CN108273520A - A kind of cadmium sulfide/sulphur composite photo-catalyst and the preparation method and application thereof - Google Patents
A kind of cadmium sulfide/sulphur composite photo-catalyst and the preparation method and application thereof Download PDFInfo
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- CN108273520A CN108273520A CN201810227790.5A CN201810227790A CN108273520A CN 108273520 A CN108273520 A CN 108273520A CN 201810227790 A CN201810227790 A CN 201810227790A CN 108273520 A CN108273520 A CN 108273520A
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- Prior art keywords
- composite photo
- cadmium sulfide
- catalyst
- cadmium
- sulphur
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000005864 Sulphur Substances 0.000 title claims abstract description 57
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 46
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 230000001699 photocatalysis Effects 0.000 claims abstract description 21
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 16
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 238000007146 photocatalysis Methods 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000013049 sediment Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 5
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical group [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 5
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 5
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 3
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 claims description 3
- 229910000331 cadmium sulfate Inorganic materials 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000007789 gas Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000011017 operating method Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 4
- 239000003643 water by type Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 238000013102 re-test Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/345—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of ultraviolet wave energy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention belongs to photocatalysis technology field, a kind of cadmium sulfide/sulphur composite photo-catalyst and the preparation method and application thereof is disclosed.It weighs cadmium source and sulphur source is dissolved in deionized water, configure forerunner's liquor；By forerunner's liquor as being irradiated under ultraviolet source, solution forms sediment under light irradiation reaction；Taking-up reaction solution is centrifuged, deionized water is washed, drying to obtain cadmium sulfide/sulphur composite photo-catalyst.The raw material that uses of preparation method of the present invention is simple, and of low cost, operating procedure is simple, and reaction condition is mild, can be reacted by ultraviolet light irradiation at room temperature, low energy consumption and environmental-friendly；Cadmium sulfide obtained/sulphur composite photo-catalyst has the characteristics that photocatalysis performance is good, stability is good；There is preferable application prospect in terms of photocatalysis hydrogen production gas.
Description
Technical field
The invention belongs to photocatalysis technology fields, and in particular to a kind of cadmium sulfide/sulphur composite photo-catalyst and its preparation side
Method and application.
Background technology
Photocatalysis technology has the characteristics that operating procedure is simple controllably, low energy consumption, is grinding for photodissociation aquatic products hydrogen technical aspect
Study carefully hot spot.Cadmium sulfide is a kind of N-type semiconductor, and there is wider forbidden band (2.42eV), unique photoelectric properties it to be made to urge
Have broad application prospects in terms of change, nonlinear optics, opto-electronic device and solar energy conversion.Sulphur be in natural environment distribution compared with
A kind of wide non-metal simple-substance, but at present for sulphur in photocatalysis technology field using less, and it is purely by way of photocatalysis
Activity is relatively low when agent.Currently, for the synthesis of Nano cadmium sulphide be still confined to hydro-thermal method, microemulsion method etc. be cumbersome, high energy consumption very
To the method for having suspicion of danger, at the same cadmium sulfide there are properties it is unstable, photocatalytic activity is low the features such as, need by with its
His Material cladding is to improve its stability and photocatalytic activity.Cadmium sulfide carries out In-situ reaction with elemental sulfur and is applied to photocatalytic water
There has been no relevant reports for the research of production hydrogen.Photo chemistry technology is a kind of technology of mild room temperature synthetic material, but is preparing sulphur
It is still blank in terms of cadmium/sulphur composite photocatalyst material.
Invention content
The object of the present invention is to provide a kind of photochemical method for preparation of cadmium sulfide/sulphur composite photo-catalyst, in ultraviolet light
Under irradiation, cadmium sulfide carries out compound in situ with sulphur, prepares cadmium sulfide/sulphur composite photo-catalyst, for solving in the prior art
Prepare the problem that cadmium sulfide photochemical catalyst property is unstable and photocatalytic activity is low.The invention also discloses by party's legal system simultaneously
Standby obtained cadmium sulfide/sulphur composite photo-catalyst and its application in terms of photocatalysis prepares hydrogen.
The technical scheme is that：
A kind of photochemical method for preparation of cadmium sulfide/sulphur composite photo-catalyst, includes the following steps：
(1) cadmium source and sulphur source are dissolved in deionized water, configure forerunner's liquor；
(2) forerunner's liquor is placed under ultraviolet source and is irradiated, solution forms sediment under light irradiation reaction；
(3) reaction solution is taken out to be centrifuged, washed, dried to get to cadmium sulfide/sulphur composite photo-catalyst.
Preferably, the cadmium source is one kind in cadmium sulfate, cadmium acetate, caddy.
Preferably, the sulphur source is sodium thiosulfate or thiocarbamide.
Preferably, a concentration of 0.05mol/L-0.4mol/L in cadmium source in forerunner's liquor.
Preferably, the molar ratio of the cadmium source and sulphur source is (0.5~2):1.
Preferably, the ultraviolet source is the ultraviolet lamp of wavelength 254nm, and ultraviolet lamp power is 8~30W, ultraviolet when irradiation
Lamp is 1.4~6.2mW/cm in the irradiation intensity of precursor liquid liquid level2。
Preferably, the irradiation time is 6-24h.
Preferably, make to be washed with deionized in step (3), it is dry at 60 DEG C.
The cadmium sulfide and sulphur composite photo-catalyst be prepared by the above method.
The application of above-mentioned cadmium sulfide and sulphur composite photo-catalyst in terms of photocatalysis prepares hydrogen.Beneficial effects of the present invention
It is as follows：
The raw material type that uses of preparation method of the present invention is simple, of low cost, reaction condition is mildly controllable, environmental-friendly
It is pollution-free.Cadmium sulfide obtained/sulphur composite photo-catalyst has the characteristics that photocatalytic activity is good, property is stablized, in photocatalysis
There is preferable application prospect in terms of preparing hydrogen.
Description of the drawings
Fig. 1 is the X ray diffracting spectrum of cadmium sulfide/sulphur composite photo-catalyst and bright sulfur cadmium；
Fig. 2 is the photocatalysis hydrogen production gas performance comparison figure of cadmium sulfide/sulphur composite photo-catalyst and bright sulfur cadmium；
Fig. 3 is the photocatalysis hydrogen production gas Repeatability test chart of cadmium sulfide/sulphur composite photo-catalyst.
Specific implementation mode
With reference to embodiment, technical scheme of the present invention is described in further detail, but do not constituted pair
Any restrictions of the present invention.
Embodiment 1
(1) caddy and 0.01mol sodium thiosulfate for weighing 0.015mol are dissolved in (forerunner in 100ml deionized waters
The molar ratio of a concentration of 0.15M in cadmium source in liquor, cadmium source and sulphur source is 1.5:1) forerunner's liquor, is configured；
(2) forerunner's liquor is placed under ultraviolet source irradiate for 24 hours (ultraviolet lamp power be 8W, the irradiation intensity of ultraviolet lamp
For 2.72mW/cm2), solution forms sediment under light irradiation reaction；
(3) taking-up reaction solution is centrifuged, deionized water is washed, 60 DEG C of dry 12h obtain cadmium sulfide/sulphur complex light
Catalyst.
Fig. 1 is the X-ray diffraction comparison diagram of cadmium sulfide and sulphur composite photo-catalyst manufactured in the present embodiment and bright sulfur cadmium
Spectrum, from the figure, it can be seen that the X-ray diffraction spectrogram of cadmium sulfide and sulphur composite photo-catalyst has the spy of sulphur in 2 θ=23.082 °
Diffraction maximum is levied, shows to contain cadmium sulfide and sulphur in the composite photo-catalyst product.
Embodiment 2
(1) cadmium sulfate and 0.02mol sodium thiosulfate for weighing 0.04mol are dissolved in (precursor liquid in 100ml deionized waters
The molar ratio of a concentration of 0.4M in cadmium source in solution, cadmium source and sulphur source is 2:1) forerunner's liquor, is configured；
(2) forerunner's liquor is placed under ultraviolet source irradiate for 24 hours (ultraviolet lamp power be 8W, the irradiation intensity of ultraviolet lamp
For 1.40mW/cm2), solution forms sediment under light irradiation reaction；
(3) taking-up reaction solution is centrifuged, deionized water is washed, 60 DEG C of dry 12h obtain cadmium sulfide/sulphur complex light
Catalyst.
Embodiment 3
(1) cadmium acetate and 0.01mol sodium thiosulfate for weighing 0.005mol are dissolved in (forerunner in 100ml deionized waters
The molar ratio of a concentration of 0.05M in cadmium source in liquor, cadmium source and sulphur source is 0.5:1) forerunner's liquor, is configured；
(2) forerunner's liquor is placed under ultraviolet source irradiate for 24 hours (ultraviolet lamp power be 8W, the irradiation intensity of ultraviolet lamp
For 5.50mW/cm2), solution forms sediment under light irradiation reaction；
(3) taking-up reaction solution is centrifuged, deionized water is washed, 60 DEG C of dry 12h obtain cadmium sulfide/sulphur complex light
Catalyst.
Cadmium sulfide/sulphur composite photo-catalyst prepares hydrogen performance test：
Fig. 2 is the photocatalysis hydrogen production gas performance pair of cadmium sulfide/sulphur composite photo-catalyst and bright sulfur cadmium prepared by embodiment 1
Than figure, it can be seen that the cadmium sulfide containing sulphur/sulphur composite photo-catalyst has better photocatalysis hydrogen production compared to bright sulfur cadmium
Gas performance.
Fig. 3 is the photocatalysis hydrogen production gas Repeatability test chart of cadmium sulfide/sulphur composite photo-catalyst prepared by embodiment 1,
It can be seen that the retest performance of cadmium sulfide/sulphur composite photo-catalyst is good, property is stablized.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of photochemical method for preparation of cadmium sulfide/sulphur composite photo-catalyst, which is characterized in that include the following steps：
(1) cadmium source and sulphur source are dissolved in deionized water, configure forerunner's liquor；
(2) forerunner's liquor is placed under ultraviolet source and is irradiated, solution forms sediment under light irradiation reaction；
(3) reaction solution is taken out to be centrifuged, washed, dried to get to cadmium sulfide/sulphur composite photo-catalyst.
2. a kind of photochemical method for preparation of cadmium sulfide/sulphur composite photo-catalyst according to claim 1, feature exist
In：The cadmium source is one kind in cadmium sulfate, cadmium acetate, caddy.
3. a kind of photochemical method for preparation of cadmium sulfide/sulphur composite photo-catalyst according to claim 1, feature exist
In：The sulphur source is sodium thiosulfate or thiocarbamide.
4. a kind of photochemical method for preparation of cadmium sulfide/sulphur composite photo-catalyst according to claim 1, feature exist
In：A concentration of 0.05mol/L-0.4mol/L in cadmium source in forerunner's liquor.
5. a kind of photochemical method for preparation of cadmium sulfide/sulphur composite photo-catalyst according to claim 1, feature exist
In：The molar ratio of the cadmium source and sulphur source is (0.5~2):1.
6. a kind of photochemical method for preparation of cadmium sulfide/sulphur composite photo-catalyst according to claim 1, feature exist
In：The ultraviolet source is the ultraviolet lamp of wavelength 254nm, and ultraviolet lamp power is 8~30W, and when irradiation, ultraviolet lamp is in precursor liquid liquid
The irradiation intensity in face is 1.4~6.2mW/cm2。
7. a kind of photochemical method for preparation of cadmium sulfide/sulphur composite photo-catalyst according to claim 1, feature exist
In：The irradiation time is 6-24h.
8. a kind of photochemical method for preparation of cadmium sulfide/sulphur composite photo-catalyst according to claim 1, feature exist
In：Step makes to be washed with deionized in (3), the dry 6-24h at 50 DEG C -80 DEG C.
9. a kind of cadmium sulfide/sulphur composite photo-catalyst, it is characterised in that：The cadmium sulfide/sulphur composite photo-catalyst is according to right
It is required that any one of 1-8 is prepared.
10. a kind of cadmium sulfide/application of the sulphur composite photo-catalyst in terms of photocatalysis prepares hydrogen described in claim 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810227790.5A CN108273520A (en) | 2018-03-20 | 2018-03-20 | A kind of cadmium sulfide/sulphur composite photo-catalyst and the preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810227790.5A CN108273520A (en) | 2018-03-20 | 2018-03-20 | A kind of cadmium sulfide/sulphur composite photo-catalyst and the preparation method and application thereof |
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| CN108273520A true CN108273520A (en) | 2018-07-13 |
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| CN201810227790.5A Pending CN108273520A (en) | 2018-03-20 | 2018-03-20 | A kind of cadmium sulfide/sulphur composite photo-catalyst and the preparation method and application thereof |
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| CN (1) | CN108273520A (en) |
Cited By (2)
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|---|---|---|---|---|
| CN112439429A (en) * | 2020-11-27 | 2021-03-05 | 华南师范大学 | Cadmium sulfide particles with cage-shaped structure and preparation method and application thereof |
| CN114989425A (en) * | 2022-05-31 | 2022-09-02 | 华南师范大学 | Photochemical preparation method and application of lamellar polyaniline |
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2018
- 2018-03-20 CN CN201810227790.5A patent/CN108273520A/en active Pending
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112439429A (en) * | 2020-11-27 | 2021-03-05 | 华南师范大学 | Cadmium sulfide particles with cage-shaped structure and preparation method and application thereof |
| CN112439429B (en) * | 2020-11-27 | 2022-10-04 | 华南师范大学 | Cadmium sulfide particles with cage-shaped structure and preparation method and application thereof |
| CN114989425A (en) * | 2022-05-31 | 2022-09-02 | 华南师范大学 | Photochemical preparation method and application of lamellar polyaniline |
| CN114989425B (en) * | 2022-05-31 | 2023-12-19 | 华南师范大学 | Photochemical preparation method and application of lamellar polyaniline |
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Application publication date: 20180713 |
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