CN109351362A - A kind of porous molecular doping carbon nitride photocatalyst and the preparation method and application thereof - Google Patents
A kind of porous molecular doping carbon nitride photocatalyst and the preparation method and application thereof Download PDFInfo
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- CN109351362A CN109351362A CN201811194356.8A CN201811194356A CN109351362A CN 109351362 A CN109351362 A CN 109351362A CN 201811194356 A CN201811194356 A CN 201811194356A CN 109351362 A CN109351362 A CN 109351362A
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 32
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 9
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 6
- ZZYXNRREDYWPLN-UHFFFAOYSA-N pyridine-2,3-diamine Chemical compound NC1=CC=CN=C1N ZZYXNRREDYWPLN-UHFFFAOYSA-N 0.000 claims abstract 6
- 239000000243 solution Substances 0.000 claims description 25
- 239000002253 acid Substances 0.000 claims description 19
- 238000012545 processing Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000003837 high-temperature calcination Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 10
- 230000015556 catabolic process Effects 0.000 abstract description 9
- 238000006731 degradation reaction Methods 0.000 abstract description 9
- 238000001354 calcination Methods 0.000 abstract description 7
- 239000011148 porous material Substances 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 2
- 238000011017 operating method Methods 0.000 abstract description 2
- VHNQIURBCCNWDN-UHFFFAOYSA-N pyridine-2,6-diamine Chemical compound NC1=CC=CC(N)=N1 VHNQIURBCCNWDN-UHFFFAOYSA-N 0.000 description 13
- 230000001699 photocatalysis Effects 0.000 description 9
- 238000007146 photocatalysis Methods 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000013019 agitation Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000002791 soaking Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229920000877 Melamine resin Polymers 0.000 description 3
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 101150079125 DCN1 gene Proteins 0.000 description 1
- 102100026982 DCN1-like protein 1 Human genes 0.000 description 1
- 101100330861 Homo sapiens DCUN1D1 gene Proteins 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- -1 dicyanodiamine Chemical compound 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- B01J35/613—
-
- B01J35/633—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention belongs to catalysis material preparation technical fields, and in particular to a kind of porous molecular doping carbon nitride photocatalyst and the preparation method and application thereof.Then carbon nitride precursor and diamino-pyridine reaction preparation mixing presoma are used HNO by this method3Solution carries out oxidation corrosion to mixing presoma, and final high temperature calcining can be obtained the photochemical catalyst.Wherein, in presoma diamino-pyridine addition, and to mixing presoma use HNO3Solution, which carries out oxidation corrosion, can dramatically increase the specific surface area of photochemical catalyst, and the photochemical catalyst specific surface area obtained is made to be up to 28.6~58.6m2/ g, pore volume are up to 0.28~0.34cm3/ g, and then increase more reaction sites.This method is not necessarily to template, and operating procedure is simple.The catalyst is used for Photocatalytic Degradation of Phenol, the degradation rate after 4 hours is up to 60%.
Description
Technical field
The invention belongs to catalysis material preparation technical fields, and in particular to a kind of porous molecular doping carbonitride photocatalysis
Agent and the preparation method and application thereof.
Background technique
With the development of modern industry, energy resources gradually decrease or even exhaustion, environmental pollution are got worse.Energy shortage
It is 21 century facing mankind and significant problem urgently to be resolved with environmental degradation.Therefore, renewable new energy and control are developed and used
System curbs environmental pollution to developing national economy, realizes that the strategy of sustainable development is of great significance.Conductor photocatalysis this
One frontier is that mankind's development and utilization solar energy opens brand-new approach.However, conventional Ti O2Base inorganic semiconductor photocatalysis
The drawbacks of that there are solar energy utilization ratios is low for agent, photo-quantum efficiency is low and easy in inactivation, seriously constrains the reality of photocatalysis technology
It promotes and applies.Therefore, it develops new and effective photochemical catalyst and widens the optical response range of photochemical catalyst, become current photocatalysis neck
The research hotspot in domain.Graphite phase carbon nitride (g-C3N4) there is good chemical inertness, thermal stability and bio-compatibility etc.,
It is possible that substituting graphitic carbon material in a variety of materials scientific application.g-C3N4It is a kind of organic semiconducting materials, forbidden bandwidth is about
2.7eV has suitable conduction band valence band location, there is tempting application prospect in photocatalysis field.G-C at present3N4Photochemical catalyst
Preparation method be high-temperature calcination thermal polycondensation process, i.e., by forerunners such as melamine, cyanamide, dicyanodiamine, cyanuric trichloride, urea
Body is heated to 500~600 DEG C, brings it about polycondensation reaction and obtains product.But the g-C obtained by this method3N4Specific surface area
It is small, therefore photocatalysis performance is often not satisfactory.
Summary of the invention
In order to overcome carbonitride small in specific surface area present on the prior art, it is seen that the deficiencies of light utilization efficiency is lower, this
The primary and foremost purpose of invention is to provide a kind of specific surface area higher, and active stronger and Pyrogentisinic Acid's sewage has superior photocatalytic activity
Porous molecular doping carbon nitride photocatalyst preparation method.
Another object of the present invention is to provide the porous moleculars obtained by above-mentioned preparation method to adulterate carbonitride photocatalysis
Agent.
A further object of the present invention is to provide the applications of above-mentioned porous molecular doping carbon nitride photocatalyst.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of preparation method of porous molecular doping carbon nitride photocatalyst, comprising the following steps:
(1) preparation of presoma
Carbon nitride precursor and diamino-pyridine (DPY) are added to the water, heating stirring, dissolve the two, clarified
Solution, solution is dried, obtain mixing presoma；
(2) the acid processing of presoma is mixed
HNO is added into mixing presoma3Solution obtains mixed solution, and reaction makes to mix presoma dissolution, dry, obtains
To the presoma of acid processing；
(3) it calcines
High-temperature calcination is carried out to the presoma of acid processing and adulterates carbon nitride photocatalyst to get to the porous molecular
(P-DCN)。
Preferably, carbon nitride precursor described in step (1) is dicyanodiamine (DCDA), melamine, cyanamide or urine
Element.
Preferably, the mass ratio of the carbon nitride precursor in solution described in step (1) and diamino-pyridine is 3:0.01
~3:0.1.
Preferably, in solution described in step (1), the matter of the quality sum and water of carbon nitride precursor and diamino-pyridine
Amount is than being 1:3~1:10.
Preferably, the temperature of heating described in step (1) is 80~100 DEG C.
Preferably, stirring described in step (1) when it is 0.5~2 hour a length of.
Preferably, the method for drying described in step (1) and step (2) is to be dried with electric hot plate or insulating box.
Preferably, the temperature of drying described in step (1) and step (2) is 100 DEG C.
Preferably, HNO described in step (2)3The concentration of solution is 0.6M.
Preferably, in mixed solution described in step (2), presoma and HNO are mixed3The solid-to-liquid ratio of solution be 1:50~
1:200g/mL。
Preferably, the heating rate of high-temperature calcination described in step (3) is 2.3~10 DEG C/min.
Preferably, the temperature of high-temperature calcination described in step (3) is 400~650 DEG C.
Preferably, high-temperature calcination described in step (3) when it is 2~6 hours a length of.
The present invention further provides the porous moleculars obtained by above-mentioned preparation method to adulterate carbon nitride photocatalyst.
The present invention further provides the applications of above-mentioned porous molecular doping carbon nitride photocatalyst, and the photochemical catalyst is used
In Photocatalytic Degradation of Phenol.
The preparation principle of porous molecular doping carbon nitride photocatalyst in the present invention are as follows:
The present invention, which first reacts dicyanodiamine (DCDA) with 2,6-diaminopyridine (DPY), is prepared into presoma, then makes
Use HNO3Solution to presoma carry out oxidation corrosion, finally by high-temperature calcination carry out polycondensation reaction come be prepared cellular,
The porous molecular of high catalytic activity adulterates carbonitride.
Compared with prior art, the present invention having the following advantages and beneficial effects:
(1) then carbon nitride precursor and diamino-pyridine reaction preparation mixing presoma are used HNO by the present invention3Solution
Oxidation corrosion is carried out to mixing presoma, final high temperature calcining can be obtained the photochemical catalyst.Wherein, diamino in presoma
The addition of yl pyridines, and HNO is used to mixing presoma3Solution, which carries out oxidation corrosion, can dramatically increase the ratio table of photochemical catalyst
The specific surface area of area, the porous molecular doping carbon nitride photocatalyst being prepared is up to 28.6~58.6m2/ g, pore volume
Up to 0.28~0.34cm3/g.It can provide more reaction sites, have it under the irradiation of visible light to organic pollutant
There is stronger photocatalytic degradation capability.
(2) method of porous molecular doping carbonitride prepared by the present invention is template-free method, and operating procedure is simple, catalyst
It is active high.
(3) the porous molecular doping carbon nitride photocatalyst that the present invention is prepared is used for Photocatalytic Degradation of Phenol, 4 is small
When after degradation rate be up to 60%.
Detailed description of the invention
Fig. 1 is the XPS spectrum figure of the C element of P-DCN3 made from embodiment 1.
Fig. 2 is the XPS spectrum figure of the O element of P-DCN3 made from embodiment 1.
Fig. 3 is the XPS spectrum figure of the N element of P-DCN3 made from embodiment 1.
Fig. 4 is the X-ray diffractogram (XRD) of DCN, P-DCN3 prepared by embodiment 1.
Fig. 5 is the infrared spectrogram (IR) of DCN, P-DCN3 made from embodiment 1.
Fig. 6 is SEM and the TEM figure of DCN, P-DCN3 made from embodiment 1, and the SEM that wherein the figure A in Fig. 6 is DCN schemes,
The SEM that figure B in Fig. 6 is P-PCN3 schemes, and the TEM that the figure C in Fig. 6 is DCN schemes, and the TEM that the figure D in Fig. 6 is P-PCN3 schemes.
Fig. 7 is the degradation effect comparison diagram of DCN, P-DCN3 Pyrogentisinic Acid made from embodiment 1.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.For not specifically specified technological parameter, routine techniques progress can refer to.
Embodiment 1
The present embodiment provides a kind of porous molecular doping carbon nitride photocatalyst P-DCN3 and preparation method thereof.
Porous molecular adulterate carbon nitride photocatalyst P-DCN3's the preparation method is as follows:
(1) 3g DCDA and 0.07g DPY are placed in conical flask, 9.21mL water is added, 80 DEG C are heated to, in 500rpm
Lower magnetic agitation is transferred in culture dish to solution clear, is placed in 100 DEG C of thermostatic drying chambers dry 5h, is mixed
Presoma.
(2) mixing presoma is pulverized, weighs 1g and is placed in a beaker, the HNO that 50mL concentration is 0.6M is added3It is molten
Liquid is placed in 100 DEG C of drying boxes dry 5h, obtains the presoma of acid processing.
(3) presoma of acid processing is placed in Muffle furnace and is calcined, calcination temperature is 550 DEG C, and soaking time is 4 small
When, heating rate is 10 DEG C/min；It pulverizes after natural cooling, obtains porous molecular doping carbon nitride photocatalyst P-
DCN3。
The specific surface area of gained photochemical catalyst P-DCN3 is 58.6m2/ g, pore volume 0.28cm3/g。
Embodiment 2
Reference examples of the present embodiment as embodiment 1 provide a kind of porous molecular doping carbonitride for not carrying out sour processing
Photochemical catalyst DCN and preparation method thereof.
DCN's the preparation method is as follows:
(1) 3g DCDA and 0.07g DPY are placed in conical flask, 9.21mL water is added, 80 DEG C are heated to, in 500rpm
Lower magnetic agitation is transferred in culture dish to solution clear, is placed in 100 DEG C of thermostatic drying chambers dry 5h, is mixed
Presoma.
(2) mixing presoma is pulverized, is calcined in Muffle furnace, calcination temperature is 550 DEG C, and soaking time is 4 small
When, heating rate is 10 DEG C/min；It pulverizes after natural cooling, obtains molecular dopant carbon nitride photocatalyst DCN.
The specific surface area of gained photochemical catalyst DCN is 18.8m2/ g, pore volume 0.018cm3/g。
The P-DCN3 and DCN photochemical catalyst manufactured in the present embodiment prepare to embodiment 1 carries out characterization of structure and properties, as a result
As shown in figs. 1 to 6.
It is the XPS figure of C, N, O of P-DCN3 respectively shown in Fig. 1~3, the bond energy and valence state and nitrogen of C, O, N is seen from figure
It is consistent to change carbon.
It is the XRD comparison diagram of DCN, P-DCN3 shown in Fig. 4, the substance that peak position may determine that from figure is all nitrogen
Change carbon.
It is the IR comparison diagram of DCN, P-DCN3 shown in Fig. 5, as can be seen from the figure the position at the peak of the two and peak type differ
Less, illustrate after molecular dopant is modified and acid is handled and have not been changed the essential groups of carbonitride.
Fig. 6 is that the SEM and TEM of DCN, P-DCN3 scheme, the surface of the P-DCN3 obtained after peracid treatment as seen from the figure compared with
There is not more multiple hole in the DCN of acid processing.
Embodiment 3
Reference examples of the present embodiment as embodiment 1 provide the porous molecular doping nitrogen in a kind of presoma not comprising DPY
Change carbon photochemical catalyst P-CN and preparation method thereof.
P-CN's the preparation method is as follows:
(1) 3g DCDA is placed in conical flask, 9.21mL water is added, is heated to 80 DEG C, magnetic agitation is extremely at 500 rpm
Solution clear, is transferred in culture dish, is placed in 100 DEG C of thermostatic drying chambers dry 5h, obtains presoma.
(2) presoma is pulverized, weighs 1g and is placed in a beaker, the HNO that 50mL concentration is 0.6M is added3Solution is set
The dry 5h in 100 DEG C of drying boxes obtains acid treated presoma.
(3) presoma of acid processing is placed in Muffle furnace and is calcined, calcination temperature is 550 DEG C, and soaking time is 4 small
When, heating rate is 10 DEG C/min；It pulverizes after natural cooling, obtains nitride porous carbon photochemical catalyst P-CN.
The specific surface area of gained photochemical catalyst P-CN is 37.3m2/ g, pore volume 0.12cm3/g.It can with the comparison of embodiment 1
Know, is remarkably improved the specific surface area and hole that porous molecular adulterates carbon nitride photocatalyst by adding DPY in presoma
Rate.
Embodiment 4
The present embodiment provides P-DCN3 prepared by embodiment 1, P-CN prepared by DCN and embodiment 3 prepared by embodiment 2 exists
Application effect in Photocatalytic Degradation of Phenol.
The phenol solution that 150ml concentration is 10mg/L is added in phototropic reaction device, take DCN obtained in 50mg embodiment 1,
P-CN or P-DCN3 investment wherein, reaches adsorption equilibrium, then irradiates under 300W xenon lamp, every 0.5h takes one after dark reaction 0.5h
Secondary sample calculates remaining phenol by the method that ultraviolet-visible spectrophotometer measures solution absorbance and contains after sampling dyeing
Amount, degradation results are shown in Fig. 7.As seen from the figure, the P-DCN3 that the present embodiment is prepared has apparent degradation of phenol effect, wherein
The degradation effect of P-DCN3 is preferable, and the degradation rate of Pyrogentisinic Acid is up to 60% after the irradiation of 4h xenon lamp, and DCN, P-CN Pyrogentisinic Acid
Degradation rate it is bad, respectively may be about 20% and 42%.
Embodiment 5
The present embodiment provides a kind of porous molecular doping carbon nitride photocatalyst P-DCN1 and preparation method thereof.
(1) 3g melamine and 0.01g DPY are placed in conical flask, 30.1mL water is added, is heated to 90 DEG C,
Magnetic agitation is transferred in culture dish to solution clear, is placed in 100 DEG C of thermostatic drying chambers dry 5h, obtains under 500rpm
To mixing presoma.
(2) mixing presoma is pulverized, weighs 1g and is placed in a beaker, the HNO that 200mL concentration is 0.6M is added3It is molten
Liquid is placed in 100 DEG C of drying boxes dry 5h, obtains the presoma of acid processing.
(3) presoma of acid processing is placed in Muffle furnace and is calcined, calcination temperature is 400 DEG C, and soaking time is 6 small
When, heating rate is 2.3 DEG C/min；It pulverizes after natural cooling, obtains porous molecular doping carbon nitride photocatalyst P-
DCN1。
The specific surface area of gained photochemical catalyst P-DCN1 is 28.6m2/ g, pore volume 0.33cm3/g。
Embodiment 6
The present embodiment provides a kind of porous molecular doping carbon nitride photocatalyst P-DCN2 and preparation method thereof.
(1) 3g urea and 0.10g DPY are placed in conical flask, 15mL water is added, is heated to 100 DEG C, at 500 rpm
Magnetic agitation is transferred in culture dish to solution clear, dry 5h is placed in 100 DEG C of thermostatic drying chambers, before obtaining mixing
Drive body.
(2) mixing presoma is pulverized, weighs 1g and is placed in a beaker, the HNO that 100mL concentration is 0.6M is added3It is molten
Liquid is placed in 100 DEG C of drying boxes dry 5h, obtains the presoma of acid processing.
(3) presoma of acid processing is placed in Muffle furnace and is calcined, calcination temperature is 650 DEG C, and soaking time is 2 small
When, heating rate is 5 DEG C/min；It pulverizes after natural cooling, obtains porous molecular doping carbon nitride photocatalyst P-DCN2.
The specific surface area of gained photochemical catalyst P-DCN2 is 38.1m2/ g, pore volume 0.34cm3/g。
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by the embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of porous molecular doping carbon nitride photocatalyst, which comprises the following steps:
(1) preparation of presoma
Carbon nitride precursor and diamino-pyridine (DPY) are added to the water, heating stirring, dissolve the two, obtain clear molten
Solution is dried in liquid, obtains mixing presoma；
(2) the acid processing of presoma
HNO is added into mixing presoma3Solution obtains mixed solution, and reaction makes to mix presoma dissolution, dry, obtains sour place
The presoma of reason；
(3) it calcines
High-temperature calcination is carried out to the presoma of acid processing and adulterates carbon nitride photocatalyst to get to the porous molecular.
2. the preparation method of porous molecular doping carbon nitride photocatalyst according to claim 1, it is characterised in that:
The mass ratio of carbon nitride precursor and diamino-pyridine in solution described in step (1) is 3:0.01~3:0.1；
In the solution, the mass ratio of the quality sum and water of carbon nitride precursor and diamino-pyridine is 1:3~1:10.
3. the preparation method of porous molecular doping carbon nitride photocatalyst according to claim 1, it is characterised in that: step
(1) temperature of the heating described in is 80~100 DEG C.
4. the preparation method of porous molecular doping carbon nitride photocatalyst according to claim 1, it is characterised in that: step
(1) and the temperature of drying described in step (2) is 100 DEG C.
5. the preparation method of porous molecular doping carbon nitride photocatalyst according to claim 1, it is characterised in that: step
(2) HNO described in3The concentration of solution is 0.6M.
6. the preparation method of porous molecular doping carbon nitride photocatalyst according to claim 1, it is characterised in that: step
(2) in the mixed solution described in, presoma and HNO are mixed3The solid-to-liquid ratio of solution is 1:50~1:200g/mL.
7. the preparation method of porous molecular doping carbon nitride photocatalyst according to claim 1, it is characterised in that: step
(3) temperature of the high-temperature calcination described in is 400~650 DEG C.
8. the preparation method of porous molecular doping carbon nitride photocatalyst according to claim 1, it is characterised in that: step
(3) high-temperature calcination described in when it is 2~6 hours a length of.
9. a kind of porous molecular adulterates carbon nitride photocatalyst, it is characterised in that: the preparation method as described in claim 1~8
It obtains.
10. the application of porous molecular doping carbon nitride photocatalyst as claimed in claim 9, it is characterised in that: by the light
Catalyst is used for Photocatalytic Degradation of Phenol.
Priority Applications (1)
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