CN103143356A - Ordered meso-porous (TiO2-Cu) nanocomplex and its hydrothermal supercritical extraction preparation technology - Google Patents
Ordered meso-porous (TiO2-Cu) nanocomplex and its hydrothermal supercritical extraction preparation technology Download PDFInfo
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- CN103143356A CN103143356A CN2013100514388A CN201310051438A CN103143356A CN 103143356 A CN103143356 A CN 103143356A CN 2013100514388 A CN2013100514388 A CN 2013100514388A CN 201310051438 A CN201310051438 A CN 201310051438A CN 103143356 A CN103143356 A CN 103143356A
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Abstract
The invention discloses an ordered meso-porous (TiO2-Cu) nanocomplex and its preparation technology. The above ordered meso-porous (TiO2-Cu) composite nanomaterial is prepared through adopting a hydrothermal method and a supercritical extraction technique. The technology is characterized in that a surfactant is treated as a soft template and the supercritical extraction technique and the hydrothermal method are adopted to prepare the ordered meso-porous (TiO2-Cu) nanocomplex having a novel structure and good physical and chemical properties. The technology provides a new way for researching the application of meso-porous TiO2-doped photocatalytic materials. The technology has the advantages of simplicity and easy industrial production; and the prepared meso-porous nanocomplex has a large specific surface area and a uniform pore distribution.
Description
Technical field
The present invention relates to a kind of order mesoporous (TiO
2-Cu) nano complex and hydro-thermal method supercritical extract preparation technology belongs to field of functional materials.
Background technology
TiO
2Because of its biologically inert and chemical inertness, photoetch and chemical attack can not occur, the advantage such as cheap, and a kind of photochemical catalyst that is proved to be to be most widely used.Due to TiO
2Electron distributions be characterised in that the existence that band gap is arranged between its conduction band and valence band.When being subject to illumination, as long as the energy of photon equals or exceeds semi-conductive band-gap energy (hv 〉=E
g), just can make electronics transit to conduction band from valence band, thereby produce conduction band electron and valence band hole.Under the electric field action of space charge layer, the free electron of conduction band moves to rapidly semiconductive particles surface and is transferred to oxidation component in solution, thereby light induced electron and hole form hydroxyl radical free radical OH through series reaction, and it can the nearly all organic matter of oxidation.Therefore, it has powerful application prospect at field of Environment Protection (as pollutant treatment).Course of reaction is as follows:
TiO
2+hv→h
++e
-
H
2O+h
+→·OH+H
+
e
-+O
2→O
2 -·
H
++O
2 -·→HO
2·
2HO
2·→H
2O
2+O
2
H
2O
2+O
2 -·→·OH+OH
-+O
2
h
++OH
-→·OH
h
++ org → intermediate → CO
2+ H
2O
OH+org → intermediate → CO
2+ H
2O
Yet, due to TiO
2Greater band gap (approximately 3.2eV), the threshold wave-length of its absorption are less than 400nm, and be not high to the utilization rate of sunshine; Affected TiO
2Practical and the industrialization process of multiphase photocatalysis reaction.Research finds, by transient metal doped or conductor oxidate is compound can improve TiO
2Photocatalytic activity and visible light utilization rate.Therefore, nano-TiO
2(X: transition metal) the doping catalysis material also just becomes one of study hotspot of photocatalysis field to-X.But, the TiO of preparation
2-X nano-powder, nanofiber specific area are little, and photocatalytic activity and photocatalysis efficiency are not high, also affect and have limited its practical application.Therefore, the orderly doped meso-porous TiO of preparation
2Nano complex is to solve photocatalysis technology to be applied to sewage degradation treatment effective method the most.Yet traditional calcination method all causes the synthetic material hole to cave in, and specific area is significantly reduced.But it is worth noting, also do not prepare so far mesoporous (TiO
2-X) the effective ways of composite Nano catalysis material.
Summary of the invention
The purpose of the embodiment of the present invention is to provide a kind of order mesoporous (TiO2-Cu) nano complex hydro-thermal method supercritical extract preparation technology, is intended to solve traditional calcination method and all causes the synthetic material hole to cave in, and specific area is significantly reduced.But it is worth noting, also do not prepare so far mesoporous (TiO
2-X) the problem of the effective ways of composite Nano catalysis material.
The embodiment of the present invention is achieved in that a kind of order mesoporous (TiO
2-Cu) the preparation technology of nano complex, this preparation technology synthesizes " surfactant-inorganic matter " precipitation by soft template method, then, adopt supercritical extraction technique with the extraction from precipitation of surfactant soft template, then process synthesizing ordered mesoporous (TiO by the distilled water rinsing
2-Cu) nano complex.
Further, this preparation technology's concrete steps are:
1), take titanium tetrachloride as initiation material, take DTAB as the surfactant soft template, under the interaction of distilled water, concentrated hydrochloric acid, by hydro-thermal reaction synthesis of nano complex;
2), take ethanol, methyl alcohol as extractant, after supercritical extract surfactant soft template, then adopt the distilled water rinsing to process, prepare order mesoporous (TiO
2-Cu) composite.
Further, the agents useful for same percentage by weight is: titanium tetrachloride, purity＞99.0,50-65%; Deionized water, 1-5%; Absolute ethyl alcohol, purity＞99.9,75-85%; Methyl alcohol, purity＞99.9,70-80%, DTAB, purity＞99.0,10-20%; The nitric acid gold, purity＞99.0,0.5-1%.
Further, by hydro-thermal method, preparation " soft template-inorganic matter " nano complex, titanium tetrachloride: the soft template control range is 4-1.5, and pH is controlled at 1-3.
Further, " soft template-inorganic matter " nano complex is put into autoclave, by supercritical extraction technique, surfactant is extracted from " soft template-inorganic matter " nano complex, heating rate 2-4 ℃, be raised to appropriate temperature range (34.1-250 ℃) and reach under appropriate pressure range (7.1-45MPa), keeping 10-15h.
Further, with order mesoporous (TiO
2-Cu) nano complex passes through distilled water rinsing 1-5 time.
Above-mentioned order mesoporous (the TiO that utilizes that provides is provided another purpose of the embodiment of the present invention
2-Cu) order mesoporous (the TiO of the preparation technology preparation of nano complex
2-Cu) nano complex.
The present invention adopts soft template method, by the synthesizing ordered mesoporous (TiO of supercritical extraction technique
2-Cu) nano complex.At present, we utilize this technique to prepare order mesoporous (TiO
2-Cu) composite nano materials has following remarkable advantage effect: (a) have high photocatalysis performance, without any toxicity; (b) specific area is large, and pore structure can be adjusted, and can carry out Quantitative design; (c) do not need calcining, preparation technology is simple, and production cost is low, is easy to suitability for industrialized production; (d) being widely used, is to solve photocatalysis technology to be applied to sewage degradation treatment effective method the most, has saved sewage degradation treatment cost.
Description of drawings
Fig. 1 is preparation technology's schematic diagram of the present invention;
Fig. 2 is order mesoporous (TiO
2-Cu) nano complex throws electromicroscopic photograph;
Fig. 3 is order mesoporous (TiO
2-Cu) the X-ray diffractogram of nano complex under treatment of different temperature;
Fig. 4 is order mesoporous (TiO
2-Cu) the infared spectrum of nano complex.
The specific embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
The invention provides a kind of order mesoporous (TiO
2-Cu) the preparation technology of nano complex comprises the following steps:
1) take titanium tetrachloride as initiation material, take " DTAB " surfactant as soft template, under the interaction of distilled water, concentrated hydrochloric acid, synthetic " surfactant-inorganic matter " precipitation.Titanium tetrachloride adds in there-necked flask at first together, and distilled water and hydrochloric acid and surfactant add simultaneously by funnel, and both rate of addition general controls are at 0.4-1.Omlmin
-1Between;
2) also join in there-necked flask synthetic " surfactant-inorganic matter " precipitation by the inorganic matter presoma of above-mentioned formula with Cu;
3) " surfactant-inorganic matter " precipitation is put into overcritical still, heating rate 1-3 ℃, be raised to appropriate temperature range (34.1-250 ℃) and reach under appropriate pressure range (7.1-45MPa), keeping 10-15h, making surfactant fully be extracted out;
4) after surfactant is extracted out fully, stopped heating makes overcritical still cooling, then takes out order mesoporous (TiO
2-Cu) nano complex;
5) to order mesoporous (TiO
2-Cu) carry out the distilled water rinsing, be treated to number 1-5 time;
6) to order mesoporous (TiO
2-Cu) chemical form etc. of nano complex specific area, aperture, crystal formation, surface topography, element carries out test analysis;
Embodiment 1: at first adopting the hydro-thermal method method, is that 99.0% titanium tetrachloride and 2g nitric acid gold are put into there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer; Secondly with DTAB (30g), after 160g distilled water and concentrated hydrochloric acid mix, slowly splash in there-necked flask by separatory funnel, controlling the pH value is between 1-3, and titanium tetrachloride forms " surfactant-inorganic matter " precipitation by hydrolysis; Then, 20g " surfactant-inorganic matter " precipitation is put in overcritical still, be warmed up to 100 ℃ according to 2 ℃/min of heating rate, after pressure is 9MPa, keep 12h; Then with overcritical still cool to room temperature, obtain order mesoporous " TiO
2-Cu " nano complex; At last, with the order mesoporous " TiO that obtains
2-Cu " nano complex carries out the distilled water rinsing and processes 4 times.Its crystal formation is anatase, and the nano particle aperture size is 2-5nm, and specific area is 85m
2/ g, order mesoporous (TiO
2-Cu) nano complex.
Embodiment 2: at first adopting the hydro-thermal method method, is that 99.0% titanium tetrachloride and 2g nitric acid gold are put into there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer; Secondly with DTAB (35g), after 160g distilled water and concentrated hydrochloric acid mix, slowly splash in there-necked flask by separatory funnel, controlling the pH value is between 1-3, and titanium tetrachloride forms " surfactant-inorganic matter " precipitation by hydrolysis; Then, 20g " surfactant-inorganic matter " precipitation is put in overcritical still, be warmed up to 100 ℃ according to 2 ℃/min of heating rate, after pressure is 9MPa, keep 12h; Then with overcritical still cool to room temperature, obtain order mesoporous " TiO
2-Cu " nano complex; At last, with the order mesoporous " TiO that obtains
2-Cu " nano complex carries out the distilled water rinsing and processes 4 times.Its crystal formation is anatase, and the nano particle aperture size is 2-5nm, and specific area is 95m
2/ g, order mesoporous (TiO
2-Cu) nano complex.
Embodiment 3: at first adopting the hydro-thermal method method, is that 99.0% titanium tetrachloride and 2g nitric acid gold are put into there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer; Secondly with DTAB (28g), after 160g distilled water and concentrated hydrochloric acid mix, slowly splash in there-necked flask by separatory funnel, controlling the pH value is between 1-3, and titanium tetrachloride forms " surfactant-inorganic matter " precipitation by hydrolysis; Then, 30g " surfactant-inorganic matter " precipitation is put in overcritical still, be warmed up to 100 ℃ according to 2 ℃/min of heating rate, after pressure is 9MPa, keep 12h; Then with overcritical still cool to room temperature, obtain order mesoporous " TiO
2-Cu " nano complex; At last, with the order mesoporous " TiO that obtains
2-Cu " nano complex carries out the distilled water rinsing and processes 4 times.Its crystal formation is anatase, and the nano particle aperture size is 2-5nm, and specific area is 83m
2/ g, order mesoporous (TiO
2-Cu) nano complex.
Embodiment 4: at first adopting the hydro-thermal method method, is that 99.0% titanium tetrachloride and 2g nitric acid gold are put into there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer; Secondly with DTAB (20g), after 160g distilled water and concentrated hydrochloric acid mix, slowly splash in there-necked flask by separatory funnel, controlling the pH value is between 1-3, and titanium tetrachloride forms " surfactant-inorganic matter " precipitation by hydrolysis; Then, 30g " surfactant-inorganic matter " precipitation is put in overcritical still, be warmed up to 100 ℃ according to 2 ℃/min of heating rate, after pressure is 9MPa, keep 12h; Then with overcritical still cool to room temperature, obtain order mesoporous " TiO
2-Cu " nano complex; At last, with the order mesoporous " TiO that obtains
2-Cu " nano complex carries out the distilled water rinsing and processes 4 times.Its crystal formation is anatase, and the nano particle aperture size is 2-5nm, and specific area is 78m
2/ g, order mesoporous (TiO
2-Cu) nano complex.
Embodiment 5: at first adopting the hydro-thermal method method, is that 99.0% titanium tetrachloride and 2g nitric acid gold are put into there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer; Secondly with DTAB (30g), after 160g distilled water and concentrated hydrochloric acid mix, slowly splash in there-necked flask by separatory funnel, controlling the pH value is between 1-3, and titanium tetrachloride forms " surfactant-inorganic matter " precipitation by hydrolysis; Then, 30g " surfactant-inorganic matter " precipitation is put in overcritical still, be warmed up to 100 ℃ according to 2 ℃/min of heating rate, after pressure is 12MPa, keep 13h; Then with overcritical still cool to room temperature, obtain order mesoporous " TiO
2-Cu " nano complex; At last, with the order mesoporous " TiO that obtains
2-Cu " nano complex carries out the distilled water rinsing and processes 3 times.Its crystal formation is anatase, and the nano particle aperture size is 2-5nm, and specific area is 96m
2/ g, order mesoporous (TiO
2-Cu) nano complex.
Embodiment 6: at first adopting the hydro-thermal method method, is that 99.0% titanium tetrachloride and 2g nitric acid gold are put into there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer; Secondly with DTAB (30g), after 160g distilled water and concentrated hydrochloric acid mix, slowly splash in there-necked flask by separatory funnel, controlling the pH value is between 1-3, and titanium tetrachloride forms " surfactant-inorganic matter " precipitation by hydrolysis; Then, 30g " surfactant-inorganic matter " precipitation is put in overcritical still, be warmed up to 100 ℃ according to 2 ℃/min of heating rate, after pressure is 15MPa, keep 15h; Then with overcritical still cool to room temperature, obtain order mesoporous " TiO
2-Cu " nano complex; At last, with the order mesoporous " TiO that obtains
2-Cu " nano complex carries out the distilled water rinsing and processes 4 times.Its crystal formation is anatase, and the nano particle aperture size is 2-5nm, and specific area is 108m
2/ g, order mesoporous (TiO
2-Cu) nano complex.
Embodiment 7: at first adopting the hydro-thermal method method, is that 99.0% titanium tetrachloride and 2g nitric acid gold are put into there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer; Secondly with DTAB (30g), after 150g distilled water and concentrated hydrochloric acid mix, slowly splash in there-necked flask by separatory funnel, controlling the pH value is between 1-3, and titanium tetrachloride forms " surfactant-inorganic matter " precipitation by hydrolysis; Then, 30g " surfactant-inorganic matter " precipitation is put in overcritical still, be warmed up to 100 ℃ according to 1 ℃/min of heating rate, after pressure is 10MPa, keep 12h; Then with overcritical still cool to room temperature, obtain order mesoporous " TiO
2-Cu " nano complex; At last, with the order mesoporous " TiO that obtains
2-Cu " nano complex carries out the distilled water rinsing and processes 4 times.Its crystal formation is anatase, and the nano particle aperture size is 2-5nm, and specific area is 89m
2/ g, order mesoporous (TiO
2-Cu) nano complex.
Embodiment 8: at first adopting the hydro-thermal method method, is that 99.0% titanium tetrachloride and 2g nitric acid gold are put into there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer; Secondly with DTAB (30g), after 180g distilled water and concentrated hydrochloric acid mix, slowly splash in there-necked flask by separatory funnel, controlling the pH value is between 1-3, and titanium tetrachloride forms " surfactant-inorganic matter " precipitation by hydrolysis; Then, 30g " surfactant-inorganic matter " precipitation is put in overcritical still, be warmed up to 100 ℃ according to 1 ℃/min of heating rate, after pressure is 12MPa, keep 14h; Then with overcritical still cool to room temperature, obtain order mesoporous " TiO
2-Cu " nano complex; At last, with the order mesoporous " TiO that obtains
2-Cu " nano complex carries out the distilled water rinsing and processes 4 times.Its crystal formation is anatase, and the nano particle aperture size is 2-5nm, and specific area is 68m
2/ g, order mesoporous (TiO
2-Cu) nano complex.
Order mesoporous (the TiO of the embodiment of the present invention
2-Cu) the nano complex physical and chemical performance is: through the synthetic mesoporous (TiO of supercritical extract
2-Cu) its crystalline structure of nano complex is anatase, crystallite dimension is between 20-40nm.Under the low power Electronic Speculum, order mesoporous (TiO
2-Cu) the nano complex surface topography is more even, and hole is arranged, under the high power Electronic Speculum, and order mesoporous (TiO
2-Cu) few surface defects only contains the seldom impurity of amount; Near the obvious UV absorption of generation turning 375nm, compare the pure TiO of P25 simultaneously
2Powder, order mesoporous (TiO
2-Cu) nano complex has obvious central hole structure.
Order mesoporous (TiO
2-Cu) nano complex, its organic matter almost extracts fully, and the O-H linkage content is relatively high, and this is mainly due to due to moisture that complex surfaces absorbs.
The above is only preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., within all should being included in protection scope of the present invention.
Claims (7)
1. order mesoporous (TiO
2-Cu) the preparation technology of nano complex, it is characterized in that, this preparation technology synthesizes " surfactant-inorganic matter " precipitation by soft template method, then, adopt supercritical extraction technique with the extraction from precipitation of surfactant soft template, then process synthesizing ordered mesoporous (TiO by the distilled water rinsing
2-Cu) nano complex.
2. order mesoporous (TiO according to claim 1
2-Cu) the preparation technology of nano complex is characterized in that, this preparation technology's concrete steps are:
1), take titanium tetrachloride as initiation material, take DTAB as the surfactant soft template, under the interaction of distilled water, concentrated hydrochloric acid, by hydro-thermal reaction synthesis of nano complex;
2), take ethanol, methyl alcohol as extractant, after supercritical extract surfactant soft template, then adopt the distilled water rinsing to process, prepare order mesoporous (TiO
2-Cu) composite.
3. order mesoporous (TiO according to claim 2
2-Cu) the preparation technology of nano complex is characterized in that the agents useful for same percentage by weight is: titanium tetrachloride, purity＞99.0,50-65%; Deionized water, 1-5%; Absolute ethyl alcohol, purity＞99.9,75-85%; Methyl alcohol, purity＞99.9,70-80%, DTAB, purity＞99.0,10-20%; The nitric acid gold, purity＞99.0,0.5-1%.
4. order mesoporous (TiO according to claim 2
2-Cu) the preparation technology of nano complex is characterized in that, by hydro-thermal method, and preparation " soft template-inorganic matter " nano complex, titanium tetrachloride: the soft template control range is 4-1.5, and pH is controlled at 1-3.
5. order mesoporous (TiO according to claim 2
2-Cu) the preparation technology of nano complex, it is characterized in that, " soft template-inorganic matter " nano complex is put into autoclave, by supercritical extraction technique, surfactant is extracted from " soft template-inorganic matter " nano complex, heating rate 2-4 ℃, be raised to appropriate temperature range (34.1-250 ℃) and reach under appropriate pressure range (7.1-45MPa), keeping 10-15h.
6. order mesoporous (TiO according to claim 2
2-Cu) the preparation technology of nano complex is characterized in that, with order mesoporous (TiO
2-Cu) nano complex passes through distilled water rinsing 1-5 time.
7. one kind is utilized order mesoporous (TiO claimed in claim 1
2-Cu) order mesoporous (the TiO of the preparation technology preparation of nano complex
2-Cu) nano complex.
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Cited By (4)
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| CN104722300A (en) * | 2015-03-02 | 2015-06-24 | 郑州大学 | Cu-TiO2 photocatalyst and preparation method thereof |
| CN105080546A (en) * | 2015-07-13 | 2015-11-25 | 吉首大学 | Conductive carbon felt loaded ferric ferric-doped mesoporous titanium oxide gas diffuse photoelectrode and preparation method therefor |
| CN105293949A (en) * | 2015-10-23 | 2016-02-03 | 苏磊 | TiO2-based photocatalytic self-cleaning glass and preparation method thereof |
| CN109126791A (en) * | 2018-07-24 | 2019-01-04 | 福州大学 | A kind of Cu (II)-mTiO2Loaded photocatalyst and its preparation and application |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104722300A (en) * | 2015-03-02 | 2015-06-24 | 郑州大学 | Cu-TiO2 photocatalyst and preparation method thereof |
| CN105080546A (en) * | 2015-07-13 | 2015-11-25 | 吉首大学 | Conductive carbon felt loaded ferric ferric-doped mesoporous titanium oxide gas diffuse photoelectrode and preparation method therefor |
| CN105080546B (en) * | 2015-07-13 | 2016-12-07 | 吉首大学 | Conduction charcoal felt loaded iron doped meso-porous titanium oxide gas diffusion optoelectronic pole and preparation method thereof |
| CN105293949A (en) * | 2015-10-23 | 2016-02-03 | 苏磊 | TiO2-based photocatalytic self-cleaning glass and preparation method thereof |
| CN105293949B (en) * | 2015-10-23 | 2019-03-12 | 苏磊 | A kind of TiO2Base optic catalytic self-cleaning glass and preparation method thereof |
| CN109126791A (en) * | 2018-07-24 | 2019-01-04 | 福州大学 | A kind of Cu (II)-mTiO2Loaded photocatalyst and its preparation and application |
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| CN103143356B (en) | 2015-03-11 |
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