CN103990488B - Two-step method prepares Cu 2the method of O/TaON composite photocatalyst material - Google Patents

Two-step method prepares Cu 2the method of O/TaON composite photocatalyst material Download PDF

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CN103990488B
CN103990488B CN201410257837.4A CN201410257837A CN103990488B CN 103990488 B CN103990488 B CN 103990488B CN 201410257837 A CN201410257837 A CN 201410257837A CN 103990488 B CN103990488 B CN 103990488B
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taon
composite photocatalyst
photocatalyst material
solid
powder
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CN103990488A (en
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陈刚
刘悦
周彦松
王力
郝临星
曾炜
黄希
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Harbin Institute of Technology
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Abstract

Two-step method prepares Cu 2the method of O/TaON composite photocatalyst material, the present invention relates to a kind of preparation method of composite photocatalyst material, it in order to the synthesis cycle solving existing composite photocatalyst material long, the problem that decomposition water oxygen performance is low.One, the Ta after grinding 2o 5put into tube furnace high temperature sintering under ammonia atmosphere, preparation TaON solid; Two, grind TaON solid and copper chloride solid, add sodium hydroxide solution in process of lapping, obtain mixed-powder; Three, in mixed-powder, glucose and deionized water is added, heating in water bath for reaction; Four, centrifugal reaction solution, solid product is through the preparation of washing, drying completes composite photocatalyst material.This synthesis technique cycle is short, and the composite photocatalyst powder granule soilless sticking obtained, output are large, show good decomposition water oxygen performance under visible light.

Description

Two-step method prepares Cu 2the method of O/TaON composite photocatalyst material
Technical field
The invention belongs to composite photocatalyst material field in functional material, be specifically related to Cu 2the preparation method of O/TaON composite photo-catalyst.
Background technology
Becoming increasingly conspicuous of aggravation of contradictions between the energy demand increased severely along with limited fossil fuel and the mankind and environmental problem, such that exploitation is clean, new forms of energy are very urgent efficiently.H 2fuel value is high, and odorless is nontoxic, and combustion product is pollution-free, is regenerative resource.H 2directly as the fuel of fuel cell, for electric motor car provides power, can solving current tail gas pollution problem, also Hydrogen Energy can be converted into electric energy, for electrical appliance is powered, is the new forms of energy having bright prospects.And utilizing solar energy photocatalytic hydrogen production by water decomposition, energy density is low, dispersed strong solar energy is converted into Hydrogen Energy, then by H that fuel cell will generate 2and O 2carry out electrochemical reaction, produce electric energy, its product water can be used as again the raw material of solar hydrogen making, and can not produce any pollution to environment, can form eucyclic energy system.Therefore, utilize solar energy photocatalytic hydrogen production by water decomposition to be called as and be referred to as " technology of 21 century dream ", receive extensively deep research.
Through 30 years of researches, up to the present have developed multiple visible light-responded photocatalysis hydrogen production system.Cuprous oxide material have energy gap little, high, nontoxic, inexpensive at visible region absorption coefficient, stablize, be easy to the advantages such as compound and be subject to the extensive attention of scientists.Tantalum base class material is because its ABSORPTION EDGE is large, and steady performance is also the study hotspot of scientist in recent years.
Semiconductors coupling a kind ofly improves separation of charge efficiency, light stable catalyst expand the effective means of visible spectrum responses scope.When different semiconductor close contacts, can be formed " knot ", in the both sides of knot due to its can with etc. the difference of character can form space potential difference.This space potential difference have the separation being beneficial to electron-hole, light-catalysed efficiency can be improved.Researcher finds that copper tantalum base has good stability and optical characteristics, but does not have it for the report of photocatalysis aspect, and the preparation method of existing report also exists complex process, synthesis cycle is long, the problem that cannot synthesize on a large scale.
Summary of the invention
The synthesis cycle that the present invention seeks to solve existing composite photocatalyst material is long, the problem that decomposition water oxygen performance is low, and provides two-step method to prepare Cu 2the method of O/TaON composite photocatalyst material.
Two-step method of the present invention prepares Cu 2the method of O/TaON composite photocatalyst material follows these steps to realize:
One, by Ta 2o 5be placed in mortar to grind, then put into tube furnace high temperature sintering under ammonia atmosphere, obtain TaON solid;
Two, TaON solid step one obtained and copper chloride solid are placed in mortar and grind, and add the sodium hydroxide solution of 1mol/L in process of lapping, and grinding 20 ~ 30min obtains mixed-powder;
Three, the mixed-powder that step 2 obtains is transferred in reaction vessel, adds glucose and deionized water, put into the water-bath magnetic agitation 20 ~ 40min of 80 ~ 100 DEG C after sealed reaction vessel, obtain reactant liquor;
Four, by reactant liquor centrifugal treating, the solid product after centrifugal obtains Cu through washing, drying 2o/TaON composite photocatalyst material.
The present invention adopts two step synthesis composite photocatalyst material Cu 2o/TaON, the synthesis technique cycle is short, and energy consumption is low, can prepare in a large number.The composite photocatalyst powder granule soilless sticking obtained, fillibility is good, output is large, and product purity can reach 100%, simultaneously by Cu that the method prepares 2o/TaON composite photocatalyst material has good visible light-responded, at about 530nm place, there is stronger absorption, this catalyst shows higher decomposition water oxygen performance under visible light simultaneously, and under the illumination of λ >400nm is penetrated, oxygen-producing amount reaches 2mmolh -1g -1, and also significantly do not reduce in the activity of the 12 hours rear catalysts that circulated, show good cycle performance.
Accompanying drawing explanation
Fig. 1 is the Cu that embodiment one obtains 2the XRD collection of illustrative plates of O/TaON composite photocatalyst material, wherein △ represents TaON, ◆ represent Cu 2o, 1-PDF#65-3288,2-Cu 2the XRD collection of illustrative plates of O/TaON composite photocatalyst material, the XRD collection of illustrative plates of 3-TaON, 4-PDF#20-1235;
Fig. 2 is the Cu that embodiment one obtains 2the SEM figure of O/TaON composite photocatalyst material;
Fig. 3 is the Cu that each embodiment obtains 2the UV-vis DRS spectrogram of O/TaON composite photocatalyst material, wherein 1 represents TaON:Cu 2the comparative example of O=1:0,8 represent TaON:Cu 2the comparative example of O=0:1,3 Cu representing embodiment one 2o/TaON composite photocatalyst material, 2 Cu representing embodiment two 2o/TaON composite photocatalyst material, 4 Cu representing embodiment three 2o/TaON composite photocatalyst material, 5 Cu representing embodiment four 2o/TaON composite photocatalyst material, 6 Cu representing embodiment five 2o/TaON composite photocatalyst material, 7 Cu representing embodiment six 2o/TaON composite photocatalyst material;
Fig. 4 is the Cu of different quality ratio 2the cycle performance resolution chart of O/TaON composite photocatalyst material, wherein 1 represents TaON:Cu 2the comparative example of O=1:0,8 represent TaON:Cu 2the comparative example of O=0:1,3 Cu representing embodiment one 2o/TaON composite photocatalyst material, 2 Cu representing embodiment two 2o/TaON composite photocatalyst material, 4 Cu representing embodiment three 2o/TaON composite photocatalyst material, 5 Cu representing embodiment four 2o/TaON composite photocatalyst material, 6 Cu representing embodiment five 2o/TaON composite photocatalyst material, 7 Cu representing embodiment six 2o/TaON composite photocatalyst material.
Detailed description of the invention
Detailed description of the invention one: present embodiment two-step method prepares Cu 2the method two-step method of O/TaON composite photocatalyst material prepares Cu 2o/TaON composite photocatalyst material follows these steps to implement:
One, by Ta 2o 5be placed in mortar to grind, then put into tube furnace high temperature sintering under ammonia atmosphere, obtain TaON solid;
Two, TaON solid step one obtained and copper chloride solid are placed in mortar and grind, and add the sodium hydroxide solution of 1mol/L in process of lapping, and grinding 20 ~ 30min obtains mixed-powder;
Three, the mixed-powder that step 2 obtains is transferred in reaction vessel, adds glucose and deionized water, put into the water-bath magnetic agitation 20 ~ 40min of 80 ~ 100 DEG C after sealed reaction vessel, obtain reactant liquor;
Four, by reactant liquor centrifugal treating, the solid product after centrifugal obtains Cu through washing, drying 2o/TaON composite photocatalyst material.
The raw material adopted in present embodiment is the pure raw material of commercially available analysis.Present embodiment obtains Cu 2in O/TaON composite photocatalyst material, the ratio of each amount of substance is
Detailed description of the invention two: present embodiment and detailed description of the invention one are unlike being sinter 700 ~ 1000min with the high-temperature of 800 ~ 1000 DEG C in step one.Other step and parameter identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment and detailed description of the invention one or two are 1:0.12 unlike the mass ratio of step 2 TaON solid and copper chloride solid.Other step and parameter identical with detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three are unlike Cu in copper chloride 2+with OH in sodium hydroxide solution -and the ratio of amount of substance is between glucose three: n (Cu 2+): n (OH -): n (glucose)=1:2.1 ~ 2.5:1 ~ 1.2.Other step and parameter identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four are first spend deionized water 2 ~ 3 times unlike the washing described in step 4, then use absolute ethanol washing 1 ~ 2 time.Other step and parameter identical with one of detailed description of the invention one to four.
Embodiment one: the present embodiment two-step method prepares Cu 2o/TaON composite photocatalyst material follows these steps to realize:
One, by the Ta of 0.88g 2o 5be placed in mortar and grind 30min, then put into tube furnace under ammonia atmosphere with 900 DEG C of high temperature sintering 900min, obtain TaON solid;
Two, 0.5gTaON solid step one obtained and 0.06g copper chloride solid are placed in mortar and grind, and add the sodium hydroxide solution that 0.9ml concentration is 1mol/L in process of lapping, and grinding 25min obtains mixed-powder;
Three, the mixed-powder that step 2 obtains is transferred in beaker, adds 0.035g glucose and 20ml deionized water, seal beaker mouth with preservative film, then beaker is put into the water-bath magnetic agitation 35min of 90 DEG C, obtain reactant liquor;
Four, by reactant liquor centrifugal treating, the solid product after centrifugal uses absolute ethanol washing 2 times again after deionized water washs 3 times, finally dries up at normal temperatures and obtains Cu 2o/TaON composite photocatalyst material.
The Cu that the present embodiment obtains 2in O/TaON composite photocatalyst material the Cu obtained 2the XRD collection of illustrative plates of O/TaON composite photocatalyst material as shown in Figure 1; SEM figure as shown in Figure 2.This Cu 2o/TaON composite photocatalyst material has good visible light-responded, can find out, at about 530nm, there is stronger absorption from its UV-vis DRS spectrogram, this catalyst shows higher decomposition water oxygen performance under visible light simultaneously, under the illumination of λ >400nm is penetrated, oxygen-producing amount reaches nearly 2mmolh -1g -1.
Embodiment two: the present embodiment two-step method prepares Cu 2the method two-step method of O/TaON composite photocatalyst material prepares Cu 2o/TaON composite photocatalyst material follows these steps to realize:
One, by the Ta of 0.88g 2o 5be placed in mortar and grind 30min, then put into tube furnace under ammonia atmosphere with 900 DEG C of high temperature sintering 900min, obtain TaON solid;
Two, 0.5gTaON solid step one obtained and 0.012g copper chloride solid are placed in mortar and grind, and add the sodium hydroxide solution that 0.18ml concentration is 1mol/L in process of lapping, and grinding 25min obtains mixed-powder;
Three, the mixed-powder that step 2 obtains is transferred in beaker, adds 0.007g glucose and 20ml deionized water, seal beaker mouth with preservative film, then beaker is put into the water-bath magnetic agitation 35min of 90 DEG C, obtain reactant liquor;
Four, by reactant liquor centrifugal treating, the solid product after centrifugal uses absolute ethanol washing 2 times again after deionized water washs 3 times, finally dries up at normal temperatures and obtains Cu 2o/TaON composite photocatalyst material.
The Cu that the present embodiment obtains 2in O/TaON composite photocatalyst material the Cu obtained 2shown in the UV-vis DRS spectrogram 3 of O/TaON composite photocatalyst material, oxygen-producing amount as shown in Figure 4.
Embodiment three: the present embodiment two-step method prepares Cu 2o/TaON composite photocatalyst material follows these steps to realize:
One, by the Ta of 0.88g 2o 5be placed in mortar and grind 30min, then put into tube furnace under ammonia atmosphere with 900 DEG C of high temperature sintering 900min, obtain TaON solid;
Two, 0.5gTaON solid step one obtained and 0.12g copper chloride solid are placed in mortar and grind, and add the sodium hydroxide solution that 1.8ml concentration is 1mol/L in process of lapping, and grinding 25min obtains mixed-powder;
Three, the mixed-powder that step 2 obtains is transferred in beaker, adds 0.07g glucose and 20ml deionized water, seal beaker mouth with preservative film, then beaker is put into the water-bath magnetic agitation 35min of 90 DEG C, obtain reactant liquor;
Four, by reactant liquor centrifugal treating, the solid product after centrifugal uses absolute ethanol washing 2 times again after deionized water washs 3 times, finally dries up at normal temperatures and obtains Cu 2o/TaON composite photocatalyst material.
The Cu that the present embodiment obtains 2in O/TaON composite photocatalyst material the Cu obtained 2shown in the UV-vis DRS spectrogram 3 of O/TaON composite photocatalyst material, oxygen-producing amount as shown in Figure 4.
Embodiment four: the present embodiment two-step method prepares Cu 2o/TaON composite photocatalyst material follows these steps to realize:
One, by the Ta of 0.88g 2o 5be placed in mortar and grind 30min, then put into tube furnace under ammonia atmosphere with 900 DEG C of high temperature sintering 900min, obtain TaON solid;
Two, 0.5gTaON solid step one obtained and 0.24g copper chloride solid are placed in mortar and grind, and add the sodium hydroxide solution that 3.6ml concentration is 1mol/L in process of lapping, and grinding 25min obtains mixed-powder;
Three, the mixed-powder that step 2 obtains is transferred in beaker, adds 0.14g glucose and 20ml deionized water, seal beaker mouth with preservative film, then beaker is put into the water-bath magnetic agitation 35min of 90 DEG C, obtain reactant liquor;
Four, by reactant liquor centrifugal treating, the solid product after centrifugal uses absolute ethanol washing 2 times again after deionized water washs 3 times, finally dries up at normal temperatures and obtains Cu 2o/TaON composite photocatalyst material.
The Cu that the present embodiment obtains 2in O/TaON composite photocatalyst material the Cu obtained 2shown in the UV-vis DRS spectrogram 3 of O/TaON composite photocatalyst material, oxygen-producing amount as shown in Figure 4.
Embodiment five: the present embodiment two-step method prepares Cu 2o/TaON composite photocatalyst material follows these steps to realize:
One, by the Ta of 0.88g 2o 5be placed in mortar and grind 30min, then put into tube furnace under ammonia atmosphere with 900 DEG C of high temperature sintering 900min, obtain TaON solid;
Two, 0.5gTaON solid step one obtained and 1.2g copper chloride solid are placed in mortar and grind, and add the sodium hydroxide solution that 18ml concentration is 1mol/L in process of lapping, and grinding 25min obtains mixed-powder;
Three, the mixed-powder that step 2 obtains is transferred in beaker, adds 0.7g glucose and 20ml deionized water, seal beaker mouth with preservative film, then beaker is put into the water-bath magnetic agitation 35min of 90 DEG C, obtain reactant liquor;
Four, by reactant liquor centrifugal treating, the solid product after centrifugal uses absolute ethanol washing 2 times again after deionized water washs 3 times, finally dries up at normal temperatures and obtains Cu 2o/TaON composite photocatalyst material.
The Cu that the present embodiment obtains 2in O/TaON composite photocatalyst material the Cu obtained 2shown in the UV-vis DRS spectrogram 3 of O/TaON composite photocatalyst material, oxygen-producing amount as shown in Figure 4.
Embodiment six: the present embodiment two-step method prepares Cu 2o/TaON composite photocatalyst material follows these steps to realize:
One, by the Ta of 0.88g 2o 5be placed in mortar and grind 30min, then put into tube furnace under ammonia atmosphere with 900 DEG C of high temperature sintering 900min, obtain TaON solid;
Two, 0.5gTaON solid step one obtained and 2.4g copper chloride solid are placed in mortar and grind, and add the sodium hydroxide solution that 36ml concentration is 1mol/L in process of lapping, and grinding 25min obtains mixed-powder;
Three, the mixed-powder that step 2 obtains is transferred in beaker, adds 1.4g glucose and 20ml deionized water, seal beaker mouth with preservative film, then beaker is put into the water-bath magnetic agitation 35min of 90 DEG C, obtain reactant liquor;
Four, by reactant liquor centrifugal treating, the solid product after centrifugal uses absolute ethanol washing 2 times again after deionized water washs 3 times, finally dries up at normal temperatures and obtains Cu 2o/TaON composite photocatalyst material.
The Cu that the present embodiment obtains 2in O/TaON composite photocatalyst material the Cu obtained 2shown in the UV-vis DRS spectrogram 3 of O/TaON composite photocatalyst material, oxygen-producing amount as shown in Figure 4.
Comparative example: adopt TaON and Cu 2o carries out the test of UV-vis DRS spectrogram and oxygen performance test, and result as shown in Figure 3, Figure 4.

Claims (4)

1. two-step method prepares Cu 2the method of O/TaON composite photocatalyst material, it is characterized in that following these steps to realize:
One, by Ta 2o 5be placed in mortar to grind, then put into tube furnace and sinter 700 ~ 1000min with the high-temperature of 800 ~ 1000 DEG C under ammonia atmosphere, obtain TaON solid;
Two, TaON solid step one obtained and copper chloride solid are placed in mortar and grind, and add the sodium hydroxide solution of 1mol/L in process of lapping, and grinding 20 ~ 30min obtains mixed-powder;
Three, the mixed-powder that step 2 obtains is transferred in reaction vessel, adds glucose and deionized water, put into the water-bath magnetic agitation 20 ~ 40min of 80 ~ 100 DEG C after sealed reaction vessel, obtain reactant liquor;
Four, by reactant liquor centrifugal treating, the solid product after centrifugal obtains Cu through washing, drying 2o/TaON composite photocatalyst material.
2. two-step method according to claim 1 prepares Cu 2the method of O/TaON composite photocatalyst material, is characterized in that the mass ratio of TaON solid and copper chloride solid in step 2 is 1:0.12.
3. two-step method according to claim 1 prepares Cu 2the method of O/TaON composite photocatalyst material, is characterized in that Cu in copper chloride 2+with OH in sodium hydroxide solution -and the ratio of amount of substance is between glucose three: n (Cu 2+): n (OH -): n (glucose)=1:2.1 ~ 2.5:1 ~ 1.2.
4. two-step method according to claim 1 prepares Cu 2the method of O/TaON composite photocatalyst material, is characterized in that the washing described in step 4 first spends deionized water 2 ~ 3 times, then uses absolute ethanol washing 1 ~ 2 time.
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