CN109794274A - A kind of titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material and preparation method - Google Patents
A kind of titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material and preparation method Download PDFInfo
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Abstract
The present invention relates to a kind of titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material and preparation methods, step are as follows: after titanium aluminium carbon and hydrofluoric acid hybrid reaction, obtained sediment A is subjected to hydro-thermal reaction, Thiomolybdate solution is added in the sediment C that hydro-thermal reaction obtains, obtains titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material by photoreduction.Application of the composite material as photochemical catalyst in photochemical catalyzing.Composite material is the efficient photocatalytic water catalyst with the double co-catalysts of non precious metal, significantly improves photocatalysis effect.
Description
Technical field
The invention belongs to catalyst material preparation technical fields, and in particular to and a kind of titanium carbide lamella/molybdenum sulfide nanometer sheet/
Titanium dioxide nanoplate composite material and preparation method.
Background technique
With the worsening of global fossil energy rapidly depleted with environment, environmental-friendly, low in cost, resource is developed
Renewable energy abundant has become the urgent problem to be solved of facing mankind.As a kind of environmentally friendly energy, hydrogen
Calorific value it is high, be readily transported, be renewable, thus convert solar energy into Hydrogen Energy be the optimal method to tap a new source of energy it
One.Photolysis water hydrogen can directly utilize decomposing water with solar energy hydrogen making, not consume other energy, and to environment without dirt
Dye, by the extensive concern of researcher, becomes optimal hydrogen manufacturing approach.TiO2Because have stable photoelectrochemical behaviour,
The excellent properties such as low in cost, corrosion-resistant, redox ability is strong, become one of most promising photochemical catalyst.
In photochemical catalyzing, co-catalyst is essential auxiliary substances in photocatalytic water, it can promote light
The transmission of raw electronics and the separation of electron hole pair, it is effective to improve photocatalytic water efficiency.But co-catalysis commonly used at present
Agent is noble metal platinum, gold etc., and since it is expensive, yield is few etc., factors, the new co-catalyst of development utilization very must
It wants.
Summary of the invention
For above-mentioned problems of the prior art, it is an object of the present invention to provide a kind of titanium carbide lamella/sulphur
Change molybdenum nanometer sheet/titanium dioxide nanoplate composite material and preparation method.
In order to solve the above technical problems, the technical solution of the present invention is as follows:
A kind of titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material preparation method, step are as follows:
After titanium aluminium carbon and hydrofluoric acid hybrid reaction, by obtained sediment A progress hydro-thermal reaction, in the sediment C that hydro-thermal reaction obtains
Thiomolybdate is added, obtains titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite wood by photoreduction
Material.
Above-mentioned titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material preparation method, specific steps
Are as follows:
1) sediment A is obtained by filtration after reacting at room temperature in hydrofluoric acid solution and titanium aluminium carbon；
2) sodium fluoborate, hydrochloric acid solution, deionized water are added in sediment A, precipitating is obtained by filtration after carrying out hydro-thermal reaction
Object C；
3) mixed liquor after mixing sediment C and Thiomolybdate solution after photoreduction is by filtering, washing
It washs, vacuum heat-preserving obtains titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material.
Preferably, the mass fraction of hydrofluoric acid solution is 35-45% in step 1)；Preferably, the powder particle of titanium aluminium carbon
Degree is 100-400 mesh, preferably 200-300 mesh；Preferably, the time of hydrofluoric acid and the reaction of titanium aluminium carbon is 65-78 hours；It is preferred that
, the volume of 1 gram of the corresponding hydrofluoric acid solution of titanium aluminium carbon is 90-110 milliliters.
Preferably, magnetic agitation is carried out after sediment A and sodium fluoborate, hydrochloric acid solution, deionized water mixing in step 2),
The time of stirring is 6-20min；Preferably, the concentration of hydrochloric acid solution is 0.05-0.15M, preferably 0.08M- in step 2)
0.1M；Preferably, the temperature of hydro-thermal reaction is 100-200 DEG C, is chosen as 120 DEG C, 140 DEG C, 160 DEG C；Preferably, hydro-thermal reaction
Time be 5-20 hours, preferably 12-14 hours；Preferably, the ratio of the quality, the quality of sodium fluoborate of sediment A is 8-
12:1；Preferably, the volume of 1 gram of the corresponding hydrochloric acid solution of sediment A is 80-120 milliliters.
Preferably, the mass ratio of sediment C and the molybdenum element in Thiomolybdate solution is 0.1-0.3 in step 3)；It is excellent
Choosing, it is stirred after sediment C and the mixing of Thiomolybdate solution, the time of stirring is 6-20 minutes；Preferably, molybdenum dithiophosphate
Hydrochlorate is ammonium thiomolybdate；Preferably, the light source of photo catalytic reduction is xenon lamp；It is further preferred that the power of xenon lamp is 280-
320 watts；It is further preferred that the time of xenon lamp irradiation is 1-5 hours, it is chosen as 2-3 hours.
Preferably, the temperature of vacuum heat-preserving is 50-70 DEG C in step 3)；Preferably, the time of vacuum heat-preserving is that 10-15 is small
When.
Titanium carbide lamella obtained by the above method/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material.
Hydrofluoric acid and titanium aluminium carbon react to obtain two-dimentional transition metal carbide, and two-dimentional transition metal carbide is anti-by hydro-thermal
It answers, two-dimentional transition metal carbide growth obtains the structure of titanium carbide lamella and titanium dioxide nanoplate, sulphur on area load
Molybdenum sulfide is obtained to obtain titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate by photo-reduction for after molybdate
Meet material.
Above-mentioned titanium carbide lamella/molybdenum sulfide nanometer sheet/application of the titanium dioxide nanoplate composite material as photochemical catalyst.
Application of the above-mentioned photochemical catalyst in photochemical catalyzing.
Beneficial effects of the present invention:
The application is reacted to obtain two-dimentional transition metal carbide using hydrofluoric acid and titanium aluminium carbon, then passes through hydro-thermal again
Method makes two-dimensional structure be grown to three-dimensional structure, and three-dimensional structure is added in ammonium thiomolybdate solution, is vulcanized by photo-reduction
Molybdenum, titanium carbide is due to its good electric conductivity, and possesses the unique lamellar structure of large specific surface area.Therefore its have at
For the potentiality of good co-catalyst.Molybdenum sulfide urges the light such as the two and titanium dioxide as known effective co-catalyst again
Agent is effectively combined, its electric conductivity is made full use of, and the application in terms of co-catalyst may be implemented.Obtaining has efficient photodissociation
The ideal photochemical catalyst of water effect；
The present invention provides a kind of titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material, the carbonization
Titanium sheet layer/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material is produced by above-mentioned preparation method, the titanium carbide
Lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material is the efficient photocatalytic water with the double co-catalysts of non precious metal
Catalyst；
A kind of titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material, passes through the thio molybdic acid of photo-reduction
Ammonium is molybdenum sulfide nanometer sheet and is selectively deposited on (101) crystal face of titanium dioxide that (101) crystal face of titanium dioxide is enriched with electricity
Son, electronics has reproducibility to which ammonium thiomolybdate is reduced to molybdenum sulfide under the action of illumination, to keep titanium dioxide sudden and violent
Reveal (001) crystal face of more high activities, TiO2The upper and lower surface of nanometer sheet is (001) crystal face of the hole-rich of high activity,
Surrounding is (101) crystal face of the electron rich of low activity.Operating process is simple, and production cost is low.Titanium carbide lamella/sulphur obtained
Change molybdenum nanometer sheet/exposure (001) crystal face titanium dioxide nanoplate composite material, realizes that double co-catalysts with non precious metal are deposited
High efficiency photocatalyst, and effectively facilitate the transmission of light induced electron and the separation of photo-generate electron-hole pairs, significantly improve
Photocatalysis effect.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 is titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material X obtained in embodiment 2
X-ray photoelectron spectroscopy X；
Fig. 2 is titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material obtained in embodiment 2
Scanning electron microscope (SEM) photograph；
Fig. 3 is titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material, carbon obtained in embodiment 2
Change titanium sheet layer/titanium dioxide nanoplate composite material and titanium dioxide nanoplate the photodissociation aquatic products hydrogen speed under simulated solar irradiation irradiation
Rate figure
Fig. 4 is titanium carbide lamella/molybdenum sulfide nanometer sheet/exposure (001) crystal face nano titania obtained in embodiment 2
Piece composite material, titanium carbide lamella/titanium dioxide nanoplate composite material and titanium dioxide nanoplate are irradiated in simulated solar irradiation
Lower photocatalytic water hydrogen output figure.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
The raw material used in following embodiment 1 to embodiment 4 is hydrofluoric acid solution, titanium aluminium carbon dust, hydrochloric acid solution, fluorine boron
Sour sodium, ammonium thiomolybdate, thiocarbamide and deionized water, used equipment have anti-for mixed beaker, magnetic stirring apparatus, hydro-thermal
Answer kettle, xenon lamp, scanning electron microscope, transmission electron microscope and gas-chromatography photocatalytic activity evaluation system.Produce titanium carbide lamella/
When molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material, hydrofluoric acid solution and titanium aluminium carbon dust are mixed with first
One mixed liquor；Then filter that the first mixed liquor will obtain sediment one and hydrochloric acid (sodium fluoborate) solution is added in deionized water
Prepare the second mixed liquor；The second mixed liquor is subsequently placed in hydro-thermal reaction in hydrothermal reaction kettle and prepares third mixed liquor；Then
Filtering third mixed liquor will obtain sediment two and ammonium thiomolybdate solution is added to deionized water and prepares the 4th mixed liquor；It connects again
The 4th mixed liquor be placed in beaker photoreduction prepare the 5th mixed liquor；Finally the 5th mixed liquor of filtering will be precipitated
The dry obtained titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst of the washing of object three.Made from taking-up
After titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst, also need through scanning electron microscope, transmission electricity
Mirror and gas-chromatography photocatalytic activity evaluation system carry out observation analysis.
Embodiment 1
The hydrofluoric acid solution for measuring 100 milliliters of mass ratioes 40% first, weighs 1 gram of titanium aluminium carbon dust, the powder of titanium aluminium carbon
Last granularity is 200 mesh, and hydrofluoric acid solution and titanium aluminium carbon dust are sufficiently mixed and preparation in 72 hours is stirred at room temperature first mixes
Close liquid.Then filter that the first mixed liquor will obtain 100 milligrams of titanium carbides of sediment and 10 milligrams of sodium fluoborates are added to 10 milliliters
0.1 mole of every liter of hydrochloric acid solution magnetic agitation, 30 minutes the second mixed liquors of preparation.It is anti-that the second mixed liquor is subsequently placed in hydro-thermal
It answers in kettle, hydro-thermal reaction 12 hours at 160 DEG C, prepares third mixed liquor.Then filtering third mixed liquor will obtain sediment carbon
Change titanium/titanium dioxide nanoplate composite material, by 60 milligrams of sediment titanium carbide/titanium dioxide nanoplate composite materials and 7.5
Milligram ammonium thiomolybdate solution is added to magnetic agitation 10 minutes in deionized water, prepares the 4th mixed liquor.Followed by by the 4th
Mixed liquor is placed in a beaker, and is irradiated 2 hours in 300 watts of xenon lamps, is prepared the 5th mixed liquor.Finally the 5th mixed liquor of filtering will obtain
Obtained final sediment is washed with deionized sediment, and 50 DEG C are dried in vacuo 10 hours, takes out the manufactured titanium sheet that is carbonized
Layer/molybdenum sulfide nanometer sheet titanium dioxide nanoplate ternary photochemical catalyst.
The lamella of titanium carbide made from above-described embodiment 1/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst,
The granularity of the titanium carbide layer chip architecture is 200 mesh, the titanium carbide/titanium dioxide nanoplate obtained by first time hydro-thermal reaction
In composite material, titanium dioxide nanoplate is interspersed to be grown in lamellar titanium carbide structure, is obtained finally by photoreduction
Titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst, wherein molybdenum sulfide nanometer sheet is selectivity point
Cloth titanium dioxide nanoplate (101) crystal face, and exposure high activity (001) crystal face.The presence of this double co-catalysts, with
And the exposure of high activity surface, so that titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst has
Higher photocatalytic water hydrogen-producing speed.
Embodiment 2
The hydrofluoric acid solution for measuring 100 milliliters of mass ratioes 40% first, weighs 1 gram of titanium aluminium carbon dust, the powder of titanium aluminium carbon
Last granularity is 200 mesh, and hydrofluoric acid solution and titanium aluminium carbon dust are sufficiently mixed and preparation in 72 hours is stirred at room temperature first mixes
Close liquid.Then filter that the first mixed liquor will obtain 100 milligrams of titanium carbides of sediment and 10 milligrams of sodium fluoborates are added to 10 milliliters
0.1 mole of every liter of hydrochloric acid solution magnetic agitation, 30 minutes the second mixed liquors of preparation.It is anti-that the second mixed liquor is subsequently placed in hydro-thermal
It answers in kettle, hydro-thermal reaction 12 hours at 160 DEG C, prepares third mixed liquor.Then filtering third mixed liquor will obtain sediment carbon
Change titanium/titanium dioxide nanoplate composite material, by 60 milligrams of sediment titanium carbide/titanium dioxide nanoplate composite materials and 15 millis
Gram ammonium thiomolybdate solution is added to magnetic agitation 10 minutes in deionized water, prepares the 4th mixed liquor.It is mixed followed by by the 4th
It closes liquid to be placed in a beaker, is irradiated 2 hours in 300 watts of xenon lamps, prepare the 5th mixed liquor.Finally the 5th mixed liquor of filtering will be sunk
Obtained final sediment is washed with deionized starch, and 50 DEG C are dried in vacuo 10 hours, takes out the manufactured titanium sheet that is carbonized
Layer/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst.
The lamella of titanium carbide made from above-described embodiment 2/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst,
The granularity of the titanium carbide layer chip architecture is 200 mesh, the titanium carbide/titanium dioxide nanoplate obtained by first time hydro-thermal reaction
In composite material, titanium dioxide nanoplate is interspersed to be grown in lamellar titanium carbide structure, is obtained finally by photoreduction
Titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst, wherein molybdenum sulfide nanometer sheet is selectivity point
Cloth titanium dioxide nanoplate (101) crystal face, and exposure high activity (001) crystal face.The presence of this double co-catalysts, with
And the exposure of high activity surface, so that titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst has
Higher photocatalytic water hydrogen-producing speed.
It is illustrated in figure 2 titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst scanning electricity
Mirror picture, its available structure are three-dimensional lamellar structure.Titanium dioxide nanoplate is plugged in titanium carbide lamella, and molybdenum sulfide is received
Rice piece is selectively supported on (101) face of titanium dioxide nanoplate, thus make more (001) active faces of titanium dioxide exposure,
Titanium carbide lamella has superior electrical conductivity, is conducive to the transmission of electronics, and molybdenum sulfide can also construct heterojunction structure with titanium dioxide
The molecule for promoting photo-generate electron-hole, to enhance the photocatalysis effect of titanium dioxide nanoplate.
Embodiment 3
The hydrofluoric acid solution for measuring 100 milliliters of mass ratioes 40% first, weighs 1 gram of titanium aluminium carbon dust, the powder of titanium aluminium carbon
Last granularity is 200 mesh, and hydrofluoric acid solution and titanium aluminium carbon dust are sufficiently mixed and preparation in 72 hours is stirred at room temperature first mixes
Close liquid.Then filter that the first mixed liquor will obtain 100 milligrams of titanium carbides of sediment and 10 milligrams of sodium fluoborates are added to 10 milliliters
0.1 mole of every liter of hydrochloric acid solution magnetic agitation, 30 minutes the second mixed liquors of preparation.It is anti-that the second mixed liquor is subsequently placed in hydro-thermal
It answers in kettle, hydro-thermal reaction 12 hours at 160 DEG C, prepares third mixed liquor.Then filtering third mixed liquor will obtain sediment carbon
Change titanium/titanium dioxide nanoplate composite material, by 60 milligrams of sediment titanium carbide/titanium dioxide nanoplate composite materials and 23 millis
Gram ammonium thiomolybdate solution is added to magnetic agitation 10 minutes in deionized water, prepares the 4th mixed liquor.It is mixed followed by by the 4th
It closes liquid to be placed in a beaker, is irradiated 2 hours in 300 watts of xenon lamps, prepare the 5th mixed liquor.Finally the 5th mixed liquor of filtering will be sunk
Obtained final sediment is washed with deionized starch, and 50 DEG C are dried in vacuo 10 hours, takes out the manufactured titanium sheet that is carbonized
Layer/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst.
The lamella of titanium carbide made from above-described embodiment 3/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst,
The granularity of the titanium carbide layer chip architecture is 200 mesh, the titanium carbide/titanium dioxide nanoplate obtained by first time hydro-thermal reaction
In composite material, titanium dioxide nanoplate is interspersed to be grown in lamellar titanium carbide structure, is obtained finally by photoreduction
Titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst, wherein molybdenum sulfide nanometer sheet is selectivity point
Cloth titanium dioxide nanoplate (101) crystal face, and exposure high activity (001) crystal face.The presence of this double co-catalysts, with
And the exposure of high activity surface, so that titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst has
Higher photocatalytic water hydrogen-producing speed.
Embodiment 4
The hydrofluoric acid solution for measuring 100 milliliters of mass ratioes 40% first, weighs 1 gram of titanium aluminium carbon dust, the powder of titanium aluminium carbon
Last granularity is 200 mesh, and hydrofluoric acid solution and titanium aluminium carbon dust are sufficiently mixed and preparation in 72 hours is stirred at room temperature first mixes
Close liquid.Then filter that the first mixed liquor will obtain 100 milligrams of titanium carbides of sediment and 10 milligrams of sodium fluoborates are added to 10 milliliters
0.1 mole of every liter of hydrochloric acid solution magnetic agitation, 30 minutes the second mixed liquors of preparation.It is anti-that the second mixed liquor is subsequently placed in hydro-thermal
It answers in kettle, hydro-thermal reaction 12 hours at 160 DEG C, prepares third mixed liquor.Then filtering third mixed liquor will obtain sediment carbon
Change titanium/titanium dioxide nanoplate composite material, by 60 milligrams of sediment titanium carbide/titanium dioxide nanoplate composite materials and 30 millis
Gram ammonium thiomolybdate solution is added to magnetic agitation 10 minutes in deionized water, prepares the 4th mixed liquor.It is mixed followed by by the 4th
It closes liquid to be placed in a beaker, is irradiated 2 hours in 300 watts of xenon lamps, prepare the 5th mixed liquor.Finally the 5th mixed liquor of filtering will be sunk
Obtained final sediment is washed with deionized starch, and 50 DEG C are dried in vacuo 10 hours, takes out the manufactured titanium sheet that is carbonized
Layer/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst.
The lamella of titanium carbide made from above-described embodiment 4/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst,
The granularity of the titanium carbide layer chip architecture is 200 mesh, the titanium carbide/titanium dioxide nanoplate obtained by first time hydro-thermal reaction
In composite material, titanium dioxide nanoplate is interspersed to be grown in lamellar titanium carbide structure, is obtained finally by photoreduction
Titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst, wherein molybdenum sulfide nanometer sheet is selectivity point
Cloth titanium dioxide nanoplate (101) crystal face, and exposure high activity (001) crystal face.The presence of this double co-catalysts, with
And the exposure of high activity surface, so that titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst has
Higher photocatalytic water hydrogen-producing speed.
Embodiment 5
The hydrofluoric acid solution for measuring 90 milliliters of mass ratioes 40% first, weighs 1 gram of titanium aluminium carbon dust, the powder of titanium aluminium carbon
Granularity is 300 mesh, hydrofluoric acid solution and titanium aluminium carbon dust is sufficiently mixed, the first mixing of preparation in 72 hours is stirred at room temperature
Liquid.Then filter that the first mixed liquor will obtain 100 milligrams of titanium carbides of sediment and 10 milligrams of sodium fluoborates are added to 10 milliliters
0.08 mole of every liter of hydrochloric acid solution magnetic agitation, 30 minutes the second mixed liquors of preparation.It is anti-that the second mixed liquor is subsequently placed in hydro-thermal
It answers in kettle, hydro-thermal reaction 14 hours at 160 DEG C, prepares third mixed liquor.Then filtering third mixed liquor will obtain sediment carbon
Change titanium/titanium dioxide nanoplate composite material, by 60 milligrams of sediment titanium carbide/titanium dioxide nanoplate composite materials and 15 millis
Gram ammonium thiomolybdate solution is added to magnetic agitation 10 minutes in deionized water, prepares the 4th mixed liquor.It is mixed followed by by the 4th
It closes liquid to be placed in a beaker, is irradiated 3 hours in 280 watts of xenon lamps, prepare the 5th mixed liquor.Finally the 5th mixed liquor of filtering will be sunk
Obtained final sediment is washed with deionized starch, and 50 DEG C are dried in vacuo 10 hours, takes out the manufactured titanium sheet that is carbonized
Layer/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst.
The lamella of titanium carbide made from above-described embodiment 5/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst,
The granularity of the titanium carbide layer chip architecture is 200 mesh, the titanium carbide/titanium dioxide nanoplate obtained by first time hydro-thermal reaction
In composite material, titanium dioxide nanoplate is interspersed to be grown in lamellar titanium carbide structure, is obtained finally by photoreduction
Titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst, wherein molybdenum sulfide nanometer sheet is selectivity point
Cloth titanium dioxide nanoplate (101) crystal face, and exposure high activity (001) crystal face.The presence of this double co-catalysts, with
And the exposure of high activity surface, so that titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst has
Higher photocatalytic water hydrogen-producing speed.
Photodissociation water test
Embodiment 1- embodiment 5, titanium carbide/titanium dioxide this six kinds of substances are respectively put into identical water, using too
Sunlight carries out illumination, photocatalytic water hydrogen-producing speed figure as shown in figure 3, photocatalytic water hydrogen output figure as shown in figure 4, can be with by Fig. 3 and Fig. 4
Obtain titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst hydrogen-producing speed and the production of embodiment 2
Hydrogen amount is maximum.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for the skill of this field
For art personnel, various changes and changes are possible in this application.Within the spirit and principles of this application, made any to repair
Change, equivalent replacement, improvement etc., should be included within the scope of protection of this application.
Claims (10)
1. a kind of titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material preparation method, feature exist
In: step are as follows: after titanium aluminium carbon and hydrofluoric acid hybrid reaction, obtained sediment A is subjected to hydro-thermal reaction, what hydro-thermal reaction obtained
Thiomolybdate is added in sediment C, obtains titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide by photoreduction and receives
Rice piece ternary photochemical catalyst.
2. a kind of titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate composite material preparation method, feature exist
In: specific steps are as follows:
1) hydrofluoric acid solution and titanium aluminium carbon obtain sediment A after reacting at room temperature；
2) sodium fluoborate, hydrochloric acid solution, deionized water progress hydro-thermal reaction are added in sediment A and obtains sediment C；
3) mixed liquor after mixing sediment C and Thiomolybdate solution, deionized water after photoreduction passed through
Filter, washing, vacuum heat-preserving obtain titanium carbide lamella/molybdenum sulfide nanometer sheet/titanium dioxide nanoplate ternary photochemical catalyst；
Preferably, the mass fraction of hydrofluoric acid solution is 35-45% in step 1)；Preferably, the powder particle size of titanium aluminium carbon is
100-400 mesh, preferably 200-300 mesh；Preferably, the time of hydrofluoric acid and the reaction of titanium aluminium carbon is 65-78 hours；Preferably, 1
Gram the corresponding hydrofluoric acid solution of titanium aluminium carbon volume be 90-110 milliliters；
Preferably, magnetic agitation is carried out after sediment A and sodium fluoborate, hydrochloric acid solution, deionized water mixing in step 2), stirred
Time be 6-20min；Preferably, the concentration of hydrochloric acid solution is 0.05-0.15M, preferably 0.08M-0.1M in step 2)；It is excellent
Choosing, the temperature of hydro-thermal reaction is 100-200 DEG C, is chosen as 120 DEG C, 140 DEG C, 160 DEG C；Preferably, the time of hydro-thermal reaction
It is 5-20 hours, preferably 12-14 hours；Preferably, the ratio of the quality, the quality of sodium fluoborate of sediment A is 8-12:1；It is excellent
Choosing, the volume of 1 gram of the corresponding hydrochloric acid solution of sediment A is 80-120 milliliters.
3. preparation method according to claim 2, it is characterised in that: sediment C and Thiomolybdate solution in step 3)
In molybdenum element mass ratio be 0.1-0.3.
4. preparation method according to claim 2, it is characterised in that: sediment C and Thiomolybdate solution in step 3)
It is stirred after mixing, the time of stirring is 6-20 minutes.
5. preparation method according to claim 2, it is characterised in that: the light source of photo catalytic reduction is xenon lamp in step 3),
The power of xenon lamp is 280-320 watts；The time of xenon lamp irradiation is 1-5 hours.
6. preparation method according to claim 5, it is characterised in that: Thiomolybdate is ammonium thiomolybdate.
7. preparation method according to claim 5, it is characterised in that: the temperature of vacuum heat-preserving is 50-70 DEG C in step 3)；
The time of vacuum heat-preserving is 10-15 hours.
8. titanium carbide lamella/molybdenum sulfide nanometer sheet/bis- that the described in any item preparation methods of claim 1- claim 7 obtain
TiOx nano piece composite material.
9. application of the composite material according to any one of claims 8 as photochemical catalyst.
10. application of the composite material according to any one of claims 8 as photochemical catalyst in photochemical catalyzing.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112121855A (en) * | 2020-10-10 | 2020-12-25 | 何刚刚 | Preparation method of photocatalytic thiourea modified two-dimensional MXene material |
| CN113578297A (en) * | 2021-08-27 | 2021-11-02 | 陕西科技大学 | Oxygen-terminated monolayer titanium carbide composite titanium dioxide photocatalyst and preparation method thereof |
| CN114512653A (en) * | 2022-02-22 | 2022-05-17 | 广东工业大学 | Preparation method of nitrogen-doped MXene-loaded molybdenum disulfide composite material, product and application of product |
| CN115624983A (en) * | 2022-10-17 | 2023-01-20 | 中山大学·深圳 | Two-dimensional Ti 3 C 2 -MoS 2 Preparation method of nano heterojunction |
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2019
- 2019-01-24 CN CN201910069875.XA patent/CN109794274A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112121855A (en) * | 2020-10-10 | 2020-12-25 | 何刚刚 | Preparation method of photocatalytic thiourea modified two-dimensional MXene material |
| CN113578297A (en) * | 2021-08-27 | 2021-11-02 | 陕西科技大学 | Oxygen-terminated monolayer titanium carbide composite titanium dioxide photocatalyst and preparation method thereof |
| CN113578297B (en) * | 2021-08-27 | 2024-02-27 | 陕西科技大学 | Oxygen-terminated monolayer titanium carbide composite titanium dioxide photocatalyst and preparation method thereof |
| CN114512653A (en) * | 2022-02-22 | 2022-05-17 | 广东工业大学 | Preparation method of nitrogen-doped MXene-loaded molybdenum disulfide composite material, product and application of product |
| CN115624983A (en) * | 2022-10-17 | 2023-01-20 | 中山大学·深圳 | Two-dimensional Ti 3 C 2 -MoS 2 Preparation method of nano heterojunction |
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