CN101428210A - Porous structured bismuth titanate microsphere, preparation method and application thereof - Google Patents

Porous structured bismuth titanate microsphere, preparation method and application thereof Download PDF

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CN101428210A
CN101428210A CNA2008102044846A CN200810204484A CN101428210A CN 101428210 A CN101428210 A CN 101428210A CN A2008102044846 A CNA2008102044846 A CN A2008102044846A CN 200810204484 A CN200810204484 A CN 200810204484A CN 101428210 A CN101428210 A CN 101428210A
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bismuth
bismuth titanate
loose structure
microsphere
preparation
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CN101428210B (en
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霍宇凝
张怡
蔡陈灵
李和兴
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Shanghai Normal University
University of Shanghai for Science and Technology
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Shanghai Normal University
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Abstract

The invention discloses a bismuth titanate microsphere with a porous structure, as well as a preparation method and the application thereof. The porous-structure bismuth titanate microsphere is characterized in that the molecular formula thereof is Bi2Ti2O7, the grain diameter thereof is 0.5-2.0 Mum, the aperture thereof is 3.1-23.8 nm, the pore volume thereof is 0.02-0.20 cm<3>/g, and the specific surface area thereof is 8.4-47.1 m<2>/g. The preparation method comprises the following steps: using glacial acetic acid of bismuth salt or a glycerin solution, a surface active agent aqueous solution and titaniumivbutoxide or titanyl sulfate to form a precursor solution, in which the spray drying technique is applied to obtain a porous-structure bismuth titanate photocatalyst. The porous-structure bismuth titanate obtained can effectively degrade organic pollutants such as para-chlorophenol and the like through photocatalysis in visible light, so that the porous-structure bismuth titanate has a potential prospect of application. The invention has the advantages of easy attainment of raw materials, low preparation cost, simple process and easy control of conditions, and meanwhile provides a preparation process, from which synthesis of other photocatalyst materials can draw on experience.

Description

Bismuth titanate microsphere of a kind of loose structure and its production and use
Technical field
The present invention relates to material and catalyst field, especially the visible light catalyst field is specifically related to a kind of bismuth titanate microsphere with loose structure and its production and use.
Background technology
Bi 2Ti 2O 7Be A with pyrochlore constitution 2B 2O 7Compounds of group, crystal structure is made up of Ti-O octahedron and Bi-O tetrahedron.Because Bi 2Ti 2O 7There is TiO in the crystal 6Therefore octahedra unit has caused the broad research interest to its photochemical properties.For example, Kudo etc. has reported by the solid phase roasting method and has prepared Bi 2Ti 2O 7, and be applied in the reaction of photodissociation water; Yao etc. have reported and have utilized the chemical solution decomposition technique to prepare Bi 2Ti 2O 7, and be applied to degradable organic pollutant.But at present institute generally the preparation method of employing still exist complex process, preparation cost height, material specific area little, pattern such as can not regulate and control at shortcoming, therefore need to explore new method to prepare the novel visible catalysis material that specific area is big, structure is controlled, provide the new technology new material for further improving photocatalysis efficiency.
Spray drying technology is as the novel process of preparation catalysis material, and it is simple to have technical process, and process conditions are easy to control, the characteristics such as particle that the particle diameter that is easy to get is even, structure is controlled.This patent adopts spray-drying cosurfactant self-assembling technique to prepare the bismuth titanate photocatalyst with loose structure.
Summary of the invention
The objective of the invention is at the existing in prior technology defective, a kind of bismuth titanate microsphere with loose structure is provided.
Another object of the present invention is to provide above-mentioned preparation method with bismuth titanate microsphere of loose structure.
The present invention also provides the purposes of the bismuth titanate microsphere of above-mentioned loose structure.
The bismuth titanate microsphere with loose structure that can be used as visible light catalyst provided by the present invention, its molecular formula is Bi 2Ti 2O 7, be spheric granules with loose structure, particle diameter is 0.5～2.0 μ m, and the aperture is 3.1～23.8nm, and pore volume is 0.02～0.20cm 3/ g, specific area is 8.4～47.1m 2/ g.
This preparation method with bismuth titanate microsphere of loose structure comprises the steps:
(1) surfactant is dissolved in the deionized water, bismuth salt is dissolved in glacial acetic acid or the glycerine; Just above-mentioned surfactant solution and bismuth salt solution mix also stir; The adding titanium-containing compound also mixes, and obtains precursor solution; Titanium-containing compound is tetrabutyl titanate or titanyl sulfate;
(2) precursor solution is carried out spray-drying, and collect formed particle;
(3) with the particle collected at 400～600 ℃ of following roasting 3～8h, promptly obtain object.
Ratio 40～the 240g/mol of bismuth element is preferably 80～160g/mol in surfactant and the bismuth salt.
Bismuth element and the contained titanium elements mol ratio of titanium-containing compound contained in step (1) the bismuth salt are 1:1.
The consumption of deionized water should make surfactant fully dissolve; The consumption of glacial acetic acid or glycerine should make bismuth salt fully dissolve.Keeping surfactant and bismuth element is under the prerequisite of aforementioned proportion, and the ratio of deionized water and glacial acetic acid or glycerine can be regulated arbitrarily.
In the step (1), after the glacial acetic acid solution of surfactant solution and bismuth salt or glycerite mixed, the concentration of bismuth element was 0.1～0.3mol/L.
Surfactant can be selected F127 (EO for use 106PO 70EO 106, Aldrich) or P123 (EO 20PO 70EO 20), be preferably F127.
The spray-dired technology of step (2) is: as carrier gas, flow velocity is 2～8L/min, makes precursor aqueous solution pass through to form droplet behind the atomizer with nitrogen or helium, and carries out drying by the quartz ampoule that is heated to 250 ℃～450 ℃.
This bismuth titanate microsphere with loose structure can be used for as visible-light photocatalyst; Especially as visible-light photocatalyst, be used for the Photocatalytic Activity for Degradation reaction of parachlorophenol.
The product of the present invention's preparation carries out structural characterization by following means: adopt the X-ray diffraction of measuring on Japan's RigakuD/Max-RB type of science X-ray diffractometer to carry out the structures of samples analysis; Adopt the specific area and the pore structure of the automatic physical adsorption appearance working sample of QuantaChrome Nova 4000e type; The appearance structure of stereoscan photograph that employing obtains at Japanese JEOL JSM-6380LV type ESEM and the transmission electron microscope photo analytic sample that obtains at Japanese JEOLJEM2010 type high-resolution-ration transmission electric-lens.
Bismuth titanate microsphere with loose structure provided by the present invention adopts 1.0 * 10 of 50.0mL -4The photocatalytic degradation of M parachlorophenol is investigated its catalytic performance.Concrete steps are: bismuth titanate photocatalyst reacted 6 hours down at 30 ℃, and a 500W Xe lamp is positioned at 18cm place, reactant liquid level top as light source, with filter plate wavelength is removed less than the light of 420nm.Reactant liquor stirs 1 hour to reach adsorption equilibrium before the illumination.The remaining parachlorophenol in reaction back is measured absorbance with ultraviolet specrophotometer (UV 7504/PC) at the 224nm place, calculate reactant concentration according to the linear relationship between absorbance and concentration.After stirring 6 hours under unglazed photograph or the catalyst condition, only there is 3% parachlorophenol to decompose, therefore can ignores the error that causes thus.
The present invention compared with prior art, have the following advantages and outstanding effect: employed chemical reagent is common agents, cheap and easy to get, preparation technology is simple, easy to operate, big, the easy control of structure of specific surface area of catalyst.The resulting bismuth titanate microsphere specific area with loose structure of the present invention reaches 47m 2/ g is much higher than commodity bismuth titanates powder, has increased substantially photocatalytic activity simultaneously.
Description of drawings
Fig. 1 is the spray-drying installation schematic diagram;
1-atomizer, 2-tube furnace, 3-quartz ampoule, 4-filter
Fig. 2 is the XRD figure spectrum of embodiment 1 prepared sample;
Fig. 3 is the nitrogen adsorption desorption thermoisopleth of embodiment 1 prepared sample, and illustration is the BJH graph of pore diameter distribution;
Fig. 4 is the ESEM (A) and transmission electron microscope (B) photo of embodiment 1 prepared sample;
Fig. 5 has the bismuth titanate microsphere of loose structure for embodiment 1-6 is prepared and the photocatalytic activity of commodity bismuth titanates compares.
The specific embodiment
Is doing further in detail of how realizing, explanation clearly and completely below in conjunction with specific embodiment to the present invention, and listed embodiment only gives further instruction to the present invention, and is not thereby limiting the invention:
Embodiment 1
With 3g surfactant F127 (EO 106PO 70EO 106Aldrich) be dissolved in the 40ml deionized water, and 12g five nitric hydrate bismuths (0.025mol) are dissolved in the 60ml glacial acetic acid, again with above-mentioned two solution mixing and stirring, add 8.5ml tetrabutyl titanate (0.025mol) and mixing, the precursor solution that obtains spraying.
The spray drying device structure comprises atomizer 1, tube furnace 2, quartz ampoule 3 and filter 4 as shown in Figure 1.Tube furnace is enclosed within quartz ampoule and is used for heating outward, and the outlet of atomizer communicates with quartz ampoule, enters quartz ampoule after carrier gas and the precursor solution atomizing, and the other end of quartz ampoule is connected to filter; The effect of filter is to collect the particle that forms after the spray-drying.
With nitrogen as carrier gas, flow velocity is 4L/min, make solution pass through to form droplet behind the atomizer, (Φ 44 * 1200mm) for quartz ampoule by being heated to 350 ℃ with tube furnace afterwards, collect the particle that forms, 500 ℃ Muffle furnace roastings 6 hours, promptly obtain object---have the bismuth titanate microsphere of loose structure.
Fig. 2 is the X-ray diffracting spectrum (x15000) of the prepared sample of present embodiment, can determine that from collection of illustrative plates the gained sample is Bi 2Ti 2O 7Fig. 3 is the nitrogen suction-desorption isotherm of the prepared sample of present embodiment, determines that from isothermal is linear the gained sample has meso-hole structure, calculates as can be known that the aperture of gained sample is 23.8nm, and pore volume is 0.15cm 3/ g, specific area is 16.6m 2/ g; Fig. 4 is the SEM and the TEM photo of the prepared sample of present embodiment, is the microballoon with loose structure from the visible gained sample of photo, and particle diameter is 0.5～2.0 μ m.
Embodiment 2
12g five nitric hydrate bismuths are dissolved in are stirred to dissolving fully in the mixed solution of 40ml deionized water and 60ml glacial acetic acid, all the other steps are described identical with embodiment 1.
Can determine that through X-ray diffracting spectrum the gained sample is Bi 2Ti 2O 7Can determine that through nitrogen suction-desorption isotherm shape the gained sample has meso-hole structure, calculate as can be known that the aperture of gained sample is 17.8nm, pore volume is 0.06cm 3/ g, specific area is 8.9m 2/ g; Through SEM scanning and the visible gained sample of TEM is the microballoon with loose structure, and particle diameter is 0.5～2.0 μ m.
Embodiment 3
2g surfactant F127 and 12g five nitric hydrate bismuths are dissolved in respectively in 30ml deionized water and the 70ml glacial acetic acid, and all the other contents are described identical with embodiment 1.
Can determine that through X-ray diffracting spectrum the gained sample is Bi 2Ti 2O 7Can determine that through nitrogen suction-desorption isotherm shape the gained sample has meso-hole structure, calculate as can be known that the aperture of gained sample is 23.6nm, pore volume is 0.09cm 3/ g, specific area is 10.4m 2/ g; Through SEM and the visible gained sample of TEM is the microballoon with loose structure, and particle diameter is 0.5～2.0 μ m.
Embodiment 4
4g surfactant F127 and 12g five nitric hydrate bismuths are dissolved in respectively in 50ml deionized water and the 50ml glacial acetic acid, and all the other contents are described identical with embodiment 1.
Can determine that through X-ray diffracting spectrum the gained sample is Bi 2Ti 2O 7Can determine that through nitrogen suction-desorption isotherm shape the gained sample has meso-hole structure, calculate as can be known that the aperture of gained sample is 22.4nm, pore volume is 0.07cm 3/ g, specific area is 17.0m 2/ g; Through SEM and the visible gained sample of TEM is the microballoon with loose structure, and particle diameter is 0.5～2.0 μ m.
Embodiment 5
6g surfactant F127 and 12g five nitric hydrate bismuths are dissolved in respectively in 40ml deionized water and the 60ml glacial acetic acid, and all the other contents are described identical with embodiment 1.
Can determine that through X-ray diffracting spectrum the gained sample is Bi 2Ti 2O 7Can determine that through nitrogen suction-desorption isotherm shape the gained sample has meso-hole structure, calculate as can be known that the aperture of gained sample is 17.1nm, pore volume is 0.13cm 3/ g, specific area is 20.8m 2/ g; Through SEM and the visible gained sample of TEM is the microballoon with loose structure, and particle diameter is 0.5～2.0 μ m.
Embodiment 6
The difference of present embodiment and embodiment 1 is: in the spray process, flow rate of carrier gas is 6L/min, and quartz ampoule is heated to 250 ℃, and all the other contents are described identical with embodiment 1.
Can determine that through X-ray diffracting spectrum the gained sample is Bi 2Ti 2O 7Can determine that through nitrogen suction-desorption isotherm shape the gained sample has meso-hole structure, calculate as can be known that the aperture of gained sample is 3.1nm, pore volume is 0.06cm 3/ g, specific area is 19.2m 2/ g; Through SEM and the visible gained sample of TEM is the microballoon with loose structure, and particle diameter is 0.5～2.0 μ m.
Embodiment 7
The difference of present embodiment and embodiment 1 is: in the spray process, quartz ampoule is heated to 300 ℃, and all the other contents are described identical with embodiment 1.
Can determine that through X-ray diffracting spectrum the gained sample is Bi 2Ti 2O 7Can determine that through nitrogen suction-desorption isotherm shape the gained sample has meso-hole structure, calculate as can be known that the aperture of gained sample is 21.5nm, pore volume is 0.11cm 3/ g, specific area is 8.4m 2/ g; Through SEM and the visible gained sample of TEM is the microballoon with loose structure, and particle diameter is 0.5～2.0 μ m.
Embodiment 8
The difference of present embodiment and embodiment 1 is: in the spray process, flow rate of carrier gas is 3L/min, and quartz ampoule is heated to 400 ℃, and all the other contents are described identical with embodiment 1.
Can determine that through X-ray diffracting spectrum the gained sample is Bi 2Ti 2O 7Can determine that by nitrogen suction-desorption isotherm shape the gained sample has meso-hole structure, calculate as can be known that the aperture of gained sample is 16.4nm, pore volume is 0.17cm 3/ g, specific area is 30.8m 2/ g; By SEM and the visible gained sample of TEM is the microballoon with loose structure, and particle diameter is 0.5～2.0 μ m.
Embodiment 9
The difference of present embodiment and embodiment 1 is: in the spray process, quartz ampoule is heated to 450 ℃, and all the other contents are described identical with embodiment 1.
Can determine that by X-ray diffracting spectrum the gained sample is Bi 2Ti 2O 7Can determine that by nitrogen suction-desorption isotherm shape the gained sample has meso-hole structure, calculate as can be known that the aperture of gained sample is 13.3nm, pore volume is 0.17cm 3/ g, specific area is 33.7m 2/ g; By SEM and the visible gained sample of TEM is the microballoon with loose structure, and particle diameter is 0.5～2.0 μ m.
Embodiment 10
The difference of present embodiment and embodiment 1 is: with resulting granules after the spray-drying, 450 ℃ Muffle furnace roastings 6 hours, all the other contents were described identical with embodiment 1.
Can determine that by X-ray diffracting spectrum the gained sample is Bi 2Ti 2O 7Can determine that by nitrogen suction-desorption isotherm shape the gained sample has meso-hole structure, calculate as can be known that the aperture of gained sample is 13.3nm, pore volume is 0.20cm 3/ g, specific area is 47.1m 2/ g; By SEM and the visible gained sample of TEM is the microballoon with loose structure, and particle diameter is 0.5～2.0 μ m.
Embodiment 11
The difference of present embodiment and embodiment 1 is: with resulting granules after the spray-drying, 550 ℃ Muffle furnace roastings 5 hours, all the other contents were described identical with embodiment 1.
Can determine that by X-ray diffracting spectrum the gained sample is Bi 2Ti 2O 7Can determine that by nitrogen suction-desorption isotherm shape the gained sample has meso-hole structure, calculate as can be known that the aperture of gained sample is 3.1nm, pore volume is 0.03cm 3/ g, specific area is 14.8m 2/ g; By SEM and the visible gained sample of TEM is the microballoon with loose structure, and particle diameter is 0.5～2.0 μ m.
Embodiment 12
With 3g surfactant F127 (EO 106PO 70EO 106, Aldrich) be dissolved in respectively in 30ml deionized water and the 70ml glacial acetic acid with 12g five nitric hydrate bismuths (0.025mol), again with two solution mixing and stirring, add 0.025mol titanyl sulfate and mixing, the precursor solution that obtains spraying.
With nitrogen as carrier gas, flow velocity is 4L/min, make solution pass through to form droplet behind the atomizer, (Φ 44 * 1200mm) to be heated to 350 ℃ quartz ampoule by tube furnace afterwards, collect the particle that forms, 600 ℃ Muffle furnace roastings 6 hours, promptly obtain object---have the bismuth titanate microsphere of loose structure.
Can determine that by X-ray diffracting spectrum the gained sample is Bi 2Ti 2O 7Can determine that by nitrogen suction-desorption isotherm shape the gained sample has meso-hole structure, calculate as can be known that the aperture of gained sample is 3.1nm, pore volume is 0.02cm 3/ g, specific area is 9.6m 2/ g; By SEM and the visible gained sample of TEM is the microballoon with loose structure, and particle diameter is 0.5～2.0 μ m.
Embodiment 13
Get the bismuth titanates that gained in the foregoing description 1,2,3,4,5 has loose structure, adopt 1.0 * 10 of 50.0mL -4The M parachlorophenol is the goal response thing, investigates its Photocatalytic Activity for Degradation performance, and compares with the photocatalytic activity of commodity bismuth titanates powder.The results are shown in Figure 5, the resulting product of the present invention all has photocatalytic activity as can be seen, and embodiment 1,3,4 prepared bismuth titanate microspheres with loose structure have increased substantially photocatalytic activity, more far above the photocatalytic activity of commodity bismuth titanates powder.

Claims (8)

1. the bismuth titanate microsphere with loose structure is characterized in that, molecular formula is Bi 2Ti 2O 7, particle diameter is 0.5～2.0 μ m, and the aperture is 3.1～23.8nm, and pore volume is 0.02～0.20cm 3/ g, specific area is 8.4～47.1m 2/ g.
2. the described preparation method with bismuth titanate microsphere of loose structure of claim 1 is characterized in that, may further comprise the steps:
(1) surfactant is dissolved in the deionized water, bismuth salt is dissolved in glacial acetic acid or the glycerine; With above-mentioned surfactant solution and bismuth salt solution mix and stir, add titanium-containing compound and also mix, obtain precursor solution; Described titanium-containing compound is tetrabutyl titanate or titanyl sulfate
(2) precursor solution is carried out spray-drying, and collect formed particle;
(3) with the particle collected at 400～600 ℃ of following roasting 3～8h, promptly obtain object.
3. the described preparation method with bismuth titanate microsphere of loose structure of claim 2 is characterized in that, in described step (1) the bismuth salt in contained bismuth element and the titanium-containing compound contained titanium elements mol ratio be 1:1.
4. the described preparation method with bismuth titanate microsphere of loose structure of claim 2 is characterized in that, the ratio of bismuth element is 40～240g/mol in described surfactant and the bismuth salt.
5. the described preparation method with bismuth titanate microsphere of loose structure of claim 2 is characterized in that, described surfactant is EO 106PO 70EO 106Or EO 20PO 70EO 20
6. the described preparation method of claim 2 with bismuth titanate microsphere of loose structure, it is characterized in that, the spray-dired technology of described step (2) is: with nitrogen or helium as carrier gas, flow velocity is 2～8L/min, make precursor aqueous solution pass through to form droplet behind the atomizer, and carry out drying by the quartz ampoule that is heated to 250～450 ℃.
7. the described purposes with bismuth titanate microsphere of loose structure of claim 1 is characterized in that described bismuth titanate microsphere with loose structure is applied to the purposes of visible-light photocatalyst.
8. the described purposes with bismuth titanate microsphere of loose structure of claim 1 is characterized in that, described bismuth titanate microsphere with loose structure is applied to the Photocatalytic Activity for Degradation reaction of parachlorophenol.
CN2008102044846A 2008-12-12 2008-12-12 Porous structured bismuth titanate microsphere preparation method Expired - Fee Related CN101428210B (en)

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CN101791558A (en) * 2010-03-19 2010-08-04 上海师范大学 Bismuth ferrite microsphere photocatalyst with hollow structure and preparation method thereof
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CN101791558B (en) * 2010-03-19 2012-09-05 上海师范大学 Bismuth ferrite microsphere photocatalyst with hollow structure and preparation method thereof
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CN102351242A (en) * 2011-08-17 2012-02-15 南京师范大学 Solvent-thermal method for preparing single-phase bismuth titanate Bi2Ti2O7
CN102659400A (en) * 2012-04-27 2012-09-12 陕西科技大学 Method for manufacturing pyrochlore phase bismuth titanate functional films on surfaces of glass substrates
CN103523823A (en) * 2013-09-22 2014-01-22 南京师范大学 Preparation method and application of bismuth titanate-titanium oxide heterojunction nano-material
CN104324713A (en) * 2014-11-20 2015-02-04 熊菊莲 Photocatalyst of graphene-bismuth titanate composite material
CN104549216A (en) * 2015-02-10 2015-04-29 合肥工业大学 Micro/nano-structure Bi4Ti3O12 photocatalyst, and preparation method and application thereof
CN106915771A (en) * 2017-02-27 2017-07-04 江苏大学 One kind is with C3N4The method that mesoporous wire bismuth titanates is prepared for template
CN106915771B (en) * 2017-02-27 2018-06-01 江苏大学 One kind is with C3N4The method that mesoporous wire bismuth titanates is prepared for template
CN107115856A (en) * 2017-03-29 2017-09-01 江苏大学 A kind of preparation method of sheet bismuth titanates chlorine oxygen bismuth composite
CN108715833A (en) * 2018-06-01 2018-10-30 天晴干细胞股份有限公司 A kind of method for preparing microsphere of load platelet lysates liquid
CN108715833B (en) * 2018-06-01 2021-09-14 天晴干细胞股份有限公司 Preparation method of microsphere loaded with platelet lysate
CN108772053A (en) * 2018-06-29 2018-11-09 辽宁石油化工大学 A kind of bismuth titanates/bismuth oxide photocatalyst and its preparation method and application
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