CN103127932A - Preparation method of nanometer niobium-series photocatalyst - Google Patents
Preparation method of nanometer niobium-series photocatalyst Download PDFInfo
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- CN103127932A CN103127932A CN2013100879692A CN201310087969A CN103127932A CN 103127932 A CN103127932 A CN 103127932A CN 2013100879692 A CN2013100879692 A CN 2013100879692A CN 201310087969 A CN201310087969 A CN 201310087969A CN 103127932 A CN103127932 A CN 103127932A
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Abstract
The invention provides a nanocrystallization preparation method for a photocatalytic material NaNbO3. According to the photocatalytic material, the weakness that the traditional photocatalytic material is low in efficiency is overcome, and the speed for preparing hydrogen by utilizing water splitting is accelerated. A NaNbO3 nanowire is controllably synthesized at low temperature by utilizing a hydrothermal method. The preparation method of the NaNbO3 nanowire comprises the steps of adding 1 g of P123 into 25 ml of distilled water, continuously stirring for 2 h at 40 DEG C, and adding 5 g of Nb(OC2H5); dropwise adding 10 mL of sodium hydroxide solution (NaOh) with the concentration of 0.8 g/ml; after stirring for 1 h, transferring the obtained solution into a high-pressure kettle, and carrying out heat treatment for 24 h at 200 DEG C; after being filtered, respectively washing obtained precipitates with the distilled water and ethanol, and drying the precipitates for 24 h in a drying oven at 70 DEG C; and then respectively calcinating obtained powder at 550 DEG C, maintaining the temperature for 4 h, and cooling to the room temperature by utilizing a natural cooling manner. The P123 is replaced by PEG (Polyethylene Glycol) to prepare nanometer square NaNbO3.
Description
Technical field
The present invention relates to semiconductor nano material preparation and application, especially a kind of preparation of catalysis material sodium niobate nano and hydrogen manufacturing performance thereof.
Background technology
The consumption of tradition fossil energy has caused the problems such as greenhouse effects of the earth, environmental pollution and energy shortage, is the significant challenge that current mankind faces.Under this background, take low energy consumption, the low focus that is just becoming whole world care and research as " low-carbon economy " on basis that pollutes.Hydrogen is described as " following oil " as a kind of secondary energy sources carrier of high-efficiency cleaning.Therefore, exploitation is pollution-free, hydrogen producing technology is subject to showing great attention to of various countries day by day cheaply.As far back as 1971, the Fujishima of Tokyo Univ Japan and Honda found at N-shaped semiconductor TiO
2On the monocrystalline optoelectronic pole, decomposition water makes the phenomenon of hydrogen, this means that people can directly utilize the hydrogen energy source of solar energy and catalysis material decomposition water preparation cleaning.The photocatalytic hydrogen production by water decomposition process from the angle of Conversion of Energy, is reproducible solar energy to be converted into the chemical energy (Hydrogen Energy) of cleaning, realizes the storage of solar energy.Hydrogen is as clean energy resource, and after its energy discharges, final product is water, and this process is there is no pollutant and greenhouse gases CO
2Produce.Therefore, it also is considered to " mankind's dream technology ", is that the mankind have great expectations of one of the energy that solution faces at present and approach of environmental problem.Early stage most photochemical catalyzing research work is mainly around titanium dioxide (TiO
2) and modifier carry out.Calendar year 2001, Zou Zhigang etc. report Ni doping InTaO on Nature
4Catalysis material has realized first that worldwide under radiation of visible light, pure water decomposes, for the breakthrough of this key technology of decomposing water with solar energy hydrogen manufacturing is laid a good foundation.2006, Domen etc. realized that take GaN/ZnO solid solution as catalysis material the quantum efficiency of decomposing pure water under 420～440nm wavelength radiation of visible light reaches 2.5%, has further confirmed the application prospect of photocatalytic hydrogen production by water decomposition.But the efficient of most catalysis material photocatalytic hydrogen production by water decomposition is on the low side, and the catalysis material of studying a kind of high efficiency hydrogen production by water decomposition becomes most important.
Summary of the invention
The present invention a kind of catalysis material NaNbO is provided
3The preparation method of nanometer.This catalysis material has overcome the inefficient weakness of traditional catalysis material, has improved the speed of hydrogen production by water decomposition gas.
Technical scheme of the present invention is: the hydrothermal method of assisting by surfactant synthesizes presoma Na
2Nb
2O
6H
2Then the O nano wire adopts the method for calcining under electric furnace Air atmosphere to prepare NaNbO
3Nano wire.Concrete steps are as follows:
(1) 1g surfactant P123 adds in 25mL distilled water, adds 5gNb (OC after continuing to stir 2h under 40 ℃
2H
5)
5
(2) mentioned solution dropwise being added 10mL concentration is the sodium hydroxide solution of 0.8g/mL.
(3) after stirring 1h, the solution that obtains is transferred in autoclave, and at 200 ℃ of lower heat treatment 24h.
(4) after resulting sedimentation and filtration, respectively with the washing of distilled water and ethanol, and in the baking oven of 70 ℃ 12h.
(5) with 550 ℃ of resulting powder calcinings, temperature retention time is 4h, and adopts the mode of nature cooling to get back to room temperature, obtains catalysis material NaNbO
3Nano wire.
(6) Pt supports the method that adopts light deposition, adds NaNbO in methanol solution (concentration 20%)
3Powder and chloroplatinic acid, after irradiation 1h under the high-pressure sodium lamp of 400W, after resulting sedimentation and filtration, with the washing of distilled water and ethanol, and in the baking oven of 70 ℃ dry 12h.Obtain Pt and support catalysis material NaNbO
3Nano wire.
In order to contrast, replace P123 with PEG, adopt the NaNbO of the synthetic square shape of hydro-thermal method
3, concrete steps are as follows:
(1) the 1g Surfactant PEG adds in 25mL distilled water, adds 5gNb (OC after continuing to stir 2h under 40 ℃
2H
5)
5
(2) mentioned solution dropwise being added 10mL concentration is the sodium hydroxide solution of 0.8g/mL.
(3) after stirring 1h, the solution that obtains is transferred in autoclave, and at 200 ℃ of lower heat treatment 24h.
(4) after resulting sedimentation and filtration, respectively with the washing of distilled water and ethanol, and in the baking oven of 70 ℃ 12h.
(5) with 550 ℃ of resulting powder calcinings, temperature retention time is 4h, and adopts the mode of nature cooling to get back to room temperature, obtains the NaNbO of square shape
3
(6) Pt supports the method that adopts light deposition, adds NaNbO in methanol solution (concentration 20%)
3Powder and chloroplatinic acid, after irradiation 1h under the high-pressure sodium lamp of 400W, after resulting sedimentation and filtration, with the washing of distilled water and ethanol, and in the baking oven of 70 ℃ dry 12h, obtain the NaNbO that Pt supports the square shape
3
Hydrothermal method of the present invention has been realized NaNbO
3The low temperature controlledly synthesis of nano wire and nano square, synthetic with wet chemistry method, realized Na, Nb, the O mixing on molecular level.The product size uniform, and be mono-crystalline structures.A step water-heat process of the present invention, technique is simple, and flow process is short, and constant product quality is easy to realize industrialization.
Description of drawings
Fig. 1 is the NaNbO of distinct methods preparation
3The activity of photocatalysis Decomposition hydrogen manufacturing contrast after Pt supports.
Fig. 2 is the circular response that catalysis material produces hydrogen.
The specific embodiment
The invention provides a kind of catalysis material NaNbO
3The preparation method of nanometer and the performance of its photocatalytic hydrogen production by water decomposition.Utilize the generating rate of hydrogen to estimate the performance of photochemical catalyzing.Reaction is to carry out in an airtight glass system.This device mainly is comprised of sampler chamber, confined reaction system, circulating pump and photo catalysis reactor.The vacuum of system shows by barometer, and the realization of vacuum is realized by extraction valve by vavuum pump.Further this programme is described by following instance.
The specific embodiment one: NaNbO
3The preparation method of nano wire.
(1) 1g P123 adds in 25mL distilled water, adds 5g Nb (OC after continuing to stir 2h under 40 ℃
2H
5)
5
(2) mentioned solution dropwise being added 10mL concentration is the sodium hydroxide solution of 0.8g/mL.
(3) after stirring 1h, the solution that obtains is transferred in autoclave, and at 200 ℃ of lower heat treatment 24h.
(4) after resulting sedimentation and filtration, respectively with the washing of distilled water and ethanol, and in the baking oven of 70 ℃ 12h.
(5) with 550 ℃ of resulting powder calcinings, temperature retention time is 4h, and adopts the mode of nature cooling to get back to room temperature, obtains catalysis material NaNbO
3Nano wire.
(6) Pt supports the method that adopts light deposition, adds NaNbO in methanol solution (concentration 20%)
3Powder and chloroplatinic acid, after irradiation 1h under the high-pressure sodium lamp of 400W, after resulting sedimentation and filtration, with the washing of distilled water and ethanol, and in the baking oven of 70 ℃ dry 12h.Obtain Pt and support catalysis material NaNbO
3Nano wire.
The specific embodiment two: the NaNbO of square shape
3Preparation.
(1) 1g PEG adds in 25mL distilled water, adds 5g Nb (OC after continuing to stir 2h under 40 ℃
2H
5)
5
(2) mentioned solution dropwise being added 10mL concentration is the sodium hydroxide solution of 0.8g/mL.
(3) after stirring 1h, the solution that obtains is transferred in autoclave, and at 200 ℃ of lower heat treatment 24h.
(4) after resulting sedimentation and filtration, respectively with the washing of distilled water and ethanol, and in the baking oven of 70 ℃ 12h.
(5) with 550 ℃ of resulting powder calcinings, temperature retention time is 4h, and adopts the mode of nature cooling to get back to room temperature.Obtain the NaNbO of square shape
3
(6) Pt supports the method that adopts light deposition, adds NaNbO in methanol solution (concentration 20%)
3Powder and chloroplatinic acid, after irradiation 1h under the high-pressure sodium lamp of 400W, after resulting sedimentation and filtration, with the washing of distilled water and ethanol, and in the baking oven of 70 ℃ dry 12h.Obtain the NaNbO that Pt supports the square shape
3
The specific embodiment three: NaNbO
3The preparation method of particle.
(1) with Nb
2O
5And NaCO
3Pressed powder mixes by the stoichiometric proportion of reaction, and pressed powder grinds in agate mortar after adding absolute ethyl alcohol.
(2) take out after the temperature lower calcination 4h of 800 ℃, calcine 5h again under 900 ℃ after again grinding.
(3) after the high-temperature calcination reaction finishes, naturally cool to room temperature, and grind standby.
The specific embodiment four: NaNbO
3The product hydrogen performance evaluation of nano wire.
(1) take the catalysis material NaNbO of 0.1g
3Nano wire joins H
2O (220mL) and CH
3In OH (50mL) solution, make under the magnetic agitation effect during catalysis material is suspended in reaction system.
(2) by vacuum pump system, the air in system is pumped, more a certain amount of argon gas that is filled with is as carrier gas.
(3) whole reaction is at room temperature carried out, and connects recirculated cooling water during reaction to avoid the mercury lamp excess Temperature to cause that system leaks.
(4) gas that produces mixes by circulating pump in closed system, and the hydrogen of generation and the amount of oxygen are taken a sample by sampler chamber, and then the method for gas chromatographic analysis detects.The speed of producing hydrogen is 13.5mmol/h.
The specific embodiment five: square shape NaNbO
3Product hydrogen performance evaluation.
Different from the specific embodiment four is, with the NaNbO in step (1)
3Nano wire changes the NaNbO of square complexion into
3, the speed of producing hydrogen is 4.0mmol/h.
The specific embodiment six: granular NaNbO
3Product hydrogen performance evaluation.
Different from the specific embodiment four is, with the NaNbO in step (1)
3Nano wire changes granular NaNbO into
3, the speed of producing hydrogen is 0.9mmol/h, well below NaNbO
3The hydrogen-producing speed of nano wire.
Claims (9)
1. catalysis material NaNbO
3The preparation method of nano wire comprises following step: (1) 1g P123 adds in 25mL distilled water, adds 5g Nb (OC after continuing to stir 2h under 40 ℃
2H
5)
5(2) dropwise adding 10mL concentration is the sodium hydroxide solution of 0.8g/mL.(3) after stirring 1h, the solution that obtains is transferred in autoclave, and at 200 ℃ of lower heat treatment 24h.(4) after resulting sedimentation and filtration, respectively with the washing of distilled water and ethanol, and in the baking oven of 70 ℃ 12h.(5) resulting powder is calcined respectively 550 ℃, temperature retention time is 4h, and adopts the mode of nature cooling to get back to room temperature.(6) in a typical case, contain and add NaNbO in methanol solution
3Powder and chloroplatinic acid, after irradiation 1h under the high-pressure sodium lamp of 400W, after resulting sedimentation and filtration, with the washing of distilled water and ethanol, and in the baking oven of 70 ℃ dry 12h.
2. the method for claim 1, is characterized in that preparing NaNbO
3Nano wire used reactant be Nb (OC
2H
5)
5, P123 and NaOH, and the gained precipitation need to be washed respectively with distilled water and ethanol.
3. the method for claim 1, is characterized in that heat treatment 24h.It is characterized in that the heat treatment bake out temperature is 923 ℃.
4. the NaNbO of a square shape
3The preparation method, comprise following step: (1) 1g PEG adds in 25mL distilled water, is adding 5g Nb (OC after continue stirring 2h under 40 ℃
2H
5)
5(2) dropwise adding 10mL concentration is the sodium hydroxide solution of 0.8g/mL.(3) after stirring 1h, the solution that obtains is transferred in autoclave, and at 200 ℃ of lower heat treatment 24h.(4) after resulting sedimentation and filtration, respectively with the washing of distilled water and ethanol, and in the baking oven of 70 ℃ 12h.(5) resulting powder is calcined respectively 550 ℃, temperature retention time is 4h, and adopts the mode of nature cooling to get back to room temperature.(6) in a typical case, contain and add NaNbO in methanol solution
3Powder and chloroplatinic acid, after irradiation 1h under the high-pressure sodium lamp of 400W, after resulting sedimentation and filtration, with the washing of distilled water and ethanol, and in the baking oven of 70 ℃ dry 12h.
5. method as claimed in claim 4 is characterized in that preparing the NaNbO of square complexion
3Reactant used is Nb (OC
2H
5)
5, PEG and NaOH, and the gained precipitation need to be washed respectively with distilled water and ethanol.
6. method as claimed in claim 4, is characterized in that heat treatment 24h.It is characterized in that the heat treatment bake out temperature is 923 ℃.
7. catalysis material NaNbO
3The preparation method of particle comprises following step: (1) is with Nb
2O
5And Na
2CO
3Pressed powder mixes by the stoichiometric proportion of reaction, and pressed powder grinds in agate mortar after adding absolute ethyl alcohol.(2) take out after the temperature lower calcination 4h of 800 ℃, calcine 5h again under 900 ℃ after again grinding.(3) after the high-temperature calcination reaction finishes, naturally cool to room temperature, and grind.
8. method as claimed in claim 7, is characterized in that preparing NaNbO
3Particle used reactant be Nb
2O
5And Na
2CO
3, and mix by stoichiometric proportion.
9. method as claimed in claim 7, is characterized in that heat treatment 4h.It is characterized in that the heat treatment bake out temperature is 800 ℃.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399418A (en) * | 2015-12-08 | 2016-03-16 | 南京航空航天大学 | Preparation method of high-performance sodium niobate dielectric ceramic powder |
| CN107758743A (en) * | 2017-11-17 | 2018-03-06 | 北京工业大学 | A kind of method that cation exchange approach prepares sodium niobate nano line |
| CN107961782A (en) * | 2017-12-14 | 2018-04-27 | 聊城大学 | A kind of cube NaNbO with square hole3The preparation method of catalysis material |
| CN109748317A (en) * | 2019-03-08 | 2019-05-14 | 淮北师范大学 | A kind of controllable synthesis method of hydrogen fluoride nano zinc oxide material |
| CN110474029A (en) * | 2019-07-11 | 2019-11-19 | 江苏师范大学 | A kind of anode composite material of lithium sulfur battery and preparation method thereof |
| CN115121261A (en) * | 2022-06-28 | 2022-09-30 | 天津城建大学 | NaNbO for photoelectrocatalysis 3 /Co(OH) 2 Preparation method of/Ag composite film material |
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| CN1946814A (en) * | 2004-04-26 | 2007-04-11 | 昭和电工株式会社 | Coating material and use thereof |
| CN101507921A (en) * | 2009-03-20 | 2009-08-19 | 华中师范大学 | Carbon-doped niobium pentaoxide nano-structure visible-light photocatalyst and non-water body low-temperature preparation method thereof |
| CN102658139A (en) * | 2012-05-08 | 2012-09-12 | 江南大学 | Sodium niobate nanowire photocatalyst and preparation method thereof |
-
2013
- 2013-03-13 CN CN2013100879692A patent/CN103127932A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1946814A (en) * | 2004-04-26 | 2007-04-11 | 昭和电工株式会社 | Coating material and use thereof |
| CN101507921A (en) * | 2009-03-20 | 2009-08-19 | 华中师范大学 | Carbon-doped niobium pentaoxide nano-structure visible-light photocatalyst and non-water body low-temperature preparation method thereof |
| CN102658139A (en) * | 2012-05-08 | 2012-09-12 | 江南大学 | Sodium niobate nanowire photocatalyst and preparation method thereof |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399418A (en) * | 2015-12-08 | 2016-03-16 | 南京航空航天大学 | Preparation method of high-performance sodium niobate dielectric ceramic powder |
| CN107758743A (en) * | 2017-11-17 | 2018-03-06 | 北京工业大学 | A kind of method that cation exchange approach prepares sodium niobate nano line |
| CN107961782A (en) * | 2017-12-14 | 2018-04-27 | 聊城大学 | A kind of cube NaNbO with square hole3The preparation method of catalysis material |
| CN107961782B (en) * | 2017-12-14 | 2020-07-10 | 聊城大学 | Cubic NaNbO with square hole3Preparation method of photocatalytic material |
| CN109748317A (en) * | 2019-03-08 | 2019-05-14 | 淮北师范大学 | A kind of controllable synthesis method of hydrogen fluoride nano zinc oxide material |
| CN109748317B (en) * | 2019-03-08 | 2021-03-16 | 淮北师范大学 | Controllable synthesis method of zinc fluoride hydroxide nano material |
| CN110474029A (en) * | 2019-07-11 | 2019-11-19 | 江苏师范大学 | A kind of anode composite material of lithium sulfur battery and preparation method thereof |
| CN110474029B (en) * | 2019-07-11 | 2022-06-10 | 江苏师范大学 | Lithium-sulfur battery positive electrode composite material and preparation method thereof |
| CN115121261A (en) * | 2022-06-28 | 2022-09-30 | 天津城建大学 | NaNbO for photoelectrocatalysis 3 /Co(OH) 2 Preparation method of/Ag composite film material |
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Application publication date: 20130605 |