CN102502814B - Application of solid-solution type sodium zirconate titanate micro/nanobelt powdery material - Google Patents
Application of solid-solution type sodium zirconate titanate micro/nanobelt powdery material Download PDFInfo
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Abstract
The invention relates to application of a solid-solution type sodium zirconate titanate micro/nanobelt material, particularly application of a solid-solution type sodium zirconate titanate micro/nanobelt powdery material. The invention provides application of the solid-solution type sodium zirconate titanate micro/nanobelt material and realizes cycle use. 0.1g of the solid-solution type sodium zirconate titanate micro/nanobelt material prepared by the application generates 7-11mumol of hydrogen for each hour. The solid-solution type sodium zirconate titanate micro/nanobelt powdery material is used for photocatalyst for hydrogen production.
Description
Technical field
The present invention relates to a kind of application of solid-solution type titanium sodium zirconate micro-/ nano carrying material.
Background technology
Energy problem and high-efficiency solar transition material are one of the research emphasis of 21st century nano material, and nano barium titanate salt material is a based semiconductor metallic compound of finding that at present photocatalytic hydrogen production activity is higher, there are the huge potential advantages as new energy materials application.In addition,, due to its unique physical and chemical performance, nano barium titanate salt material has important application prospect too in fields such as gas adsorption, degraded harmful ion and pollutent and ionization celies.Its microtexture is depended in the performance of titanate material and application, and particle size and specific surface area are also the key factors that affects its performance.Nano strip titanate powder is due to its unique one-dimentional structure and large specific surface area, aspect photocatalytic activity and the manufacture micro-nano Primary Component of hypersensitization (as transistor, opto-electronic device, gas sensor and biosensor etc.), show excellent performance advantage.Therefore, design, research and development nano strip titanate powder are such material to be further applied to the crucial matter of science and technology of photocatalysis hydrogen production and hypersensitization devices field.
Our group patent applied for < < amorphous metal surface titanium zirconium solid solution micro-/ nano film and preparation method thereof > > (application number: 201110153429.0) although in solved the problem of preparing solid-solution type titanate material, but because the titanium zirconium solid solution micro-/ nano film of preparation is film like product, exist photocatalytic activity limited, amorphous metal matrix can not reuse, prepare the first-class limitation of matrix used material list with not enough, if and this film like product is transformed into Powdered, exist converting process method complicated, be difficult to the difficulties such as batch production, particularly can not obtain completely single, pure dusty material.In addition, in transition process, destroy microtexture and the tissue of original film like product, can reduce the photocatalysis performance of product, and increased preparation cost.Therefore prior art is prepared the problem that solid-solution type titanate powder exists that raw material types is limited and utilization ratio is low, prepared material purity is low and photocatalysis performance is low and separation method is difficult, is difficult to batch production, cost is high.
Summary of the invention
The invention provides a kind of application of solid-solution type sodium zirconate titanate micro/nanobelt powdery material, realization recycles, and the amounts of hydrogen of the solid-solution type sodium zirconate titanate micro/nanobelt powdery material production hourly prepared of every 0.1g the application is 7～11 μ mol.
A kind of preparation method of solid-solution type sodium zirconate titanate micro/nanobelt powdery material, specifically complete according to the following steps: one, sodium hydroxide and deionized water are put into closed reaction vessel, then adding diameter is the titanium zirconium base alloy powder of 5～150 μ m, in temperature, be that 110 ℃～190 ℃, pressure are under 1MPa～40MPa, to react 3～200 hours, then naturally cool to room temperature, obtain reaction product mixed system; Two, in the reaction product mixed system of preparing to step 1, add deionized water, the pH value of reaction product mixed system prepared by step 1 is reconciled to neutral, then isolate the throw out of closed reaction container bottom, in temperature, be at 50 ℃～90 ℃, isolated throw out to be dried to constant weight, obtain the titanium zirconium base alloy powder of surface growth solid-solution type titanium sodium zirconate micro-/ nano band; Three, in the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of the preparation in step 2, add deionized water, then under greenhouse, stirring velocity with 60～800rpm stirs 2～60min, the suspension liquid evaporate to dryness that separation is obtained, obtains solid-solution type sodium zirconate titanate micro/nanobelt powdery material; The mass ratio of the sodium hydroxide described in step 1 and deionized water is (0.01～0.5): 1; The mass ratio of the sodium hydroxide described in step 1 and titanium zirconium base alloy powder is (0.5～50): 1; The mass ratio of the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of the deionized water adding described in step 3 and the preparation in step 2 is (15～1500): 1.
Advantage of the present invention: the solid-solution type sodium zirconate titanate micro/nanobelt powdery material that, prepared by the present invention can recycle as photocatalysis hydrogen production, and has improved photocatalytic hydrogen production activity; Two, simple, the cleanliness without any pollution of technique of the present invention, can be for industrialized mass production solid-solution type sodium zirconate titanate micro/nanobelt powdery material; Three, the titanium zirconium base alloy powder that the present invention uses can recycle, and has improved material use efficiency, has reduced production cost.
Accompanying drawing explanation
Fig. 1 is 1500 times of scanning electronic microscope (SEM) figure that tests the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of preparing in a step 2; Fig. 2 is the optical photograph figure of the solid-solution type sodium zirconate titanate micro/nanobelt powdery material prepared of test one step 3; Fig. 3 is the photocatalysis hydrogen production performance map of the solid-solution type sodium zirconate titanate micro/nanobelt powdery material prepared of test one step 3, A in figure represents primary detected result, B in figure represents secondary detected result, and the C in figure represents detected result for the third time; Fig. 4 is 3000 times of scanning electronic microscope (SEM) figure that tests the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of preparing in two step 2.
Embodiment
Embodiment one: present embodiment is a kind of preparation method of solid-solution type sodium zirconate titanate micro/nanobelt powdery material, specifically completes according to the following steps:
One, sodium hydroxide and deionized water are put into closed reaction vessel, then adding diameter is the titanium zirconium base alloy powder of 5～150 μ m, in temperature, be that 110 ℃～190 ℃, pressure are under 1MPa～40MPa, to react 3～200 hours, then naturally cool to room temperature, obtain reaction product mixed system; Two, in the reaction product mixed system of preparing to step 1, add deionized water, the pH value of reaction product mixed system prepared by step 1 is reconciled to neutral, then isolate the throw out of closed reaction container bottom, in temperature, be at 50 ℃～90 ℃, isolated throw out to be dried to constant weight, obtain the titanium zirconium base alloy powder of surface growth solid-solution type titanium sodium zirconate micro-/ nano band; Three, in the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of the preparation in step 2, add deionized water, then under greenhouse, stirring velocity with 60～800rpm stirs 2～60min, the suspension liquid evaporate to dryness that separation is obtained, obtains solid-solution type sodium zirconate titanate micro/nanobelt powdery material.
The mass ratio of the sodium hydroxide described in present embodiment step 1 and deionized water is (0.01～0.5): 1; The mass ratio of the sodium hydroxide described in present embodiment step 1 and titanium zirconium base alloy powder is (0.5～50): 1.
The mass ratio of the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of the deionized water adding described in present embodiment step 3 and the preparation in step 2 is (15～1500): 1.
Because present embodiment adopts titanium zirconium base alloy, powder is spherical, therefore be the solid-solution type titanium sodium zirconate micro-/ nano band in spherical surface growth, with comparing very easily separated peeling off containing the epontic solid-solution type titanium of the titanium-based amorphous tinsel of zirconium sodium zirconate micro-/ nano band, and adopt simple and convenient magnetic agitation method can reach separated object; And the solid-solution type sodium zirconate titanate micro/nanobelt powdery material obtaining has kept the solid-solution type titanium sodium zirconate original microtexture of micro-/ nano band and tissue, keep to greatest extent the good photocatalysis performance of solid-solution type titanium sodium zirconate micro-/ nano band.And the solid-solution type sodium zirconate titanate micro/nanobelt powdery material of preparation is compared the performance with recycling with film like product.Can be in addition, because separated powdered alloy matrix and micro-/ nano carrying material have density difference, micro-/ nano band will be suspended in aqueous solution upper strata, and powdered alloy matrix will be deposited in rapidly aqueous solution bottom, this is also convenient to further separated solid-solution type titanium sodium zirconate micro-/ nano band be taken out to obtain highly purified dusty material.Prior, in present embodiment step 3, through separated, the dry titanium zirconium base alloy powder obtaining, can be used as new titanium zirconium body material recycling, be that the powdered alloy that present embodiment is used can recycle, improved material use efficiency, reduced production cost.
In present embodiment step 3, the separated precipitation obtaining can be used as the titanium zirconium base alloy powder continuation use of producing solid-solution type sodium zirconate titanate micro/nanobelt powdery material next time after drying, although can there is the solid-solution type titanium sodium zirconate micro-/ nano band of not peeling off completely in the separated titanium zirconium base alloy powder surface obtaining, but because the product of preparation is constant, still can not affect purity and the quality of product; And present embodiment solved and prepared the problem that thin-film material amorphous metal matrix can not reuse, improved utilization rate of raw materials, reduced cost.
Solid-solution type sodium zirconate titanate micro/nanobelt powdery material prepared by present embodiment can recycle as photocatalysis hydrogen production, and has improved photocatalytic hydrogen production activity.
Present embodiment technique is simple, cleanliness without any pollution, can be for industrialized mass production solid-solution type sodium zirconate titanate micro/nanobelt powdery material.
Adopt following verification experimental verification invention effect:
Test one: a kind of preparation method of solid-solution type sodium zirconate titanate micro/nanobelt powdery material, specifically completes according to the following steps:
One, sodium hydroxide and deionized water are put into closed reaction vessel, then adding diameter is the titanium zirconium base alloy powder of 70～100 μ m, in temperature, be that 140 ℃, pressure are under 30MPa, to react 24 hours, then naturally cool to room temperature, obtain reaction product mixed system; Two, in the reaction product mixed system of preparing to step 1, add deionized water, the pH value of reaction product mixed system prepared by step 1 is reconciled to neutral, then isolate the throw out of closed reaction container bottom, in temperature, be at 80 ℃, isolated throw out to be dried to constant weight, obtain the titanium zirconium base alloy powder of surface growth solid-solution type titanium sodium zirconate micro-/ nano band; Three, in the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of the preparation in step 2, add deionized water, then under greenhouse, stirring velocity with 60rpm stirs 15min, the suspension liquid evaporate to dryness that separation is obtained, obtains solid-solution type sodium zirconate titanate micro/nanobelt powdery material.
The mass ratio of the sodium hydroxide described in this testing sequence one and deionized water is 0.3:1; The mass ratio of the sodium hydroxide described in this testing sequence one and titanium zirconium base alloy powder is 25:1.
Titanium zirconium base alloy powder described in this testing sequence one is to adopt industrial aerosolization method, with industrial pure material, prepares.Adopting industrial aerosolization method and industrial pure material to prepare titanium zirconium base alloy powder has advantages of pollution-free and with low cost.
In titanium zirconium base alloy powder described in this testing sequence one, titanium and zirconium mass ratio are 20:1, and titanium zirconium base alloy powder is titanium zirconium-base amorphous alloy powder.
The mass ratio of the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of the deionized water adding described in this testing sequence three and the preparation in step 2 is 200:1.
In this testing sequence two, the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of preparation carries out electron-microscope scanning, obtains 1500 times of scanning electronic microscope (SEM) figure, as shown in Figure 1.As can be seen from Figure 1, the thickness of the independent a slice solid-solution type titanium sodium zirconate micro-/ nano band in this testing sequence two on the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of preparation is 1～100nm, length is 1～150 μ m, and the diameter of micro-flowers is at 20～150 μ m.
The optical photograph figure of the solid-solution type sodium zirconate titanate micro/nanobelt powdery material of this test preparation as shown in Figure 2.As can be seen from Figure 2, the solid-solution type sodium zirconate titanate micro/nanobelt powdery material of this test preparation is white powder product.
Adopt following methods to detect the photocatalytic hydrogen production activity of the solid-solution type sodium zirconate titanate micro/nanobelt powdery material of this test preparation:
Detect one:
First 40ml methanol aqueous solution is poured in quartz container, then the solid-solution type sodium zirconate titanate micro/nanobelt powdery material that takes this test of 0.1g preparation immerses in 40ml methanol aqueous solution, under ultraviolet source irradiation, every sampling in 30 minutes once, adopt chromatogram to measure the hydrogen content producing, in wherein said methanol aqueous solution, the volume ratio of methyl alcohol and deionized water is 1:9, and wherein said ultraviolet source is mercury lamp.
Detect two:
40ml methanol aqueous solution is poured in quartz container, then solid-solution type sodium zirconate titanate micro/nanobelt powdery material is immersed in 40ml methanol aqueous solution, under ultraviolet source irradiation, every sampling in 30 minutes once, adopt chromatogram to measure the hydrogen content producing, in wherein said methanol aqueous solution, the volume ratio of methyl alcohol and deionized water is 1:9, wherein said ultraviolet source is mercury lamp, wherein said solid-solution type sodium zirconate titanate micro/nanobelt powdery material is to detect used solid-solution type sodium zirconate titanate micro/nanobelt powdery material in to separate, oven dry obtains.
Detect three:
40ml methanol aqueous solution is poured in quartz container, then solid-solution type sodium zirconate titanate micro/nanobelt powdery material is immersed in 40ml methanol aqueous solution, under ultraviolet source irradiation, every sampling in 30 minutes once, adopt chromatogram to measure the hydrogen content producing, in wherein said methanol aqueous solution, the volume ratio of methyl alcohol and deionized water is 1:9, wherein said ultraviolet source is mercury lamp, wherein said solid-solution type sodium zirconate titanate micro/nanobelt powdery material is to detect used solid-solution type sodium zirconate titanate micro/nanobelt powdery material in two to separate, oven dry obtains.
The photocatalysis hydrogen production performance map obtaining by above-mentioned detection as shown in Figure 3, as can be seen from Figure 3, the solid-solution type sodium zirconate titanate micro/nanobelt powdery material of this test preparation has good hydrogen production activity, stability and repeatability, by calculating the amounts of hydrogen of the solid-solution type sodium zirconate titanate micro/nanobelt powdery material production hourly of known every this test of 0.1g preparation, is 7～11 μ mol.
Test two: a kind of preparation method of solid-solution type sodium zirconate titanate micro/nanobelt powdery material, specifically completes according to the following steps:
One, sodium hydroxide and deionized water are put into closed reaction vessel, then adding diameter is the titanium zirconium base alloy powder of 5～40 μ m, in temperature, be that 160 ℃, pressure are under 20MPa, to react 12 hours, then naturally cool to room temperature, obtain reaction product mixed system; Two, in the reaction product mixed system of preparing to step 1, add deionized water, the pH value of reaction product mixed system prepared by step 1 is reconciled to neutral, then isolate the throw out of closed reaction container bottom, in temperature, be at 70 ℃, isolated throw out to be dried to constant weight, obtain the titanium zirconium base alloy powder of surface growth solid-solution type titanium sodium zirconate micro-/ nano band; Three, in the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of the preparation in step 2, add deionized water, then under greenhouse, stirring velocity with 120rpm stirs 5min, the suspension liquid evaporate to dryness that separation is obtained, obtains solid-solution type sodium zirconate titanate micro/nanobelt powdery material.
The mass ratio of the sodium hydroxide described in this testing sequence one and deionized water is 0.2:1; The mass ratio of the sodium hydroxide described in this testing sequence one and titanium zirconium base alloy powder is 15:1.
Titanium zirconium base alloy powder described in this testing sequence one is separated, dried titanium zirconium base alloy powder in test one step 3.
The mass ratio of the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of the deionized water adding described in this testing sequence three and the preparation in step 2 is 300:1.
In this testing sequence two, the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of preparation carries out electron-microscope scanning, obtains 3000 times of scanning electronic microscope (SEM) figure, as shown in Figure 4.As can be seen from Figure 4, the thickness of the independent a slice solid-solution type titanium sodium zirconate micro-/ nano band in this testing sequence two on the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of preparation is 5～50nmnm, length is 10～100 μ m, and the diameter of micro-flowers is at 20～100 μ m.
Embodiment two: the difference of present embodiment and embodiment one is: the titanium zirconium base alloy powder described in step 1 is to adopt industrial aerosolization method, prepares with industrial pure material.Other is identical with embodiment one.
Present embodiment adopts industrial aerosolization method and industrial pure material to prepare titanium zirconium base alloy powder to have advantages of pollution-free and with low cost.
Embodiment three: present embodiment and one of embodiment one or two difference are: in the titanium zirconium base alloy powder described in step 1, titanium and zirconium mass ratio are (0.2～30): 1.Other is identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three difference is: the titanium zirconium base alloy powder described in step 1 be titanium zirconium-base amorphous alloy powder, titanium Zirconium-base nano peritectic alloy powder or titanium zirconium-base amorphous/nanometer crystal alloy composite powder.Other is identical with embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four difference is: the mass ratio of the sodium hydroxide described in step 1 and deionized water is (0.1～0.4): 1; The mass ratio of the sodium hydroxide described in step 1 and titanium zirconium base alloy powder is (5～45): 1.Other is identical with embodiment one to four.
Embodiment six: present embodiment with one of embodiment one to five difference is: be that 130 ℃～170 ℃, pressure are to react under 5MPa～35MPa 10～100 hours in temperature in step 1, then naturally cool to room temperature, obtain reaction product mixed system.Other is identical with embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six difference is: be at 60 ℃～80 ℃, isolated throw out to be dried to constant weight in temperature in step 2.Other is identical with embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven difference is: the mass ratio of the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of the deionized water adding described in step 3 and the preparation in step 2 is (50～1000): 1.Other is identical with embodiment one to seven.
Claims (1)
1. the application of a solid-solution type sodium zirconate titanate micro/nanobelt powdery material, it is characterized in that solid-solution type sodium zirconate titanate micro/nanobelt powdery material is for the photocatalyst as hydrogen manufacturing, described solid-solution type sodium zirconate titanate micro/nanobelt powdery material completes according to the following steps: one, sodium hydroxide and deionized water are put into closed reaction vessel, then adding diameter is the titanium zirconium base alloy powder of 70～100 μ m, in temperature, be that 140 ℃, pressure are under 30MPa, to react 24 hours, then naturally cool to room temperature, obtain reaction product mixed system; Two, in the reaction product mixed system of preparing to step 1, add deionized water, the pH value of reaction product mixed system prepared by step 1 is adjusted to neutrality, then isolate the throw out of closed reaction container bottom, in temperature, be at 80 ℃, isolated throw out to be dried to constant weight, obtain the titanium zirconium base alloy powder of surface growth solid-solution type titanium sodium zirconate micro-/ nano band; Three, in the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of the preparation in step 2, add deionized water, then under greenhouse, stirring velocity with 60rpm stirs 15min, the suspension liquid evaporate to dryness that separation is obtained, obtains solid-solution type sodium zirconate titanate micro/nanobelt powdery material; The mass ratio of the sodium hydroxide described in step 1 and deionized water is 0.3:1; The mass ratio of the sodium hydroxide described in step 1 and titanium zirconium base alloy powder is 25:1; Titanium zirconium base alloy powder described in step 1 is to adopt industrial aerosolization method, with industrial pure material, prepares; In titanium zirconium base alloy powder described in step 1, titanium and zirconium mass ratio are 20:1, and titanium zirconium base alloy powder is titanium zirconium-base amorphous alloy powder; The mass ratio of the titanium zirconium base alloy powder of the surface growth solid-solution type titanium sodium zirconate micro-/ nano band of the deionized water adding described in step 3 and the preparation in step 2 is 200:1.
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