CN108380230A - The preparation method and application of ultra-thin graphite phase carbon nitride - Google Patents
The preparation method and application of ultra-thin graphite phase carbon nitride Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 14
- 239000010439 graphite Substances 0.000 title claims abstract description 14
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- 230000000593 degrading effect Effects 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 10
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 9
- 239000004065 semiconductor Substances 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 21
- 238000006731 degradation reaction Methods 0.000 description 8
- 101100165323 Drosophila melanogaster bgcn gene Proteins 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 101100054306 Arabidopsis thaliana ABCF3 gene Proteins 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 102100022846 Histone acetyltransferase KAT2B Human genes 0.000 description 1
- 101001046967 Homo sapiens Histone acetyltransferase KAT2A Proteins 0.000 description 1
- 101001047006 Homo sapiens Histone acetyltransferase KAT2B Proteins 0.000 description 1
- 206010028813 Nausea Diseases 0.000 description 1
- 206010033799 Paralysis Diseases 0.000 description 1
- 101100279457 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) GCN3 gene Proteins 0.000 description 1
- 239000004098 Tetracycline Substances 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
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- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
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- 231100000869 headache Toxicity 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 101150111648 mtnA gene Proteins 0.000 description 1
- 230000008693 nausea Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
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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
-
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
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- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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
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- Inorganic Chemistry (AREA)
- Toxicology (AREA)
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Abstract
The invention belongs to semiconductor catalyst preparing technical fields, refer in particular to the synthesis and application of ultra-thin graphite phase carbon nitride, the grinding of the urea of certain mass is put into crucible and is built in after 60 80 DEG C of 20 30h of drying in oven by profit calcines 3 5h, 23 DEG C/min of heating rate in Muffle furnace at 500 600 DEG C.Obtain sample A.It calcines obtained A powder to be put into the salpeter solution of pH=1, stirs 20 25h, the sample after being washed with deionized water makes pH value improve, and no more than neutrality, is dried in vacuum drying chamber and obtains sample B.Powder B obtained above is placed in Muffle furnace at 400 500 DEG C and continues to calcine 2 4h, 23 DEG C/min of heating rate.Obtain final ultra-thin g C3N4.The present invention is used under visible light 2 mercaptobenzothiazolers of degrading.
Description
Technical field
The invention belongs to semiconductor catalyst preparing technical fields, and synthesizing ultra-thin graphite phase carbon nitride light using calcination method urges
Agent, for 2-mercaptobenzothiazole of degrading under visible light.
Background technology
Recently as the fast development of world economy, global environmental degradation and problems of energy consumption become increasingly conspicuous, because
This accelerates non-fossil energy, actively pushes forward clean energy resource and have become countries in the world to face and key subjects mesh urgently to be resolved hurrily
Before, Hydrogen Energy becomes because having many advantages, such as that fuel value is high, efficient and cleanliness without any pollution and substitutes a kind of of traditional fossil energy and relatively manage
The new cleaning fuel thought.Meanwhile with the development of chemical industry, mercaptan is as a kind of important chemical products, extensively
Applied to every field, such as medicine, the vulcanization of rubber, synthesizing fungicide.Benzothiazole mercaptan (MBT), as a kind of mercaptan, quilt
It is widely used in the rubber products such as manufacture tire, rubber overshoes.In addition, MBT also can be sensitive as one reagent for testing metal.But
It is worth noting that, the toxicity of MBT is difficult to eliminate, low concentration MBT leads to people's nausea and headache, and the MBT of higher concentration will band
Carry out fatal respiratory tract paralysis.Therefore, it has been that researcher is urgent to eliminate and reduce the problem of MBT brings environment and the mankind
Need the significant problem solved.
Photocatalitic Technique of Semiconductor because reaction condition is mild, oxidability is strong, non-toxic inexpensive, using solar energy as the energy
The advantages that become research hotspot in recent years.It studies at present in more semiconductor, TiO2With activity it is high, stable, nontoxic and
It is inexpensive to be considered as best photochemical catalyst and obtained extensive research, however TiO2It is merely able to absorb ultraviolet light, in the sun
In spectrum, ultraviolet light only accounts for 5%, and the ratio of visible light is up to 43%, therefore, develop can the visible light of practical application ring
The semiconductor light-catalyst answered is the hot issue of current photocatalysis research field.Carbonitride (g-C3N4) as a kind of nonmetallic
Semiconductor catalyst, energy gap 2.7eV, due to the spies such as its good thermal stability, cheap cost, safe and non-toxic
Point gradually causes the favor of researcher in photocatalysis field.But more body phase g-C is studied at present3N4Due to specific surface
Product is smaller, and photo-generated carrier is easily compound so that its photocatalytic activity is relatively low.Therefore the present invention prepares the ultra-thin g- of different-thickness
C3N4For Photocatalyzed Hydrogen Production and degradation MBT.
Invention content
In order to overcome above-mentioned body phase g-C3N4Existing deficiency, the present invention synthesize ultra-thin graphite phase carbon nitride using calcination method
Photochemical catalyst, for 2-mercaptobenzothiazole of degrading under visible light.
The preparation method of ultra-thin graphite phase carbon nitride, includes the following steps：
The ultra-thin g-C of different-thickness3N4Preparation
(1) grinding of the urea of certain mass crucible is put into be built in after 60-80 DEG C of drying in oven 20-30h in Muffle
3-5h, 2-3 DEG C of heating rate/min are calcined in stove at 500-600 DEG C.Obtain sample A.
(2) the A powder that calcining obtains is put into the salpeter solution of pH=1, stirs 20-25h,
(3) sample after being washed with deionized water makes pH value improve, and no more than neutrality, in vacuum drying chamber
Interior drying obtains sample B.
(4) powder B obtained above is placed in Muffle furnace at 400-500 DEG C and continues to calcine 2-4h, heating rate 2-3
℃/min.Obtain final ultra-thin g-C3N4。
Preferably, in above-mentioned steps (1), 80 DEG C of baking oven drying temperature, the time is for 24 hours；550 DEG C of calcination temperature, calcination time
4h, 2.3 DEG C/min of heating rate.
Preferably, in above-mentioned steps (2), powders A mixing time is for 24 hours.
Preferably, in above-mentioned steps (4), 500 DEG C, calcination time 4h in Muffle furnace, 2.3 DEG C/min of heating rate.
In addition, the technology of the present invention compared to existing technology, is removed to obtain two-dimensional ultrathin g-C using sour processing method3N4,
Solve the disadvantages such as existing method difficulty recycles, cyclical stability is poor, catalytic activity is low at present.The present invention is because method is simple, yield
It is higher, be more advantageous to practical application.It removes to obtain two-dimensional ultrathin g-C using sour processing method simultaneously3N4Thickness only has 4nm, ultra-thin
Two-dimentional g-C3N4The specific surface area for greatly improving material provides more reactivity sites, improves electronics-sky
The separative efficiency in cave, finally enhances photocatalytic activity.
Advantageous effect
Ultra-thin graphite phase carbon nitride photochemical catalyst is synthesized using calcination method, 2-mercaptobenzothiazole of degrading under visible light is aobvious
Excellent photocatalytic activity is shown；Present invention process is simple, and reaction cost is low, convenient for batch production, meets environmental-friendly requirement.
Description of the drawings
Fig. 1 is body phase g-C prepared by calcination method3N4(BGCN) the ultra-thin g-C and under different PH3N4(GCN) light is urged
The XRD diffraction spectrograms for changing material, the diffraction maximum of the GCN after it can be seen that BGCN and stripping in the test result of XRD is not
Apparent variation occurs.And prepared all samples all occur without miscellaneous peak, illustrate the g-C that we prepare3N4Crystal form does not change
Become.
Fig. 2 is body phase g-C3N4(BGCN) the ultra-thin g-C and under different PH3N4(GCN) catalysis material scanning figure and
Transmission plot.It can be seen that the g-C not obtained through peracid treatment from Fig. 2 a3N4(BGCN) block structure is presented.However, Fig. 2 b can be with
It is apparent to observe the g-C obtained after sour process3N4(GCN) laminated structure is presented.In order to further prove it is acidified after
The g-C of two-dimensional sheet is arrived3N4.By Fig. 2 c we have further found that body phase g-C3N4(BGCN) it is bulk, is obtained after acidification
Fig. 2 d be two-dimensional sheet g-C3N4。
Fig. 3 shows body phase g-C3N4(BGCN), the ultra-thin g-C of PH 1,3,5 and 73N4(GCN) it is dropped in visible light catalytic
Solve the relational graph of degradation time-degradation rate of 2-mercaptobenzothiazole solution.It can be seen from the figure that 2-mercaptobenzothiazole sheet
It can be stabilized in radiation of visible light, body phase g-C3N4(BGCN) 120 minutes lower degradation rates only have under visible light
48.3%, however the g-C after being acidified3N4Material can significantly improve photocatalysis effect.When pH value is washed to 7 with deionized water,
Degradation 2-mercaptobenzothiazole activity highest, lower degradation rate can reach 84.9% within 120 minutes.
Specific implementation mode
Embodiment 1
The ultra-thin g-C of different-thickness3N4Preparation
(1) grinding of the urea of certain mass is put into after crucible is built in 80 DEG C of drying in oven for 24 hours in Muffle furnace
4h, 2.3 DEG C/min of heating rate are calcined at 550 DEG C.Obtain sample A.
(2) the A powder that calcining obtains is put into the salpeter solution of PH=1, and stirring is for 24 hours.
(3) it is washed with deionized water, until PH=3, collects sample and dried in vacuum drying chamber.Obtain sample B
(4) powder B obtained above is placed in Muffle furnace at 500 DEG C and continues to calcine 4h, 2.3 DEG C/min of heating rate.
Obtain final ultra-thin GCN3.
Embodiment 2
The ultra-thin g-C of different-thickness3N4Preparation
(1) grinding of the urea of certain mass is put into after crucible is built in 80 DEG C of drying in oven for 24 hours in Muffle furnace
4h, 2.3 DEG C/min of heating rate are calcined at 550 DEG C.Obtain sample A.
(2) the A powder that calcining obtains is put into the salpeter solution of PH=1, and stirring is for 24 hours.
(3) it is washed with deionized water, until PH=5, collects sample and dried in vacuum drying chamber.Obtain sample B
(4) powder B obtained above is placed in Muffle furnace at 500 DEG C and continues to calcine 4h, 2.3 DEG C/min of heating rate.
Obtain final ultra-thin GCN5.
Embodiment 3
The ultra-thin g-C of different-thickness3N4Preparation
(1) grinding of the urea of certain mass is put into after crucible is built in 80 DEG C of drying in oven for 24 hours in Muffle furnace
4h, 2.3 DEG C/min of heating rate are calcined at 550 DEG C.Obtain sample A.
(2) the A powder that calcining obtains is put into the salpeter solution of PH=1, and stirring is for 24 hours.
(3) it is washed with deionized water, until PH=7, collects sample and dried in vacuum drying chamber.Obtain sample B
(4) powder B obtained above is placed in Muffle furnace at 500 DEG C and continues to calcine 4h, 2.3 DEG C/min of heating rate.
Obtain final ultra-thin GCN7.
Embodiment 4
Compound concentration is the tetracycline of 10mg/L, and the solution prepared is placed in dark place.Photochemical catalyst 50mg is weighed,
It is respectively placed in photo catalysis reactor, above-mentioned the prepared target descending liquid of 100mL steps is added, magnetic agitation 30min is to be composite
After photochemical catalyst is uniformly dispersed, water source is opened, light source carries out photocatalytic degradation experiment.The light drawn per 20min in reactor is urged
Change degradation solution, the measurement of UV-visible absorbance is used for after centrifugation.Prepared two-dimensional ultrathin g-C as seen from Figure 33N4
2-mercaptobenzothiazole of degrading under 120min has excellent visible light catalysis activity.
Claims (6)
1. the preparation method of ultra-thin graphite phase carbon nitride, which is characterized in that steps are as follows：
(1) urea grinding crucible is put into be built in after 60-80 DEG C of drying in oven 20-30h in Muffle furnace at 500-600 DEG C
3-5h is calcined, 2-3 DEG C of heating rate/min obtains sample A；
(2) the A powder that calcining obtains is put into the salpeter solution of pH=1, stirs 20-25h；
(3) sample after being washed with deionized water makes pH value improve, and no more than neutrality, is dried in vacuum drying chamber
It is dry to obtain sample B；
(4) powder B obtained above is placed in Muffle furnace at 400-500 DEG C and continues to calcine 2-4h, 2-3 DEG C of heating rate/
Min obtains ultra-thin graphite phase carbon nitride.
2. the preparation method of ultra-thin graphite phase carbon nitride as described in claim 1, which is characterized in that in step (1), baking oven dries
Dry 80 DEG C of temperature, the time is for 24 hours；550 DEG C, calcination time 4h of calcination temperature, 2.3 DEG C/min of heating rate.
3. the preparation method of ultra-thin graphite phase carbon nitride as described in claim 1, which is characterized in that in step (2), powders A
Mixing time is for 24 hours.
4. the preparation method of ultra-thin graphite phase carbon nitride as described in claim 1, which is characterized in that in step (4), Muffle furnace
Interior 500 DEG C, calcination time 4h, 2.3 DEG C/min of heating rate.
5. the preparation method of ultra-thin graphite phase carbon nitride as described in claim 1, which is characterized in that in step (2), pH value is
7。
6. the purposes of ultra-thin graphite phase carbon nitride prepared by method as described in claim 1, for 2- sulfydryls of degrading under visible light
Benzothiazole.
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| CN109225303A (en) * | 2018-10-23 | 2019-01-18 | 江苏大学 | A kind of dimensional thinlayer Au/g-C3N4The Preparation method and use of composite photo-catalyst |
| CN109395758A (en) * | 2018-11-12 | 2019-03-01 | 江苏大学 | A kind of dimensional thinlayer CdS/g-C3N4The Preparation method and use of composite photo-catalyst |
| CN109759108A (en) * | 2018-11-19 | 2019-05-17 | 江苏大学 | A kind of Three-element composite photocatalyst and preparation method and application |
| CN110252370A (en) * | 2019-05-23 | 2019-09-20 | 江苏大学 | A kind of two dimension ZnO/g-C3N4The Preparation method and use of composite photo-catalyst |
| CN110420656A (en) * | 2019-08-13 | 2019-11-08 | 合肥工业大学 | A kind of gas phase acidification g-C3N4 nanometer sheet and preparation method thereof |
| CN110743599A (en) * | 2019-11-11 | 2020-02-04 | 盐城工学院 | Preparation method and application of near-infrared light response type thin-layer carbon nitride photocatalytic material |
| CN111871442A (en) * | 2020-07-31 | 2020-11-03 | 江苏大学 | Niobium-tantalum sulfide/carbon nitride nanosheet photocatalytic material and preparation method and application thereof |
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| CN114345388A (en) * | 2022-01-11 | 2022-04-15 | 广州亦盛环保科技有限公司 | Modification method of graphite-like phase carbon nitride |
| CN114870880A (en) * | 2022-05-26 | 2022-08-09 | 江苏省农业科学院 | Preparation and application of adsorption-catalysis dual-function material capable of synchronously removing COD (chemical oxygen demand), antibiotics and phosphorus in aquaculture sewage |
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