CN106824228B - A kind of flower-shaped cobalt sulfide photochemical catalyst and preparation method thereof - Google Patents
A kind of flower-shaped cobalt sulfide photochemical catalyst and preparation method thereof Download PDFInfo
- Publication number
- CN106824228B CN106824228B CN201710170526.8A CN201710170526A CN106824228B CN 106824228 B CN106824228 B CN 106824228B CN 201710170526 A CN201710170526 A CN 201710170526A CN 106824228 B CN106824228 B CN 106824228B
- Authority
- CN
- China
- Prior art keywords
- flower
- photochemical catalyst
- cobalt sulfide
- preparation
- shaped cobalt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 39
- INPLXZPZQSLHBR-UHFFFAOYSA-N cobalt(2+);sulfide Chemical compound [S-2].[Co+2] INPLXZPZQSLHBR-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 229940011182 cobalt acetate Drugs 0.000 claims description 9
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 9
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 7
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 7
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 7
- 239000005864 Sulphur Substances 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 3
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 2
- PMUIBVMKQVKHBE-UHFFFAOYSA-N [S].NC(N)=O Chemical group [S].NC(N)=O PMUIBVMKQVKHBE-UHFFFAOYSA-N 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 16
- 239000002994 raw material Substances 0.000 abstract description 2
- 150000001868 cobalt Chemical class 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 229910052717 sulfur Inorganic materials 0.000 abstract 1
- 239000011593 sulfur Substances 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 11
- 229910052739 hydrogen Inorganic materials 0.000 description 11
- 239000001257 hydrogen Substances 0.000 description 11
- 239000011941 photocatalyst Substances 0.000 description 11
- 229910000510 noble metal Inorganic materials 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical group NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 7
- 239000006185 dispersion Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 239000010953 base metal Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 229960001124 trientine Drugs 0.000 description 1
- 238000004073 vulcanization Methods 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
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
It is to be made using inorganic cobalt salt and sulfur-containing compound as raw material through simple hydro-thermal reaction the invention discloses a kind of flower-shaped cobalt sulfide photochemical catalyst and preparation method thereof.Preparation method of the invention has the characteristics that simple, efficient, environmentally friendly, controllable, low in cost, the prepared flower-like structure cobalt sulfide stability height come out, large specific surface area, photocatalytic activity height.
Description
Technical field
The invention belongs to catalyst preparation technical fields, in particular to a kind of to prepare efficient base metal transition elements vulcanization
The method of object light catalyst.
Background technique
Currently, global energy supply depends on limited and non-renewable fossil fuel, such as coal, petroleum and day
Right gas etc..However the burning of fossil fuel brings a series of environmental problem, the continuous deterioration of environment leads to biological existence ring
Border is increasingly harsh, therefore readjusting the energy structure is the vital task of current mankind, explores and becomes scientist using new energy
Urgent need to resolve the problem of.
Solar energy is referred to as " technology of 21 century dream " as a kind of green, pollution-free and sufficient energy, its utilization.
Solar use is classified as the important content of " National Program for Medium-to Long-term Scientific and Technological Development (2006-2020) " by China
One of.Be using the advantages of solar energy: energy reserves is sufficient, it is estimated that the total storage of solar energy can maintain over ten billion year；Nothing
Pollution, is to be completely environmentally friendly；Solar energy is taken conveniently, and it is a kind of global-type energy that light radiation range, which covers the whole world,
There is no territory restrictions.
Photocatalysis technology is the new technology that chemical energy is converted solar energy into the help of photochemical catalyst, that is, utilizes the sun
It can be H by water decomposition2, by CO2Carbon monoxide, methane and methanol etc. are transformed into, organic matter is decomposed into pollution-free substance.It is existing
Stage common photochemical catalyst is the noble metals based photocatalysts such as golden (Au), platinum (Pt), although these photochemical catalysts are with higher
Activity, but by it is expensive, shortage of resources is limited, noble metal based photocatalyst can not widespread adoption.Phase
For noble metal based photocatalyst, the non-noble metal j elements such as nickel (Ni), iron (Fe) and cobalt (Co) rich reserves, valence on earth
Lattice are cheap, are very suitable to large-scale industrial application, but the application in photocatalysis field is considerably less, for base metal base light
The research of catalyst is still insufficient.If can be obtained in terms of the base metals based photocatalyst preparation such as efficient nickel, iron, cobalt prominent
It is broken, it will huge impetus is played to the development of photocatalysis field.
Summary of the invention
To solve above-mentioned existing deficiencies in the technology, the present invention provides a kind of flower-shaped cobalt sulfide photochemical catalysts
Preparation method, it is intended to efficient base metal transition elements sulfide photocatalyst is made using hydro-thermal method.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of preparation method of flower-shaped cobalt sulfide photochemical catalyst, includes the following steps:
(1) cobalt acetate and sulphur source are uniformly mixed in the in the mixed solvent being made of organic amine and hydrazine hydrate, and sufficiently stirred
It mixes to dissolution, obtains mixed reaction solution；
(2) by the mixed reaction solution, hydro-thermal reaction for 24 hours, is centrifuged products therefrom, is washed under the conditions of 100-200 DEG C
It washs and dries, that is, obtain flower-shaped cobalt sulfide photochemical catalyst.
Wherein:
The sulphur source is thiocarbamide, thioacetamide or vulcanized sodium.
The molar ratio of cobalt acetate and sulphur source is 1:0.5-5 in step (1).
The organic amine is diethylenetriamine, triethylene tetramine or tetraethylenepentamine.
The beneficial effects of the present invention are embodied in:
1, preparation method of the invention is compared with the traditional method with the obvious advantage: conventional method need to use high-temperature roasting, roasting
Temperature is greater than 400 DEG C, this be easy to cause catalyst agglomeration, and leads to catalyst dispersity difference and crystal defect, urges to reduce
The photocatalysis performance of agent；And the preparation method is that carry out hydro-thermal reaction in the range of 100-200 DEG C, reaction temperature
It is low, do not need high-temperature roasting, and it is easy to operate, low energy consumption.Photochemical catalyst good dispersion prepared by the present invention, crystal be perfect,
Photocatalytic activity is high, photocatalysis is stablized, suitable for mass production.
2, raw material of the present invention is non-precious metal salt, cheap, resourceful, be widely used.
3, the base metal photochemical catalyst good dispersion prepared by the present invention, crystal are perfect, photocatalytic activity is high, photocatalysis
Stability is good, suitable for mass production.
Detailed description of the invention
Fig. 1 is the electron scanning micrograph of the 1 flower-shaped cobalt sulfide of gained of embodiment；
Fig. 2 is the X-ray diffraction spectrogram (XRD) of the 1 flower-shaped cobalt sulfide of gained of embodiment；
Fig. 3 is activity of the 1 flower-shaped cobalt sulfide of gained of embodiment in photocatalytic water splitting reaction.
Specific embodiment
It elaborates with reference to the accompanying drawing to the embodiment of the present invention, following embodiments are being with technical solution of the present invention
Under the premise of implemented, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to
Following embodiments.
Agents useful for same is purchased from Sinopharm Chemical Reagent Co., Ltd. in following embodiments.
Embodiment 1
The present embodiment is prepared as follows flower-shaped cobalt sulfide photochemical catalyst:
It successively weighs 249.08mg cobalt acetate and 38.06mg thiocarbamide is placed in 4mL hydrazine hydrate, be uniformly mixed and sufficiently molten
Then solution is added 36mL diethylenetriamine, after being uniformly mixed, resulting dark solution is added to the polytetrafluoroethyl-ne of 50mL
In alkene reaction kettle, reaction kettle is placed in 180 DEG C of baking ovens hydro-thermal reaction 24 hours, subsequent cooled to room temperature, and to product
It is centrifuged, washed and dried, that is, obtain flower-shaped cobalt sulfide photochemical catalyst.
Fig. 1 and Fig. 2 is respectively the electron scanning micrograph and X-ray diffraction spectrogram of product.It will be seen from figure 1 that
The catalyst is in a kind of flower-like structure, is made of 2-3 μm of micron chip；It is clearly visible from Fig. 2, the catalyst spectrogram is not
There is apparent diffraction maximum in place, is amorphous state.
The flower-shaped cobalt sulfide photochemical catalyst sample of the present embodiment is used in photocatalytic water splitting to produce in hydrogen reaction, while with expensive
Metal based photocatalyst Pt as a comparison, to test its catalytic performance, method particularly includes: by 10mg sample and 20mg CdS quantum
Point combines, and 10mL lactic acid is added as sacrifice agent, 90mL deionized water as solvent and catalysis substrate.After tested, sample
Hydrogen output is as shown in figure 3, as can be seen from the figure the flower-shaped cobalt sulfide photochemical catalyst sample of the present embodiment has preferable photocatalysis
Activity.It is computed, the hydrogen-producing speed of the flower-shaped cobalt sulfide photochemical catalyst sample of the present embodiment is 1083.93 μm of ol/h, is much higher than
It uses noble metal based photocatalyst (about 326.6 μm of ol/h).
Embodiment 2
The present embodiment is prepared as follows flower-shaped cobalt sulfide photochemical catalyst:
It successively weighs 249.08mg cobalt acetate and 75.13mg thioacetamide is placed in 4mL hydrazine hydrate, be uniformly mixed and fill
Divide dissolution, 36mL diethylenetriamine is then added, after being uniformly mixed, resulting dark solution is added to poly- the four of 50mL
In vinyl fluoride reaction kettle, reaction kettle is placed in 180 DEG C of baking ovens hydro-thermal reaction 24 hours, subsequent cooled to room temperature, and right
Product is centrifuged, is washed and is dried, that is, obtains flower-shaped cobalt sulfide photochemical catalyst.
The pattern of sample obtained by the present embodiment is similar to Example 1, and pattern is uniform, good dispersion, crystal are perfect.
After tested, it is produced in hydrogen reaction in photocatalytic water splitting, the hydrogen-producing speed of the cobalt sulfide photochemical catalyst of the present embodiment is
730.5 μm of ol/h are higher than and use noble metal based photocatalyst (about 326.6 μm of ol/h).
Embodiment 3
The present embodiment is prepared as follows flower-shaped cobalt sulfide photochemical catalyst:
It successively weighs 249.08mg cobalt acetate and nine water vulcanized sodium of 240.18mg is placed in 4mL hydrazine hydrate, be uniformly mixed simultaneously
Then 36mL diethylenetriamine is added in sufficiently dissolution, after being uniformly mixed, resulting dark solution is added to the poly- of 50mL
In tetrafluoroethene reaction kettle, reaction kettle is placed in 180 DEG C of baking ovens hydro-thermal reaction 24 hours, subsequent cooled to room temperature, and
Product is centrifuged, washed and is dried, that is, obtains flower-shaped cobalt sulfide photochemical catalyst.
The pattern of sample obtained by the present embodiment is similar to Example 1, and uniform particle sizes, good dispersion, crystal are perfect.
After tested, it is produced in hydrogen reaction in photocatalytic water splitting, the hydrogen-producing speed of the cobalt sulfide photochemical catalyst of the present embodiment is
890.6 μm of ol/h are higher than and use noble metal based photocatalyst (about 326.6 μm of ol/h).
Embodiment 4
The present embodiment is prepared as follows flower-shaped cobalt sulfide photochemical catalyst:
It successively weighs 249.08mg cobalt acetate and 76.12mg thiocarbamide is placed in 4mL hydrazine hydrate, be uniformly mixed and sufficiently molten
Then solution is added 36mL diethylenetriamine, after being uniformly mixed, resulting dark solution is added to the polytetrafluoroethyl-ne of 50mL
In alkene reaction kettle, reaction kettle is placed in 180 DEG C of baking ovens hydro-thermal reaction 24 hours, subsequent cooled to room temperature, and to product
It is centrifuged, washed and dried, that is, obtain flower-shaped cobalt sulfide photochemical catalyst.
The pattern of sample obtained by the present embodiment is similar to Example 1, and pattern is uniform, good dispersion, crystal are perfect.
After tested, it is produced in hydrogen reaction in photocatalytic water splitting, the hydrogen-producing speed of the cobalt sulfide photochemical catalyst of the present embodiment is
927.25 μm of ol/h are higher than and use noble metal based photocatalyst (about 326.6 μm of ol/h).
Embodiment 5
The present embodiment is prepared as follows flower-shaped cobalt sulfide photochemical catalyst:
It successively weighs 249.08mg cobalt acetate and 15.22mg thiocarbamide is placed in 4mL hydrazine hydrate, be uniformly mixed and sufficiently molten
Then solution is added 36mL diethylenetriamine, after being uniformly mixed, resulting dark solution is added to the polytetrafluoroethyl-ne of 50mL
In alkene reaction kettle, reaction kettle is placed in 180 DEG C of baking ovens hydro-thermal reaction 24 hours, subsequent cooled to room temperature, and to product
It is centrifuged, washed and dried, that is, obtain flower-shaped cobalt sulfide photochemical catalyst.
The pattern of sample obtained by the present embodiment is similar to Example 1, and pattern is uniform, good dispersion, crystal are perfect.
After tested, it is produced in hydrogen reaction in photocatalytic water splitting, the hydrogen-producing speed of the cobalt sulfide photochemical catalyst of the present embodiment is
817.62 μm of ol/h are higher than and use noble metal based photocatalyst (about 326.6 μm of ol/h).
Claims (3)
1. a kind of preparation method of flower-shaped cobalt sulfide photochemical catalyst, which comprises the steps of:
(1) cobalt acetate and sulphur source are uniformly mixed in the in the mixed solvent being made of diethylenetriamine and hydrazine hydrate, and sufficiently stirred
It mixes to dissolution, obtains mixed reaction solution；Wherein, the molar ratio of cobalt acetate and sulphur source is 1:0.5-5；
(2) by the mixed reaction solution under the conditions of 100-200 DEG C hydro-thermal reaction for 24 hours, products therefrom is centrifuged, wash and
It is dry, that is, obtain flower-shaped cobalt sulfide photochemical catalyst.
2. the preparation method of flower-shaped cobalt sulfide photochemical catalyst according to claim 1, it is characterised in that: the sulphur source is sulphur
Urea, thioacetamide or vulcanized sodium.
3. flower-shaped cobalt sulfide photochemical catalyst obtained by preparation method described in a kind of any one of claim 1~2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710170526.8A CN106824228B (en) | 2017-03-21 | 2017-03-21 | A kind of flower-shaped cobalt sulfide photochemical catalyst and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710170526.8A CN106824228B (en) | 2017-03-21 | 2017-03-21 | A kind of flower-shaped cobalt sulfide photochemical catalyst and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106824228A CN106824228A (en) | 2017-06-13 |
| CN106824228B true CN106824228B (en) | 2019-06-18 |
Family
ID=59130098
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710170526.8A Active CN106824228B (en) | 2017-03-21 | 2017-03-21 | A kind of flower-shaped cobalt sulfide photochemical catalyst and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106824228B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109589990B (en) * | 2017-09-30 | 2022-02-11 | 中国科学院金属研究所 | Cobalt-based heterogeneous catalytic material and preparation method and application thereof |
| CN110404562A (en) * | 2018-04-27 | 2019-11-05 | 天津大学 | A kind of Co of richness defect3S4Ultra-thin porous nanometer sheet material and the preparation method and application thereof |
| CN109192951B (en) * | 2018-09-06 | 2021-03-09 | 中国科学技术大学 | Preparation method and application of nanometer flower-shaped spherical cobalt disulfide composite material |
| CN110400938A (en) * | 2019-07-30 | 2019-11-01 | 河南师范大学 | A kind of Co of porous surface club shaped structure3S4The preparation method of zinc and air cell catalyst |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000246110A (en) * | 1999-03-01 | 2000-09-12 | Agency Of Ind Science & Technol | Hydrogenation catalyst and its production |
| CN103214041A (en) * | 2013-03-01 | 2013-07-24 | 浙江理工大学 | Cobalt sulfide preparation method |
| CN104016419A (en) * | 2014-06-14 | 2014-09-03 | 哈尔滨工业大学 | Method for preparing three-dimensional flower-shaped CoS hierarchy counter electrode of dye-sensitized solar cell |
| CN104549374A (en) * | 2014-12-16 | 2015-04-29 | 中国科学院理化技术研究所 | Cadmium selenide flower-shaped microspheres prepared from nanosheets with hydrophilic surfaces as well as preparation method and application of microspheres |
| CN106099126A (en) * | 2016-06-11 | 2016-11-09 | 北京化工大学 | A kind of flower-like structure cobalt sulfide/carbon composite and preparation method thereof |
| CN106238072A (en) * | 2016-08-01 | 2016-12-21 | 湖南大学 | Cobalt sulfide photocatalyst and its preparation method and application |
-
2017
- 2017-03-21 CN CN201710170526.8A patent/CN106824228B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000246110A (en) * | 1999-03-01 | 2000-09-12 | Agency Of Ind Science & Technol | Hydrogenation catalyst and its production |
| CN103214041A (en) * | 2013-03-01 | 2013-07-24 | 浙江理工大学 | Cobalt sulfide preparation method |
| CN104016419A (en) * | 2014-06-14 | 2014-09-03 | 哈尔滨工业大学 | Method for preparing three-dimensional flower-shaped CoS hierarchy counter electrode of dye-sensitized solar cell |
| CN104549374A (en) * | 2014-12-16 | 2015-04-29 | 中国科学院理化技术研究所 | Cadmium selenide flower-shaped microspheres prepared from nanosheets with hydrophilic surfaces as well as preparation method and application of microspheres |
| CN106099126A (en) * | 2016-06-11 | 2016-11-09 | 北京化工大学 | A kind of flower-like structure cobalt sulfide/carbon composite and preparation method thereof |
| CN106238072A (en) * | 2016-08-01 | 2016-12-21 | 湖南大学 | Cobalt sulfide photocatalyst and its preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| "Architectural Control Syntheses of CdS and CdSe Nanoflowers, Branched Nanowires, and Nanotrees via a Solvothermal Approach in a Mixed Solution and Their Photocatalytic Property";Wei-Tang Yao et al.;《J. Phys. Chem. B》;20060527;第110卷;第11704-11710页 * |
| "In Situ Grown Pristine Cobalt Sulfide as Bifunctional Photocatalyst for Hydrogen and Oxygen Evolution";Min Zheng et al;《Adv. Funct. Mater.》;20170206;第27卷(第1605846期);第1-11页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106824228A (en) | 2017-06-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107649150B (en) | A kind of preparation method and applications of the Cd/CdS hetero-junctions visible light catalyst rich in sulphur vacancy | |
| CN106824228B (en) | A kind of flower-shaped cobalt sulfide photochemical catalyst and preparation method thereof | |
| Zhang et al. | Fabricating 1D/2D Co3O4/ZnIn2S4 core–shell heterostructures with boosted charge transfer for photocatalytic hydrogen production | |
| CN104324733B (en) | The preparation method of non precious metal high activity photolytic hydrogen production catalyst | |
| CN107321368B (en) | Au atom modified CoSe2Nanobelt and preparation method and application thereof | |
| CN102407147A (en) | Preparation method and application of ZnIn2S4-graphene composited photochemical catalyst | |
| CN109985666B (en) | Surface modified MoS2Application of catalyst in piezoelectric catalytic hydrogen production | |
| CN106807404B (en) | A kind of preparation method and applications of base metal base carbon coating nickel sulfide photochemical catalyst | |
| CN107486221B (en) | Copper sulfide photocatalyst and preparation method thereof | |
| Li et al. | MoC quantum dots modified by CeO2 dispersed in ultra-thin carbon films for efficient photocatalytic hydrogen evolution | |
| CN106362774A (en) | Preparation method for 1D/2D vertical Cds/MoS2 catalyst used for hydrogen production | |
| CN110227500A (en) | A kind of Cd1-xZnxS-Ni/MoS2Composite photo-catalyst and preparation method thereof, application | |
| CN108745382A (en) | A kind of preparation method and applications of the CdS visible light catalysts of NiCd double non-noble metals modification | |
| CN106622322A (en) | Two-dimensional nanosheet composite photocatalyst with bimetallic nanoparticles as heterojunction and preparation method thereof | |
| CN104959153A (en) | Auxiliary agent for photocatalytic production of hydrogen, and photocatalyst and preparation method and application thereof | |
| CN107321372B (en) | CoS nano particle/N doping RGO liberation of hydrogen composite material preparation method | |
| Wang et al. | Synthesis of Ni-silicate superficially modified CdS and its highly improved photocatalytic hydrogen production | |
| Fan et al. | Construction of 0D/2D Ni2P/Ni2P homophase Schottky junction by molten salt-assisted strategy for enhanced photocatalytic H2 evolution | |
| CN110116015B (en) | Photocatalyst for completely decomposing water, preparation method and application thereof, reaction method for completely decomposing water through photocatalysis and catalytic mixed solution | |
| Wang et al. | Dual-metal sites CuInS2/g-C3N4 Z-scheme heterojunction with efficient photocatalytic CO2 reduction selectivity | |
| Li et al. | ZIF‐67 derived hollow double‐shell core Co3O4 modified g‐C3N4 to construct p‐n heterojunction for efficient photocatalytic hydrogen evolution | |
| Feng et al. | Integrating carbon vacancy modified carbon quantum dots with carbon nitride for efficient photocatalytic CO2 reduction to syngas with tunable hydrogen to carbon monoxide ratio | |
| CN107185556B (en) | Preparation method of high-efficiency photocatalyst based on non-noble metal transition element sulfide | |
| Zhang et al. | Construction of graphdiyne (CnH2n-2) based Co-SP/CuI double S-scheme heterojunctions proved with in situ XPS characterization for efficient photocatalytic hydrogen production | |
| Liu et al. | Mechanochemical Synthesis of Pyrenyl Graphdiyne Coupling CdS/CeO2, Constructing a Ternary Photocatalyst toward Efficient Hydrogen Evolution |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |