CN1821088A - Process for preparing bismuth silicate nano powder and use - Google Patents
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Abstract
The present invention relates to preparation process and application of nanometer Bi12SiO20 powder. The preparation process of nanometer Bi12SiO20 powder includes the first dissolving Bi salt in one solvent to form Bi containing solution of Bi salt concentration 0.5-5 M, adding organic Si compound in the Bi/Si molar ratio of 12 into the Bi containing solution to form homogeneous sol through full stirring, evaporating the sol at normal or negative pressure to obtain dry precursor powder, and final sintering the precursor powder in aerobic condition to obtain the nanometer Bi12SiO20 powder. The present invention realizes the homogeneous mixing of initial materials in molecular size, so as to prepare nanometer Bi12SiO20 powder with high purity and high crystallization degree in relatively low temperature and relatively short time. The nanometer Bi12SiO20 powder has high photocatalytic activity and may be used in photocatalysis to degrade one pollutant.
Description
Technical Field
The invention relates to bismuth silicate (Bi)12SiO20) The preparation method of the nano powder, the prepared bismuth silicate nano powder can be used as a photocatalyst, and belongs to the technical field of material science photocatalysts.
Background
Bismuth silicate (Bi)12SiO20) The crystal belongs to a cubic crystal system, I23 point group, gamma-Bi2O3And (5) structure. It has excellent electrooptical, photoconductive, photorefractive and piezoelectric effectsThe method has wide application prospect in the fields of electronics, optical information storage, optical calculation and the like.
At present, the method for growing bismuth silicate single crystal at home and abroad adopts a self-melting liquid pulling method. The method adopts high-purity Bi2O3And SiO2The powder is used as raw material, mixed according to the mol ratio of 6: 1, melted at the high temperature of about 900 ℃, and then the bismuth silicate single crystal is prepared by a pulling method.
And few documents relate to the preparation method and the application of the bismuth silicate nano powder. The traditional solid phase reaction sintering method can be used for preparing bismuth silicate powder, namely Bi2O3And SiO2Mixing the powders, and performing solid phase reaction Thus obtaining the product. The method has the disadvantages that the two raw materials are difficult to be uniformly mixed, so that the solid-phase sintering needs higher temperature (above 800 ℃) and longer time (5-15 hours) to obtain a single-phase target product, and crystal grains grow up and agglomerate at high temperature, so that nano-scale powder is difficult to obtain. At the same time due to Bi2O3Unavoidable volatilization occurs at temperatures in excess of 800 c, andthus heat treatment at high temperatures can cause the synthesized product to deviate from the ideal stoichiometric ratio.
Among the known documents, only the document (Journal of Materials Science Letters 18(1999)1871-1874) discloses a method for preparing bismuth silicate nanopowders by mechanical alloying. The method is to use Bi2O3And SiO2The powder is used as raw material to prepare bismuth silicate nano powder directly by high-energy ball milling, and is characterized in that the target product is synthesized by utilizing the mechanical alloying reaction of the two powders in the process of repeatedly colliding and crushing, so that Bi can be obtained without additional high-temperature heat treatment12SiO20Nano powder, so that the defects of the solid-phase reaction sintering method can be avoided. However, the mechanical alloying method requires a long time (more than 7 hours), has low production efficiency, and is not suitable for a practical method for producing bismuth silicate nano powder in batches. Moreover, the high-energy ball milling process for a long time inevitably leads to a grinding systemImpurities are introduced into the grinding container and the grinding ball to cause pollution, so that the high-purity bismuth silicate nano powder is difficult to obtain. This is very disadvantageous for the use of bismuth silicates in the fields of optoelectronics and photocatalysis.
In recent years, semiconductor photocatalysis technology has attracted much attention in the aspects of environmental governance, hydrogen production by photocatalytic water decomposition, and the like. Broadening the spectral response of the photocatalyst, improving the photocatalytic quantum efficiency and the photocatalytic reaction speed are the main directions for developing novel photocatalysts.
Hitherto, as to Bi12SiO20Theapplication of the nano powder in the field of the photocatalyst is not reported in relevant documents.
Disclosure of Invention
The invention aims to provide a preparation method of bismuth silicate nano powder, which adopts simple process and equipment to obtain high-purity bismuth silicate nano powder with small particle size and good crystallization and can be used as a photocatalyst.
In order to achieve the purpose, the technical scheme adopted by the invention is that bismuth salt is firstly dissolved in an organic solvent to form a bismuth-containing solution with the bismuth salt concentration of 0.5-5M, then an organic silicon compound is added into the bismuth-containing solution according to the molar ratio of Bi to Si of 12 to 1, the mixture is fully stirred to form uniform sol, the sol is evaporated at normal pressure or negative pressure to obtain dry precursor powder, and finally the precursor powder is sintered in an aerobic environment to prepare Bi with good purity and crystallinity in a lower temperature and a shorter time12SiO20And (3) nano powder. Bi12SiO20The nano powder shows high-efficiency photocatalytic activity and can be used for photocatalytic degradation of organic pollutants.
The method specifically comprises the following steps:
1. dissolving bismuth salt in an organic solvent to form a bismuth-containing solution with the bismuth salt concentration of 0.5-5M.
2. Adding the organic silicon compound into the bismuth-containing solution according to the molar ratio Bi to Si of 12 to 1, and fully stirring to form uniform sol.
3. And (3) evaporating the sol at normal pressure or negative pressure, wherein the evaporation temperature is controlled tobe 100-350 ℃, and thus dry precursor powder is obtained.
4. Sintering the precursor powder in an aerobic environment, wherein the sintering temperature is 500-700 ℃, and the sintering time is 0.5-4 hours, so as to obtain the bismuth silicate nano powder.
The bismuth silicate nano powder prepared by the method of the invention shows excellent performance and good application prospect in the aspect of photocatalytic degradation of organic pollutants.
The bismuth salt is nitrate, acetate or carbonate of bismuth. If the aforementioned bismuth salt contains crystal water, the crystal water should be removed by drying before use. When glacial acetic acid is used as the organic solvent, the bismuth salt containing the water of crystallization can be used without having to remove the water of crystallization beforehand.
The organosilicon compounds of the invention are alkoxysilanes, including tetramethoxysilane (CH)2O)4Si, tetraethoxysilane (C)2H5O)4Si and tetrapropoxysilane (C)3H7O)4Si, or the corresponding silanes after substitution of the alkoxy group (i.e. methoxy, ethoxy or propoxy) with an alkyl moiety, e.g. methyltrimethoxysilane CH3Si(OCH2)3Methyl triethoxysilane CH3Si(OC2H5)3Dimethyl dimethoxy silane (CH)3)2Si(OCH3)2Dimethyl diethoxy silane CH3)2Si(OC2H5)2And the like.
The organic solvent is glacial acetic acid, absolute ethyl alcohol, absolute isopropanol or absolute acetone. Glacial acetic acid is preferred. Glacial acetic acid has good solubility to bismuth salt, and acetate has strong complexation effect to bismuth ions, and can effectively inhibit hydrolysis of bismuth salt, so that when glacial acetic acid is used as organic solvent, bismuth salt containing crystal water can be used.
The evaporation in the invention refers to normal pressure evaporation or negative pressure evaporation. The evaporation temperature may be selected depending on the boiling point of the solvent. A relatively low evaporation temperature is selected for the lower boiling solvent and a higher evaporation temperature is selected for the higher boiling solvent. In the case of negative pressure evaporation, a lower evaporation temperature may be selected than in normal pressure evaporation. During the evaporation and drying process of the precursor sol, reactions such as crystal water, volatilization of small molecular organic matters, decomposition and combustion of nitrate radicals and organic matters occur, so that the solvent and part of organic groups are removed, and dry solid precursor powder is obtained.
The organic solvent of the present invention may be ethylene glycol dimethyl ether (CH) other than the organic solvent described above3OCH2CH2OH) or diethylene glycol dimethyl ether (CH)3OCH2CH2)2O as a co-solvent. The glycol dimethyl ether or the diethylene glycol dimethyl ether can promote the dissolution of bismuth salt and silicon salt and can also play a role in regulating the viscosity of the sol. The ratio of the cosolvent to the organic solvent can be adjusted to be 1: 2-1: 5.
The sintering according to the present invention is performed in an oxygen atmosphere, and therefore, the sintering may be performed in air or in an oxygen atmosphere. The sintering temperature can be 500-700 ℃, preferably 550-650 ℃. At too low a temperature, i.e. below 500 ℃, Bi in pure phase is not obtained12SiO20In the case of nano-powder, when the temperature exceeds 700 ℃, Bi iseasily volatilized, so that it is difficult to obtain Bi in a strict stoichiometric ratio12SiO20And (3) nano powder. When the sintering temperature is 500-700 ℃, the sintering time is within 0.5-4 hours. The sintering time can be adjusted according to the sintering temperature, when sintering is carried out at a lower temperature, the sintering time needs to be properly prolonged to ensure the purity of a crystal phase and the crystallization quality, and the specific time can be determined by XRD analysis of a final product. When the temperature is 550-650 ℃ for sintering, the Bi with good crystallization and light yellow color can be obtained within 0.75-1.5 hours of sintering time12SiO20And (3) nano powder.
The method can be used for preparing Bi with the particle size of 20-200 nm12SiO20And (3) nano powder.The particle size of the powder is determined by sintering time and sintering temperature, and nano-powder with different particle sizes can be obtained by different sintering systems. Increasing the sintering temperature and extending the sintering time can lead to grain growth. Therefore, the appropriate sintering temperature and sintering time can be determined according to actual needs.
Bi prepared by the method of the invention12SiO20The semiconductor energy gap of the nano powder is about 2.6-2.8 eV, and the nano powder can absorb visible light with the wavelength of less than 550 nm. Compared with the traditional titanium dioxide (the semiconductor energy gap of which is about 3.2eV and can only absorb ultraviolet light below 400 nm), the light response interval of the photocatalyst is greatly widened, and good conditions are created for photocatalysis by using solar natural light as a light source.
The method has simple process flow and low requirement on equipment, and simultaneously overcomes the defect of uneven mixing of the traditional solid-phase reaction method because the initial raw materials, namely the Bi salt and the Si salt, can achieve the uniform mixing of molecular scale, thereby obtaining the target product with good crystallization at lower temperature in shorter time. Meanwhile, the method can obtain the nano powder with smaller particle size and larger specific surface area.
Bi of the present invention12SiO20The nano powder is applied to a photocatalyst, has excellent photocatalytic activity and good chemical stability, and has good application prospects in the aspects of organic pollutant degradation, indoor air purification, automobile exhaust treatment, photocatalytic water decomposition and the like.
Drawings
FIG. 1 shows Bi prepared by the method of the present invention12SiO20X-ray diffraction pattern of the powder.
FIG. 2 shows Bi prepared by the method of the present invention12SiO20Transmission electron micrograph of the powder.
FIG. 3 shows Bi prepared by the method of the present invention12SiO20Absorption spectrum of the powder.
FIG. 4 shows Bi in the present invention12SiO20In the process of photocatalytic degradation of Congo red dye by powder, the ultraviolet-visible light absorption spectrum of the Congo red aqueous solution changes along with the light irradiation time.
Detailed Description
The technical solution of the present invention is further described below with reference to the accompanying drawings and examples. The following examples are not to be construed as limiting the invention.
Example 1
0.12mol of bismuth nitrate pentahydrate (Bi (NO)3)3·5H2O) dissolved in 180ml of glacial acetic acid (CH)3COOH), and then 0.01mol of tetraethoxysilane ((C)2H5O)4Si) with addition of 60ml of ethylene glycol dimethyl ether (CH)3OCH2CH2OH) is used as a cosolvent to adjust the viscosity of the solution, and the solution is fully stirred to form uniform sol. Evaporating and drying the sol at 150 ℃ to obtain precursor powder. Sintering the precursor powder at 650 ℃ under normal pressure for 0.75 h to obtain Bi12SiO20And (3) nano powder.
Example 2
0.12mol of bismuth acetate (Bi (CH)3COO)3) Dissolved in 60ml of absolute ethanol (CH)3CH2OH) and then 0.01mol of tetrapropoxysilane ((C)3H7O)4Si), stirred well to form a homogeneous sol. Evaporating and drying the sol at 250 ℃ to obtain precursor powder. Sintering the obtained precursor powder at the temperature of 550 ℃ under normal pressure for 1.5 hours to obtain Bi12SiO20 nanometer powder.
Example 3
0.12mol of bismuth carbonate (Bi (CO)3)3) Dissolved in 100ml of anhydrous isopropanol ((CH)3)2CHOH), then 0.01mol of tetramethoxysilane ((CH)2O)4Si) with addition of 20ml of ethylene glycol dimethyl ether (CH)3OCH2CH2OH) is used as a cosolvent to adjust the viscosity of the solution, and the solution is fully stirred to form uniform sol.And (3) evaporating the sol at 100 ℃ under negative pressure, wherein the vacuum degree is-0.1 MPa, and obtaining precursor powder. Sintering the precursor powder at the temperature of 700 ℃ under normal pressure for 0.5 hour to obtain Bi12SiO20And (3) nano powder.
Example 4
0.12mol of bismuth nitrate (Bi (NO)3)3) Dissolved in 60ml of anhydrous acetone (CH)3COCH3) Then, 0.01mol of dimethyldimethoxysilane ((CH) was added dropwise3)2Si(OCH3)2) While adding 30ml of diethylene glycol dimethyl ether (CH)3OCH2CH2)2And O is used as a cosolvent to adjust the viscosity of the solution, and the solution is fully stirred to form uniform sol. Evaporating and drying the sol at 350 ℃ to obtain precursor powder. Sintering the obtained precursor powder at the temperature of 500 ℃ under normal pressure for 4 hours to obtain Bi12SiO20 nanometer powder.
FIG. 1 shows Bi obtained by the process of the present invention12SiO20The X-ray diffraction pattern of the nano powder has the advantages that the positions of all diffraction peaks are in good accordance with JCPDS standard card No.37-0485 of International Union of powder diffraction standards, and the peak shape is sharp, which indicates that the prepared sample is composed of single Bi12SiO20Phase composition and good crystallization.
FIG. 2 shows Bi obtained in example 1 according to the present invention12SiO20A Transmission Electron Microscope (TEM) photograph of the nano-powder can be seen from FIG. 2, the nano-powder is irregular, the particle size is between 20 nm and 100nm, and the average particle size is about 50 nm. The particle size of the powder is determined by sintering time and sintering temperature, and nano-powder with different particle sizes can be obtained by differentsintering systems. Increasing the sintering temperature and extending the sintering time can lead to grain growth. Therefore, an appropriate sintering schedule can be determined according to actual needs.
Bi prepared by the method of the invention12SiO20The semiconductor energy gap of the nano powder is about 2.6 eV. FIG. 3 shows Bi prepared by the method of the present invention12SiO20Absorption spectra of the powders, Bi produced by the method of the present invention can be seen in FIG. 312SiO20The nano powder can absorb the wavelength range between 400nm and 550nmVisible light. Compared with the traditional titanium dioxide (the semiconductor energy gap of which is about 3.2eV, the titanium dioxide can only absorb ultraviolet light below 400nm, the light response interval of the photocatalyst is greatly widened, and good conditions are created for photocatalysis by using solar natural light as a light source.
For evaluation of Bi prepared by the method of the invention12SiO20The nano powder is used as the photocatalytic activity of the photocatalyst, the typical organic compound Congo red containing nitrogen dye which is difficult to degrade is used as a model organic pollutant, and the Bi prepared in the embodiment 1 is used12SiO20The nano powder is used as a photocatalyst to carry out photocatalytic degradation experiments on the Congo red aqueous solution. Accurately weighing 5g/l of Bi12SiO20Adding the nano powder photocatalyst into a beaker filled with 40mg/l Congo red aqueous solution, ultrasonically dispersing for 30 minutes at the dark at room temperature to ensure that the adsorption-desorption balance is achieved between the catalyst and the Congo red solution, and then carrying out a photocatalytic degradation experiment under the condition of magnetic stirring. The light source used was a 250W high pressure mercury lamp, which was about 10cm from the liquid surface. Under the irradiation of a light source, sampling is carried out once every 10 minutes, part of the solution is taken to be subjected to high-speed centrifugal separation, and then the upper layer solution is taken to be detected on a 756MC spectrophotometer to detect the change of the absorbance of the Congo red solution at the position with the maximum absorption peak (500 nm) with time before and after degradation.
FIG. 4 shows Bi in the present invention12SiO20In the process of photocatalytic degradation of Congo red dye by powder, the ultraviolet-visible light absorption spectrum of the Congo red aqueous solution changes along with time. The concrete conditions are as follows: congo red solution with concentration of 40mg/l and Bi12SiO20The loading was 5 g/l. The light irradiation time for each curve in the figure was (a)0 minutes; (b)10 minutes; (c)20 minutes; (d)30 minutes; (e)40 minutes; (f)50 minutes; (g)60 minutes; (h)90 minutes; (i)120 minutes. As can be seen from FIG. 4, the absorbance at the characteristic absorption peaks (. about.500 nm and. about.340 nm) of the Congo red solution gradually decreased with the increase of the irradiation time, and the maximum absorption peak (. about.500 nm) of Congo red gradually decreased until it finally disappeared completely after 1 hour of the photocatalytic reaction,it is shown that azo bonds (-N ═ N-) in Congo red molecules are broken by photocatalytic oxidation, and the color of the solution gradually becomes lighter from orange yellow until finally becoming a colorless transparent solution. Further prolonging the photocatalytic reaction time, another characteristic absorption peak (340 nm) in the ultraviolet region is also gradually reduced. The above experimental results show that in Bi12SiO20Under the photocatalysis of the nano powder, Congo red molecules are effectively degraded, thereby verifying the Bi of the invention12SiO20The photocatalytic effect of the nanopowder.
Claims (8)
1. A preparation method of bismuth silicate nano powder is characterized by comprising the following steps:
1) dissolving bismuth salt in an organic solvent to form a bismuth-containing solution with the bismuth salt concentration of 0.5-5M;
2) adding an organic silicon compound into the bismuth-containing solution according to the molar ratio of Bi to Si of 12 to 1, and fully stirring to form uniform sol;
3) evaporating the sol at normal pressure or negative pressure, and controlling the evaporation temperature to be 100-350 ℃ to obtain dry precursor powder;
4) sintering the precursor powder in an aerobic environment, wherein the sintering temperature is 500-700 ℃, and the sintering time is 0.5-4 hours, so as to obtain the bismuth silicate nano powder.
2. The method for preparing bismuth silicate nanopowder according to claim 1, characterized in that the bismuth salt is bismuth nitrate, acetate or carbonate.
3. The method for preparing bismuth silicate nanopowder according to claim 1, characterized in that the organosilicon compound is alkoxysilane.
4. The method for preparing bismuth silicate nanopowder according to claim 3, characterized in that said alkoxysilane is tetramethoxysilane, tetraethoxysilane or tetrapropoxysilane, or a corresponding silane in which alkoxy groups thereof are partially substituted with alkyl groups.
5. The method for preparing bismuth silicate nanopowder according to claim 1, characterized in that the organic solvent is glacial acetic acid, anhydrous ethanol, anhydrous isopropanol or anhydrous acetone.
6. The method for preparing bismuth silicate nanopowder according to claim 1, wherein the sintering temperature is 550-650 ℃ and the sintering time is 0.75-1.5 hours.
7. The method for preparing bismuth silicate nano powder according to claim 1, characterized in that the bismuth-containing solution further uses ethylene glycol dimethyl ether or diethylene glycol dimethyl ether as a cosolvent, and the ratio of the cosolvent to the organic solvent is controlled to be 1: 2-1: 5.
8. Use of bismuth silicate nanopowders prepared by the process of claim 1 or 7, characterized by being used as a photocatalyst.
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| CN101709508B (en) * | 2009-11-10 | 2011-10-26 | 陕西科技大学 | Preparation method of bismuth-containing eulytite bismuth silicate crystals |
| CN102249252A (en) * | 2011-04-11 | 2011-11-23 | 烟台大学 | New preparation method of Bi12SiO20 |
| CN102275942A (en) * | 2011-07-06 | 2011-12-14 | 陕西科技大学 | Preparation method of bismuth silicate nanopowder |
| CN102275944A (en) * | 2011-07-06 | 2011-12-14 | 陕西科技大学 | Preparation method of new scintillating bismuth silicate powder |
| CN102351513A (en) * | 2011-07-06 | 2012-02-15 | 陕西科技大学 | Preparation method for bismuth silicate powder for utilization of optical performance |
| CN101792181B (en) * | 2010-02-09 | 2012-07-25 | 陕西科技大学 | Preparation method of bismuth silicate nanocrystalline |
| CN103949655A (en) * | 2014-04-11 | 2014-07-30 | 西安建筑科技大学 | Bismuth silicate powder preparation method using stoichiometric ratio raw materials and sol-gel method |
| CN104986947A (en) * | 2015-07-13 | 2015-10-21 | 江苏圣达石英制品有限公司 | Photosensitive quartz tube preparation method |
| CN105924144A (en) * | 2016-05-05 | 2016-09-07 | 陕西科技大学 | Preparing method for porous metastable stable Bi2SiO5 block |
| CN105948118A (en) * | 2016-05-05 | 2016-09-21 | 陕西科技大学 | Preparation method of porous Bi4Si3O12 bulk |
| CN105948806A (en) * | 2016-05-05 | 2016-09-21 | 陕西科技大学 | Preparation method of porous steady-state Bi4Si3O12 bulk |
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| JPS5260986A (en) * | 1975-11-13 | 1977-05-19 | Matsushita Electric Ind Co Ltd | Manufacturing of dielectric thin film |
| JPS5259900A (en) * | 1975-11-13 | 1977-05-17 | Matsushita Electric Ind Co Ltd | Manufacture of dielectric film |
| JPS5954615A (en) * | 1982-09-20 | 1984-03-29 | Univ Kyoto | Composite polycrystalline bismuth compound and its preparation |
| JPH02144A (en) * | 1988-12-16 | 1990-01-05 | Nisshin Flour Milling Co Ltd | Decaprenyl-substituted amino acid derivative and antiviral agent |
| CN1072221A (en) * | 1991-11-01 | 1993-05-19 | 中国科学院上海硅酸盐研究所 | The Bridgman-Stockbarge method for growing of bismuth silicate (BSO) monocrystalline |
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| CN101709508B (en) * | 2009-11-10 | 2011-10-26 | 陕西科技大学 | Preparation method of bismuth-containing eulytite bismuth silicate crystals |
| CN101792181B (en) * | 2010-02-09 | 2012-07-25 | 陕西科技大学 | Preparation method of bismuth silicate nanocrystalline |
| CN102249252A (en) * | 2011-04-11 | 2011-11-23 | 烟台大学 | New preparation method of Bi12SiO20 |
| CN102249252B (en) * | 2011-04-11 | 2013-06-05 | 烟台大学 | New preparation method of Bi12SiO20 |
| CN102275944A (en) * | 2011-07-06 | 2011-12-14 | 陕西科技大学 | Preparation method of new scintillating bismuth silicate powder |
| CN102351513A (en) * | 2011-07-06 | 2012-02-15 | 陕西科技大学 | Preparation method for bismuth silicate powder for utilization of optical performance |
| CN102275942A (en) * | 2011-07-06 | 2011-12-14 | 陕西科技大学 | Preparation method of bismuth silicate nanopowder |
| CN103949655A (en) * | 2014-04-11 | 2014-07-30 | 西安建筑科技大学 | Bismuth silicate powder preparation method using stoichiometric ratio raw materials and sol-gel method |
| CN103949655B (en) * | 2014-04-11 | 2016-04-20 | 西安建筑科技大学 | A kind of raw material of stoichiometric proportion and sol-gal process prepare the method for bismuth silicate powder |
| CN104986947A (en) * | 2015-07-13 | 2015-10-21 | 江苏圣达石英制品有限公司 | Photosensitive quartz tube preparation method |
| CN104986947B (en) * | 2015-07-13 | 2018-03-16 | 江苏圣达石英制品有限公司 | A kind of photosensitive quartzy tube preparation method |
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| CN105948806A (en) * | 2016-05-05 | 2016-09-21 | 陕西科技大学 | Preparation method of porous steady-state Bi4Si3O12 bulk |
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