CN109806901A - A kind of hollow tubular g-C3N4Photochemical catalyst and preparation method and application - Google Patents
A kind of hollow tubular g-C3N4Photochemical catalyst and preparation method and application Download PDFInfo
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- CN109806901A CN109806901A CN201910141462.8A CN201910141462A CN109806901A CN 109806901 A CN109806901 A CN 109806901A CN 201910141462 A CN201910141462 A CN 201910141462A CN 109806901 A CN109806901 A CN 109806901A
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- 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
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Abstract
The present invention relates to photochemical catalysts, refer in particular to a kind of hollow tubular g-C3N4Photochemical catalyst and preparation method and application.Melamine is add to deionized water, stirs 5-10min at 80-90 DEG C of water-bath.In water-heat process, melamine decomposition can generate intermediate cyanuric acid, and cyanuric acid can be acted on melamine, be quickly generated poly cyanamid-cyanuric acid precursor.Then obtained solution is fitted into reaction kettle, at 170-190 DEG C, hydro-thermal 16-24h.Sample is obtained after centrifugation, washing, drying to be put into tube furnace, is passed through nitrogen, is warming up to 500-550 DEG C with the heating rate of 3-5 DEG C/min, and calcine 4h at 500-550 DEG C.By hydro-thermal, hydrone plays an important role, and by poly cyanamid-cyanuric acid precursor along longitudinal growth, by overcoming the direction of hydrogen bond, finally obtains hollow tubular carbonitride after calcining.
Description
Technical field
The present invention relates to photochemical catalysts, refer in particular to a kind of hollow tubular g-C3N4Photochemical catalyst and preparation method and application.It utilizes
Simple hydro-thermal and calcination method have synthesized hollow tubular graphite phase carbon nitride (mg-C3N4) photochemical catalyst, and will be prepared hollow
The g-C of tubulose3N4Photocatalyst applications decompose water hydrogen making under visible light.
Background technique
With the sustainable development of a large amount of consumption and modern industry of fossil fuel, energy shortage has become 21 century restriction
The main bugbear of mankind's socio-economic development.In addition, the huge pollution problem of combustion of fossil fuel bring brought to the mankind it is heavy
The disaster of weight.Therefore, angle long-range from human society, sustainable development, there is an urgent need to develop a kind of environment friend for we
Good, the reproducible green production that can be used in the energy and the technology for solving environmental problem.In numerous strategies of proposition, have
Economic, cleaning, it is safe and sustainable the advantages that photocatalysis technology be considered as solve energy shortage and environmental problem effective
Approach it-.In the presence of photochemical catalyst, photocatalysis technology solar energy can be converted into can directly utilize it is clear
Clean chemical energy source (hydrogen)；In addition to this, photocatalysis technology can also be by a kind of environmentally protective chemical process substantially effectively
It is nontoxic substance by the contaminant degradation in environment.
In recent years, nonmetallic polymer-class g-C3N4Since raw material is cheap, preparation is simple, by visible optical drive, (band gap is about
2.7eV), nontoxic, there are the series of advantages such as unique electronic band structure and excellent physical and chemical stability, obtained section
Boundary is ground widely to pay close attention to.In spite of the above plurality of advantages, for simple, unmodified g-C3N4For photochemical catalyst, advantage
Still it not can overcome the disadvantages that the fact that the separative efficiency of photo-generated carrier is lower in light-catalyzed reaction, lower separation of charge efficiency are straight
It connects and results in that its photocatalysis performance is low, far from the standard for reaching practical application.Therefore, it is necessary to single g-C3N4It carries out
Modification is modified, its photocatalysis efficiency and photochemical reaction stability is improved, to meet the needs of human society.And pass through
Change g-C3N4Pattern improve the approach that its photocatalysis performance is a kind of very simple and effective.So far people have prepared
The g-C of different morphologies3N4, such as thin layer, stub, ball.
Summary of the invention
The object of the present invention is to provide a kind of hollow tubular graphite phase carbon nitride (mg-C3N4) photochemical catalyst and its preparation side
Method, and its application for decomposing water hydrogen making under visible light has been investigated, by changing g-C3N4Pattern, make to be prepared
mg-C3N4Photochemical catalyst has higher light utilization efficiency, and has decomposition water under superior visible light to produce fuel hydrogen performance.
The present invention is to realize above-mentioned purpose by following technological means.
A kind of preparation method of hollow tubular graphite phase carbon nitride photochemical catalyst, includes the following steps:
Step S1: body phase g-C3N4(bg-C3N4) preparation
Melamine is put into tube furnace first, is passed through nitrogen, 500- is warming up to the heating rate of 3-5 DEG C/min
550 DEG C, and 4h is calcined at 500-550 DEG C.
Step S2: nanometer sheet g-C3N4(ug-C3N4) preparation
Melamine is add to deionized water, 0.5-1.0h is stirred.Then obtained solution is fitted into reaction kettle,
At 170-190 DEG C, hydro-thermal 20-24h.Centrifugation, washing, it is dry after obtain sample and be put into tube furnace, be passed through nitrogen, with 3-5 DEG C/
The heating rate of min is warming up to 500-550 DEG C, and calcines 4h at 500-550 DEG C.
Step S3: hollow tubular graphite phase carbon nitride (mg-C3N4) preparation
Melamine is add to deionized water, stirs 5-10min at 80-90 DEG C of water-bath.During water-bath, trimerization
Cyanamide, which decomposes, generates intermediate cyanuric acid, and cyanuric acid can be acted on melamine, before being quickly generated poly cyanamid-cyanuric acid
Body.Then obtained solution is fitted into reaction kettle, at 170-190 DEG C, hydro-thermal 16-24h passes through hydro-thermal reaction, hydrone
It plays an important role, it can by overcoming the direction of hydrogen bond along longitudinal growth by poly cyanamid-cyanuric acid precursor
Form tubular nanometer stick.After centrifugation, washing, drying, obtained sample is put into tube furnace, nitrogen is passed through, with 3-5 DEG C/min
Heating rate be warming up to 500-550 DEG C, and calcine 4h at 500-550 DEG C, obtain hollow tubular g-C3N4Photochemical catalyst.
Preferably, in step S1, the amount of melamine is 0.5g, and calcination temperature is 550 DEG C, and heating rate is 5 DEG C/min.
Preferably, in step S2, the mass ratio of melamine and deionized water is 0.5-1.0:20-30；Preferred amounts are
0.5:30, mixing time 1.0h, hydrothermal temperature are 180 DEG C, and when hydro-thermal is a length of for 24 hours.The calcination temperature of tube furnace is 550 DEG C,
Heating rate is 5 DEG C/min.
Preferably, in step S3, the mass ratio of melamine and deionized water is 0.5-1.0:20-30；Preferred amounts are
0.5:30, bath temperature are 90 DEG C, mixing time 10min, and hydrothermal temperature is 180 DEG C, and when hydro-thermal is a length of for 24 hours.Tube furnace
Calcination temperature is 550 DEG C, and heating rate is 5 DEG C/min.
Beneficial effects of the present invention
The advantage of the invention is that easy has synthesized mg-C3N4Catalysis material, and water is decomposed as photochemical catalyst
Hydrogen manufacturing has good photocatalysis performance.Mg-C provided by the present invention3N4Compared to traditional g-C3N4Specific surface area is bigger,
Available active site is more, so that the efficient photocatalytic activity of prepared photochemical catalyst is played, this method will not be made
At the wasting of resources, and it is easy to operate, cost is relatively low, is a kind of environmentally protective efficient process technology.
Detailed description of the invention
Fig. 1 a is the X-ray diffractogram of prepared catalyst, as can be seen from the figure mg-C3N4With ug-C3N4It is in 2 θ
13 ° of diffraction maximums and bg-C with 27 °3N4It fits like a glove, illustrates prepared catalyst consisting of g-C3N4.Fig. 1 b is made
The infrared absorption spectrum of standby catalyst, it can be seen from the figure that in 1800-1200cm-1In range, mg-C3N4、ug-C3N4With
bg-C3N4Absorption peak fit like a glove, also turn out that prepared catalyst is g-C3N4。
Fig. 2 a is bg-C3N4Scanning electron microscope (SEM) photograph, it can be seen that bg-C3N4Pattern be irregular particle.Fig. 2 b is
ug-C3N4Scanning electron microscope (SEM) photograph, it can be seen that ug-C3N4Pattern be thin layer nanometer sheet.Fig. 2 c is the presoma after hydro-thermal
Scanning electron microscope (SEM) photograph, it can be seen that cuboid stick made of the pattern thin slice accumulation of the presoma after hydro-thermal.Fig. 2 d, 2e mg-
C3N4- 16 scanning electron microscope (SEM) photograph and partial enlarged view, it can be seen that the piece of half curling is made of the curling sheet of multilayer.
Fig. 3 f is mg-C3N4- 24 scanning electron microscope (SEM) photograph, it can be seen that hollow tube is constituted by the thin slice of several layers.
Fig. 4 g-i is mg-C3N4-16、mg-C3N4-20、mg-C3N4- 24 scanning electron microscope (SEM) photograph, it can be seen that when with hydro-thermal
Between extension, by calcining after, sheet g-C3N4Gradually curl into the pattern of hollow tubular.
Fig. 5 a is 5 hours hydrogen output curves of prepared catalyst, as can be seen from the figure mg-C3N4- 24 in the same time
Hydrogen output highest, illustrate mg-C3N4- 24 performance is best.Fig. 5 b is to produce hydrogen reaction to prepared catalyst to carry out first order kinetics
The rate constant figure that fitting obtains is learned, as can be seen from the figure mg-C3N4- 24 rate constants are maximum, illustrate mg-C3N4- 24 production
Hydrogen rate is most fast, and photocatalysis performance is best.Fig. 5 c, 5d are mg-C3N4Quantum efficiency figure and wink under -24 different band logicals
State photocurrent response figure, the mg-C under as can be seen from the figure difference with is logical3N4- 24 quantum efficiency and transient photocurrents compares
It is lower, illustrate mg-C3N4- 24 photocatalysis performance is mainly due to its wider spectral absorption rather than the suction of single wavelength light
It receives.Fig. 5 e is mg-C3N4- 24 circulation hydrogen output figures, as can be seen from the figure after 5 cyclic tests, mg-C3N4- 24 hydrogen output
It does not significantly decrease, illustrates prepared mg-C3N4- 24 have preferable stability.Fig. 5 f is mg-C3N4Before -24 circulation experiments
X-ray diffractogram afterwards, as can be seen from the figure mg-C3N4The diffraction of -24 circulation front and backs does not change significantly, illustrates mg-
C3N4- 24 have preferable stability.
Fig. 6 a is the BET adsorption curve of prepared catalyst, as can be seen from the figure mg-C3N4- 24 there are micropore distributions.
The specific surface area data of Fig. 6 b prepared catalyst, it can be seen that mg-C3N4- 24 have biggish specific surface area, can provide compared with
More active sites, thus have preferable photocatalysis performance.
Fig. 7 a is mg-C3N4- 24 and bg-C3N4Steady-state fluorescence figure, as can be seen from the figure mg-C3N4- 24 fluorescence is strong
Degree is smaller, illustrates mg-C3N4The recombination rate in -24 light induced electron and hole is lower.Fig. 7 b is that the electrochemistry of prepared catalyst hinders
Anti- spectrum, as can be seen from the figure mg-C3N4- 24 radius is minimum, illustrates mg-C3N4- 24 impedance is minimum, carrier separation effect
Rate is best, and performance is best.
Specific embodiment
Embodiment 1
mg-C3N4The preparation of -16 photochemical catalysts:
0.5g melamine is added in the deionized water of 30mL, stirs 10min at 90 DEG C of water-bath.It will then obtain
Solution is fitted into reaction kettle, at 180 DEG C, hydro-thermal 16h.Sample is obtained after centrifugation, washing, drying to be put into tube furnace, is passed through nitrogen
Gas, calcines 4h at 550 DEG C, and heating rate is 5 DEG C/min.
Embodiment 2
mg-C3N4The preparation of -20 photochemical catalysts:
0.5g melamine is added in the deionized water of 30mL, stirs 10min at 90 DEG C of water-bath.It is then molten by what is obtained
Liquid is fitted into reaction kettle, at 180 DEG C, hydro-thermal 20h.Sample is obtained after centrifugation, washing, drying to be put into tube furnace, is passed through nitrogen,
4h is calcined at 550 DEG C, heating rate is 5 DEG C/min.
Embodiment 3
mg-C3N4The preparation of -24 photochemical catalysts:
0.5g melamine is added in the deionized water of 30mL, stirs 10min at 90 DEG C of water-bath.It is then molten by what is obtained
Liquid is fitted into reaction kettle, and at 180 DEG C, hydro-thermal is for 24 hours.Sample is obtained after centrifugation, washing, drying to be put into tube furnace, is passed through nitrogen,
4h is calcined at 550 DEG C, heating rate is 5 DEG C/min.
Embodiment 4
The experimentation of photocatalytic hydrogen production by water decomposition: it weighs 0.05g catalyst and is dispersed in 50mL solution, wherein 50mL is molten
It include 20% (10mL) triethanolamine, 3wt% (0.0015g) Pt in liquid.Before illumination, argon gas, purpose are passed through in reaction vessel
It is the air exhausted in reactor, avoids influence of the air to water generation hydrogen is decomposed.Every 1h, injected into gas-chromatography anti-
The hydrogen that should be generated, finally calculates hydrogen output.By the visible prepared mg-C of Fig. 5 a3N4- 24 photochemical catalysts can with excellent
Decompose in light water hydrogen production activity.
Claims (6)
1. a kind of hollow tubular g-C3N4The preparation method of photochemical catalyst, which is characterized in that specific step is as follows: by melamine
It is add to deionized water, stirring in water bath makes during water-bath, and melamine, which decomposes, generates intermediate cyanuric acid, trimerization
Cyanic acid can be acted on melamine, be quickly generated poly cyanamid-cyanuric acid precursor；Obtained solution is then packed into reaction kettle
In, hydro-thermal reaction, by hydro-thermal reaction, hydrone plays an important role, by poly cyanamid-cyanuric acid precursor along vertical
Tubular nanometer stick is capable of forming by overcoming the direction of hydrogen bond to growth；Centrifugation, washing, drying, obtained sample is put into
In tube furnace, it is passed through nitrogen, obtains hollow tubular g-C after heating calcining3N4Photochemical catalyst.
2. a kind of hollow tubular g-C as described in claim 13N4The preparation method of photochemical catalyst, which is characterized in that water-bath temperature
80-90 DEG C of degree, mixing time 5-10min；170-190 DEG C of hydrothermal temperature, reaction time 16-24h；Heating rate is
3-5 DEG C/min, calcination temperature is 500-550 DEG C, calcination time 4h.
3. a kind of hollow tubular g-C as claimed in claim 23N4The preparation method of photochemical catalyst, which is characterized in that water-bath temperature
Degree is 90 DEG C, mixing time 10min；Hydrothermal temperature is 180 DEG C, and the reaction time is for 24 hours；Calcination temperature is 550 DEG C, is risen
Warm rate is 5 DEG C/min.
4. a kind of hollow tubular g-C as described in claim 13N4The preparation method of photochemical catalyst, which is characterized in that melamine
Amine and the mass ratio of deionized water are 0.5-1.0:20-30.
5. a kind of hollow tubular g-C as claimed in claim 43N4The preparation method of photochemical catalyst, which is characterized in that melamine
Amine and the mass ratio of deionized water are 0.5:30.
6. the hollow tubular g-C of preparation method preparation as described in claim 13N4The purposes of photochemical catalyst, which is characterized in that use
In decomposition water hydrogen making under visible light.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110064430A (en) * | 2019-05-31 | 2019-07-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of sulfur doping hollow tubular carbonitride and products thereof and application |
| CN110170330A (en) * | 2019-05-31 | 2019-08-27 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method and products thereof and application of filiform carbonitride |
| CN110697667A (en) * | 2019-10-08 | 2020-01-17 | 河海大学 | Visible light responsive tubular g-C3N4Preparation method of (1) |
| CN110882714A (en) * | 2019-12-16 | 2020-03-17 | 吉林大学 | Curled carbon nitride thin sheet, preparation method and application thereof in hydrogen production through photocatalytic water decomposition |
| CN110947405A (en) * | 2019-11-08 | 2020-04-03 | 武汉科技大学 | Regularly arranged g-C3N4Nanotube catalyst and method for preparing the same |
| CN111085238A (en) * | 2020-01-10 | 2020-05-01 | 生态环境部华南环境科学研究所 | Hollow tubular graphite phase carbon nitride photocatalyst containing nitrogen defects and preparation method and application thereof |
| CN111470482A (en) * | 2020-04-07 | 2020-07-31 | 南方科技大学 | Multistage tubular carbon nitride and preparation method and application thereof |
| CN112023965A (en) * | 2020-07-30 | 2020-12-04 | 江苏大学 | Regulation and control g-C3N4Method for producing crystallinity |
| WO2021003520A1 (en) * | 2019-07-05 | 2021-01-14 | Newsouth Innovations Pty Limited | Hydrogen storage material |
| CN112675894A (en) * | 2021-01-04 | 2021-04-20 | 中国人民解放军陆军军医大学第二附属医院 | Hollow annular carbon nitride photocatalyst and preparation method thereof |
| CN113509949A (en) * | 2021-03-24 | 2021-10-19 | 大连工业大学 | Preparation of porous hollow carbon nitride nanotube photocatalyst and application of photocatalyst in synthesis of lactic acid by photocatalytic oxidation of xylose |
| CN114524420A (en) * | 2022-03-09 | 2022-05-24 | 重庆大学 | Preparation method of carbon nitride nanotube array |
| CN114558601A (en) * | 2022-01-20 | 2022-05-31 | 南京林业大学 | Donor-acceptor unit modified porous ultrathin g-C3N4Tubular photocatalyst and preparation method and application thereof |
| CN114632535A (en) * | 2022-03-31 | 2022-06-17 | 国家电投集团山西铝业有限公司 | Graphite-phase carbon nitride photocatalyst for sewage treatment and preparation method thereof |
| CN115301267A (en) * | 2021-09-08 | 2022-11-08 | 南京工业大学 | Porous tubular carbon nitride catalyst suitable for visible light catalysis and preparation method and application thereof |
| CN116212918A (en) * | 2022-12-28 | 2023-06-06 | 四川启睿克科技有限公司 | CABI@C 3 N 4 Heterojunction catalyst and preparation method and application thereof |
| CN116571265A (en) * | 2023-05-16 | 2023-08-11 | 长沙学院 | Boron-doped graphite-phase carbon nitride and preparation method and application thereof |
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| CN110064430A (en) * | 2019-05-31 | 2019-07-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of sulfur doping hollow tubular carbonitride and products thereof and application |
| CN110170330A (en) * | 2019-05-31 | 2019-08-27 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method and products thereof and application of filiform carbonitride |
| WO2021003520A1 (en) * | 2019-07-05 | 2021-01-14 | Newsouth Innovations Pty Limited | Hydrogen storage material |
| EP3994096A4 (en) * | 2019-07-05 | 2022-09-14 | NewSouth Innovations Pty Limited | Hydrogen storage material |
| CN113874319A (en) * | 2019-07-05 | 2021-12-31 | 新南创新私人有限公司 | Hydrogen storage material |
| CN110697667A (en) * | 2019-10-08 | 2020-01-17 | 河海大学 | Visible light responsive tubular g-C3N4Preparation method of (1) |
| CN110947405A (en) * | 2019-11-08 | 2020-04-03 | 武汉科技大学 | Regularly arranged g-C3N4Nanotube catalyst and method for preparing the same |
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| CN111085238A (en) * | 2020-01-10 | 2020-05-01 | 生态环境部华南环境科学研究所 | Hollow tubular graphite phase carbon nitride photocatalyst containing nitrogen defects and preparation method and application thereof |
| CN111470482A (en) * | 2020-04-07 | 2020-07-31 | 南方科技大学 | Multistage tubular carbon nitride and preparation method and application thereof |
| CN112023965A (en) * | 2020-07-30 | 2020-12-04 | 江苏大学 | Regulation and control g-C3N4Method for producing crystallinity |
| CN112023965B (en) * | 2020-07-30 | 2023-08-22 | 江苏大学 | Regulation and control g-C 3 N 4 Preparation method of crystallinity |
| CN112675894A (en) * | 2021-01-04 | 2021-04-20 | 中国人民解放军陆军军医大学第二附属医院 | Hollow annular carbon nitride photocatalyst and preparation method thereof |
| CN112675894B (en) * | 2021-01-04 | 2022-12-06 | 中国人民解放军陆军军医大学第二附属医院 | Hollow annular carbon nitride photocatalyst and preparation method thereof |
| CN113509949B (en) * | 2021-03-24 | 2023-08-11 | 大连工业大学 | Preparation of porous hollow carbon nitride nanotube photocatalyst and application of photocatalyst in synthesis of lactic acid by photocatalytic oxidation of xylose |
| CN113509949A (en) * | 2021-03-24 | 2021-10-19 | 大连工业大学 | Preparation of porous hollow carbon nitride nanotube photocatalyst and application of photocatalyst in synthesis of lactic acid by photocatalytic oxidation of xylose |
| CN115301267A (en) * | 2021-09-08 | 2022-11-08 | 南京工业大学 | Porous tubular carbon nitride catalyst suitable for visible light catalysis and preparation method and application thereof |
| CN114558601B (en) * | 2022-01-20 | 2023-10-24 | 南京林业大学 | Porous ultrathin g-C modified by donor-acceptor unit 3 N 4 Tube photocatalyst, preparation method and application thereof |
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| CN114524420A (en) * | 2022-03-09 | 2022-05-24 | 重庆大学 | Preparation method of carbon nitride nanotube array |
| CN114632535A (en) * | 2022-03-31 | 2022-06-17 | 国家电投集团山西铝业有限公司 | Graphite-phase carbon nitride photocatalyst for sewage treatment and preparation method thereof |
| CN116212918A (en) * | 2022-12-28 | 2023-06-06 | 四川启睿克科技有限公司 | CABI@C 3 N 4 Heterojunction catalyst and preparation method and application thereof |
| CN116212918B (en) * | 2022-12-28 | 2024-09-03 | 四川启睿克科技有限公司 | CABI@C3N4Heterojunction catalyst and preparation method and application thereof |
| CN116571265A (en) * | 2023-05-16 | 2023-08-11 | 长沙学院 | Boron-doped graphite-phase carbon nitride and preparation method and application thereof |
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Application publication date: 20190528 |