CN106744743A - A kind of one-step synthesis water solubility g C3N4The preparation method of material - Google Patents
A kind of one-step synthesis water solubility g C3N4The preparation method of material Download PDFInfo
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- CN106744743A CN106744743A CN201611104012.4A CN201611104012A CN106744743A CN 106744743 A CN106744743 A CN 106744743A CN 201611104012 A CN201611104012 A CN 201611104012A CN 106744743 A CN106744743 A CN 106744743A
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- 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
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
A kind of one-step synthesis water solubility g C3N4The preparation method of material, belongs to materials synthesis and environmental monitoring.The method comprises the following steps：(1) one kind in melamine or dicyandiamide is well mixed with sodium chloride, potassium chloride and adds distilled water, water bath with thermostatic control stirring and dissolving is carried out at 60~90 DEG C；(2) step (1) solution is carried out into rotary evaporation treatment, 650~690 DEG C of calcinings are obtained in atmosphere after drying, and calcining heating rate is 2 DEG C/min~10 DEG C/min, obtains final product the water-soluble g C3N4Material；(3) by step (2) gained g C3N4Material is purified three times with isopropanol.The g C that the present invention is provided3N4Material has good water solubility and trace metal ion detection performance；The preparation method that the present invention is provided, its raw material is inexpensive, process is simple, with application prospect and practical value very high.
Description
Technical field
The present invention relates to a kind of one-step synthesis water solubility g-C3N4The preparation method of material, belongs to materials synthesis and environment prison
Survey field.
Background technology
C3N4Material is the class that pole attracts attention in new function material family, it is generally the case that g-C3N4Material be its most
The allotrope of stabilization.g-C3N4Material connects stacking by orderly triazine ring structure, forms the layer structure of graphite-like.g-
C3N4Material causes the great interest of researcher due to its characteristic of semiconductor, and it is in photocatalysis and photodissociation hydrogen preparation field
Using great potential.g-C3N4Electronic band structure and band gap depend on the extent of polymerization of material, and band gap can be with
It is adjusted by protonating technique or doping metals cation, just because metal cation can adjust band gap, from
And its photoluminescence property can be adjusted, it is g-C3N4Materials application is laid a good foundation in metal ion sensor field.
Optical pickocff belongs to molecular receptor, is bonded with it by other ions and changes its optical characteristics.Optics is passed
Sensing system has benefited from its high-sensitivity detection, quick detectability, biocompatibility and gentle testing conditions.Optics is passed
It is exactly for monitoring trace metal ion that sensor has a very important application.It is a large amount of poisonous, carcinogenic in industrial circle
Metal ion be directly discharged in environment, thus people need the angle from biological and environment to carry out these metal ions
Monitoring.Most of monitoring metal ion optical pickocff materials contain azo ring, porphyrin and face phenanthroline derivative.These points
The Lewis sites of sub- receptor surface can with metal ion formed it is extremely strong be bonded, electronics turns from the luminophore of receptor surface
Metal ion is moved on to, by the change of luminous intensity, qualitative, Semi-qualitative detection metal ion.In recent years, the development of mesoporous material
The performance of sensing material is improved, more fluorescence molecules are adsorbed so as to reach lower detection limit by increasing specific surface area.
By contrast, g-C3N4Material more has the prospect of application.Due to g-C3N4Electronic structure can by protonation and doping metals
Be adjusted, and by functional group chelate can more adsorbing metal ions, so as to there is metal ion detection higher
Sensitivity.
The content of the invention
It is an object of the invention to provide a kind of environmental protection, simple controllable water-soluble g-C3N4Material preparation method, this hair
Bright method is prepared using fused salt environment, can be with Effective Regulation g-C3N4The microcosmic thickness and surface potential of nanometer sheet, so as to ensure
Its good water solubility；G-C prepared by the method for the present invention3N4Material has good trace metal ion detection performance.
A kind of one-step synthesis water solubility g-C3N4The preparation method of material, comprises the following steps：
(1) one kind of melamine or dicyandiamide is well mixed with sodium chloride, potassium chloride and adds distilled water, 60~
90 DEG C carry out water bath with thermostatic control stirring；
(2) step (1) slurry is carried out into rotary evaporation treatment, 650~690 DEG C of calcinings in atmosphere, are incubated 1-4 after drying
Hour, calcining heating rate is 2 DEG C/min~10 DEG C/min, obtains final product the water-soluble g-C3N4Material；
(3) by step (2) gained g-C3N4Material is purified three times with isopropanol.
In step (1), the melamine or dicyandiamide and the mol ratio of sodium chloride, potassium chloride are 1：(0.5~4)：
(0.5~4), preferably 1:1:1.
In step (1), the water bath processing temperature is 60~90 DEG C, and preferably constant temperature time is 0.5~2 hour.
In step (2), calcining heat be 650~690 DEG C, preferably 670 DEG C, calcining heating rate for 2 DEG C/min~10 DEG C/
Min, preferably heating rate are 5 DEG C/min, and the soaking time of step (2) calcining is 2 hours.
The g-C that the present invention is provided3N4Material has good water solubility and trace metal ion detection performance, can be used for many
The detection of metal ion species absorbs, and is respectively provided with good effect；The preparation method that the present invention is provided, its raw material is inexpensive, work
Skill is simple, with application prospect and practical value very high.
Brief description of the drawings
Fig. 1 is g-C in embodiment 33N4The XRD spectra of sample；
Fig. 2 is the g-C of preparation in embodiment 33N4TEM figure；
Fig. 3 is g-C in embodiment 33N4The PL spectrograms of each metal ion species of sample detection；
Fig. 4 is g-C in embodiment 33N4Sample detection metal-ion fluorescent is quenched rate spectrogram；
Fig. 5 is the g-C prepared in embodiment 33N4Material tests various concentrations Fe3+PL spectrograms；
Fig. 6 is the g-C prepared in embodiment 33N4Material digital photograph；
Fig. 7 is the g-C prepared in embodiment 33N4Material water dissolution properties matter digital photograph.
Specific embodiment
With reference to embodiment, the present invention will be further described, but the present invention is not limited to following examples.
Experimental example 1：
Melamine 0.06mol is taken, it is dissolved in distilled water with 0.03mol NaCl, 0.03mol KCl, 60 DEG C of water
Bath stirring 0.5h, mixture then is transferred into eggplant type bottle carries out rotary evaporation treatment, and powder is placed in crucible after drying, and uses aluminium
Foil paper is tight by crucible parcel, is placed in Muffle furnace 650 DEG C of calcinings in air atmosphere, and heating rate is 2 DEG C/min, is incubated 2h
Natural cooling afterwards, gained powder is water-soluble g-C3N4Material, by gained g-C3N4Material is purified three times with isopropanol, is designated as
CNMS-1.Take Cd2+, Co2+, Cr3+, Cu2+, Fe2+, Ni2+, Zn2+, Hg2+, Pb2+, as metal ion target detection thing, take g-
C3N4Material (CNMS-1) 5mg is added in the metal ion solution that 5ml concentration is 1mM, stirs 0.5h, makes up to absorption flat
Weighing apparatus, after adsorption equilibrium process, solution is injected to be placed in XRF in four-way cuvette and tests its fluorescence intensity, according to formula
1- (C/C0) calculate its fluorescent quenching rate.Wherein C is the fluorescence intensity of solution after addition metal ion, C0It is original g-C3N4It is molten
The fluorescence intensity of liquid,.
Experimental example 2：
Melamine 0.06mol is taken, it is dissolved in distilled water with 0.045mol NaCl, 0.045mol KCl, 60 DEG C
Stirring in water bath 2h, mixture then is transferred into eggplant type bottle carries out rotary evaporation treatment, and powder is placed in crucible after drying, and uses aluminium
Foil paper is tight by crucible parcel, is placed in Muffle furnace 650 DEG C of calcinings in air atmosphere, and heating rate is 10 DEG C/min, insulation
Natural cooling after 2h, gained powder is water-soluble g-C3N4Material, by gained g-C3N4Material is purified three times with isopropanol, note
It is CNMS-2.Take Cd2+, Co2+, Cr3+, Cu2+, Fe2+, Ni2+, Zn2+, Hg2+, Pb2+, as metal ion target detection thing, take g-
C3N4Material (CNMS-2) 5mg is added in the metal ion solution that 5ml concentration is 1mM, stirs 0.5h, makes up to absorption flat
Weighing apparatus, after adsorption equilibrium process, solution is injected to be placed in XRF in four-way cuvette and tests its fluorescence intensity, according to formula
1- (C/C0) calculate its fluorescent quenching rate.Wherein C is the fluorescence intensity of solution after addition metal ion, C0It is original g-C3N4It is molten
The fluorescence intensity of liquid.
Experimental example 3：
Melamine 0.06mol is taken, it is dissolved in distilled water with 0.06mol NaCl, 0.06mol KCl, 80 DEG C of water
Bath stirring 1h, mixture then is transferred into eggplant type bottle carries out rotary evaporation treatment, and powder is placed in crucible after drying, and uses aluminium foil
Paper is tight by crucible parcel, is placed in Muffle furnace 670 DEG C of calcinings in air atmosphere, and heating rate is 5 DEG C/min, after insulation 2h
Natural cooling, gained powder is water-soluble g-C3N4Material, by gained g-C3N4Material is purified three times with isopropanol, is designated as
CNMS-3.Take Cd2+, Co2+, Cr3+, Cu2+, Fe2+, Ni2+, Zn2+, Hg2+, Pb2+, as metal ion target detection thing, take g-
C3N4Material (CNMS-3) 5mg is added in the metal ion solution that 5ml concentration is 1mM, stirs 0.5h, makes up to absorption flat
Weighing apparatus, after adsorption equilibrium process, solution is injected to be placed in XRF in four-way cuvette and tests its fluorescence intensity, according to formula
1- (C/C0) calculate its fluorescent quenching rate.Wherein C is the fluorescence intensity of solution after addition metal ion, C0It is original g-C3N4It is molten
The fluorescence intensity of liquid.
Experimental example 4：
Melamine 0.06mol is taken, it is dissolved in distilled water with 0.09mol NaCl, 0.09mol KCl, 90 DEG C of water
Bath stirring 0.5h, mixture then is transferred into eggplant type bottle carries out rotary evaporation treatment, and powder is placed in crucible after drying, and uses aluminium
Foil paper is tight by crucible parcel, is placed in Muffle furnace 690 DEG C of calcinings in air atmosphere, and heating rate is 2 DEG C/min, is incubated 2h
Natural cooling afterwards, gained powder is water-soluble g-C3N4Material, by gained g-C3N4Material is purified three times with isopropanol, is designated as
CNMS-4.Take Cd2+, Co2+, Cr3+, Cu2+, Fe2+, Ni2+, Zn2+, Hg2+, Pb2+, as metal ion target detection thing, take g-
C3N4Material (CNMS-4) 5mg is added in the metal ion solution that 5ml concentration is 1mM, stirs 0.5h, makes up to absorption flat
Weighing apparatus, after adsorption equilibrium process, solution is injected to be placed in XRF in four-way cuvette and tests its fluorescence intensity, according to formula
1- (C/C0) calculate its fluorescent quenching rate.Wherein C is the fluorescence intensity of solution after addition metal ion, C0It is original g-C3N4It is molten
The fluorescence intensity of liquid.
Experimental example 5：
Melamine 0.06mol is taken, it is dissolved in distilled water with 0.24mol NaCl, 0.24mol KCl, 90 DEG C of water
Bath stirring 2h, mixture then is transferred into eggplant type bottle carries out rotary evaporation treatment, and powder is placed in crucible after drying, and uses aluminium foil
Paper is tight by crucible parcel, is placed in Muffle furnace 690 DEG C of calcinings in air atmosphere, and heating rate is 10 DEG C/min, is incubated 2h
Natural cooling afterwards, gained powder is water-soluble g-C3N4Material, by gained g-C3N4Material is purified three times with isopropanol, is designated as
CNMS-5.Take Cd2+, Co2+, Cr3+, Cu2+, Fe2+, Ni2+, Zn2+, Hg2+, Pb2+, as metal ion target detection thing, take g-
C3N4Material (CNMS-5) 5mg is added in the metal ion solution that 5ml concentration is 1mM, stirs 0.5h, makes up to absorption flat
Weighing apparatus, after adsorption equilibrium process, solution is injected to be placed in XRF in four-way cuvette and tests its fluorescence intensity, according to formula
1- (C/C0) calculate its fluorescent quenching rate.Wherein C is the fluorescence intensity of solution after addition metal ion, C0It is original g-C3N4It is molten
The fluorescence intensity of liquid.
Experimental example 6：
Dicyandiamide 0.06mol is taken, it is dissolved in distilled water with 0.03mol NaCl, 0.03mol KCl, 60 DEG C of water-baths
Stirring 0.5h, mixture then is transferred into eggplant type bottle carries out rotary evaporation treatment, and powder is placed in crucible after drying, and uses aluminium foil
Paper is tight by crucible parcel, is placed in Muffle furnace 690 DEG C of calcinings in air atmosphere, and heating rate is 2 DEG C/min, after insulation 2h
Natural cooling, gained powder is water-soluble g-C3N4Material, is designated as CNMS-6.Take Cd2+, Co2+, Cr3+, Cu2+, Fe2+, Ni2+,
Zn2+, Hg2+, Pb2+, by gained g-C3N4Material is purified three times with isopropanol, as metal ion target detection thing, takes g-C3N4
Material (CNMS-6) 5mg is added in the metal ion solution that 5ml concentration is 1mM, stirs 0.5h, makes up to adsorption equilibrium,
After adsorption equilibrium process, solution is injected to be placed in XRF in four-way cuvette and tests its fluorescence intensity, according to formula 1-
(C/C0) calculate its fluorescent quenching rate.Wherein C is the fluorescence intensity of solution after addition metal ion, C0It is original g-C3N4Solution
Fluorescence intensity.
Experimental example 7：
Dicyandiamide 0.06mol is taken, it is dissolved in distilled water with 0.06mol NaCl, 0.06mol KCl, 60 DEG C of water-baths
Stirring 2h, mixture then is transferred into eggplant type bottle carries out rotary evaporation treatment, and powder is placed in crucible after drying, and uses aluminium-foil paper
Crucible parcel is tight, 680 DEG C of calcinings in air atmosphere are placed in Muffle furnace, heating rate is 10 DEG C/min, after insulation 2h
Natural cooling, gained powder is water-soluble g-C3N4Material, by gained g-C3N4Material is purified three times with isopropanol, is designated as
CNMS-7.Take Cd2+, Co2+, Cr3+, Cu2+, Fe2+, Ni2+, Zn2+, Hg2+, Pb2+, as metal ion target detection thing, take g-
C3N4Material (CNMS-7) 5mg is added in the metal ion solution that 5ml concentration is 1mM, stirs 0.5h, makes up to absorption flat
Weighing apparatus, after adsorption equilibrium process, solution is injected to be placed in XRF in four-way cuvette and tests its fluorescence intensity, according to formula
1- (C/C0) calculate its fluorescent quenching rate.Wherein C is the fluorescence intensity of solution after addition metal ion, C0It is original g-C3N4It is molten
The fluorescence intensity of liquid.
Experimental example 8：
Dicyandiamide 0.06mol is taken, it is dissolved in distilled water with 0.12mol NaCl, 0.12mol KCl, 60 DEG C of water-baths
Stirring 1h, mixture then is transferred into eggplant type bottle carries out rotary evaporation treatment, and powder is placed in crucible after drying, and uses aluminium-foil paper
Crucible is wrapped up tight, 670 DEG C of calcinings in air atmosphere are placed in Muffle furnace, heating rate is 5 DEG C/min, after insulation 2h certainly
So cooling, gained powder is water-soluble g-C3N4Material, by gained g-C3N4Material is purified three times with isopropanol, is designated as CNMS-
8.Take Cd2+, Co2+, Cr3+, Cu2+, Fe2+, Ni2+, Zn2+, Hg2+, Pb2+, as metal ion target detection thing, take g-C3N4Material
(CNMS-8) 5mg is added in the metal ion solution that 5ml concentration is 1mM, stirs 0.5h, makes up to adsorption equilibrium, is adsorbed
After equilibrium process, solution is injected to be placed in XRF in four-way cuvette and tests its fluorescence intensity, according to formula 1- (C/
C0) calculate its fluorescent quenching rate.Wherein C is the fluorescence intensity of solution after addition metal ion, C0It is original g-C3N4Solution it is glimmering
Luminous intensity.
Experimental example 9：
Dicyandiamide 0.06mol is taken, it is dissolved in distilled water with 0.18mol NaCl, 0.18mol KCl, 60 DEG C of water-baths
Stirring 0.5h, mixture then is transferred into eggplant type bottle carries out rotary evaporation treatment, and powder is placed in crucible after drying, and uses aluminium foil
Paper is tight by crucible parcel, is placed in Muffle furnace 670 DEG C of calcinings in air atmosphere, and heating rate is 2 DEG C/min, after insulation 2h
Natural cooling, gained powder is water-soluble g-C3N4Material, by gained g-C3N4Material is purified three times with isopropanol, is designated as
CNMS-9.Take Cd2+, Co2+, Cr3+, Cu2+, Fe2+, Ni2+, Zn2+, Hg2+, Pb2+, as metal ion target detection thing, take g-
C3N4Material (CNMS-9) 5mg is added in the metal ion solution that 5ml concentration is 1mM, stirs 0.5h, makes up to absorption flat
Weighing apparatus, after adsorption equilibrium process, solution is injected to be placed in XRF in four-way cuvette and tests its fluorescence intensity, according to formula
1- (C/C0) calculate its fluorescent quenching rate.Wherein C is the fluorescence intensity of solution after addition metal ion, C0It is original g-C3N4It is molten
The fluorescence intensity of liquid.
Experimental example 10：
Dicyandiamide 0.06mol is taken, it is dissolved in distilled water with 0.24mol NaCl, 0.24mol KCl, 60 DEG C of water-baths
Stirring 2h, mixture then is transferred into eggplant type bottle carries out rotary evaporation treatment, and powder is placed in crucible after drying, and uses aluminium-foil paper
Crucible parcel is tight, 670 DEG C of calcinings in air atmosphere are placed in Muffle furnace, heating rate is 10 DEG C/min, after insulation 2h
Natural cooling, gained powder is water-soluble g-C3N4Material, by gained g-C3N4Material is purified three times with isopropanol, is designated as
CNMS-10.Take Cd2+, Co2+, Cr3+, Cu2+, Fe2+, Ni2+, Zn2+, Hg2+, Pb2+, as metal ion target detection thing, take g-
C3N4Material (CNMS-10) 5mg is added in the metal ion solution that 5ml concentration is 1mM, stirs 0.5h, makes up to absorption flat
Weighing apparatus, after adsorption equilibrium process, solution is injected to be placed in XRF in four-way cuvette and tests its fluorescence intensity, according to formula
1- (C/C0) calculate its fluorescent quenching rate.Wherein C is the fluorescence intensity of solution after addition metal ion, C0It is original g-C3N4It is molten
The fluorescence intensity of liquid.
The wherein g-C of embodiment 33N4The XRD spectra of sample is shown in Fig. 1, and TEM figures are shown in Fig. 2, the g-C of embodiment 33N4Sample is examined
The PL spectrograms for surveying each metal ion species are shown in Fig. 3；The g-C of embodiment 33N4Sample detection metal-ion fluorescent is quenched rate spectrogram and sees figure
4, the g-C in other embodiments of the invention3N4Sample is to Co2+, Cr3+, Cu2+, Fe2+, Ni2+Metal-ion fluorescent is quenched rate also base
This is higher than 90%；g-C3N4Material tests various concentrations Fe3+PL spectrograms are shown in Fig. 5；g-C3N4Material digital photograph is shown in Fig. 6；g-C3N4
Material water dissolution properties matter digital photograph is shown in Fig. 7.
Claims (9)
1. a kind of one-step synthesis water solubility g-C3N4The preparation method of material, it is characterised in that comprise the following steps：
(1) one kind in melamine or dicyandiamide is well mixed with sodium chloride, potassium chloride and adds distilled water, 60~90
DEG C carry out water bath with thermostatic control stirring；
(2) step (1) slurry is carried out into rotary evaporation treatment, 650~690 DEG C of calcinings are obtained in atmosphere after drying, and calcining rises
Warm speed is 2 DEG C/min~10 DEG C/min, obtains final product the water-soluble g-C3N4Material；
(3) by step (2) gained g-C3N4Material is purified with isopropanol.
2. according to the method for claim 1, it is characterised in that in step (1), melamine or dicyandiamide and sodium chloride, chlorination
The mol ratio of potassium is 1：(0.5~4)：(0.5~4).
3. according to the method for claim 1, it is characterised in that in step (1), melamine or dicyandiamide and sodium chloride, chlorination
The mol ratio of potassium is 1:1:1.
4., according to the method for claim 1, it is characterised in that in step (1), the water bath processing temperature is 60~90 DEG C, permanent
The warm time is 0.5~2 hour.
5., according to the method for claim 1, it is characterised in that in step (2), calcining heat is 650~690 DEG C, and calcining heats up
Speed is 2 DEG C/min~10 DEG C/min.
6. according to the method for claim 1, it is characterised in that in step (2), calcining heat is 670 DEG C, and calcining heating rate is
5 DEG C/min, the soaking time of calcining is 2 hours.
7. the water-soluble g-C for being obtained according to the either method of claim 1-63N4Material.
8. the water-soluble g-C for being obtained according to the either method of claim 1-63N4The application of material, for trace metal ion inspection
Survey.
9. according to the application of claim 8, it is characterised in that for Cd2+, Co2+, Cr3+, Cu2+, Fe2+, Ni2+, Zn2+, Hg2+,
Pb2+Detection.
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| CN108557784A (en) * | 2018-05-16 | 2018-09-21 | 武汉科技大学 | A kind of high-specific surface area atomic layers thick azotized carbon nano piece and preparation method thereof |
| CN109765225A (en) * | 2019-01-30 | 2019-05-17 | 扬州工业职业技术学院 | A kind of g-C of load silver ion3N4Nano material and its application in the detection of kitchen abandoned oil |
| CN111250042A (en) * | 2020-02-18 | 2020-06-09 | 上海电力大学 | Carbon-based adsorbent for demercuration and preparation method and application thereof |
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Application publication date: 20170531 |