CN104549500A - Method for preparing B-doped g-C3N4 photocatalyst through nonmetal liquid-phase doping - Google Patents
Method for preparing B-doped g-C3N4 photocatalyst through nonmetal liquid-phase doping Download PDFInfo
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- CN104549500A CN104549500A CN201410836957.XA CN201410836957A CN104549500A CN 104549500 A CN104549500 A CN 104549500A CN 201410836957 A CN201410836957 A CN 201410836957A CN 104549500 A CN104549500 A CN 104549500A
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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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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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- Y02P20/133—Renewable energy sources, e.g. sunlight
Abstract
The invention discloses a method for preparing a B-doped g-C3N4 photocatalyst through nonmetal liquid-phase doping, and belongs to the technical field of hydrogen production through photocatalytic materials. According to the prepared organic polymer semiconductor material g-C3N4 photocatalyst, cheap chemical material urea is taken as a reactant source, sodium tetraphenylborate is taken as a doping source, PEI (polyethyleneimine) is taken as a surface charge modifier, and the B-doped g-C3N4 photocatalyst is successively prepared with a pyrolysis and polymerization method easy to operate. The nonmetal liquid-phase doping modified g-C3N4 photocatalyst has novel organization structure appearance, good response of visible light with wavelength larger than 420 nm and good photocatalytic hydrogen generation property, and promotes solar energy conversion into new energy under the photocatalysis action at a low cost; the provided preparation method has the advantages of cheap raw materials, simple and convenient technology and the like and has an important research value and a wide industrialized application prospect.
Description
Technical field
The present invention relates to photocatalysis field, a kind of nonmetal liquid phase doping prepares B doping g-C
3n
4the method of photocatalyst, belongs to photocatalyst material and produces hydrogen technical field.
Background technology
Hydrogen Energy by becoming a kind of very important energy, is subject to the attention of various countries on 21 century energy stage.Utilize Hydrogen Energy to be the effective way solving energy problem of China and challenge, be also the important guarantee realizing China's Sustainable development simultaneously, have bright prospect in China.But hydrogen is secondary energy, the method preparing hydrogen is at present very many, and is the effective ways that both environmental protection is economic by solar photolysis water hydrogen.
In energy shortage and environmental pollution day by day serious today, exploitation Hydrogen Energy has very major and immediate significance.Each state has all dropped into substantial contribution and has solved future source of energy supply structure problem in scientific research, finds novel renewable energy source.Self-discovery TiO
2photoelectrochemistry energy water of decomposition produces H
2and O
2since, scientific researcher is being made unremitting efforts to for realizing solar photolysis water hydrogen always.But up to the present, the photocatalyst ubiquity photoelectric transformation efficiency that people develop is low, mostly only can absorb ultraviolet, and ultraviolet only accounts for about 3% in sunlight, and maximum sunlight intensity is at 500nm.Therefore the solution water catalyzer how formulating efficient absorption and conversion visible ray then becomes current theme in this research field, and how realizing the extensive hydrogen manufacturing of cheapness then becomes research emphasis from now on and ultimate aim.
Polymer semiconductor g-C
3n
4as a kind of novel nonmetal visible-light photocatalyst, because of its tool uniqueness, there is the laminate structure that is similar to graphite and conjugated electrons structure, high catalytic activity, chemistry and Heat stability is good, nontoxic and prepare simple and easy, the not feature such as containing metal, receive the concern of whole world researchist, there is boundless application prospect.But monomer g-C
3n
4electron-hole pair recombination rate is higher, causes its activity to be restricted, therefore by improving to the modification of photocatalyst the focus that photocatalytic activity becomes research.
Summary of the invention
The object of the invention is to for non-metallic element liquid phase B doping controllable g-C
3n
4appearance structure, improve mesoporous quantity, reduce the features such as the right recombination rate of photo-generate electron-hole, provide a kind of nonmetal liquid phase B doping and modification g-C by simple pyrolysis polyreaction
3n
4the preparation method of photocatalyst.The method production cost is low, and operating procedure is simple, and the catalyzer of preparation has good photocatalysis performance.
The B doping g-C that nonmetal liquid phase doping provided by the present invention is modified
3n
4photocatalyst calcines by urea the g-C obtained
3n
4in aqueous after positive electricity in surface charge modifying dose of PEI load, more fully adsorb with tetraphenyl boron anion, finally adopt the synthesis of pyrolysis polymerization process.
The nonmetal liquid phase doping of one provided by the present invention prepares B doping g-C
3n
4the method of photocatalyst, is characterized in that, comprises the following steps:
(1) by a certain amount of g-C
3n
4after being placed in the ultrasonic 0.5 ~ 2h of distilled water, continuing stirring 12 ~ 24h, make it fully mix, obtain g-C
3n
4suspension.
(2) a certain amount of polymine (Polyethyleneimine, PEI) is joined above-mentioned g-C
3n
4in suspension, stir 1 ~ 3h, centrifugal and after toppling over supernatant liquid, add the water of equivalent, and fully stir, obtain CNP solution.
(3) get above-mentioned CNP solution, the sodium tetraphenylborate solution configured dropwise instilled in above-mentioned got solution, and centrifugal after stirring 1 ~ 3h, by gained solid at the temperature of 60 ~ 80 DEG C dry 8 ~ 12 hours, both presoma.
(4) dried presoma grinding is evenly placed in crucible, be placed in retort furnace and calcine at air atmosphere, calcining temperature to be 500 DEG C ~ 520 DEG C temperature rise rates be 1 DEG C/min ~ 5 DEG C/min, be incubated naturally cooling after 4 hours, gained powder is nonmetal liquid phase doping and modifies the B doping g-C obtained
3n
4photocatalyst.
In step (1), described g-C
3n
4by urea, 550 DEG C of calcinings are obtained in atmosphere, and calcining temperature rise rate is 10 DEG C/min.Preferred m (g-C
3n
4): v (H
2o)=10mg:1ml.
In step (2), preferred m (g-C
3n
4): m (PEI)=10:1.
In step (3), the concentration of sodium tetraphenylborate solution is 1mg/ml, sodium tetraphenylborate solution: g-C
3n
4than being (20-110) ml:0.2g, preferred 70ml:0.2g.
The B doping g-C prepared according to the nonmetal liquid phase doping of the inventive method gained
3n
4photocatalyst.The g-C that nonmetal liquid phase doping prepared by the inventive method is modified
3n
4photocatalyst is used for photochemical catalysis sun power.
The present invention selects cheap industrial chemicals urea to be presoma, take sodium tetraphenylborate as doped source, with polymine (Polyethyleneimine, PEI) be surface charge modifying dose, adopt simple pyrolysis polymerization process, successfully prepared and there is visible light-responded (>420nm), the boron doped carboritride of organic polymer semiconductor material (the B-doped g-C that thermally-stabilised and chemical stability is superior
3n
4), with pure g-C
3n
4compare, this material has novel weave construction pattern (having more mesoporous quantity), and hydrogen manufacturing characteristic shows advantageous characteristic, under a small amount of promotor and sacrifice agent participate in, to obtain under solar light irradiation hydrogen-producing speed 4280 μm of olh faster
-1/ g, low cost realizes photochemical catalysis solar energy converting new forms of energy, has very high application prospect.
Liquid phase doping is better than solid phase mechanical doping, wherein passes through g-C
3n
4the modification of nonmetal liquid phase B doping and modification, mesoporous quantity can be improved, suppress g-C
3n
4light induced electron and the compound in hole, improve g-C
3n
4photocatalytic activity, these advantages make g-C
3n
4in the application great potential of photochemical catalysis and photodissociation hydrogen preparation field, simultaneously to g-C
3n
4industrial applications important in inhibiting.Therefore nonmetal liquid phase doping modification g-C
3n
4the preparation of photocatalyst has great importance.
Accompanying drawing illustrates:
The pure g-C of Fig. 1
3n
4and embodiment 2, example 4 product X-ray diffraction curve, wherein a is pure g-C
3n
4x-ray diffraction curve, b, c are respectively the X-ray diffraction curve of embodiment 2, example 4 product.
The pure g-C of Fig. 2
3n
4and the scanning electron microscope image of embodiment 3 product, wherein a, b, c are pure g-C
3n
4surface sweeping sem image, d, e, f are the scanning electron microscope image of embodiment 3 product.
The images of transmissive electron microscope of the CNPB-3 sample of preparation in Fig. 3 embodiment 3.
Fig. 4 embodiment (1 ~ 3) product infrared spectra curve, wherein a is the infrared spectra curve of embodiment 1 product, and b is the infrared spectra curve of embodiment 2 product, and c is the infrared spectra curve of embodiment 3 product.
The X-ray photoelectron spectroscopic analysis figure of Fig. 5 embodiment 3 product
The pure g-C of Fig. 6
3n
4and the fluorescence spectrum of embodiment 2,3 product under 400nm optical excitation.
The graphic representation of Fig. 7 embodiment (1 ~ 4) Photocatalyzed Hydrogen Production amount.
Fig. 8 embodiment (1 ~ 4) Photocatalyzed Hydrogen Production speed bar graph.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, but the present invention is not limited to following examples.
Embodiment 1:
Accurately take the g-C of 2g
3n
4after being placed in the ultrasonic 0.5h of distilled water of 200ml, continuing to stir 12h, make it fully mix, obtain g-C
3n
4suspension.The PEI accurately taking 0.2g joins above-mentioned g-C
3n
4in suspension, stir 1h, centrifugal and add a certain amount of water after toppling over supernatant liquid to 200ml, and fully stir, obtain CNP solution.Get the CNP solution of 20ml, the sodium tetraphenylborate solution of the 1mg/ml configured by 20ml dropwise instills in above-mentioned got solution, stirs after 1h centrifugal, by gained solid at the temperature of 60 DEG C dry 8 hours, both presoma.Dried presoma grinding be evenly placed in crucible, be placed in air atmosphere calcining in retort furnace, calcining temperature is 500 DEG C, and temperature rise rate is 5 DEG C/min, and be incubated naturally cooling after 4 hours, gained powder is the g-C of nonmetal liquid phase B doping and modification
3n
4photocatalyst, is designated as CNPB-1.Get this catalyzer 50mg, the deionized water of 90ml, the trolamine of 10ml (10vol.%) does sacrifice agent, 4mg Platinic chloride (Pt of 3wt.%) makes promotor, join altogether in reactor, use the 300WXe lamp carrying 420nm spectral filter as visible light source, adopt in the airtight glass circulation system for producing hydrogen of gas chromatography luxuriant and rich with fragrance Lay on the berth and carry out Photocatalyzed Hydrogen Production experiment, record hydrogen output curve as the CNPB-1 line in Fig. 7.
Embodiment 2:
Accurately take the g-C of 2g
3n
4after being placed in the ultrasonic 1h of distilled water of 200ml, continuing to stir 12h, make it fully mix, obtain g-C
3n
4suspension.The PEI accurately taking 0.2g joins above-mentioned g-C
3n
4in suspension, stir 2h, centrifugal and add a certain amount of water after toppling over supernatant liquid to 200ml, and fully stir, obtain CNP solution.Get the CNP solution of 20ml, the sodium tetraphenylborate solution of the 1mg/ml configured by 50ml dropwise instills in above-mentioned got solution, stirs after 2h centrifugal, by gained solid at the temperature of 60 DEG C dry 12 hours, both presoma.Dried presoma grinding be evenly placed in crucible, be placed in air atmosphere calcining in retort furnace stove, calcining temperature is 520 DEG C, and temperature rise rate is 1 DEG C/min, and be incubated naturally cooling after 4 hours, gained powder is the g-C of nonmetal liquid phase B doping and modification
3n
4photocatalyst, is designated as CNPB-2.Get this catalyzer 50mg, the deionized water of 90ml, the trolamine of 10ml (10vol.%) does sacrifice agent, 4mg Platinic chloride (Pt of 3wt.%) makes promotor, join altogether in reactor, use the 300WXe lamp carrying 420nm spectral filter as visible light source, adopt in the airtight glass circulation system for producing hydrogen of gas chromatography luxuriant and rich with fragrance Lay on the berth and carry out Photocatalyzed Hydrogen Production experiment, record hydrogen output curve as the CNPB-2 line in Fig. 7.
Embodiment 3:
Accurately take the g-C of 2g
3n
4after being placed in the ultrasonic 2h of distilled water of 200ml, continuing to stir 24h, make it fully mix, obtain g-C
3n
4suspension.The PEI accurately taking 0.2g joins above-mentioned g-C
3n
4in suspension, stir 3h, centrifugal and add a certain amount of water after toppling over supernatant liquid to 200ml, and fully stir, obtain CNP solution.Get the CNP solution of 20ml, the sodium tetraphenylborate solution of the 1mg/ml configured by 70ml dropwise instills in above-mentioned got solution, stirs after 2h centrifugal, by gained solid at the temperature of 80 DEG C dry 8 hours, both presoma.Dried presoma grinding be evenly placed in crucible, be placed in air atmosphere calcining in retort furnace stove, calcining temperature is 500 DEG C, and temperature rise rate is 1 DEG C/min, and be incubated naturally cooling after 4 hours, gained powder is the g-C of nonmetal liquid phase B doping and modification
3n
4photocatalyst, is designated as CNPB-3.Get this catalyzer 50mg, the deionized water of 90ml, the trolamine of 10ml (10vol.%) does sacrifice agent, 4mg Platinic chloride (Pt of 3wt.%) makes promotor, join altogether in reactor, use the 300WXe lamp carrying 420nm spectral filter as visible light source, adopt in the airtight glass circulation system for producing hydrogen of gas chromatography luxuriant and rich with fragrance Lay on the berth and carry out Photocatalyzed Hydrogen Production experiment, record hydrogen output curve as the CNPB-3 line in Fig. 7.
Embodiment 4:
Accurately take the g-C of 2g
3n
4after being placed in the ultrasonic 2h of distilled water of 200ml, continuing to stir 24h, make it fully mix, obtain g-C
3n
4suspension.The PEI accurately taking 0.2g joins above-mentioned g-C
3n
4in suspension, stir 3h, centrifugal and add a certain amount of water after toppling over supernatant liquid to 200ml, and fully stir, obtain CNP solution.Get the CNP solution of 20ml, the sodium tetraphenylborate solution of the 1mg/ml configured by 110ml dropwise instills in above-mentioned got solution, stirs after 3h centrifugal, by gained solid at the temperature of 80 DEG C dry 12 hours, both presoma.Dried presoma grinding be evenly placed in crucible, be placed in air atmosphere calcining in retort furnace stove, calcining temperature is 500 DEG C, and temperature rise rate is 5 DEG C/min, and be incubated naturally cooling after 4 hours, gained powder is the g-C of nonmetal liquid phase B doping and modification
3n
4photocatalyst, is designated as CNPB-4.Get this catalyzer 50mg, the deionized water of 90ml, the trolamine of 10ml (10vol.%) does sacrifice agent, 4mg Platinic chloride (Pt of 3wt.%) makes promotor, join altogether in reactor, use the 300WXe lamp carrying 420nm spectral filter as visible light source, adopt in the airtight glass circulation system for producing hydrogen of gas chromatography luxuriant and rich with fragrance Lay on the berth and carry out Photocatalyzed Hydrogen Production experiment, record hydrogen output curve as the CNPB-4 line in Fig. 7.
Note: CNUB-JX is sample as a comparison, for solid phase machinery B adulterates optimum sample
Table 1 is that CNPB-X sample specific surface area, pore volume and the hydrogen-producing speed prepared in embodiment compares.
Claims (7)
1. a nonmetal liquid phase doping prepares B doping g-C
3n
4the method of photocatalyst, is characterized in that, comprises the following steps:
(1) by a certain amount of g-C
3n
4after being placed in the ultrasonic 0.5 ~ 2h of distilled water, continuing stirring 12 ~ 24h, make it fully mix, obtain g-C
3n
4suspension;
(2) a certain amount of polymine (Polyethyleneimine, PEI) is joined above-mentioned g-C
3n
4in suspension, stir 1 ~ 3h, centrifugal and after toppling over supernatant liquid, add the water of equivalent, and fully stir, obtain CNP solution;
(3) get above-mentioned CNP solution, the sodium tetraphenylborate solution configured dropwise instilled in above-mentioned got solution, and centrifugal after stirring 1 ~ 3h, by gained solid at the temperature of 60 ~ 80 DEG C dry 8 ~ 12 hours, both presoma;
(4) dried presoma grinding is evenly placed in crucible, be placed in retort furnace and calcine at air atmosphere, calcining temperature to be 500 DEG C ~ 520 DEG C temperature rise rates be 1 DEG C/min ~ 5 DEG C/min, be incubated naturally cooling after 4 hours, gained powder is nonmetal liquid phase doping and modifies the B doping g-C obtained
3n
4photocatalyst.
2., according to the method for claim 1, it is characterized in that, in step (1), described g-C
3n
4by urea, 550 DEG C of calcinings are obtained in atmosphere, and calcining temperature rise rate is 10 DEG C/min.
3., according to the method for claim 1, it is characterized in that, in step (1), m (g-C
3n
4): v (H
2o)=10mg:1ml.
4., according to the method for claim 1, it is characterized in that, in step (2), m (g-C
3n
4): m (PEI)=10:1.
5. according to the method for claim 1, it is characterized in that, the concentration of sodium tetraphenylborate solution is 1mg/ml, sodium tetraphenylborate solution: g-C
3n
4than being (20-110) ml:0.2g.
6. according to the either method gained B doping g-C of claim 1-5
3n
4photocatalyst.
7. according to the either method gained B doping g-C of claim 1-5
3n
4photocatalyst be used for photocatalysis hydrogen production.
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| CN106629639A (en) * | 2016-12-03 | 2017-05-10 | 南昌大学 | Preparation method for boron-sulfur codoped graphene carbon nitride and application in detecting Hg<2+> |
| CN106732508A (en) * | 2016-12-26 | 2017-05-31 | 阜阳师范学院 | A kind of photochemical catalyst alkali metal CNB and preparation method thereof |
| CN106732710A (en) * | 2016-11-17 | 2017-05-31 | 阜阳师范学院 | A kind of metal oxide CNB composite photo-catalysts and preparation method thereof |
| CN106732736A (en) * | 2017-01-20 | 2017-05-31 | 济南大学 | One species tubulose boron doped graphite phase carbon nitride nano material and preparation method thereof |
| CN107029787A (en) * | 2017-05-24 | 2017-08-11 | 河海大学 | A kind of PEI carbonitride floats the preparation method of catalysis material |
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| CN110433844A (en) * | 2019-08-08 | 2019-11-12 | 盐城工学院 | One kind containing Cr for efficient process6+(B, O) the codope g-C of waste water3N4The preparation method of photochemical catalyst |
| CN110813345A (en) * | 2019-08-16 | 2020-02-21 | 济南大学 | Method for preparing novel carbon-nitrogen nonmetal photocatalyst by utilizing p/n junction principle |
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