CN107352519B - A kind of C3N4The preparation method of nano wire - Google Patents
A kind of C3N4The preparation method of nano wire Download PDFInfo
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- 239000002070 nanowire Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003504 photosensitizing agent Substances 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000005119 centrifugation Methods 0.000 claims abstract description 6
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 229920000877 Melamine resin Polymers 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 6
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 4
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical group [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 4
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 4
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims description 3
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 2
- 239000012965 benzophenone Substances 0.000 claims description 2
- SURLGNKAQXKNSP-DBLYXWCISA-N chlorin Chemical compound C\1=C/2\N/C(=C\C3=N/C(=C\C=4NC(/C=C\5/C=CC/1=N/5)=CC=4)/C=C3)/CC\2 SURLGNKAQXKNSP-DBLYXWCISA-N 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- -1 cyanogen Amine Chemical class 0.000 claims 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- JMANVNJQNLATNU-UHFFFAOYSA-N glycolonitrile Natural products N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims 1
- 150000002475 indoles Chemical group 0.000 claims 1
- 229910001950 potassium oxide Inorganic materials 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 6
- 229960000907 methylthioninium chloride Drugs 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- MOFVSTNWEDAEEK-UHFFFAOYSA-M indocyanine green Chemical group [Na+].[O-]S(=O)(=O)CCCCN1C2=CC=C3C=CC=CC3=C2C(C)(C)C1=CC=CC=CC=CC1=[N+](CCCCS([O-])(=O)=O)C2=CC=C(C=CC=C3)C3=C2C1(C)C MOFVSTNWEDAEEK-UHFFFAOYSA-M 0.000 description 1
- 229960004657 indocyanine green Drugs 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of C3N4The preparation method of nano wire by rich nitrogen forerunner and salt or na oxide mixing high-temperature calcination, then is washed, is filtered, drying to get C is arrived3N4Nano wire.Photosensitizer and graphene powder can also be added into water, be protected from light ultrasonic vibration 30min~90min, then 2000 turns~2800 turns 12~20min of centrifugation in washing；System of the present invention is mixed using rich nitrogen forerunner and salt or oxide for the first time, is led to high-temperature calcination, washing method, is prepared C3N4Nano wire, preparation process is simple, and the reaction time is short, environmental friendly, reproducible, easy to industrialized production, prepared C3N4Nano wire has large specific surface area, and photocatalytic activity is up to 86.56%, and C3N4Nano wire pattern, dimensional homogeneity are preferable, reproducible.
Description
Technical field
The invention belongs to material preparation and photocatalysis technology field, and in particular to be a kind of C3N4The preparation side of nano wire
Method.
Background technique
Semiconductor light-catalyst has been a concern in the past few decades.It is obtained because it is widely used in direct hydrolysis
Obtain the environmental protection of renewable energy hydrogen and organic polluting water.
In numerous semiconductors, TiO2Since its nontoxic, inexpensive, high stability and excellent photo-catalysis capability become
Most study and most promising semiconductor material.But due to big (such as Detitanium-ore-type TiO of its energy gap23.2eV),
Can only be using the part ultraviolet light (UV) for accounting for sunlight 3%~4%, and quantum efficiency is low, to limit TiO2Application.
Therefore, the methods of doping, metal deposit and preparation of composite material are applied to TiO2Modification, with expectation improve its visible light
Photocatalytic activity.
In recent years, a kind of new function material-graphitic carbon nitride (g-C3N4) due to being moved with nonmetal character, high electronics
The characteristics of shifting rate, low band gap (2.73eV) and be caused extensive concern.g-C3N4With superior reducing power, photoresponse wave
Long reachable 450nm, is expanded to visible-range.But its oxidability ratio TiO2It is weak, in addition, electricity in the photocatalytic process
Son-hole further increases separation rate needs.
Summary of the invention
To solve graphitic carbon nitride (g-C of the existing technology3N4) oxidability ratio TiO2It is weak, in photocatalysis
The defect that electron-hole pair separation rate in journey needs to further increase, the present invention provide a kind of C3N4The preparation side of nano wire
Method.
A kind of C3N4The preparation method of nano wire, by rich nitrogen forerunner and salt or na oxide mixing high-temperature calcination, then wash,
Filtering is dried to get C is arrived3N4Nano wire.
Preferably, the rich nitrogen forerunner is any one or more of cyanamide, dicyandiamide and melamine etc..
Further, when washing, photosensitizer and graphene powder are added into water, be protected from light ultrasonic vibration 30min~
90min, then 2000 turns~2800 turns 12~20min of centrifugation.Preferred photosensitizer is indocyanine green, chlorin e 6 or is two
Benzophenone.
Further, the salt be sodium hydroxide, potassium hydroxide, sodium carbonate and sodium bicarbonate etc. any one or it is more
Kind.
Further, the na oxide is sodium oxide molybdena or/and sodium peroxide etc..
Further, the mass ratio of rich nitrogen forerunner and salt or na oxide is 0.01~10:0.01~10.
Further, it is 0.01~20 DEG C/min that the condition of high-temperature calcination, which is heating rate, and calcination temperature is 400~550
DEG C, calcination time is 0.5~4h.
The utility model has the advantages that the present invention is mixed using rich nitrogen forerunner and salt or oxide for the first time, lead to high-temperature calcination, washing method, system
Standby C out3N4Nano wire, preparation process is simple, and the reaction time is short, environmental friendly, reproducible, easy to industrialized production, prepared
C3N4Nano wire has large specific surface area, and photocatalytic activity is up to 86.56%, and C3N4Nano wire pattern, dimensional homogeneity
Preferably, reproducible.By the way that photosensitizer is added into water lotion, so that C3N4Nanowire supported a certain amount of photosensitizer, in laser
Irradiation under photosensitizer can by oxygen molecule effectively and rapidly be converted into singlet oxygen；The graphene powder in being protected from light ultrasonic vibration
But so that C3N4 nano wire is fluffy, spacing is ideal, greatly improves the yield of C3N4 nano wire.
Detailed description of the invention
Fig. 1 is the C of preparation3N4The SEM spectrum of nano wire.
Fig. 2 is the C of preparation3N4The XRD diffracting spectrum of nano wire.
Specific embodiment
Embodiment 1
By 5g melamine forerunner and 1g sodium hydroxide ground and mixed in crucible, it is placed in Muffle furnace with 5 DEG C/min liter
Temperature to 500 DEG C of calcining 2h, it is cold go after the deionized water of 10mL is added, refilter, wash, drying to get to C3N4Nano wire.
In order to examine C manufactured in the present embodiment3N4The photocatalysis performance of nano wire carries out photocatalytic degradation methylene to it
Blue test: light-catalyzed reaction carries out in cylindrical glass reactor, and using 300W xenon lamp as light source, light source is away from liquid level
20cm；Add magnetic agitation below reaction vessel, be sufficiently mixed solution, keeps concentration and temperature uniformity, catalyst C3N4
Nano wire dosage is 1g/L, methylene blue initial concentration is 20mg/L, and through detecting after 1h, the photocatalytic activity of methylene blue reaches
To 84.56%.
Embodiment 2
By 5g melamine forerunner and 5g potassium hydroxide ground and mixed in crucible, it is placed in Muffle furnace with 10 DEG C/min liter
Temperature to 520 DEG C of calcining 2.5h, it is cold go after the deionized water of 10mL is added, refilter, wash, drying to get to C3N4Nano wire,
The photocatalytic activity of methylene blue reaches 85.67%.
Embodiment 3
5g melamine forerunner and 2g sodium oxide molybdena are mixed in crucible, is placed in Muffle furnace and is warming up to 500 with 4 DEG C/min
DEG C calcining 2.5h, it is cold go after the deionized water of 10mL is added, refilter, wash, drying to get to C3N4Nano wire, methylene blue
Photocatalytic activity reach 86.56%.
Embodiment 4
5g melamine forerunner and 1.5g sodium carbonate are mixed in crucible, is placed in Muffle furnace and is warming up to 8 DEG C/min
510 DEG C of calcining 2h, it is cold go after the deionized water of 10mL is added, refilter and photosensitizer be added into water and graphene powder carries out water
It washes, is protected from light ultrasonic vibration 30min, then 2000 turns of centrifugation 20min dry to get C is arrived3N4Receive nano wire, the light of methylene blue is urged
Change degradation rate and reaches 83.21%.
Embodiment 5
1g cyanamide forerunner and 10g sodium peroxide are mixed in crucible, are placed in Muffle furnace with 0.01 DEG C/min heating
To 400 DEG C of calcining 4h, it is cold go after the deionized water of 10mL is added, refilter, photosensitizer 0.1mg and Graphene powder be added into water
3mg is washed at end, and ultrasonic vibration 90min is protected from light, and then 2800 turns of centrifugation 12min dry to get C is arrived3N4Receive nano wire, it is sub-
The photocatalytic activity of methyl blue reaches 81.29%.
Embodiment 6
2g dicyandiamide forerunner and 9g sodium oxide molybdena are mixed in crucible, is placed in Muffle furnace and is warming up to 550 with 20 DEG C/min
DEG C calcining 0.5h, it is cold go after the deionized water of 10mL is added, refilter, photosensitizer 0.05mg and graphene powder be added into water
5mg is washed, and ultrasonic vibration 60min is protected from light, and then 2400 turns of centrifugation 16min dry to get C is arrived3N4Nano wire, methylene
Blue photocatalytic activity reaches 84.93%.
Claims (6)
1. a kind of C3N4The preparation method of nano wire, which is characterized in that forge rich nitrogen forerunner and salt or na oxide mixing high temperature
It burns, then washes, filters, drying to get C is arrived3N4Nano wire；
When washing, photosensitizer and graphene powder are added into water, is protected from light ultrasonic vibration 30min~90min, then 2000 turns~
2800 turns of 12~20min of centrifugation.
2. C according to claim 13N4The preparation method of nano wire, it is characterised in that: the rich nitrogen forerunner is single cyanogen
Amine, dicyandiamide and melamine any one or more.
3. C according to claim 13N4The preparation method of nano wire, it is characterised in that: the photosensitizer is indoles cyanines
Green, chlorin e 6 is benzophenone.
4. C according to claim 13N4The preparation method of nano wire, it is characterised in that: the salt is sodium hydroxide, hydrogen
Potassium oxide, sodium carbonate and sodium bicarbonate any one or more；The na oxide is sodium oxide molybdena or/and sodium peroxide.
5. C according to claim 13N4The preparation method of nano wire, it is characterised in that: rich nitrogen forerunner and salt or sodium aoxidize
The mass ratio of object is 0.01~10:0.01~10.
6. C according to claim 1 or 53N4The preparation method of nano wire, it is characterised in that: the condition of high-temperature calcination is to rise
Warm rate is 0.01~20 DEG C/min, and calcination temperature is 400~550 DEG C, and calcination time is 0.5~4h.
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| CN109999874A (en) * | 2019-03-11 | 2019-07-12 | 江苏大学 | A kind of richness nitrogen azotized carbon nano pipe photochemical catalyst and preparation method and application |
| CN113418900A (en) * | 2021-07-16 | 2021-09-21 | 电子科技大学 | Synthesis method of molecular probe with ultrahigh specific surface area and ultrahigh fluorescence intensity |
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| CN103708430B (en) * | 2013-12-20 | 2015-04-08 | 武汉理工大学 | Preparation method for super-hard composite-phase carbon nitride nanowires |
| CN104801326A (en) * | 2015-03-25 | 2015-07-29 | 天津大学 | Surface-hydroxylated nano-pore carbon nitride photocatalytic material as well as preparation method and application thereof |
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Application publication date: 20171117 Assignee: Jiangsu Ningda environmental protection Co.,Ltd. Assignor: JIANGSU University OF TECHNOLOGY Contract record no.: X2023980054656 Denomination of invention: A method for preparing C3N4nanowires Granted publication date: 20190823 License type: Common License Record date: 20240103 |