CN110124716A - A kind of one-step method preparation sheet TiO2/g-C3N4The method of hetero-junctions - Google Patents
A kind of one-step method preparation sheet TiO2/g-C3N4The method of hetero-junctions Download PDFInfo
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- CN110124716A CN110124716A CN201910378493.5A CN201910378493A CN110124716A CN 110124716 A CN110124716 A CN 110124716A CN 201910378493 A CN201910378493 A CN 201910378493A CN 110124716 A CN110124716 A CN 110124716A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 4
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000009987 spinning Methods 0.000 claims abstract description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 11
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 11
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 11
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 8
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine powder Natural products NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 6
- 239000010935 stainless steel Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000835 fiber Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 239000000356 contaminant Substances 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 3
- 239000001257 hydrogen Substances 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000010842 industrial wastewater Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- 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—
-
- B01J35/61—
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
A kind of one-step method preparation sheet TiO2/g‑C3N4The method of hetero-junctions includes the following steps: that (1) sequentially adds acetylacetone,2,4-pentanedione and butyl titanate into dehydrated alcohol, obtains solution A；(2) polyvinylpyrrolidone is added into solution A, obtains solution B after dissolution completely；(3) appropriate melamine powder is added into solution B, mixed liquor C is obtained after being completely dissolved；(4) mixed liquor C is fitted into syringe, carries out electrostatic spinning under certain condition, spinning product is collected with stainless steel disc；(5) it after spinning product is dry, is roasted 4 hours at 550 DEG C in air atmosphere.The present invention has method simple and fast, and low in cost, product fibre diameter is small, and large specific surface area is widely used in Photocatalyzed Hydrogen Production and contaminant degradation.
Description
Technical field
The present invention relates to material molding mode technical field, in particular to a kind of one-step method prepares sheet TiO2/g-C3N4It is different
The method of matter knot.
Background technique
Industrial processes generate a large amount of industrial wastewater, these waste water not only pollute environment, and have to human health
Larger harm, it is necessary to can just discharge after treatment.Traditional process for treating industrial waste water mainly includes physical method, chemical method
And bioanalysis, the disadvantages of there are processing capacity is limited and processing cost is higher.
In recent years, photocatalysis oxidation technique is widely used in the processing of industrial wastewater.TiO2Photocatalysis oxidation technique has
Oxidative degradation ability is strong, performance is stable, processing cost is low and the advantages such as without secondary pollution, but its greater band gap (3.2eV), to too
The utilization rate of positive energy is lower.g-C3N4Band gap is relatively narrow (2.7eV), and spectral response range is wider, but its photo-generate electron-hole is easily multiple
It closes.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of one-step method to prepare sheet
TiO2/g-C3N4The method of hetero-junctions has method simple and fast, and low in cost, product fibre diameter is small, large specific surface area, extensively
It is general to be applied to Photocatalyzed Hydrogen Production and contaminant degradation.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of one-step method preparation sheet TiO2/g-C3N4The method of hetero-junctions, includes the following steps:
Step 1: sequentially adding acetylacetone,2,4-pentanedione and butyl titanate into dehydrated alcohol, obtain solution A；
Step 2: polyvinylpyrrolidone being added into solution A, solution B is obtained after being completely dissolved；
Step 3: appropriate melamine powder being added into solution B, mixed liquor C is obtained after being completely dissolved；
Step 4: mixed liquor C being fitted into 5mL syringe, syringe is mounted on electrostatic spinning apparatus, in certain item
Electrostatic spinning is carried out under part, product is collected with stainless steel disc；
Step 5: after spinning product is dry, being roasted 4 hours at 550 DEG C in air atmosphere.
The volume ratio of dehydrated alcohol and acetylacetone,2,4-pentanedione and butyl titanate is between 1:1:1~1:1:3 in the step 1.
Polyvinylpyrrolidone and solution A mass ratio are between 8%~12% in the step 2.
Melamine powder and solution B mass ratio are between 12.5%~17.5% in the step 3.
Spinning condition is voltage 20KV in the step 4, and solution feed speed is 50 μ L/min, receives distance and is
20cm。
Heating rate is 5 DEG C/min in the step 5.
Beneficial effects of the present invention:
Polyethylene glycol oxide of the present invention is soft template, and method is simple and fast, and low in cost, product fibre diameter is small, specific surface
Product is big, is widely used in Photocatalyzed Hydrogen Production and contaminant degradation.
Select polyvinylpyrrolidone for soft template in the present invention, be because are as follows: 1) polyvinylpyrrolidone is to spinning process
Favorably；2) polyvinylpyrrolidone easily removes in annealing process.g-C3N4For narrow gap semiconductor catalyst, TiO2With g-C3N4
In conjunction with hetero-junctions is formed, TiO can reduce2Band gap width, widen TiO2Optical response range, improve TiO2Absorptivity.
TiO2/g-C3N4Hetero-junctions can be realized efficiently separating for electron-hole pair, improve the carrier concentration in photochemical catalyst.This
Outside, lamellar structure can be improved biggish specific surface area, increase active site quantity, to make the photo-catalysis capability of photochemical catalyst
Increase
Detailed description of the invention
Fig. 1 is 20KV, under the conditions of 50 μ L/min, 20cm, obtains TiO2/g-C3N4Hetero-junctions spinning fibre SEM photograph.
Fig. 2 is 20KV, under the conditions of 50 μ L/min, 20cm, roasts 4 hours at 550 DEG C in air atmosphere, obtains sheet
TiO2/g-C3N4Hetero-junctions SEM photograph.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Embodiment 1
1) acetylacetone,2,4-pentanedione is sequentially added into dehydrated alcohol and its volume ratio of butyl titanate is 1:1:3, after mixing
Obtain solution A；
2) polyvinylpyrrolidone that mass ratio is 8% is added into solution A, solution B is obtained after being completely dissolved；
3) melamine powder that mass ratio is 12.5% is added into solution B, obtains mixed liquor C after mixing evenly；
4) mixed liquor C is fitted into 5mL syringe, syringe is mounted on electrostatic spinning apparatus, it is molten in voltage 20KV
Electrostatic spinning is carried out under the conditions of 50 μ L/min of liquid feed speed, reception distance 20cm, product is collected with stainless steel disc；
5) it after product is dry, roasts 4 hours for 550 DEG C in air atmosphere；
Embodiment 2
1) acetylacetone,2,4-pentanedione is sequentially added into dehydrated alcohol and its volume ratio of butyl titanate is 1:1:2, after mixing
Obtain solution A；
2) polyvinylpyrrolidone that mass ratio is 10% is added into solution A, solution B is obtained after being completely dissolved；
3) melamine powder that mass ratio is 15% is added into solution B, obtains mixed liquor C after mixing evenly；
4) mixed liquor C is fitted into 5mL syringe, syringe is mounted on electrostatic spinning apparatus, it is molten in voltage 20KV
Electrostatic spinning is carried out under the conditions of 50 μ L/min of liquid feed speed, reception distance 20cm, product is collected with stainless steel disc；
5) it after product is dry, roasts 4 hours for 550 DEG C in air atmosphere；
Embodiment 3
1) acetylacetone,2,4-pentanedione is sequentially added into dehydrated alcohol and its volume ratio of butyl titanate is 1:1:3, after mixing
Obtain solution A；
2) polyvinylpyrrolidone that mass ratio is 12% is added into solution A, solution B is obtained after being completely dissolved；
3) melamine powder that mass ratio is 17.5% is added into solution B, obtains mixed liquor C after mixing evenly；
4) mixed liquor C is fitted into 5mL syringe, syringe is mounted on electrostatic spinning apparatus, it is molten in voltage 20KV
Electrostatic spinning is carried out under the conditions of 50 μ L/min of liquid feed speed, reception distance 20cm, product is collected with stainless steel disc；
5) it after product is dry, roasts 4 hours for 550 DEG C in air atmosphere；
Construct TiO2/g-C3N4Hetero-junctions can reduce TiO2Band gap width, improve light abstraction width, while reducing light
Raw electron-hole combined efficiency, improves photocatalysis efficiency.
Spinning is carried out under the conditions of 20KV, 50 μ L/min, 20cm as shown in Figure 1: and obtains TiO after spinning product is dry2/g-
C3N4Hetero-junctions spinning fibre SEM photograph.
It is as shown in Figure 2: under the conditions of 20KV, 50 μ L/min, 20cm, to roast 4 hours for 550 DEG C in air atmosphere, obtain piece
Shape TiO2/g-C3N4Hetero-junctions SEM photograph.
Claims (6)
1. a kind of one-step method prepares sheet TiO2/g-C3N4The method of hetero-junctions, which comprises the steps of:
Step 1: sequentially adding acetylacetone,2,4-pentanedione and butyl titanate into dehydrated alcohol, obtain solution A；
Step 2: polyvinylpyrrolidone being added into solution A, solution B is obtained after being completely dissolved；
Step 3: appropriate melamine powder being added into solution B, mixed liquor C is obtained after being completely dissolved；
Step 4: mixed liquor C being fitted into syringe, carries out electrostatic spinning under certain condition, spinning product is received with stainless steel disc
Collection；
Step 5: after spinning product is dry, being roasted 4 hours at 550 DEG C in air atmosphere.
2. a kind of one-step method according to claim 1 prepares sheet TiO2/g-C3N4The method of hetero-junctions, which is characterized in that
The volume ratio of dehydrated alcohol and acetylacetone,2,4-pentanedione and butyl titanate is between 1:1:1~1:1:3 in the step 1.
3. a kind of one-step method according to claim 1 prepares sheet TiO2/g-C3N4The method of hetero-junctions, which is characterized in that
Polyvinylpyrrolidone and the mass ratio of solution A are between 8%~12% in the step 2.
4. a kind of one-step method according to claim 1 prepares sheet TiO2/g-C3N4The method of hetero-junctions, which is characterized in that
Melamine powder and solution B mass ratio are between 12.5%~17.5% in the step 3.
5. a kind of one-step method according to claim 1 prepares sheet TiO2/g-C3N4The method of hetero-junctions, which is characterized in that
Spinning condition is voltage 20KV in the step 4, and solution feed speed is 50 μ L/min, and receiving distance is 20cm.
6. a kind of one-step method according to claim 1 prepares sheet TiO2/g-C3N4The method of hetero-junctions, which is characterized in that
Heating rate is 5 DEG C/min in the step 5.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111185219A (en) * | 2020-03-19 | 2020-05-22 | 东北大学秦皇岛分校 | Preparation method of bismuth vanadate/graphite phase carbon nitride nano-fiber |
| CN111229285A (en) * | 2020-03-24 | 2020-06-05 | 电子科技大学 | ZnO/TiO2/g-C3N4Composite photocatalyst and preparation method thereof |
| CN111330624A (en) * | 2020-03-25 | 2020-06-26 | 陕西科技大学 | One-step method for preparing hierarchical mesoporous-porous TiO2/g-C3N4Nanofiber photocatalytic material |
| CN112708966A (en) * | 2020-12-08 | 2021-04-27 | 四川大学 | Method for preparing two-dimensional lamellar structure nano titanium dioxide fiber through electrostatic spinning |
| CN112915987A (en) * | 2021-01-26 | 2021-06-08 | 宿州学院 | TiO with formaldehyde degrading effect2@C3N4Photocatalyst and preparation method thereof |
| CN113181919A (en) * | 2021-04-27 | 2021-07-30 | 吉林化工学院 | Preparation and application of fibrous cobalt titanate and carbon nitride composite photocatalyst |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111185219A (en) * | 2020-03-19 | 2020-05-22 | 东北大学秦皇岛分校 | Preparation method of bismuth vanadate/graphite phase carbon nitride nano-fiber |
| CN111229285A (en) * | 2020-03-24 | 2020-06-05 | 电子科技大学 | ZnO/TiO2/g-C3N4Composite photocatalyst and preparation method thereof |
| CN111229285B (en) * | 2020-03-24 | 2023-03-14 | 电子科技大学 | ZnO/TiO 2 /g-C 3 N 4 Composite photocatalyst and preparation method thereof |
| CN111330624A (en) * | 2020-03-25 | 2020-06-26 | 陕西科技大学 | One-step method for preparing hierarchical mesoporous-porous TiO2/g-C3N4Nanofiber photocatalytic material |
| CN112708966A (en) * | 2020-12-08 | 2021-04-27 | 四川大学 | Method for preparing two-dimensional lamellar structure nano titanium dioxide fiber through electrostatic spinning |
| CN112915987A (en) * | 2021-01-26 | 2021-06-08 | 宿州学院 | TiO with formaldehyde degrading effect2@C3N4Photocatalyst and preparation method thereof |
| CN113181919A (en) * | 2021-04-27 | 2021-07-30 | 吉林化工学院 | Preparation and application of fibrous cobalt titanate and carbon nitride composite photocatalyst |
| CN113181919B (en) * | 2021-04-27 | 2022-06-07 | 吉林化工学院 | Preparation and application of fibrous cobalt titanate and carbon nitride composite photocatalyst |
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