CN106925299B - Conversion produces hydrogen system and its construction method and application on a kind of T-T annihilation - Google Patents
Conversion produces hydrogen system and its construction method and application on a kind of T-T annihilation Download PDFInfo
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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Abstract
The invention discloses conversions on a kind of T-T annihilation to produce hydrogen system, and conversion produces hydrogen system and includes photosensitizer, acceptor molecule, produces hydrogen catalyst and sacrificial body on this；The photosensitizer is palladium porphyrin；The acceptor molecule is 9,10- tolans base anthracene；The production hydrogen catalyst is Cd0.5Zn0.5S；The sacrificial body is Na2SO3And Na2S.The stability that conversion produces that hydrogen system has had on this produces hydrogen activity with efficient catalysis.The invention also discloses construction method and its applications in Photocatalyzed Hydrogen Production that conversion on this produces hydrogen system.
Description
Technical field
The present invention relates to energy sciences and catalytic science field.More particularly, on a kind of T-T annihilation
Conversion produces hydrogen system and its construction method and application.
Background technique
Energy problem and environmental problem are the two large problems of face of mankind nowadays.Fossil fuel is as main energy source
There is extremely important effect in the industrial production, but since its is non-renewable and to the pollution of environment, finds renewable
Economical clean energy resource just become world subject (Armaroli, N.et al.Angew.Chem.Int.Ed.2007,46
(1-2),52-66).Solar energy gets more and more people's extensive concerning as sustainable clean energy resource.Effectively not using solar energy
But it can partially solve fossil energy and face the crisis exhausted, pollution of the combustion of fossil fuel to environment can also be reduced.To,
The energy that effectively converting solar energy to can directly utilize becomes the emphasis of people's research.
Hydrogen is considered as optimal clean energy resource, its combustion product is water, not can cause environmental pollution, simultaneously
With calorific value height, the features such as being readily transported and store, the effective use of solar energy may be implemented using solar hydrogen making.Last decade
In, people successfully constructed it is numerous Photocatalyzed Hydrogen Production system, the sub- efficiency of hydrogen output can also be stepped up (for example,
Pfeffer, M.G., Kowacs, T., Wachtler, M., Guthmuller, J., Dietzek, B., Vos, J.G., Rau, S.,
Angewandte Chemie-International Edition,2015,54(22),6627-6631；Das,A.,Han,
Z.J.,Brennessel,W.W.,Holland,P.L.,Eisenberg,R.,Acs Catalysis,2015,5(3),1397-
1406) production hydrogen system constructed, but at present is concentrated mainly on short-wave band to the utilization of solar energy, for long-wave band sunlight
Using limited.
Converted on T-T annihilation (triplet-triplet annihilation, abbreviation TTA) earliest by
Parker and Hatchard proposes (Parker, C.A., Proceedings of the Royal in the 1960s
Society of London Series a-Mathematical and Physical Sciences,1963,276,125-
135；Parker,C.A.,Hatchard,C.G.,Proceedings of the Royal Society of London
Series a-Mathematical and Physical Sciences, 1962,269,574-584.), they are luxuriant and rich with fragrance and naphthalene
By selective excitation phenanthrene in mixed solution, the anti-stoke delayed fluorescence of naphthalene observed.Based on the mechanism converted on TTA
Are as follows: triplet photosensitizer, which is stimulated, reaches excited singlet state, and by passing through arrival triplet between being, triplet photosensitizer is by energy
Acceptor molecule is passed to, receptor obtains energy and reaches triplet, after the acceptor molecule in triplet reaches a certain concentration, two
A triplet acceptor molecule mutually collides, and the acceptor molecule of a singlet excited, another receptor point are generated with certain probability
Sub then reach ground state, the acceptor molecule for being now in singlet excited can issue fluorescence, realize up-conversion luminescence.
So far, there is not the relevant report that hydrogen is produced using switch technology catalysis on TTA photon also.
Summary of the invention
The first purpose of this invention is to provide conversion on a kind of T-T annihilation and produces hydrogen system, the system
Stability is good, and switch technology on T-T annihilation is used for Photocatalyzed Hydrogen Production for the first time, realizes originally cannot be by
Producing the long wavelength light that hydrogen system utilizes can be used to be catalyzed production hydrogen.
Second object of the present invention is to provide a kind of side for constructing conversion on T-T annihilation and producing hydrogen system
Method.
Third object of the present invention is to provide conversion on T-T annihilation and produces hydrogen system in Photocatalyzed Hydrogen Production
In application.
In order to achieve the above first purpose, the present invention adopts the following technical solutions:
Conversion produces hydrogen system on a kind of T-T annihilation, and it includes photosensitizer, receptor that the upper conversion, which produces hydrogen system,
Molecule produces hydrogen catalyst and sacrificial body；The photosensitizer is palladium porphyrin；The acceptor molecule is 9,10- tolans base anthracene；Institute
Stating and producing hydrogen catalyst is Cd0.5Zn0.5S；The sacrificial body is Na2SO3And Na2S。
Wherein, the structural formula of palladium porphyrin is as follows:
The structural formula of 9,10- tolans base anthracene is as follows:
In the present invention, by being selected photosensitizer, acceptor molecule, production hydrogen catalyst and sacrificial body, being cooperated, thus
Conversion produces hydrogen system on the T-T annihilation good to Photocatalyzed Hydrogen Production effect.
Preferably, the upper production hydrogen system absorbing wavelength of converting is triple by triplet-into the luminous energy of 550nm~650nm
Conversion process in state, Catalytic Proton generate hydrogen.
To reach above-mentioned second purpose, the present invention provides conversion on a kind of building T-T annihilation and produces hydrogen body
The method of system, this method comprises the following steps:
1) by photosensitizer, 1:20~1:100 is dissolved in tetrahydrofuran in molar ratio with acceptor molecule, and tween-is then added
80, it stirs evenly；
2) solution for stirring evenly step 1) is slowly injected into water, while quickly stirring the aqueous solution, obtained liquid
The as stable nano-micelle up-conversion luminescence system of Tween-80；
3) by Cd0.5Zn0.5S is added to the water, and ultrasonic disperse 10~30 minutes, Na is then added2SO3、Na2S and step
2) the stable nano-micelle up-conversion luminescence system of the Tween-80 obtained produces hydrogen body to get conversion on T-T annihilation
System.
Preferably, in step 1), the additional amount of the Tween-80 is 10~50 times of molar equivalents of acceptor molecule；It is more excellent
The additional amount of Tween-80 described in selection of land is 50 times of molar equivalents of acceptor molecule.Tween-80 can divide stable receptor well
Son prevents acceptor molecule from assembling.However excessive addition Tween-80, then the triplet-between photosensitizer and receptor can be made triple
State buries in oblivion the difficulty that upper conversion process becomes, and influences to be catalyzed hydrogen generation efficiency.
Preferably, in step 1), the molar ratio of the photosensitizer and acceptor molecule is 1:50~1:100, is obtained at this time
Conversion produces the better effect that hydrogen system catalysis visible light produces hydrogen on T-T annihilation, and hydrogen output is higher；It is highly preferred that
In step 1), the molar ratio of the photosensitizer and acceptor molecule is 1:100, and gained produces hydrogen system and is catalyzed visible light hydrogen output at this time
It is more excellent.
Preferably, in step 3), the Cd0.5Zn0.5The additional amount of S (catalyst) is 1mg/mL~20mg/mL, wherein on
The additional amount for stating catalyst is that the volume of hydrogen system is produced relative to conversion on gained.The T-T annihilation obtained at this time
Upper conversion produces the better effect that hydrogen system catalysis visible light produces hydrogen, and hydrogen output is higher；It is highly preferred that in step 3), the catalysis
The additional amount of agent is 10mg/mL, and it is more excellent to produce hydrogen system catalysis visible light hydrogen output for gained at this time.
Preferably, in step 3), the additional amount Na of the sacrificial body2SO3For 0.1g/mL~1.0g/mL, Na2S is 0.1g/
ML~1.0g/mL, wherein the additional amount of above-mentioned sacrificial body is to produce the volume of hydrogen system relative to conversion on gained.It obtains at this time
Conversion produces the better effect that hydrogen system catalysis visible light produces hydrogen on T-T annihilation, and hydrogen output is higher；It is highly preferred that
In step 3), the additional amount Na of the sacrificial body2SO3For 0.3g/mL, Na2S is 0.2g/mL, and gained produces hydrogen system catalysis at this time
Visible light hydrogen output is more excellent.
To reach above-mentioned third purpose, the present invention, which provides conversion on a kind of T-T annihilation and produces hydrogen system, to exist
Application in Photocatalyzed Hydrogen Production.
Preferably, conversion produces hydrogen system and produces the application in hydrogen in visible light catalytic on the T-T annihilation.Institute
It states conversion on T-T annihilation and produces hydrogen system as catalyst applied in visible light catalytic production hydrogen.
Preferably, the wave-length coverage of the visible light is 550nm~650nm.
Preferably, the application includes the following steps:
(1) conversion on T-T annihilation is produced hydrogen system to be added in transparency reactor, obtains reaction solution, reacted
It is atmosphere of inert gases in device, squeezes into methane as interior standard gas；
(2) visible light illumination reaction liquid is used, hydrogen is obtained.
Specifically, the application includes the following steps:
S1: by photosensitizer, 1:20~1:100 is dissolved in tetrahydrofuran in molar ratio with acceptor molecule, and tween-is then added
80, it stirs evenly；
S2: the step S1 solution stirred evenly being slowly injected into water, while quickly stirring the aqueous solution, obtained liquid
The as stable nano-micelle up-conversion luminescence system of Tween-80；
S3: by Cd0.5Zn0.5S is added to the water, and ultrasonic disperse 10~30 minutes, Na is then added2SO3、Na2S and step
The stable nano-micelle up-conversion luminescence system of the Tween-80 that rapid S2 is obtained；
S4: the reaction solution in step S3 is added in transparency reactor, obtains reaction solution, and deoxygenation is carried out in reactor, is filled
Nitrogen is maintained at atmosphere of inert gases, squeezes into methane as interior standard gas；
S5: visible light illumination reaction liquid is used, hydrogen is obtained.
Above-mentioned steps S1~S3 produces step 1)~3 in the construction method of hydrogen system with above-mentioned upper conversion in the present invention) phase
Together.
Preferably, the visible light is LED light；The more preferably wavelength LED light that is 629nm, photocatalysis effect is more at this time
It is good.
Preferably, the visible light light application time is 0~10 hour；More preferably 2~8 hours, more preferably 2~6 is small
When, most preferably 3~6 hours.
Preferably, with after visible light illumination reaction liquid, the hydrogen in reaction solution overhead gas is measured using gas chromatography
With the peak area of methane, the volume of output hydrogen can be calculated.
In the present invention, unless otherwise specified, it is raw materials used can be by commercially available commercially available.
Beneficial effects of the present invention are as follows:
It is realized for the first time in the present invention and conversion on T-T annihilation is used to construct Photocatalyzed Hydrogen Production system, it should
System stability is good, and by converting system on T-T annihilation, the long wave that script cannot be utilized by production hydrogen system
Long luminous energy is converted to short-wavelength light energy, and the energy sources conversion of Hydrogen Energy can be converted to by realizing long wavelength light.
What conversion produced hydrogen system on the T-T annihilation in the present invention constructs that process is simple, is easy to largely prepare.
Conversion produces hydrogen system in Photocatalyzed Hydrogen Production using production hydrogen process on T-T annihilation in the present invention
In, it produces hydrogen system property and stablizes, and there is catalysis well to produce hydrogen activity.
Switch technology on photon is produced hydrogen system with artificial photosynthesis in the present invention to combine, effectively utilizes long wavelength
Luminous energy produces hydrogen, has improved artificial production hydrogen system to the utilization efficiency of luminous energy.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1 shows in the embodiment of the present invention 4 system hydrogen output with the change curve of light application time.
Fig. 2 shows system hydrogen outputs in the embodiment of the present invention 5 with the change curve of light application time.
Fig. 3 shows in the embodiment of the present invention 6 system hydrogen output with the change curve of light application time.
Fig. 4 shows in the embodiment of the present invention 7 system hydrogen output with the change curve of light application time.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further below with reference to preferred embodiments and drawings
It is bright.Similar component is indicated in attached drawing with identical appended drawing reference.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1
The preparation that micella is converted on T-T annihilation, includes the following steps:
Photosensitizer palladium porphyrin and acceptor molecule 9,10- tolans base anthracene are dissolved in four according to the ratio of molar ratio 1:100
In hydrogen furans, then to the Tween-80 that 50 times of molar equivalents of acceptor molecule are added in solution is obtained, stir evenly, then will stir equal
Solution after even is slowly driven into water, while quickly stirring aqueous solution, is obtained the stable triplet-triplet of Tween-80 and is fallen into oblivion
Go out upper conversion nano micella luminescence system.
Wherein, above-mentioned photosensitizer palladium porphyrin and acceptor molecule 9, the structural formula of 10- tolans base anthracene is respectively following (I)
(II) shown in:
Embodiment 2
With embodiment 1, difference is, by photosensitizer palladium porphyrin and acceptor molecule 9, the molar ratio of 10- tolans base anthracene
It is changed to 1:50, the additive amount of Tween-80 is 30 times of molar equivalents of photosensitizer, remaining condition is constant, and it is steady that Tween-80 is prepared
Conversion nano micella luminescence system on fixed T-T annihilation.
Embodiment 3
With embodiment 1, difference is, by photosensitizer palladium porphyrin and acceptor molecule 9, the molar ratio of 10- tolans base anthracene
It is changed to 1:20, the additive amount of Tween-80 is 10 times of molar equivalents of acceptor molecule, remaining condition is constant, and Tween-80 is prepared
Conversion nano micella luminescence system on stable T-T annihilation.
Embodiment 4
By 20mgCd0.5Zn0.5S is added in 10mL water, ultrasonic disperse 10 minutes, rear that 0.3g Na is added2SO3With
0.2gNa2S, stirring and dissolving.It takes the upper conversion micellar solution prepared in 10mL embodiment 1 to be added in foregoing catalytic systems, subtracts
Pressure vacuumizes-inflated with nitrogen, recycles the oxygen in removing system three times.10mL nitrogen in extraction system squeezes into 10mL methane conduct
Internal standard carries out illumination under 629nm LED light.Extracting container overhead gas at regular intervals, gas chromatographic detection calculate and produce hydrogen
Amount.System hydrogen output is as shown in Figure 1 with the change curve of light application time.
Embodiment 5
With embodiment 4, difference is, selects to carry out illumination under 590nm LED light.Gas above extracting container at regular intervals
Body, gas chromatographic detection calculate hydrogen output.System hydrogen output is as shown in Figure 2 with the change curve of light application time.
Embodiment 6
By 20mgCd0.5Zn0.5S is added in 10mL water, ultrasonic disperse 10 minutes, rear that 0.3g Na is added2SO3With
0.2gNa2S, stirring and dissolving.It takes the upper conversion micellar solution prepared in 10mL embodiment 2 to be added in foregoing catalytic systems, subtracts
Pressure vacuumizes-inflated with nitrogen, recycles the oxygen in removing system three times.10mL nitrogen in extraction system squeezes into 10mL methane conduct
Internal standard carries out illumination under 629nm LED light.Extracting container overhead gas at regular intervals, gas chromatographic detection calculate and produce hydrogen
Amount.System hydrogen output is as shown in Figure 3 with the change curve of light application time.
Embodiment 7
By 10mg Cd0.5Zn0.5S is added in 10mL water, ultrasonic disperse 30 minutes, rear that 0.3g Na is added2SO3And 0.2g
Na2S, stirring and dissolving.The upper conversion micellar solution prepared in 10mL embodiment 3 is taken to be added in foregoing catalytic systems, decompression is taken out
Vacuum-inflated with nitrogen recycles the oxygen in removing system three times.10mL nitrogen in extraction system, squeezes into 10mL methane as internal standard,
Illumination is carried out under 629nm LED light.Extracting container overhead gas at regular intervals, gas chromatographic detection calculate hydrogen output.Body
It is that hydrogen output is as shown in Figure 4 with the change curve of light application time.
Hydrogen system is produced for visible light catalytic it is found that converting on T-T annihilation of the invention from Fig. 1~4
The effect for producing hydrogen is obvious, and the hydrogen output in the short time is higher.When selected photosensitizer and acceptor molecule molar ratio are 1:100, tween-
When 80 additive amount is 100 times of photosensitizer additive amount, wavelength is used to produce hydrogen body for conversion on the LED light of 629nm irradiation gained
It is that liquor-saturated words visible light catalytic production hydrogen effect is best.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is all to belong to this hair
The obvious changes or variations that bright technical solution is extended out are still in the scope of protection of the present invention.
Claims (10)
1. conversion produces hydrogen system on a kind of T-T annihilation, which is characterized in that it includes light that the upper conversion, which produces hydrogen system,
Quick dose, acceptor molecule, production hydrogen catalyst and sacrificial body；
The photosensitizer is palladium porphyrin；The acceptor molecule is 9,10- tolans base anthracene；The production hydrogen catalyst is
Cd0.5Zn0.5S；The sacrificial body is Na2SO3And Na2S；
The molar ratio of the photosensitizer and acceptor molecule is 1:20~1:100；
The Cd0.5Zn0.5The additional amount of S is 1mg/mL~20mg/mL；
The additional amount Na of the sacrificial body2SO3For 0.1g/mL~1.0g/mL, Na2S is 0.1g/mL~1.0g/mL, wherein above-mentioned
Cd0.5Zn0.5The additional amount of S and sacrificial body is that the volume of hydrogen system is produced relative to conversion on gained.
2. conversion produces hydrogen system on T-T annihilation according to claim 1, which is characterized in that described upper turn
The luminous energy for producing that hydrogen system absorbing wavelength is 550nm~650nm is changed, by conversion process in triplet-triplet, Catalytic Proton is raw
At hydrogen.
3. constructing the method that conversion produces hydrogen system on T-T annihilation as described in claim 1, which is characterized in that
Include the following steps:
1) by photosensitizer, 1:20~1:100 is dissolved in tetrahydrofuran in molar ratio with acceptor molecule, and Tween-80 is then added, stirs
It mixes uniformly；
2) solution for stirring evenly step 1) is slowly injected into water, while quickly stirring the aqueous solution, and obtained liquid is
The stable nano-micelle up-conversion luminescence system of Tween-80；
3) by Cd0.5Zn0.5S is added to the water, and ultrasonic disperse 10~30 minutes, Na is then added2SO3、Na2S and step 2) obtain
To the stable nano-micelle up-conversion luminescence system of Tween-80 produce hydrogen system to get conversion on T-T annihilation.
4. according to the method described in claim 3, it is characterized in that, the additional amount of the Tween-80 is receptor point in step 1)
10~50 times of molar equivalents of son.
5. according to the method described in claim 3, it is characterized in that, in step 3), the Cd0.5Zn0.5The additional amount of S is 1mg/
ML~20mg/mL；The Na2SO3Additional amount be 0.1g/mL~1.0g/mL, Na2The additional amount of S is 0.1g/mL~1.0g/
mL。
6. as conversion produces hydrogen system in Photocatalyzed Hydrogen Production on the described in any item T-T annihilations of claim 1~2
Application.
7. application according to claim 6, which is characterized in that conversion produces hydrogen system on the T-T annihilation
The application in hydrogen is produced in visible light catalytic.
8. application according to claim 7, which is characterized in that the wave-length coverage of the visible light is 550nm~650nm.
9. according to the described in any item applications of claim 6~8, which is characterized in that the application includes the following steps:
(1) conversion it will produce hydrogen system on T-T annihilation and be added in transparency reactor, and reaction solution be obtained, in reactor
For atmosphere of inert gases, methane is squeezed into as interior standard gas；
(2) visible light illumination reaction liquid is used, hydrogen is obtained.
10. application according to claim 9, which is characterized in that the visible light is LED light.
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| CN111943135B (en) * | 2019-05-17 | 2022-05-17 | 中国科学院理化技术研究所 | Red light catalytic water decomposition hydrogen production system and preparation method and application thereof |
| CN112500849B (en) * | 2020-10-30 | 2022-11-22 | 中国科学院理化技术研究所 | Hydrophilic crosslinked polymer up-conversion microsphere, preparation method thereof and application thereof in photocatalytic hydrogen production |
| CN113769784B (en) * | 2021-10-11 | 2024-02-20 | 山东能源集团有限公司 | Lignin model compound degradation method and up-conversion catalyst |
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