth vanadate powder prepared by the method, wherein the bismuth vanadate powder prepared by the method has superfine granularity (the average granularity is less than 100nm) and is not agglomerated.
In order to achieve the above object, a first aspect of the present invention provides a method for preparing bismuth vanadate ultrafine powder by a gel combustion method, comprising the following steps:
(1) gel formation: dissolving bismuth nitrate, vanadyl nitrate and citric acid in absolute ethyl alcohol and deionized water, stirring and mixing, and heating and evaporating the obtained mixed solution to obtain transparent gel;
(2) and (3) combustion reaction: heating the transparent gel obtained in the step (1) to enable the transparent gel to be self-ignited, so as to obtain loose orange-red precursor powder;
(3) and (3) calcining: and (3) calcining the precursor powder obtained in the step (2) to obtain bright yellow bismuth vanadate powder.
The invention provides bismuth vanadate powder prepared by the method.
In the method for preparing bismuth vanadate ultrafine powder by the gel combustion method, the sol-gel process and the low-temperature self-combustion process are combined together, so that the method has the advantages of the sol-gel process and the low-temperature self-combustion process, is simple in operation process, relatively low in cost, high in crystallinity, ultrafine in synthesized powder granularity, and has a good application prospect. The bismuth vanadate powder prepared by the method has superfine particle size (average particle size is less than 100nm), does not agglomerate and has wider practicability.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for preparing bismuth vanadate superfine powder by adopting a gel-combustion method, which mainly comprises the steps of forming gel, carrying out combustion reaction and calcining to prepare bismuth vanadate. Specifically, the method for preparing the bismuth vanadate superfine powder by the gel combustion method comprises the following steps:
(1) gel formation: dissolving bismuth nitrate, vanadyl nitrate and citric acid in absolute ethyl alcohol and deionized water, stirring and mixing, and heating and evaporating the obtained mixed solution to obtain transparent gel;
(2) and (3) combustion reaction: heating the transparent gel obtained in the step (1) to enable the transparent gel to be self-ignited, so as to obtain loose orange-red precursor powder;
(3) and (3) calcining: and (3) calcining the precursor powder obtained in the step (2) to obtain bright yellow bismuth vanadate powder.
In step (1), the amounts of bismuth nitrate and vanadyl nitrate may be selected within a wide range, for example, bismuth nitrate may be in a suitable excess or vanadyl nitrate may be in a suitable excess. However, in order to fully utilize the raw materials and avoid material waste, it is most preferable that the amounts of bismuth nitrate and vanadyl nitrate are such that n is satisfiedBi/nV＝1:1。
In step (1), the volume ratio of the absolute ethanol to the deionized water may be 0.8:1 to 1:0.8, preferably 0.95:1 to 1: 0.95. In the most preferred embodiment, anhydrous ethanol and deionized water are used in a volume ratio of 1: 1.
In the step (1), the mass ratio of the total amount of bismuth nitrate and vanadyl nitrate to the amount of citric acid may be 1: 0.1 to 5, preferably 1: 0.2 to 4, most preferably 1: 0.4-3.
In step (1), most preferably, the heating and evaporating process is carried out in a water bath at 60-90 ℃ under magnetic stirring.
In step (2), the process of heating the transparent gel is carried out in an oven. More preferably, the temperature in the oven is 200 ℃.
In step (3), the temperature of the calcination is preferably 400-450 ℃.
In step (3), the calcination time is preferably 0.5 to 2 hours.
According to a preferred embodiment of the present invention, the method for preparing bismuth vanadate ultrafine powder by using a gel combustion method comprises:
(1) gel formation: according to nBi/nV1:1 scaleDissolving a certain amount of bismuth nitrate, vanadyl nitrate and citric acid in absolute ethyl alcohol and deionized water, and stirring to uniformly mix the bismuth nitrate, the vanadyl nitrate and the citric acid, wherein the volume ratio of the absolute ethyl alcohol to the deionized water is 1:1, mixing, and continuously evaporating in a water bath at 60-90 ℃ under magnetic stirring to obtain transparent gel;
(2) and (3) combustion reaction: placing the transparent gel prepared in the step (1) in an oven at 200 ℃, and spontaneous combustion can occur after several minutes to obtain loose orange-red precursor powder;
(3) and (3) calcining: calcining the precursor powder prepared in the step (2) at the temperature of 400-450 ℃ for 0.5-2h to obtain bright yellow bismuth vanadate superfine powder.
The invention also provides bismuth vanadate superfine powder prepared by the gel combustion method. The bismuth vanadate powder has superfine granularity (average granularity is less than 100nm), does not agglomerate and has wider practicability.
The present invention will be described in detail below by way of examples. In the following examples, bismuth nitrate, vanadyl nitrate, citric acid, absolute ethanol, and deionized water were all commercially available.
In the following examples and comparative examples, the particle size of bismuth vanadate powder products was measured using a nanometer particle sizer.
Example 1
This example is provided to illustrate the process of preparing bismuth vanadate powder by the gel combustion method according to the present invention.
According to nBi/nVWeighing 7.9g of bismuth nitrate, 2.9g of vanadyl nitrate and 10g of citric acid in 1:1, dissolving in 100ml of absolute ethanol and 100ml of deionized water, stirring to mix uniformly, and continuously evaporating in a water bath at 60 ℃ under magnetic stirring to obtain transparent gel.
And (3) placing the transparent gel in an oven at 200 ℃, and spontaneous combustion occurs after a plurality of minutes to obtain loose orange-red precursor powder.
And calcining the precursor powder at 400 ℃ for 2h to obtain bright yellow bismuth vanadate powder with the average particle size of less than 100nm, wherein the bismuth vanadate powder is fully dispersed and does not have an agglomeration phenomenon.
Example 2
This example is provided to illustrate the process of preparing bismuth vanadate powder by the gel combustion method according to the present invention.
According to nBi/nV23.7g of bismuth nitrate, 8.7g of vanadyl nitrate and 14g of citric acid were weighed out in 1:1 and dissolved in 100ml of absolute ethanol and 100ml of deionized water, and the mixture was stirred to be uniformly mixed and continuously evaporated in a water bath at 90 ℃ under magnetic stirring to obtain a transparent gel.
And (3) placing the transparent gel in an oven at 200 ℃, and spontaneous combustion occurs after a plurality of minutes to obtain loose orange-red precursor powder.
And calcining the precursor powder at the temperature of 450 ℃ for 1h to obtain bright yellow bismuth vanadate powder with the average particle size of less than 100nm, wherein the bismuth vanadate powder is fully dispersed and does not have an agglomeration phenomenon.
Example 3
This example is provided to illustrate the process of preparing bismuth vanadate powder by the gel combustion method according to the present invention.
According to nBi/nVWeighing 3.95g of bismuth nitrate, 1.45g of vanadyl nitrate and 8g of citric acid in 1:1, dissolving in 100ml of absolute ethanol and 100ml of deionized water, stirring to mix uniformly, and continuously evaporating in a water bath at 70 ℃ under magnetic stirring to obtain transparent gel.
And (3) placing the transparent gel in an oven at 200 ℃, and spontaneous combustion occurs after a plurality of minutes to obtain loose orange-red precursor powder.
And calcining the precursor powder at 400 ℃ for 2h to obtain bright yellow bismuth vanadate powder with the average particle size of less than 100nm, wherein the bismuth vanadate powder is fully dispersed and does not have an agglomeration phenomenon.
Comparative example 1
This comparative example is used to illustrate the process of preparing bismuth vanadate powder by the existing coprecipitation method.
Weighing Bi (NO)3)348.5 g, NH4VO312.87 g, dissolved in 50ml of 1mol/L nitric acid, filtered, and added with water to reach the constant concentration of 0.5 mol/L. Ammonium molybdate 1.94 g was weighed, dissolved in 100ml of water and filtered for use.
Weighing Zn (NO)3)32.86 g of cerium nitrate, 0.85 g of cerium nitrate and 2.5 g of aluminum nitrate are dissolved in 1mol/L of dilute nitric acid and filteredAnd (5) standby. And respectively adding the prepared solutions into a bismuth nitrate solution, continuously stirring for 10min, uniformly mixing, and heating to 50 ℃.
Dropping 28 wt% ammonia water into the reaction solution at 30ml/min, with the increase of pH, a large amount of light yellow precipitate appeared, detecting the change by a pH meter, when the pH value is 6, stopping titrating the precipitant, and keeping stirring at the temperature for 2 hours until the precipitate is complete.
The temperature was raised to 90 ℃ and the titration of ammonia was continued until pH 8, at which point the titration was stopped and stirring was continued for 1 hour until a pale yellow precipitate appeared.
And (3) carrying out vacuum filtration on the reaction liquid at room temperature, and drying the filter cake in an oven at 85 ℃ for 4 hours to obtain an orange bismuth vanadate pigment precursor.
And (3) placing the precursor in a muffle furnace, heating to 650 ℃ at the speed of 60 ℃/min, preserving the temperature for 2 hours, and naturally cooling to room temperature to obtain orange bismuth vanadate powder, wherein the orange bismuth vanadate powder has a serious agglomeration phenomenon.
It can be seen from the results of the above examples and comparative examples that the bismuth vanadate powder prepared by the gel combustion method of the present invention has the advantages of fine particle size and no agglomeration.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for preparing bismuth vanadate superfine powder by a gel combustion method is characterized by comprising the following steps:
(1) gel formation: dissolving bismuth nitrate, vanadyl nitrate and citric acid in absolute ethyl alcohol and deionized water, stirring and mixing, and heating and evaporating the obtained mixed solution to obtain transparent gel;
(2) and (3) combustion reaction: heating the transparent gel obtained in the step (1) to enable the transparent gel to be self-ignited, so as to obtain loose orange-red precursor powder;
(3) and (3) calcining: and (3) calcining the precursor powder obtained in the step (2) to obtain bright yellow bismuth vanadate powder.
2. The method according to claim 1, wherein in step (1), the bismuth nitrate and the vanadyl nitrate are used in amounts such that nBi/nV＝1:1。
3. The method according to claim 1 or 2, wherein, in step (1), anhydrous ethanol and deionized water are used in a volume ratio of 1: 1.
4. The method according to claim 1 or 2, wherein in step (1), the mass ratio of the total amount of bismuth nitrate and vanadyl nitrate to the amount of citric acid is 1: 0.4-3.
5. The method according to any one of claims 1 to 4, wherein in step (1), the heating and evaporating process is carried out in a water bath at 60 to 90 ℃ under magnetic stirring.
6. The method according to claim 1, wherein, in the step (2), the process of heating the transparent gel is performed in an oven.
7. The method of claim 6, wherein the oven is operated at a temperature of 200 ℃.
8. The method as claimed in claim 1, wherein, in the step (3), the temperature of the calcination is 400-450 ℃.
9. The method according to claim 1, wherein in step (3), the calcination is carried out for a time of 0.5 to 2 hours.
10. Bismuth vanadate powder prepared by the method of any one of claims 1 to 9.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116178990A (en) * | 2022-12-05 | 2023-05-30 | 成都先进金属材料产业技术研究院股份有限公司 | Preparation method of coated bismuth vanadate powder |
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| WO2014005491A1 (en) * | 2012-07-03 | 2014-01-09 | 广东先导稀材股份有限公司 | Method for preparing bismuth vanadate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2014005491A1 (en) * | 2012-07-03 | 2014-01-09 | 广东先导稀材股份有限公司 | Method for preparing bismuth vanadate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116178990A (en) * | 2022-12-05 | 2023-05-30 | 成都先进金属材料产业技术研究院股份有限公司 | Preparation method of coated bismuth vanadate powder |
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