CN104588040A - Photocatalyst and preparation method thereof - Google Patents
Photocatalyst and preparation method thereof Download PDFInfo
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- CN104588040A CN104588040A CN201310529447.3A CN201310529447A CN104588040A CN 104588040 A CN104588040 A CN 104588040A CN 201310529447 A CN201310529447 A CN 201310529447A CN 104588040 A CN104588040 A CN 104588040A
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Abstract
The invention discloses a photocatalyst. The photocatalyst is composed of RuO2 and Mn1-xCdxS composite metal sulfide according to a mass ratio of 0.01-8:100 and preferably 0.02-4:100, and x in the Mn1-xCdxS composite metal sulfide is 0-1 and preferably 0.5-0.9. A preparation method of the photocatalyst comprises a preparation process of the composite metal sulfide and a RuO2 loading process. The photocatalyst has high active stability, and solves the problem of low stability of CdS photocatalysts.
Description
Technical field
The present invention relates to a kind of photochemical catalyst and preparation method thereof, relate in particular to a kind of visible light catalyst and preparation method thereof.
Background technology
Hydrogen Energy is a kind of desirable green energy resource, solar energy and water is converted into the Hydrogen Energy of high-efficiency cleaning, is to solve one of future source of energy and the most promising method of environmental problem.Within 1972, Japanese scholars Fujishima and Honda has found at TiO
2the phenomenon of photochemical catalyzing on electrode, for photocatalytic hydrogen production by water decomposition provides foundation, also accelerate light energy conversion is the research steps of chemical energy simultaneously.Conductor photocatalysis hydrogen production by water decomposition swims in water by semiconductive particles, splits water into hydrogen and oxygen under illumination condition.Whole process converts solar energy into chemical energy, has environmental protection, economic dispatch advantage, receives increasing concern, and preparing highly active photochemical catalyst is the key improving photocatalysis hydrogen production efficiency.
Sulfide and oxymtride material have excellent visible light-responded performance, are the catalysis materials most with application prospect.CdS intrinsic material is
ntype direct band-gap semicondictor material, pay close attention to widely because its superior optical property causes in recent years, CdS itself is as body phase material, band gap is 2.42 eV, have wider visible light-responded interval and suitable oxidation-reduction potential, it has good assimilation effect to the visible ray being positioned at 400-550 nm scope.
(the functional material such as Du Juan, 2005,10,1603) hydro-thermal and solvent-thermal method is used to prepare the Nano cadmium sulphide semiconductor light-catalyst of different-grain diameter, inquired into reactant, solvent and temperature etc. and can affect cadmium sulfide crystal formation and degree of crystallinity, thus caused the factor that its photocatalytic activity changes, result shows, CdS photoetch is relevant with its crystal formation, and significantly reduces with the raising of degree of crystallinity.Multicomponent catalyst became a new direction in solar hydrogen making catalysis material in recent years, can regulate the band structure of catalyst by forming solid solution between broad-band gap and narrow gap semiconductor.Coating precious metals pt on CdS surface, when there being sacrifice reagent, there is very high hydrogen production efficiency.Domen research group of Japan prepares porous nanometer structure CdS(Chem. Mater.2008,20,110), its supporting Pt hydrogen production rate is up to 16mmol/hg, and the sub-efficiency of hydrogen output reaches 60%.Li Can academician's project team system is standby Pt-PdS/CdS ternary photochemical catalyst (Journal of Catalysis, 2009,266,165), and its photocatalytic water hydrogen generation efficiency, up to 93%, close to photosynthesis, is the photochemical catalyst that quantum efficiency is the highest up to now.But both there is the problem of photochemical catalyst instability, the catalyst of Domen research group is after use 12h, and photocatalysis efficiency reduces by 20%; Pt-PdS/CdS ternary photochemical catalyst is after use 25h, and photochemical catalyst also starts to decompose gradually.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of photochemical catalyst and preparation method thereof.This photochemical catalyst has high-activity stable, solves a difficult problem for CdS class photochemical catalyst poor stability.
A kind of photochemical catalyst, by RuO
2and Mn
1-xcd
xs composition metal sulfide forms, RuO in catalyst
2quality be Mn
1-xcd
xthe 0.01-8% of S composition metal sulfide quality, preferred 0.02-4%, described Mn
1-xcd
x0 <x< 1 in S composition metal sulfide, preferably 0.5 <x< 0.9.
In catalyst of the present invention, can also containing appropriate silver in described composition metal sulfide, composition metal sulfide consist of Ag
ymn
1-x-y/2cd
xs, wherein 0<x<1,0<y<1, preferred x=0.2 ~ 0.8, y=0.001 ~ 0.02.
A preparation method for photochemical catalyst, comprises preparation process and the RuO of composition metal sulfide
2loading process.
In the inventive method, described composition metal sulfide adopts hydrothermal synthesis method preparation, and step is as follows:
(1) preparation is containing the mixed liquor of cadmium salt, manganese salt and thioacetamide;
(2) mixed liquor of step (1) is placed in hydrothermal synthesis reaction still, 130-250 DEG C of reaction 10-30h;
(3) centrifugal treating is carried out to the sediment of step (2) hydrothermal synthesis reaction, get the single-phase obtained composition metal sulfide of yellow green.
In mixed liquor described in said method step (1), the molar concentration of cadmium is 0.3-0.5mol/L, and the molar concentration of manganese is 0.2-0.4 mol/L, and the molar concentration of thioacetamide is 0.1-0.2 mol/L.Can also be the silver of 0.001-0.1 mol/L containing molar concentration in mixed liquor.Described salt comprises the various soluble-salts such as nitrate, sulfate or acetate, preferred acetate.
In said method step (2), hydrothermal reaction condition is preferably at 150-210 DEG C of reaction 16-24h.
Carry out centrifugal treating after preferably adopting distilled water and ethanol repeatedly to rinse sediment in said method step (3), wash number is 3-5 time repeatedly.
RuO described in the inventive method
2loading process is as follows: adopt the tetrahydrofuran solution dipping Ag containing ruthenium
ymn
1-x-y/2cd
xs composition metal sulfide, obtains RuO through dry, roasting after dipping
2ag
ymn
1-x-y/2cd
xs photochemical catalyst.
In above-mentioned loading process, ruthenium comprises Ru
3(CO)
12, Ru(CO)
3cl
2or Ru (C
5h
7o
2)
3, preferred Ru
3(CO)
12.The preferred vacuum drying of described drying, described roasting is roasting 12-24h under 180-220 DEG C of condition.
Compared with prior art, the RuO for preparing of the present invention
2ag
ymn
1-x-y/2cd
xthe variant component interaction of S photochemical catalyst significantly enhances the stability of catalyst while improving visible ray producing hydrogen, catalyzing activity.
Detailed description of the invention
Further illustrate preparation process and the effect of catalyst of the present invention below in conjunction with embodiment and comparative example, but following examples do not form the restriction to technical solution of the present invention.
Embodiment 1
Take 4.3g Cd (CH
3cOO)
22H
2o, 3.94g Mn (CH
3cOO)
24H
2o is dissolved in 30ml water, adds 2.42g thioacetamide; Add in stainless steel water thermal synthesis reactor and heat 18h under 160 DEG C of conditions; Taking-up precipitation distilled water and ethanol rinse for several times repeatedly, and be divided into two-layer after sample is centrifugal, upper strata is the single-phase Mn of yellow green
0.46cd
0.54s composition metal sulfide, lower floor is bottle-green α-MnS; Separation obtains yellow green Mn
0.46cd
0.54s sample, by Mn
0.46cd
0.54s sample joins the Ru of oxolane
3(CO)
12dipping 5h in solution (0.2mol/L), filter, then vacuum drying, reacts sample to 12h, makes Ru under 220 DEG C of conditions
3(CO)
12transform into RuO
2, final products are RuO
2mn
0.46cd
0.54s, wherein, RuO
2quality be Mn
0.46cd
0.540.5% of S composition metal sulfide quality.This catalyst 0.2g is joined the Na of 200ml 0.5mol/L
2the Na of S and 0.5mol/L
2sO
3in mixed solution, slowly stir, use the xenon lamp of 500W to irradiate this sample, its hydrogen-producing speed is 2835 μm of olh
-1g
-1, use continuously after 1d, the catalytic activity of this catalyst starts to decline.
Embodiment 2
5mg Ag (CH is added in the material of Hydrothermal Synthesis
3cOO), all the other conditions are with embodiment 1, and obtaining final products is RuO
2ag
0.001mn
0.4598cd
0.5397s, RuO
2quality be Ag
0.001mn
0.4598cd
0.53970.5% of S composition metal sulfide quality.Catalyst hydrogen production reaction condition is identical with embodiment 1, and the hydrogen-producing speed of this catalyst hydrogen production by water decomposition is under visible light 3324 μm of olh
-1g
-1, use after 2d continuously, the catalytic activity of this catalyst does not change.
Embodiment 3
By Cd (CH
3cOO)
22H
2the quality of O becomes 5g, Mn (CH
3cOO)
24H
2the quality of O becomes 3.28g, Ag (CH
3cOO) quality becomes 5mg, and all the other conditions are with embodiment 2, and obtaining final products is RuO
2ag
0.001mn
0.3698cd
0.6297s, wherein, RuO
2quality be Ag
0.001mn
0.3698cd
0.62970.5% of S composition metal sulfide quality.Catalyst hydrogen production reaction condition is identical with embodiment 1, and the hydrogen-producing speed of this catalyst hydrogen production by water decomposition is under visible light 3567 μm of olh
-1g
-1, use after 2d continuously, the catalytic activity of this catalyst does not change.
Embodiment 4
By Cd (CH
3cOO)
22H
2the quality of O becomes 5g, Mn (CH
3cOO)
24H
2the quality of O becomes 3.28g, Ag (CH
3cOO) quality becomes 25mg, and all the other conditions are with embodiment 2, and obtaining final products is RuO
2ag
0.005mn
0.3685cd
0.629s, wherein, RuO
2quality be Ag
0.005mn
0.3685cd
0.6290.5% of S composition metal sulfide quality.Catalyst hydrogen production reaction condition is identical with embodiment 1, and the hydrogen-producing speed of this catalyst hydrogen production by water decomposition is under visible light 3842 μm of olh
-1g
-1, use after 2d continuously, the catalytic activity of this catalyst does not change.
Embodiment 5
By Cd (CH
3cOO)
22H
2the quality of O becomes 4.9g, Mn (CH
3cOO)
24H
2the quality of O becomes 3.28g, Ag (CH
3cOO) quality becomes 0.1g, and all the other conditions are with embodiment 2, and obtaining final products is RuO
2ag
0.02mn
0.363cd
0.627s, wherein, RuO
2quality be Ag
0.02mn
0.363cd
0.6270.5% of S composition metal sulfide quality.Catalyst hydrogen production reaction condition is identical with embodiment 1, and the hydrogen-producing speed of this catalyst hydrogen production by water decomposition is under visible light 4137 μm of olh
-1g
-1, use after 2d continuously, the catalytic activity of this catalyst does not change.
Embodiment 6
By Cd (CH
3cOO)
22H
2the quality of O becomes 4.9g, Mn (CH
3cOO)
24H
2the quality of O becomes 3.21g, Ag (CH
3cOO) quality becomes 0.2g, and all the other conditions are with embodiment 2, and obtaining final products is RuO
2ag
0.04mn
0.36cd
0.62s, wherein, RuO
2quality be RuO
2ag
0.04mn
0.36cd
0.620.5% of S composition metal sulfide quality.Catalyst hydrogen production reaction condition is identical with embodiment 1, and the hydrogen-producing speed of this catalyst hydrogen production by water decomposition is under visible light 4258 μm of olh
-1g
-1, use after 2d continuously, the catalytic activity of this catalyst does not change.
Embodiment 7
By Cd (CH
3cOO)
22H
2the quality of O becomes 4.9g, Mn (CH
3cOO)
24H
2the quality of O becomes 3.13g, Ag (CH
3cOO) quality becomes 0.3g, and all the other conditions are with embodiment 2, and obtaining final products is RuO
2ag
0.06mn
0.35cd
0.62s, wherein, RuO
2quality be Ag
0.06mn
0.35cd
0.620.5% of S composition metal sulfide quality.Catalyst hydrogen production reaction condition is identical with embodiment 1, and the hydrogen-producing speed of this catalyst hydrogen production by water decomposition is under visible light 4580 μm of olh
-1g
-1, use after 2d continuously, the catalytic activity of this catalyst does not change.
Embodiment 8
By Cd (CH
3cOO)
22H
2the quality of O becomes 4.9g, Mn (CH
3cOO)
24H
2the quality of O becomes 3.13g, Ag (CH
3cOO) quality becomes 0.4g, and all the other conditions are with embodiment 2, and obtaining final products is RuO
2ag
0.08mn
0.35cd
0.61s, wherein, RuO
2quality be Ag
0.08mn
0.35cd
0.610.5% of S composition metal sulfide quality.Catalyst hydrogen production reaction condition is identical with embodiment 1, and the hydrogen-producing speed of this catalyst hydrogen production by water decomposition is under visible light 3820 μm of olh
-1g
-1, use after 2d continuously, the catalytic activity of this catalyst does not change.
Embodiment 9
By Cd (CH
3cOO)
22H
2the quality of O becomes 4.9g, Mn (CH
3cOO)
24H
2the quality of O becomes 3.06g, Ag (CH
3cOO) quality becomes 0.5g, and all the other conditions are with embodiment 1, and obtaining final products is RuO
2ag
0.1mn
0.34cd
0.61s, wherein, RuO
2quality be Ag
0.1mn
0.34cd
0.610.5% of S composition metal sulfide quality.Catalyst hydrogen production reaction condition is identical with embodiment 2, and the hydrogen-producing speed of this catalyst hydrogen production by water decomposition is under visible light 3375 μm of olh
-1g
-1, use after 2d continuously, the catalytic activity of this catalyst does not change.
Embodiment 10
By the Ag in embodiment 7
0.06mn
0.35cd
0.62s is dissolved in the Ru of oxolane
3(CO)
12solution concentration changes 0.1mol/L into, obtained RuO
2quality be Ag
0.06mn
0.35cd
0.62s composition metal sulfide quality
0.2%, all the other conditions are with embodiment 7, and the hydrogen-producing speed of this catalyst hydrogen production by water decomposition is under visible light 3698 μm of olh
-1g
-1, use after 2d continuously, the catalytic activity of this catalyst does not change.
Embodiment 11
By the Ag in embodiment 7
0.06mn
0.35cd
0.62s is dissolved in the Ru of oxolane
3(CO)
12solution concentration changes 0.8mol/L into, obtained RuO
2quality be Ag
0.06mn
0.35cd
0.623.2% of S composition metal sulfide quality, all the other conditions are with embodiment 7, and the hydrogen-producing speed of this catalyst hydrogen production by water decomposition is under visible light 3078 μm of olh
-1g
-1, use after 2d continuously, the catalytic activity of this catalyst does not change.
Comparative example 1
Replace manganese acetate with zinc acetate, all the other conditions, with embodiment 1, obtain RuO
2zn
0.46cd
0.54s photochemical catalyst.RuO in photochemical catalyst
2quality be Zn
0.46cd
0.540.5% of S composition metal sulfide quality.Catalyst hydrogen production reaction condition is identical with embodiment 1, and the hydrogen-producing speed of this catalyst hydrogen production by water decomposition is under visible light 1943 μm of olh
-1g
-1, use continuously after 12h, the catalytic activity of this catalyst starts to decline.
Comparative example 2
Replace manganese acetate with zinc acetate, all the other conditions, with embodiment 7, obtain RuO
2ag
0.06zn
0.35cd
0.62s photochemical catalyst.RuO in photochemical catalyst
2quality be Ag
0.06zn
0.35cd
0.620.5% of S composition metal sulfide quality.Catalyst hydrogen production reaction condition is identical with embodiment 1, and the hydrogen-producing speed of this catalyst hydrogen production by water decomposition is under visible light 2144 μm of olh
-1g
-1, use continuously after 12h, the catalytic activity of this catalyst starts to decline.
Claims (13)
1. a photochemical catalyst, is characterized in that: this catalyst is by RuO
2and Mn
1-xcd
xs composition metal sulfide forms, RuO in catalyst
2quality be Mn
1-xcd
xthe 0.01-8% of S composition metal sulfide quality, preferred 0.02-4%, described Mn
1-xcd
x0 <x< 1 in S composition metal sulfide, preferably 0.5 <x< 0.9.
2. catalyst according to claim 1, is characterized in that: RuO in catalyst
2quality be Mn
1-xcd
xthe 0.02-4% of S composition metal sulfide quality, described Mn
1-xcd
x0.5 <x< 0.9 in S composition metal sulfide.
3. catalyst according to claim 1, is characterized in that: in described composition metal sulfide also containing silver, composition metal sulfide consist of Ag
ymn
1-x-y/2cd
xs, wherein 0<x<1,0<y<1, preferred x=0.2 ~ 0.8, y=0.001 ~ 0.02.
4. the preparation method of catalyst described in claim 1, is characterized in that: the preparation process and the RuO that comprise composition metal sulfide
2loading process.
5. method according to claim 4, is characterized in that: described composition metal sulfide adopts hydrothermal synthesis method preparation, and step is as follows:
(1) preparation is containing the mixed liquor of cadmium salt, manganese salt and thioacetamide;
(2) mixed liquor of step (1) is placed in hydrothermal synthesis reaction still, 130-250 DEG C of reaction 10-30h;
(3) centrifugal treating is carried out to the sediment of step (2) hydrothermal synthesis reaction, get the single-phase obtained composition metal sulfide of yellow green.
6. method according to claim 5, is characterized in that: in the mixed liquor described in step (1), the molar concentration of cadmium is 0.3-0.5mol/L, and the molar concentration of manganese is 0.2-0.4 mol/L, and the molar concentration of thioacetamide is 0.1-0.2 mol/L.
7. method according to claim 5, is characterized in that: also containing the silver that molar concentration is 0.001-0.1 mol/L in mixed liquor.
8. method according to claim 5, is characterized in that: described salt comprises nitrate, sulfate, acetate.
9. method according to claim 5, is characterized in that: in step (2), hydrothermal reaction condition is 150-210 DEG C of reaction 16-24h.
10. method according to claim 5, is characterized in that: carry out centrifugal treating after adopting distilled water and ethanol repeatedly to rinse sediment in step (3), wash number is 3-5 time repeatedly.
11. methods according to claim 4, is characterized in that: described RuO
2loading process is as follows: adopt the tetrahydrofuran solution dipping composition metal sulfide containing ruthenium, obtain photochemical catalyst after dipping through dry, roasting.
12. methods according to claim 11, is characterized in that: in loading process, ruthenium comprises Ru
3(CO)
12, Ru(CO)
3cl
2or Ru (C
5h
7o
2)
3.
13. methods according to claim 11, is characterized in that: described drying is vacuum drying, and described roasting is roasting 12-24h under 180-220 DEG C of condition.
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CN104923264A (en) * | 2015-05-28 | 2015-09-23 | 淮北师范大学 | Preparation method and application of precious metal-modified CdS nanorod photocatalyst |
CN107376944A (en) * | 2017-07-25 | 2017-11-24 | 山东大学 | Transient metal sulfide loads application of the Mn Cd S solid solution in terms of Photocatalyzed Hydrogen Production |
CN107684917A (en) * | 2017-09-05 | 2018-02-13 | 广西科技师范学院 | A kind of Mn1Cd3S4The preparation method of photochemical catalyst |
CN110252359A (en) * | 2019-06-17 | 2019-09-20 | 四川大学 | A kind of preparation method of sulfur-bearing cadmium hetero-junctions photodissociation aquatic products hydrogen catalyst |
CN111036249A (en) * | 2019-12-23 | 2020-04-21 | 华南理工大学 | FexP/Mn0.3Cd0.7S composite photocatalyst and preparation method and application thereof |
CN111905761A (en) * | 2020-07-29 | 2020-11-10 | 广西科技师范学院 | Mn (manganese)1Cd3S4Method for preparing photocatalyst |
CN114100633A (en) * | 2020-08-31 | 2022-03-01 | 中国石油化工股份有限公司 | Catalyst for hydrogen production by visible light catalytic decomposition of hydrogen sulfide and preparation method thereof |
CN114749189A (en) * | 2022-05-20 | 2022-07-15 | 常州大学 | MCS/ZCO composite photocatalyst for photocatalytic hydrogen production and preparation method thereof |
CN115364871A (en) * | 2022-08-03 | 2022-11-22 | 三峡大学 | Preparation method and application of transition metal molybdate heterojunction photocatalytic material |
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CN104923264B (en) * | 2015-05-28 | 2017-05-10 | 淮北师范大学 | Preparation method and application of precious metal-modified CdS nanorod photocatalyst |
CN104923264A (en) * | 2015-05-28 | 2015-09-23 | 淮北师范大学 | Preparation method and application of precious metal-modified CdS nanorod photocatalyst |
CN107376944B (en) * | 2017-07-25 | 2019-12-17 | 山东大学 | Application of transition metal sulfide loaded Mn-Cd-S solid solution in aspect of photocatalytic hydrogen production |
CN107376944A (en) * | 2017-07-25 | 2017-11-24 | 山东大学 | Transient metal sulfide loads application of the Mn Cd S solid solution in terms of Photocatalyzed Hydrogen Production |
CN107684917A (en) * | 2017-09-05 | 2018-02-13 | 广西科技师范学院 | A kind of Mn1Cd3S4The preparation method of photochemical catalyst |
CN110252359B (en) * | 2019-06-17 | 2020-04-03 | 四川大学 | Preparation method of catalyst for photolysis of water to produce hydrogen by using cadmium sulfide-containing heterojunction |
CN110252359A (en) * | 2019-06-17 | 2019-09-20 | 四川大学 | A kind of preparation method of sulfur-bearing cadmium hetero-junctions photodissociation aquatic products hydrogen catalyst |
CN111036249A (en) * | 2019-12-23 | 2020-04-21 | 华南理工大学 | FexP/Mn0.3Cd0.7S composite photocatalyst and preparation method and application thereof |
CN111905761A (en) * | 2020-07-29 | 2020-11-10 | 广西科技师范学院 | Mn (manganese)1Cd3S4Method for preparing photocatalyst |
CN114100633A (en) * | 2020-08-31 | 2022-03-01 | 中国石油化工股份有限公司 | Catalyst for hydrogen production by visible light catalytic decomposition of hydrogen sulfide and preparation method thereof |
CN114100633B (en) * | 2020-08-31 | 2023-10-20 | 中国石油化工股份有限公司 | Catalyst for preparing hydrogen by catalyzing and decomposing hydrogen sulfide by visible light and preparation method thereof |
CN114749189A (en) * | 2022-05-20 | 2022-07-15 | 常州大学 | MCS/ZCO composite photocatalyst for photocatalytic hydrogen production and preparation method thereof |
CN114749189B (en) * | 2022-05-20 | 2023-08-22 | 常州大学 | MCS/ZCO composite photocatalyst for photocatalytic hydrogen production and preparation method thereof |
CN115364871A (en) * | 2022-08-03 | 2022-11-22 | 三峡大学 | Preparation method and application of transition metal molybdate heterojunction photocatalytic material |
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