CN107617443A - A kind of g C3N4The NiCoP nano particles of surface in situ growth, preparation method and applications - Google Patents

A kind of g C3N4The NiCoP nano particles of surface in situ growth, preparation method and applications Download PDF

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CN107617443A
CN107617443A CN201711038710.3A CN201711038710A CN107617443A CN 107617443 A CN107617443 A CN 107617443A CN 201711038710 A CN201711038710 A CN 201711038710A CN 107617443 A CN107617443 A CN 107617443A
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nano particles
situ growth
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谢腾峰
毕玲玲
孟德栋
王德军
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Jilin University
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    • 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

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Abstract

A kind of g C3N4NiCoP nano particles, preparation method and its application in photocatalytic hydrogen production by water decomposition of surface in situ growth, belong to photocatalytic hydrogen production by water decomposition technical field.It is to prepare g C first3N4Powder particle, then by the above-mentioned g C of 200~400mg3N4Powder particle, 10~30mL redistilled waters are added, 1~3h is stirred after 1~3h of ultrasound；10~150mg nickel sources, 10~150mg cobalt sources are added, 5~20min is stirred after 5~20min of ultrasound, 50~600mg phosphorus sources is added, 1~3h is stirred after 1~3h of ultrasound；Then dry under the conditions of 50~80 DEG C, be fully ground product after water completely volatilization；1~3h is calcined under the conditions of nitrogen atmosphere, 200~400 DEG C again；Redistilled water and ethanol centrifuge washing are finally used, centrifugation product dries 10~20h under vacuum, so as to obtain g C3N4The NiCoP nano particles of surface in situ growth.

Description

A kind of g-C3N4Surface in situ growth NiCoP nano particles, preparation method and its Using
Technical field
The invention belongs to photocatalytic hydrogen production by water decomposition technical field, and in particular to a kind of g-C3N4Surface in situ growth NiCoP nano particles, preparation method and its application in photocatalytic hydrogen production by water decomposition.
Background technology
In face of increasingly serious problem of environmental pollution and energy shortage problem, find replaceable new, pollution-free, environmentally friendly The type energy is our urgent problems.Clean energy resource Hydrogen Energy due to it is environmentally friendly, pollution-free, cleaning many advantages, such as and enjoy pass Note, can alleviate energy and environment problem to a certain extent.And photocatalytic hydrogen production by water decomposition is a kind of means of effectively hydrogen manufacturing.
For light-catalyzed reaction, select suitable photochemical catalyst particularly important.At present, semiconductor light-catalyst such as CdS, TiO2, ZnO etc. is widely studied and in photocatalytic hydrogen production by water decomposition field, shows excellent photocatalytic activity.However, due to system It is standby it is complicated, visible light utilization efficiency is low etc., and shortcoming makes it be restricted in the application.In recent years, graphite phase carbon nitride (g-C3N4) by In without metal, suitably lead valence band location, prepare simple, stable chemical property and macroscopic property, in photocatalysis field Research receives much concern.But due to the compound phenomenon of the serious photogenerated charge of body phase, simple g-C3N4Photolysis water hydrogen activity also It is less desirable.
Precious metals pt is good photocatalysis co-catalyst, can improve photogenerated charge separative efficiency first, is effectively suppressed Photogenerated charge it is compound, while Pt can reduce reaction overpotential and then be advantageous to the progress of evolving hydrogen reaction.But high valency Lattice and earth content is rare limits its large-scale application.Therefore, finding replaceable base metal co-catalyst turns into light The key issue of catalytic reaction.Transition metal (Fe, Co, Ni) base co-catalyst due to it is cheap, earth rich content is extensive Apply in photocatalysis and electrocatalytic decomposition wate research.
Compared to NiP and CoP, bimetallic base NiCoP can significantly reduce reaction overpotential, display more in electrochemistry Big current density, but, also research not in photochemical catalyzing seldom in optical electro-chemistry research.Tradition prepares phosphatization The method of thing is more complicated, and experiment preparation condition requires harsher, usually prepares in organic solvent and need to be organic Centrifuge washing in solvent.In addition, in order to prevent phosphide nanoparticle agglomerates phenomenon, prepare or preservation phosphide is generally required and added Entering surfactant prevents its reunion.Moreover, the phosphide prepared is mixed with major catalyst under mechanical stirring in document Together, due between two materials tight binding ability not enough and activity it is not good enough.We are using simple one-step method directly in g- C3N4Surface in situ grows NiCoP nano particles, effectively avoids NiCoP agglomeration traits.
The content of the invention
The purpose of the present invention is to overcome the preparation method that conventional phosphatizing thing is more complicated, experiment condition is harsher, a step Method is by NiCoP growth in situ in g-C3N4On, so as to provide a kind of simple easily preparation, inexpensive g-C3N4Surface in situ grows NiCoP nano particles, preparation method and its application in photocatalytic hydrogen production by water decomposition.
A kind of g-C of the present invention3N4The preparation method of the NiCoP nano particles of surface in situ growth, its step is such as Under：
(1) g-C is prepared3N4Powder particle：5~20g melamines are weighed, 1~3h is calcined under the conditions of 500~600 DEG C, Programming rate is 3~8 DEG C/min；After calcining end naturally cools to room temperature, product is ground to uniform powder；In order to obtain more Uniform powder particle, above-mentioned 300~600mg of sample is weighed, add 30~50mL redistilled waters, stirred again after 1~3h of ultrasound 10~20h is mixed, is then centrifuged for, centrifugation product is ground again after drying, and obtains g-C3N4Powder particle；
(2) g-C is prepared3N4NiCoP nano particles (the NiCoP/g-C of surface in situ growth3N4)：
1. weigh the above-mentioned g-C of 200~400mg3N4Powder particle, 10~30mL redistilled waters are added, after 1~3h of ultrasound Stir 1~3h；
2. 10~150mg nickel sources (NiCl is added in the solution 1. obtained to step2·6H2) and 10~150mg cobalt sources (Co O (NO3)2·6H2O), 5~20min is stirred after 5~20min of ultrasound, 50~600mg phosphorus sources are added after obtaining settled solution (NaH2PO2·3H2O), 1~3h is stirred after 1~3h of ultrasound；
3. 2. solution that step obtains is dried under the conditions of 50~80 DEG C, product is fully ground after water completely volatilization Mill；
4. 3. grinding product that step obtains is calcined into 1~3h, heating rate under the conditions of nitrogen atmosphere, 200~400 DEG C For 1~3 DEG C/min；
5. 4. calcined product that step is obtained is turned with redistilled water and ethanol with 8000~12000r/min respectively Fast centrifuge washing, centrifugation product dries 10~20h under vacuum, so as to obtain g-C3N4The NiCoP of surface in situ growth receives Rice grain.The material, such as simple g-C are named with the addition of nickel source3N4NiCoP0 is named as, adds 20mg nickel sources, life Entitled NiCoP20.
(3) photocatalytic hydrogen production by water decomposition is tested
Weigh g-C3N4NiCoP 5~20mg of nano particle of surface in situ growth, are added to 50~200mL triethanolamine water In solution (wherein, the volume fraction of triethanolamine is 5%~20%), 5~20min of ultrasonic agitation obtains homogeneous aaerosol solution, It is then added in 50~200mL light-catalyzed reactions pond (boiling flask for carrying quartz window), in order to obtain the environment of anaerobism, Light-catalyzed reaction pond is continuously passed through 20~50min of nitrogen before irradiation, ventilation rapidly seals reaction tank with plug after terminating；So Afterwards with 300~600W xenon lamp irradiations, 0.5~2h, caused hydrogen content gas chromatographic detection, wherein nitrogen is as carrier gas.
(4) XRD is characterized：X-ray diffractometer is primarily used to analyze g-C3N4The NiCoP nano particles of surface in situ growth Crystal structure and material composition.Scanning range is 10~70 °, and it is 5~20 °/min to sweep speed.Light source be Cu K α (20~100kV, 100~300mA).Correspondingly detect whether product is NiCoP according to NiCoP aspect cards.
5th, ESEM characterizes：ESEM is mainly used to observe g-C3N4The NiCoP nano particles of surface in situ growth Appearance structure.
The present invention prepares g-C using redistilled water using simple one-step method3N4The NiCoP nanometers of surface in situ growth Particle, preparation method is simple and convenient, overcomes tradition to add the complex operations of organic solvent, and NiCoP nano particle uniform loads exist g-C3N4Surface, its reunion is effectively prevented, show good photochemical catalyzing activity.
Brief description of the drawings
Fig. 1：Simple g-C3N4And g-C (NiCoP0)3N4Surface in situ growth different quality NiCoP (NiCoP20, NiCoP50, NiCoP100) nano particle XRD diffraction patterns.
Fig. 2：Simple g-C3N4And g-C (NiCoP0)3N4Surface in situ growth different quality NiCoP (NiCoP20, NiCoP50, NiCoP100) nano particle photocatalytic hydrogen production by water decomposition rate diagram.
Fig. 3：Simple g-C3N4And g-C (NiCoP0)3N4Surface in situ growth different quality NiCoP (NiCoP20, NiCoP50, NiCoP100) nano particle scanning electron microscope (SEM) photograph.
Embodiment
Embodiment 1
1st, g-C is prepared3N4：10g melamines are weighed, 2h is calcined under the conditions of 550 DEG C, programming rate is 5 DEG C/min；Treat After reaction naturally cools to room temperature, product is ground to uniform powder.In order to obtain powder particle evenly, above-mentioned sample is weighed Product 500mg, 40mL redistilled waters are added, 12h is stirred for after ultrasonic 2h, is then centrifuged for, centrifugation product is ground again after drying, and is obtained To g-C3N4。
2nd, NiCoP20 is prepared：
(1) the above-mentioned g-C of 300mg are weighed3N4, 20mL redistilled waters are added, then ultrasonic 2h stirs 12h；
(2) 20mg nickel sources (NiCl is added in the solution obtained to step (1)2·6H2) and 20mg cobalt sources (Co (NO O3)2· 6H2O), ultrasonic 10min and then stir 10min, obtain clarifying it is molten after add 100mg phosphorus sources (NaH2PO2·3H2O), ultrasonic 2h Then 2h is stirred；
(3) solution for obtaining step (2) dries 48h under the conditions of 60 DEG C, fully grinds product after water completely volatilization Mill；
(4) grinding product that step (3) obtains is calcined into 1h under the conditions of nitrogen atmosphere, 300 DEG C, heating rate is 2 DEG C/ min；
(5) calcined product for obtaining step (4) is centrifuged with redistilled water and ethanol with 9000r/min rotating speed respectively Washing, centrifugation product dries 12h under vacuum, so as to obtain g-C3N4The NiCoP nano particles of surface in situ growth, production Amount is about 270mg, is named as NiCoP20.
3rd, NiCoP20XRD is tested：X-ray diffractometer is primarily used to analyze NiCoP20 crystal structure and material group Into.Scanning range is 10-70 °, and it is 10 °/min to sweep speed.Light source be Cu K α (50kV, 200mA).Three main The angle of diffraction be located at 40.98 °, 44.84 ° and 47.4 °, correspond respectively to hexagonal wurtzite type NiCoP (JCPDS No.71- 2336) (111), (201) and (210) three crystal faces, it was demonstrated that NiCoP presence.
4th, NiCoP20 photocatalysis Decompositions aquatic products hydrogen is tested：NiCoP20 sample 10mg is weighed in 100mL beakers, is added The 100mL triethanolamine aqueous solution (wherein, triethanolamine volumes：Water volume=1：9), successively ultrasonic agitation 10min obtain it is homogeneous Aaerosol solution, it is then added in 100mL reaction tanks (the 100mL boiling flasks for carrying quartz window), in order to obtain anaerobism ring Border, is continuously passed through nitrogen half an hour before irradiation by light-catalyzed reaction pond, and ventilation rapidly seals reaction tank with plug after terminating. 500W xenon lamp irradiations 1h, caused hydrogen content gas chromatographic detection, wherein nitrogen is as carrier gas.NiCoP20 hydrogen-producing speeds For 476 μm of olh-1g-1。
5th, NiCoP20 ESEMs：It is mainly base material g-C in block structure3N4.The surface marked in figure has few Perhaps nano particle, it was demonstrated that NiCoP formation.
Embodiment 2
1st, g-C is prepared3N4：10g melamines are weighed, 2h is calcined under the conditions of 550 DEG C, programming rate is 5 DEG C/min；Treat After reaction naturally cools to room temperature, product is ground to uniform powder.In order to obtain powder particle evenly, above-mentioned sample is weighed Product 500mg, 40mL redistilled waters are added, 12h is stirred for after ultrasonic 2h, is then centrifuged for, centrifugation product is ground again after drying, and is obtained To g-C3N4。
2nd, NiCoP50 is prepared：
(1) the above-mentioned g-C of 300mg are weighed3N4, 20mL redistilled waters are added, then ultrasonic 2h stirs 12h；
(2) 50mg nickel sources (NiCl is added in the solution obtained to step (1)2·6H2) and 50mg cobalt sources (Co (NO O3)2· 6H2O), ultrasonic 10min and then stir 10min, obtain clarifying it is molten after add 250mg phosphorus sources (NaH2PO2·3H2O), ultrasonic 2h Then 2h is stirred；
(3) solution for obtaining step (2) dries 48h under the conditions of 60 DEG C, fully grinds product after water completely volatilization Mill；
(4) grinding product that step (3) obtains is calcined into 1h under the conditions of nitrogen atmosphere, 300 DEG C, heating rate is 2 DEG C/ min；
(5) calcined product for obtaining step (4) is centrifuged with redistilled water and ethanol with 9000r/min rotating speed respectively Washing, centrifugation product dries 12h under vacuum, so as to obtain g-C3N4The NiCoP nano particles of surface in situ growth, production Amount is about 300mg, is named as NiCoP50.
3rd, NiCoP50XRD is tested：X-ray diffractometer is primarily used to analyze NiCoP50 crystal structure and material group Into.Scanning range is 10~70 °, and it is 10 °/min to sweep speed.Light source be Cu K α (50kV, 200mA).The angle of diffraction Hexagonal wurtzite type NiCoP (JCPDS are corresponded respectively to positioned at 40.98 °, 44.84 °, 47.4 °, 54.28 °, 54.4 ° and 55.32 ° No.71-2336 (111), (201), (210), (300), (002) and (211) crystal face), it was demonstrated that NiCoP presence.
4th, NiCoP50 photocatalysis Decompositions aquatic products hydrogen is tested：NiCoP50 samples 10mg is weighed in 100mL beakers, is added The 100mL triethanolamines aqueous solution (triethanolamine volume：Water volume=1：9), successively ultrasonic agitation 10min obtain it is homogeneous suspend it is molten Liquid, it is then added in 100mL reaction tanks (the 100mL boiling flasks for carrying quartz window), in order to obtain the environment of anaerobism, shines Light-catalyzed reaction pond is continuously passed through nitrogen half an hour before light, ventilation rapidly seals reaction tank with plug after terminating.500W xenons Lamp irradiation 1h, caused hydrogen content gas chromatographic detection, wherein nitrogen is as carrier gas.NiCoP50 hydrogen-producing speeds are 1643 μ molh-1g-1。
5th, NiCoP50 ESEMs：It is mainly base material g-C in block structure3N4。g-C3N4Surface is uniform-distribution with 10nm or so nano particle, further prove NiCoP formation.
Embodiment 3
1st, g-C is prepared3N4：10g melamines are weighed, 2h is calcined under the conditions of 550 DEG C, programming rate is 5 DEG C/min；Treat After reaction naturally cools to room temperature, product is ground to uniform powder.In order to obtain powder particle evenly, above-mentioned sample is weighed Product 500mg, 40mL redistilled waters are added, 12h is stirred for after ultrasonic 2h, is then centrifuged for, centrifugation product is ground again after drying, and is obtained To g-C3N4。
2nd, NiCoP100 is prepared：
(1) the above-mentioned g-C of 300mg are weighed3N4, 20mL redistilled waters are added, then ultrasonic 2h stirs 12h；
(2) 100mg nickel sources (NiCl is added in the solution obtained to step (1)2·6H2) and 100mg cobalt sources (Co O (NO3)2·6H2O), ultrasonic 10min and then stir 10min, obtain clarifying it is molten after add 500mg phosphorus sources (NaH2PO2· 3H2O), then ultrasonic 2h stirs 2h；
(3) solution for obtaining step (2) dries 48h under the conditions of 60 DEG C, fully grinds product after water completely volatilization Mill；
(4) grinding product that step (3) obtains is calcined into 1h under the conditions of nitrogen atmosphere, 300 DEG C, heating rate is 2 DEG C/ min；
(5) calcined product for obtaining step (4) is centrifuged with redistilled water and ethanol with 9000r/min rotating speed respectively Washing, centrifugation product dries 12h under vacuum, so as to obtain g-C3N4The NiCoP nano particles of surface in situ growth, production Amount is about 400mg, is named as NiCoP100.
3rd, NiCoP100XRD is tested：X-ray diffractometer is primarily used to analyze NiCoP100 crystal structure and material group Into.Scanning range is 10-70 °, and it is 10 °/min to sweep speed.Light source be Cu K α (50kV, 200mA).Angle of diffraction position Hexagonal wurtzite type NiCoP (JCPDS are corresponded respectively in 40.98 °, 44.84 °, 47.4 °, 54.28 °, 54.4 ° and 55.32 ° No.71-2336 (111), (201), (210), (300), (002) and (211) crystal face), it was demonstrated that NiCoP presence.
4th, NiCoP100 photocatalysis Decompositions aquatic products hydrogen is tested：NiCoP100 samples 10mg is weighed in 100mL beakers, is added The 100mL triethanolamine aqueous solution (wherein, triethanolamine volumes：Water volume=1：9), successively ultrasonic agitation 10min obtain it is homogeneous Aaerosol solution, it is then added in 100mL reaction tanks (the 100mL boiling flasks for carrying quartz window), in order to obtain anaerobism Environment, is continuously passed through nitrogen half an hour before irradiation by light-catalyzed reaction pond, and ventilation rapidly seals reaction tank with plug after terminating. 500W xenon lamp irradiations 1h, caused hydrogen content gas chromatographic detection, wherein nitrogen is as carrier gas.NiCoP100 hydrogen-producing speeds For 819 μm of olh-1g-1。
5th, NiCoP100 ESEMs：It is mainly base material g-C in block structure3N4。g-C3N4Surface is uniform-distribution with 10nm or so nano particle, further prove NiCoP formation.

Claims (6)

  1. A kind of 1. g-C3N4The preparation method of the NiCoP nano particles of surface in situ growth, its step are as follows：
    (1) g-C is prepared3N4Powder particle
    5~20g melamines are weighed, 1~3h is calcined under the conditions of 500~600 DEG C；After calcining end naturally cools to room temperature, Product is ground to uniform powder；Above-mentioned 300~600mg of powder is weighed, adds 30~50mL redistilled waters, 1~3h of ultrasound After be stirred for 10~20h, be then centrifuged for, centrifugation product dry after grind again, obtain g-C3N4Powder particle；
    (2) g-C is prepared3N4The NiCoP nano particles of surface in situ growth
    1. weigh the above-mentioned g-C of 200~400mg3N4Powder particle, 10~30mL redistilled waters are added, 1 is stirred after 1~3h of ultrasound ~3h；
    2. adding 10~150mg nickel sources and 10~150mg cobalt sources in the solution 1. obtained to step, stirred after 5~20min of ultrasound 5~20min, 50~600mg phosphorus sources are added after obtaining settled solution, 1~3h is stirred after 1~3h of ultrasound；
    3. 2. solution that step obtains is dried under the conditions of 50~80 DEG C, product is fully ground after water completely volatilization；
    4. 3. grinding product that step obtains is calcined into 1~3h under the conditions of nitrogen atmosphere, 200~400 DEG C；
    5. 4. calcined product that step is obtained uses redistilled water and ethanol centrifuge washing respectively, centrifugation product is in vacuum condition 10~20h of lower drying, so as to obtain g-C3N4The NiCoP nano particles of surface in situ growth.
  2. A kind of 2. g-C as claimed in claim 13N4The preparation method of the NiCoP nano particles of surface in situ growth, its feature It is：Programming rate in step (1) is 3~8 DEG C/min.
  3. A kind of 3. g-C as claimed in claim 13N4The preparation method of the NiCoP nano particles of surface in situ growth, its feature It is：Step (2) 2. described in nickel source be NiCl2.6H2O, cobalt source are Co (NO3)2·6H2O, phosphorus source NaH2PO2·3H2O。
  4. A kind of 4. g-C as claimed in claim 13N4The preparation method of the NiCoP nano particles of surface in situ growth, its feature It is：Step (2) 4. described in heating rate be 1~3 DEG C/min.
  5. A kind of 5. g-C3N4The NiCoP nano particles of surface in situ growth, it is characterised in that：It is by Claims 1 to 4 any one Method described in is prepared.
  6. 6. the g-C described in claim 53N4The NiCoP nano particles of surface in situ growth answering in photocatalytic hydrogen production by water decomposition With.
CN201711038710.3A 2017-10-30 2017-10-30 A kind of g C3N4The NiCoP nano particles of surface in situ growth, preparation method and applications Pending CN107617443A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109746018A (en) * 2018-12-28 2019-05-14 西安交通大学 A kind of preparation method of the graphite phase carbon nitride photochemical catalyst of the phosphorus doping of metal phosphide modification
CN109759099A (en) * 2019-03-04 2019-05-17 河南城建学院 A kind of photochemical catalyst and preparation method thereof, application
CN111195526A (en) * 2018-11-16 2020-05-26 天津大学 Catalyst and application thereof in photocatalytic ammonia borane hydrolysis hydrogen production
CN113117718A (en) * 2021-03-29 2021-07-16 安徽建筑大学 NiCoP-g-C3N4/CdS composite photocatalyst, preparation method and application thereof
CN114768855A (en) * 2022-05-10 2022-07-22 安徽工业技术创新研究院 Heterojunction composite photocatalyst with atomic-level channel, preparation method and application
CN116459850A (en) * 2023-04-04 2023-07-21 常州大学 NiCoP/g-C for degrading tetracycline 3 N 4 Preparation method of composite photocatalyst

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LINGLING BI等: "Enhanced Photocatalytic Hydrogen Evolution of NiCoP/g-C3N4 with Improved Separation Efficiency and Charge Transfer Efficiency", 《CHEMSUSCHEM》 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111195526A (en) * 2018-11-16 2020-05-26 天津大学 Catalyst and application thereof in photocatalytic ammonia borane hydrolysis hydrogen production
CN111195526B (en) * 2018-11-16 2023-08-25 天津大学 Catalyst and application thereof in photocatalytic ammonia borane hydrolysis hydrogen production
CN109746018A (en) * 2018-12-28 2019-05-14 西安交通大学 A kind of preparation method of the graphite phase carbon nitride photochemical catalyst of the phosphorus doping of metal phosphide modification
CN109759099A (en) * 2019-03-04 2019-05-17 河南城建学院 A kind of photochemical catalyst and preparation method thereof, application
CN113117718A (en) * 2021-03-29 2021-07-16 安徽建筑大学 NiCoP-g-C3N4/CdS composite photocatalyst, preparation method and application thereof
CN113117718B (en) * 2021-03-29 2023-03-14 安徽建筑大学 NiCoP-g-C 3 N 4 CdS composite photocatalyst, preparation method and application thereof
CN114768855A (en) * 2022-05-10 2022-07-22 安徽工业技术创新研究院 Heterojunction composite photocatalyst with atomic-level channel, preparation method and application
CN114768855B (en) * 2022-05-10 2023-11-24 安徽工业技术创新研究院 Heterojunction composite photocatalyst with atomic-scale channel and preparation method and application thereof
CN116459850A (en) * 2023-04-04 2023-07-21 常州大学 NiCoP/g-C for degrading tetracycline 3 N 4 Preparation method of composite photocatalyst

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