CN108043439A - A kind of preparation method of cobalt sulfide/class graphene carbon nitrogen compound composite catalyst - Google Patents
A kind of preparation method of cobalt sulfide/class graphene carbon nitrogen compound composite catalyst Download PDFInfo
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- CN108043439A CN108043439A CN201711177642.9A CN201711177642A CN108043439A CN 108043439 A CN108043439 A CN 108043439A CN 201711177642 A CN201711177642 A CN 201711177642A CN 108043439 A CN108043439 A CN 108043439A
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- nitrogen compound
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- graphene carbon
- carbon nitrogen
- cobalt sulfide
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 39
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910017464 nitrogen compound Inorganic materials 0.000 title claims abstract description 38
- INPLXZPZQSLHBR-UHFFFAOYSA-N cobalt(2+);sulfide Chemical compound [S-2].[Co+2] INPLXZPZQSLHBR-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000003054 catalyst Substances 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 10
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims abstract description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000005864 Sulphur Substances 0.000 claims abstract description 3
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 3
- 239000010941 cobalt Substances 0.000 claims abstract description 3
- 229940011182 cobalt acetate Drugs 0.000 claims abstract description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052724 xenon Inorganic materials 0.000 claims description 7
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000005286 illumination Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 24
- 239000001257 hydrogen Substances 0.000 abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 24
- 238000004519 manufacturing process Methods 0.000 abstract description 15
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 239000010970 precious metal Substances 0.000 abstract description 2
- 238000002256 photodeposition Methods 0.000 abstract 1
- 239000003504 photosensitizing agent Substances 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical class OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 4
- 238000007872 degassing Methods 0.000 description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000001678 irradiating effect Effects 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 238000000151 deposition Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- -1 graphene carbon nitrogen compounds Chemical class 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- 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
- B01J27/24—Nitrogen compounds
-
- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- 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
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- 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
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
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- 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
- B01J35/396—Distribution of the active metal ingredient
- B01J35/399—Distribution of the active metal ingredient homogeneously throughout the support particle
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- 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
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
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- 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
- B01J37/349—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 flames, plasmas or lasers
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- 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
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- 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
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Abstract
The invention aims to alleviate the energy shortage of getting worse and problem of environmental pollution, cobalt sulfide without precious metal/class graphene carbon nitrogen compound composite catalyst is prepared for by mild Photodeposition in situ, for efficiently photocatalysis Decomposition aquatic products hydrogen.For the present invention using class graphene carbon nitrogen compound as photosensitizer, cobalt sulfide/class graphene carbon nitrogen compound composite catalyst is made as sulphur source as cobalt source, thiocarbamide in cobalt acetate.This preparation method is simple and efficient, low-carbon environment-friendly, of low cost, and the Photocatalyzed Hydrogen Production rate of catalyst is high.Thus, this cobalt sulfide/class graphene carbon nitrogen compound composite catalyst has good industrial applications prospect in Photocatalyzed Hydrogen Production field.
Description
Technical field
The present invention proposes a kind of easy preparation side of the cobalt sulfide of tufted/class graphene carbon nitrogen compound composite catalyst
Method belongs to materials science field and photocatalysis hydrogen production field.
Background technology
As energy dilemmas and problem of environmental pollution are increasingly serious, exploitation green regenerative energy sources have caused greatly
Concern.Hydrogen energy source has many advantages, such as fuel value height, product cleanliness without any pollution, renewable, can as the substitute of fossil energy, into
And help to mitigate environmental problem.Using sunlight hydrogen production by water decomposition under the effect of the catalyst, can convert solar energy into
Chemical energy (Hydrogen Energy), effectively stores solar energy, has very high researching value.Exploitation have good stability and
Photoactive photochemical catalyst is the key that photocatalysis hydrogen production field.
Class graphene carbon nitrogen compound (also known as g-C3N4) it is a kind of covalent compound being made of two kinds of carbon, nitrogen elements,
Thermal stability and chemical stability are good, and energy gap is relatively narrow, can absorb visible ray.And its raw material is cheap and easy to get, preparation side
Method is simple.However, pure g-C3N4In photocatalytic hydrogen production by water decomposition system, light induced electron and hole are easy to occur compound, production hydrogen
Activity is low.In g-C3N4Nanometer sheet area load composite nano metal sulfide particle can effectively inhibit the compound of photo-generated carrier,
So as to improve Photocatalyzed Hydrogen Production activity.
There is the cobalt sulfide of tufted prepared by the present invention/class graphene carbon nitrogen compound composite catalyst excellent light to urge
Change production hydrogen activity and stability.As far as we know, the light deposition method that this experiment uses is in g-C3N4Area load cobalt sulfide, still
Have no document report.
The content of the invention
The invention aims to alleviate the energy shortage of getting worse and problem of environmental pollution, pass through mild light in situ
Sedimentation is prepared for cobalt sulfide/class graphene carbon nitrogen compound composite catalyst of tufted without precious metal, for efficiently
Decomposing water with solar energy produces hydrogen.This preparation method is simple and efficient, low-carbon environment-friendly, of low cost, and the Photocatalyzed Hydrogen Production speed of catalyst
Rate is high, stability is good.
It is an object of the invention to provide a kind of letters of cobalt sulfide/class graphene carbon nitrogen compound composite catalyst of tufted
Just preparation method can be achieved through the following technical solutions：
(1) weigh appropriate thiocarbamide and be put into crucible and be capped, heated under 550 DEG C of air atmospheres 2 it is small when, heating rate 2
DEG C/min. will gained yellow powder grind after be put into the crucible not being capped, at 500 DEG C heat 2 it is small when, heating rate is still
Last for 2 DEG C/min., obtained pale yellow powder is that class graphene carbon nitrogen compound (and can be described as g-C3N4, it is nanometer sheet
Structure)；
(2) in the single necked round bottom flask of 25mL, a certain amount of class graphene carbon nitrogen compound is added in, cobalt acetate (as
Cobalt source) and thiocarbamide (as sulphur source), suitable quantity of water and ethyl alcohol are added, ultrasound makes its dispersion mixing uniform.It is passed through 40 minutes nitrogen
The oxygen in reaction system is removed, is subsequently placed under xenon lamp and carries out illumination；
(3) after reaction, solid is separated using centrifugation, is washed for several times with deionized water and ethyl alcohol, by obtained solid
It is put in vacuum drying chamber to be dried, it is that cobalt sulfide/class graphene carbon nitrogen compound is compound is urged to obtain grey black solid matter
Agent.
The remarkable advantage of the present invention is：g-C3N4It is a kind of light absorbent cheap and easy to get, nontoxic, stability is good, and has
There is suitable energy gap.Cobalt sulfide raw material sources enrich, cheap, can effectively facilitate the separation of photo-generated carrier；Make
Cobalt sulfide/class graphene carbon nitrogen compound composite catalyst of tufted is made with the method for light deposition, compared to other methods, this hair
Bright method is simple and efficient, and energy conservation and environmental protection.Cobalt sulfide nano particle is uniformly dispersed in g-C3N4In nanometer sheet, and size is very
It is small, it is about 2-3nm, the number of the active atomic exposed is more, and atom utilization is high, has excellent production hydrogen activity and stabilization
Property.
Description of the drawings
Fig. 1 is 1 gained class graphene carbon nitrogen compound of embodiment and cobalt sulfide/class graphene carbon nitrogen compound composite catalyzing
The transmission electron microscope picture of agent and high resolution TEM picture.
Fig. 2 is 1 gained class graphene carbon nitrogen compound of embodiment and cobalt sulfide/class graphene carbon nitrogen compound composite catalyzing
Agent Photocatalyzed Hydrogen Production performance map under natural sunlight.
Fig. 3 is 1 gained class graphene carbon nitrogen compound of embodiment and cobalt sulfide/class graphene carbon nitrogen compound composite catalyzing
The Photocatalyzed Hydrogen Production performance map of agent under visible light.
Specific embodiment
With reference to some examples and attached drawing, the present invention is described further, but the application of the present invention is without being limited thereto.
Embodiment 1
(1) 20g thiocarbamides weighed be put into crucible and be capped, heated under 550 DEG C of air atmospheres 2 it is small when, heating rate 2
DEG C/min. will gained yellow powder grind after be put into the crucible not being capped, at 500 DEG C heat 2 it is small when, heating rate is still
Last for 2 DEG C/min., obtained pale yellow powder is class graphene carbon nitrogen compound；
(2) in the single necked round bottom flask of 25mL, addition 20mg class graphene carbon nitrogen compounds, 12.5mg cobalt acetates,
38mg thiocarbamides, 4mL absolute ethyl alcohols, 6mL ultra-pure waters, being ultrasonically treated 5min makes its dispersion mixing uniform.40 minutes nitrogen is passed through to remove
Oxygen in dereaction system.
(3) flask is put under 300W xenon lamps, after irradiating 15min, solid is separated using centrifugation, is washed with deionized
Twice, ethyl alcohol washed once, and obtained solid is put in vacuum drying chamber, 80 DEG C are dried overnight, and obtain pale solid substance i.e.
For cobalt sulfide/class graphene carbon nitrogen compound composite catalyst.Prepared cobalt sulfide/class graphene carbon nitrogen compound is compound is urged
The mass percentage of cobalt sulfide is 0.88wt% in agent.
Embodiment 2
(1) the class graphene carbon nitrogen compound 20mg prepared in Example 1 is placed in the round-bottomed flask of 25mL, is added in
12.5mg cobalt acetates, 38mg thiocarbamides, 4mL absolute ethyl alcohols, 6mL ultra-pure waters, being ultrasonically treated 5min makes its dispersion mixing uniform.It is passed through
Nitrogen removes the oxygen in reaction system within 40 minutes.
(2) flask is put under 300W xenon lamps, after irradiating 10min, solid is separated using centrifugation, is washed with deionized
Twice, ethyl alcohol washed once, and obtained solid is put in vacuum drying chamber, 80 DEG C are dried overnight, and obtain pale solid substance i.e.
For cobalt sulfide/class graphene carbon nitrogen compound composite catalyst.Prepared cobalt sulfide/class graphene carbon nitrogen compound is compound is urged
The mass percentage of cobalt sulfide is 0.34wt% in agent.
Embodiment 3
(1) the class graphene carbon nitrogen compound 20mg prepared in Example 1 is placed in the round-bottomed flask of 25mL, is added in
12.5mg cobalt acetates, 38mg thiocarbamides, 4mL absolute ethyl alcohols, 6mL ultra-pure waters, being ultrasonically treated 5min makes its dispersion mixing uniform.It is passed through
Nitrogen removes the oxygen in reaction system within 40 minutes.
(2) flask is put under 300W xenon lamps, after irradiating 20min, solid is separated using centrifugation, is washed with deionized
Twice, ethyl alcohol washed once, and obtained solid is put in vacuum drying chamber, 80 DEG C are dried overnight, and obtain pale solid substance i.e.
For cobalt sulfide/class graphene carbon nitrogen compound composite catalyst.Prepared cobalt sulfide/class graphene carbon nitrogen compound is compound is urged
The mass percentage of cobalt sulfide is 1.10wt% in agent.
The cobalt sulfide prepared in Example 1/class graphene carbon nitrogen compound composite catalyst 5mg is placed in 25mL round bottoms burning
In bottle, 1mL triethanolamines (98%), 9mL water are added in；5min is ultrasonically treated, is removed with nitrogen degassing 40min in reaction system
Oxygen；Round-bottomed flask is put in 300W xenon lamps, illumination under 420nm optical filters, after reaction, with thermal conductivity-gas chromatograph
The hydrogen of detection reaction generation.React 2 it is small when hydrogen-producing speed be 721 μm of ol g-1 h-1。
The cobalt sulfide prepared in Example 1/class graphene carbon nitrogen compound composite catalyst 5mg is placed in 25mL round bottoms burning
In bottle, 1mL triethanolamines (98%), 9mL water are added in；5min is ultrasonically treated, is removed with nitrogen degassing 40min in reaction system
Oxygen；Round-bottomed flask is put under nature sunlight and irradiates 2h, hydrogen-producing speed has reached 1035.5 μm of ol g-1h-1(Fig. 2).
The cobalt sulfide prepared in Example 1/class graphene carbon nitrogen compound composite catalyst 5mg is placed in 25mL round bottoms burning
In bottle, 1mL triethanolamines (98%), 9mL water are added in；5min is ultrasonically treated, is removed with nitrogen degassing 40min in reaction system
Oxygen；Round-bottomed flask is put in 300W xenon lamps, illumination under 420nm optical filters.It is detected every 1 h thermal conductivity-gas chromatographs
The hydrogen of generation is reacted, the oxygen in once gas removing system is taken off every 4h, the triethanolamine of 1ml is added every 8h, it is 16 small
Shi Hou, the production hydrogen activity of catalyst do not significantly decrease (Fig. 3).
By the cobalt sulfide prepared by the present invention it can be seen from above-mentioned each example/class graphene carbon nitrogen compound composite catalyzing
Agent has many advantages, such as that synthetic method is simple, hydrogen-producing speed is high, stability is good, has industrialization well in Photocatalyzed Hydrogen Production field
Application prospect.
Claims (1)
1. a kind of preparation method being simple and efficient of cobalt sulfide/class graphene carbon nitrogen compound composite catalyst, it is characterised in that
It is carried out according to following scheme：
(1) weigh appropriate thiocarbamide and be put into crucible and be capped, heated under 550 DEG C of air atmospheres 2 it is small when, heating rate for 2 DEG C/
Min. it is put into after the yellow powder of gained is ground in the crucible not being capped, when heating 2 is small at 500 DEG C, heating rate is still 2
DEG C/min. is last, obtained pale yellow powder is that class graphene carbon nitrogen compound (and can be described as g-C3N4, it is nanometer sheet knot
Structure)；
(2) in the single necked round bottom flask of 25mL, a certain amount of class graphene carbon nitrogen compound, cobalt acetate are added in (as cobalt source)
With thiocarbamide (as sulphur source), suitable quantity of water and ethyl alcohol are added, ultrasound makes its dispersion mixing uniform.40 minutes nitrogen is passed through to remove instead
The oxygen in system is answered, is subsequently placed under xenon lamp and carries out illumination；
(3) after reaction, solid is separated using centrifugation, is washed for several times with deionized water and ethyl alcohol, obtained solid is put in
Vacuum drying chamber is dried, and it is cobalt sulfide/class graphene carbon nitrogen compound composite catalyst to obtain grey black solid matter.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110586160A (en) * | 2019-09-20 | 2019-12-20 | 济南大学 | Preparation method of cage-shaped cobalt sulfide/graphite phase carbon nitride composite photocatalyst |
| CN111199834A (en) * | 2020-01-08 | 2020-05-26 | 杭州电子科技大学 | Cobalt sulfide/multilayer graphene composite material and preparation method thereof |
| CN113731458A (en) * | 2020-05-29 | 2021-12-03 | 山东海科创新研究院有限公司 | Graphene/carbon nitride composite material and preparation method and application thereof |
| CN114758903A (en) * | 2022-04-14 | 2022-07-15 | 南京信息工程大学 | Preparation method of supercapacitor electrode material |
| CN115999584A (en) * | 2022-12-16 | 2023-04-25 | 广州大学 | Carbon-based-sulfide heterogeneous point compound and preparation method and application thereof |
| CN116673057A (en) * | 2023-06-08 | 2023-09-01 | 福州大学 | In-situ photo-deposition supported cobalt molybdenum polysulfide/carbon nitride composite catalyst |
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| CN111199834A (en) * | 2020-01-08 | 2020-05-26 | 杭州电子科技大学 | Cobalt sulfide/multilayer graphene composite material and preparation method thereof |
| CN113731458A (en) * | 2020-05-29 | 2021-12-03 | 山东海科创新研究院有限公司 | Graphene/carbon nitride composite material and preparation method and application thereof |
| CN114758903A (en) * | 2022-04-14 | 2022-07-15 | 南京信息工程大学 | Preparation method of supercapacitor electrode material |
| CN115999584A (en) * | 2022-12-16 | 2023-04-25 | 广州大学 | Carbon-based-sulfide heterogeneous point compound and preparation method and application thereof |
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