CN105435762A - Preparation method of TiO2 photocatalytic material - Google Patents
Preparation method of TiO2 photocatalytic material Download PDFInfo
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- CN105435762A CN105435762A CN201510869833.6A CN201510869833A CN105435762A CN 105435762 A CN105435762 A CN 105435762A CN 201510869833 A CN201510869833 A CN 201510869833A CN 105435762 A CN105435762 A CN 105435762A
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Abstract
The invention provides a preparation method of a TiO2 photocatalytic material. The preparation method comprises steps as follows: step 1, acetylacetone and glacial acetic acid are added to isopropyl alcohol during stirring, and a solution I is obtained; step 2, the solution I has a hydrothermal reaction for 8-20 h at the temperature of 120-200 DEG C, and an intermediate product is obtained; step 3, the intermediate product obtained in the step 2 is washed with water and ethyl alcohol for multiple times and then is dried for 2 h at temperature of 60-150 DEG C in air atmosphere, and the TiO2 photocatalytic material is obtained. According to the preparation method of the TiO2 photocatalytic material, the method is simple and environment-friendly and is suitable for large-scale production, and the synthesized material is stable in structure, has large specific surface area and even morphology and has better visible light photocatalytic performance on a dye RhB; besides, the photocatalytic material has very good stability and recycling performance.
Description
Technical field
The present invention relates to field of material technology, particularly relate to a kind of TiO
2the preparation method of catalysis material.
Background technology
Day by day serious along with environmental problem, water treatment becomes one of key content that people pay close attention to, and catalysis material is subject to pursuing of scientific circles, wherein TiO because of its environmental protection
2the representative in this field has been become as the material used the earliest.But due to TiO
2there is larger energy gap, make it can only could catalyzing organic matter under the irradiation of ultraviolet light, and sunshine medium ultraviolet light only accounts for little ratio.Therefore, people are devoted to develop visible-light photocatalyst in recent years, and by noble metal compound, metal ion mixing, nonmetallic ion-doped, oxide compound and material with carbon element compound improve the visible light photocatalysis performance of material.
At present, TiO
2complex carbon material is a kind of visible-light photocatalysis material be widely studied, and because of material with carbon element wide material sources, performance is remarkable and receive much concern, such as: C doped Ti O
2, CNT, fullerene and Graphene composite Ti O
2material etc., but these materials majority in preparation process needs high-temperature process, or preparation process is complicated.At present about the preparation method of carbon containing poriferous titanium dioxide mainly adopts liquid phase method more, these method courses of reaction are complicated, if obtain loose structure often need follow-up high-temperature process.Zhang etc. (Chem.Commu., 2014,50,13971-13974) report one and prepare carbon containing TiO
2preparation method (the method be the ethanolic solution of butyl titanate is joined by nitre acid for adjusting pH be 1.5 acetic acid, absolute ethyl alcohol, deionized water mixed solution in, obtain colloidal sol.Colloidal sol obtains gel through stirring ageing, drying, eventually passes through the TiO that 400 degree of calcinings obtain carbon containing
2photochemical catalyst).Preparation process is comparatively complicated, and the time is longer, finally also needs high-temperature process, and prepared material does not possess multilevel hierarchy.(the J.Mater.Chem.A such as Panda, 2013,1,9122-9131) report a kind of method preparing multilevel hierarchy microballoon (with isopropyl alcohol oxygen titanium for titanium source, first prepare the predecessor of titanium, then by this predecessor and ammoniacal liquor hydro-thermal reaction, the sample obtained obtains the TiO of porous after 400 degree of calcinings
2multilevel structure material).This reaction condition is more complicated, needs high-temperature process equally, and not carbon containing in end product.
Summary of the invention
The object of the invention is to the defect solving the existence of above-mentioned prior art, that a kind of low-temperature growth carbon containing is provided, that there is multilevel hierarchy, porous TiO
2the preparation method of catalysis material.
A kind of TiO
2the preparation method of catalysis material, comprises the following steps:
Step 1: add titanium acetylacetone and glacial acetic acid under agitation in isopropyl alcohol, obtain solution I;
Step 2: by solution I at 120-200 DEG C of hydro-thermal reaction 8-20 hour, obtain intermediate product;
Step 3: by the intermediate product of step 2 respectively with water and ethanol washing for several times, then 60-150 ° of dry 2h in air atmosphere, namely obtains TiO of the present invention
2catalysis material.
Further, TiO as above
2the preparation method of catalysis material, the volume ratio of described isopropyl alcohol, titanium acetylacetone, glacial acetic acid three is: 30-35:0.2-0.8:0.1-0.5.
TiO provided by the invention
2the preparation method of catalysis material, its method is simple, environmental protection, be easy to large-scale production, the material structure synthesized is stablized, specific area is large, pattern is homogeneous, has good visible light photocatalysis performance to dye, rhodamine B (RhB), and this catalysis material has good stability and can reusing.
Accompanying drawing explanation
Fig. 1 is the XRD figure of microballoon after treatment of different temperature prepared by the embodiment of the present invention 1;
Fig. 2 is the IR figure of microballoon after treatment of different temperature prepared by the embodiment of the present invention 1;
Fig. 3 is the embodiment of the present invention 1 carbon containing TiO
2the low range scanning electron microscope (SEM) photograph of microballoon;
Fig. 4 is the embodiment of the present invention 1 carbon containing TiO
2the high magnification SEM of microballoon schemes;
Fig. 5 is the embodiment of the present invention 1 carbon containing TiO
2the transmission electron microscope picture of microballoon low range;
Fig. 6 is the embodiment of the present invention 1 carbon containing TiO
2the TEM of microballoon, HRTEM and FFT Transformation Graphs;
Fig. 7 is that the embodiment of the present invention 1 different temperatures post-calcination sample and P25 are to the catalytic degradation figure of rhodamine B.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearly, below technical scheme in the present invention be clearly and completely described, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1:
In the hydrothermal reaction kettle of 50mL, add 30mL isopropyl alcohol, add 0.458mL titanium acetylacetone under agitation, add 0.2mL glacial acetic acid, obtain solution, 150 DEG C of hydro-thermal reactions 12 hours.Obtain product respectively with water and ethanol washing, 150 degree of dry 2h in air atmosphere, the multilevel hierarchy microballoon of the carbon containing that the porous nano lamella that can obtain being constructed by nano particle is piled up further, microsphere diameter is about 100-200nm, nano-particles size is about 8nm, hole dimension is about 3.4nm, specific area 338m
2g
-1.
Embodiment 2:
In the hydrothermal reaction kettle of 50mL, add 35mL isopropyl alcohol, add 0.2mL titanium acetylacetone under agitation, add 0.1mL glacial acetic acid, obtain solution, 200 DEG C of hydro-thermal reactions 10 hours.Obtain product respectively with water and ethanol washing, 100 degree of dry 2h in air atmosphere, the multilevel hierarchy microballoon of the carbon containing that the porous nano lamella that can obtain being constructed by nano particle is piled up further, microsphere diameter is about 100-200nm, nano-particles size is about 8nm, hole dimension is about 3.4nm, specific area 338m
2g
-1.
Embodiment 3:
In the hydrothermal reaction kettle of 50mL, add 30mL isopropyl alcohol, add 0.8mL titanium acetylacetone under agitation, add 0.5mL glacial acetic acid, obtain solution, 120 DEG C of hydro-thermal reactions 8 hours.Obtain product respectively with water and ethanol washing, 60 degree of dry 2h in air atmosphere, the multilevel hierarchy microballoon of the carbon containing that the porous nano lamella that can obtain being constructed by nano particle is piled up further, microsphere diameter is about 100-200nm, nano-particles size is about 8nm, hole dimension is about 3.4nm, specific area 338m
2g
-1.
Photocatalysis is tested, and selects rhodamine B (RhB) for Contaminant measurement carbon containing TiO
2the visible light photocatalysis performance of multilevel hierarchy microballoon.Certain density RhB solution is put into measuring cup, then adds carbon containing TiO
2multilevel hierarchy microballoon is as attached dose of catalysis, at room temperature magnetic agitation uses visible light source to irradiate sample simultaneously, after stirring the regular hour, get fixed volume supernatant soln to sample, then utilize ultraviolet-uisible spectrophotometer to detect the residual concentration of RhB in the intensity of 554nm place characteristic absorption peak according to RhB.
Fig. 1 prepared by the embodiment of the present invention 1 microballoon after treatment of different temperature XRD figure, as shown in Figure 1, the diffraction maximum in figure and standard card (JCPDSNo.65-5714) comparison known, products therefrom is TiO
2.Along with the rising of heat treatment temperature, TiO in sample
2crystallinity improve gradually.
Fig. 2 is the IR figure of microballoon after treatment of different temperature prepared by the embodiment of the present invention 1, as shown in Figure 2, from the IR curve of K cryogenic treatment in figure, at 1000-1700cm
-1and 3000cm
-1near there is the flexible vibrations peak of carbonaceous organic material.After high-temperature process, organic vibrations peak disappears.
Fig. 3 is the embodiment of the present invention 1 carbon containing TiO
2the low range scanning electron microscope (SEM) photograph of microballoon, as shown in Figure 3, can find out in figure that product is more homogeneous micro-sphere structure.
Fig. 4 is the embodiment of the present invention 1 carbon containing TiO
2the high magnification SEM of microballoon schemes; As shown in Figure 4, clearly can find out in figure that this microballoon is constructed by a large amount of 2D nanometer sheet to form, microsphere diameter is about 100-200nm.
Fig. 5 is the embodiment of the present invention 1 carbon containing TiO
2the transmission electron microscope picture of microballoon low range; As shown in Figure 5, this microballoon regular appearance can be found out, size uniformity.
Fig. 6 is the embodiment of the present invention 1 carbon containing TiO
2the TEM of microballoon, HRTEM and FFT Transformation Graphs; As shown in Figure 6, scheming visible interplanar distance by high-resolution TEM is 0.35nm, corresponding TiO
2(101) crystal face, upper right illustration is Fourier transformation figure, and wherein point diffraction correspondence (101) crystal face, matches with XRD result, can see the existence of carbonaceous material in square frame line simultaneously.
Fig. 7 be the embodiment of the present invention 1 different temperatures post-calcination sample and P25 to the catalytic degradation figure of rhodamine B, (a, b, c, d, e, f, g corresponding 60 DEG C respectively, 100 DEG C, 150 DEG C, 200 DEG C, 300 DEG C, 500 DEG C, P25), carbon containing TiO as seen from the figure
2phase pure material compared by microballoon and P25 has good catalytic performance.And along with the rising of heat treatment temperature, catalytic performance first raises rear reduction.15mg150 degree heat treated sample, by 15mL20mgg after radiation of visible light 180min
-1rhodamine B degradable.
Last it is noted that above embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (2)
1. a TiO
2the preparation method of catalysis material, is characterized in that, comprises the following steps:
Step 1: add titanium acetylacetone and glacial acetic acid under agitation in isopropyl alcohol, obtain solution I;
Step 2: by solution I at 120-200 DEG C of hydro-thermal reaction 8-20 hour, obtain intermediate product;
Step 3: by the intermediate product of step 2 respectively with water and ethanol washing for several times, then 60-150 ° of dry 2h in air atmosphere, namely obtains TiO of the present invention
2catalysis material.
2. TiO according to claim 1
2the preparation method of catalysis material, is characterized in that, the volume ratio of described isopropyl alcohol, titanium acetylacetone, glacial acetic acid three is: 30-35:0.2-0.8:0.1-0.5.
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|---|---|---|---|
| CN201510869833.6A CN105435762A (en) | 2015-07-29 | 2015-12-01 | Preparation method of TiO2 photocatalytic material |
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|---|---|---|---|
| CN2015104555761 | 2015-07-29 | ||
| CN201510455576 | 2015-07-29 | ||
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108927126A (en) * | 2018-09-06 | 2018-12-04 | 中国药科大学 | A kind of visible light-responded titanium dioxide optical catalyst and preparation method thereof |
| CN111704161A (en) * | 2020-06-15 | 2020-09-25 | 闽江学院 | Hierarchical titanium dioxide microspheres and preparation method and application thereof |
-
2015
- 2015-12-01 CN CN201510869833.6A patent/CN105435762A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108927126A (en) * | 2018-09-06 | 2018-12-04 | 中国药科大学 | A kind of visible light-responded titanium dioxide optical catalyst and preparation method thereof |
| CN111704161A (en) * | 2020-06-15 | 2020-09-25 | 闽江学院 | Hierarchical titanium dioxide microspheres and preparation method and application thereof |
| CN111704161B (en) * | 2020-06-15 | 2022-09-13 | 闽江学院 | Hierarchical titanium dioxide microspheres and preparation method and application thereof |
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Application publication date: 20160330 |