CN113559906A - Method for preparing semiconductor coupling composite photocatalyst for treating refractory wastewater - Google Patents
Method for preparing semiconductor coupling composite photocatalyst for treating refractory wastewater Download PDFInfo
- Publication number
- CN113559906A CN113559906A CN202110822107.4A CN202110822107A CN113559906A CN 113559906 A CN113559906 A CN 113559906A CN 202110822107 A CN202110822107 A CN 202110822107A CN 113559906 A CN113559906 A CN 113559906A
- Authority
- CN
- China
- Prior art keywords
- reaction
- composite photocatalyst
- semiconductor
- preparing
- product
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004065 semiconductor Substances 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 40
- 239000002351 wastewater Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000008878 coupling Effects 0.000 title claims abstract description 19
- 238000010168 coupling process Methods 0.000 title claims abstract description 19
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 28
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 12
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims description 47
- 239000000047 product Substances 0.000 claims description 30
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- 239000003960 organic solvent Substances 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000005457 ice water Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 3
- 101710134784 Agnoprotein Proteins 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims 1
- 230000000630 rising effect Effects 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000004043 dyeing Methods 0.000 description 5
- 238000007639 printing Methods 0.000 description 5
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 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
- 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
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (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
The invention discloses a method for preparing a semiconductor coupling composite photocatalyst for treating refractory wastewater, wherein the semiconductor coupling composite photocatalyst is PPy/Ag/g-C3N4The preparation method comprises the following steps: (1) nano-layered g-C3N4Preparing; (2) Ag/g-C3N4Preparing; (3) semiconductor coupling composite photocatalyst PPy/Ag/g-C3N4And (4) preparing. The invention has the advantages that the nano-layered g-C is finished by one-step calcination of urea3N4Preparation of (A) havingThe preparation method has the advantages that the specific surface area is higher, the integral photocatalytic activity is improved, the introduction of ppy is realized through sodium dodecyl benzene sulfonate and ferric trichloride subsequently, the preparation method is simple, the cost of raw materials is low, and the purity of the finished product obtained subsequently is high.
Description
Technical Field
The invention relates to the technical field of photocatalysts, in particular to a method for preparing a semiconductor coupled composite photocatalyst for treating refractory wastewater.
Background
The dye wastewater mainly comprises dye production wastewater and printing and dyeing industrial wastewater. At present, the dye mainly takes aromatic hydrocarbon and heterocyclic compounds as parent bodies and is provided with a chromogenic group and a color assisting group. The structure of the dye is increasingly complex, and the property is more and more stable, so that the treatment of the dye wastewater is more difficult. The dye wastewater has the characteristics of complex components, high chromaticity, large change of water quality and water quantity, more difficultly-degraded substances and the like. The printing and dyeing wastewater is extremely polluted, and the discharge amount of the printing and dyeing wastewater accounts for 1/10 which is the total discharge amount of industrial wastewater. Therefore, the comprehensive treatment of the printing and dyeing wastewater becomes a problem which needs to be solved urgently. Among them, methyl orange is a common pollutant in printing and dyeing wastewater, and with the increasing prominence of the problem of water environment pollution, the problem of degradation of organic pollutants of methyl orange in water becomes the key point of environmental chemistry research. Therefore, the reasonable treatment of the methyl orange in the wastewater is an important link. At present, the photocatalytic technology has been widely used for the technology of wastewater treatment studied in the environment. People modify semiconductors and compound semiconductors to treat environmental pollution, and particularly solve the problem of photodegradation activity limited to an ultraviolet region, so that the modified semiconductors can effectively treat pollutants such as wastewater, waste gas and the like in life under visible light.
Existing semiconductor coupling composite photocatalyst PPy/Ag/g-C3N4The composite material is formed by combining noble metal, semiconductor and conductive polymer, the PPy is used as an organic semiconductor, Ag conductivity and other self advantages to form an electron-hole rapid separation system with carbon nitride, the effect of synergistic photocatalytic degradation is achieved, the absorption and utilization of light are enhanced, the photocatalytic degradation capability of the system is promoted, and the existing PPy/Ag/g-C3N4The preparation method is complex, has more impurities and high cost, and is difficult to obtain a high-purity sample.
Disclosure of Invention
The invention aims to provide a method for preparing a semiconductor coupled composite photocatalyst for treating refractory wastewater, which is simple and effective and has lower cost and higher purity.
The technical purpose of the invention is realized by the following technical scheme:
a method for preparing a semiconductor coupled composite photocatalyst for treating refractory wastewater is characterized in that the semiconductor coupled composite photocatalyst is PPy/Ag/g-C3N4The preparation method comprises the following steps:
(1) nano-layered g-C3N4The preparation of (1): weighing urea, grinding, placing the ground urea in an alumina crucible for calcination, keeping the temperature for reaction for a period of time, finishing the reaction, naturally cooling the alumina crucible to room temperature, placing the calcined blocky product in absolute ethyl alcohol for ultrasonic dispersion, then performing centrifugal separation and drying to obtain the nano-layered g-C3N4；
（2）Ag/g-C3N4The preparation of (1): taking the nano-layered g-C prepared in the step (1)3N4Adding organic solvent, stirring, ultrasonic dispersing, and collecting AgNO3The same organic solvent is adopted to prepare AgNO3The solution is again AgNO3The solution is dropwise added into the nano-layered g-C3N4Stirring the dispersion liquid at room temperature, pouring the mixed solution into a reaction kettle for reaction, cooling the reaction product to the room temperature after the reaction is finished, washing the product obtained by the reaction for a plurality of times by using deionized water and absolute ethyl alcohol, and freeze-drying the product to obtain the product Ag/g-C3N4；
(3) Semiconductor coupling composite photocatalyst PPy/Ag/g-C3N4The preparation of (1): taking Ag/g-C prepared in the step (2)3N4Dissolving the semiconductor coupling composite photocatalyst and sodium dodecyl benzene sulfonate in ultrapure water, dripping pyrrole under the ice-water bath condition after ultrasonic dispersion, taking a ferric trichloride solution to drip and drip after slow stirring reaction, standing for reaction for 1h after dripping, washing the product for a plurality of times by deionized water and absolute ethyl alcohol after suction filtration to obtain a product, and drying the product to obtain the semiconductor coupling composite photocatalyst PPy/Ag/g-C3N4。
Preferably, the urea in the step (1) needs to be pre-dried before grinding, the drying temperature is 75-82 ℃, and the drying time is 16-18 h.
Preferably, the calcination temperature in the step (1) is 480-520 ℃, the temperature rise speed is 2.5-3.2 ℃/min, and the heat preservation time is 2-2.5 h.
Preferably, the ultrasonic dispersion time in the step (1) is 12-16h, and the centrifugal rotation speed is controlled at 3500-4000 rmp.
Preferably, the organic solvent in (2) is selected from one of absolute ethyl alcohol, acetone or isopropanol.
Preferably, AgNO in the (2)3、g-C3N4The dosage ratio of the organic solvent to the total organic solvent is as follows: 0.009-0.099g of 1g and 80-140mL of the total weight.
Preferably, the reaction kettle in the step (2) is filled with nitrogen for protection, the reaction temperature is 500-550 ℃, and the reaction time is 2-3 h.
Preferably, Ag/g-C in the (3)3N4The mass ratio of the sodium dodecyl benzene sulfonate and the sodium dodecyl benzene sulfonate is 400-420:1, and the ultrasonic dispersion time is 30-45 min.
Preferably, Ag/g-C in the (3)3N4The dosage ratio of pyrrole to ferric trichloride is: 1g of 2-3 mu L of 0.015-0.02 g.
In conclusion, the beneficial effects of the invention are as follows: the invention completes the preparation of the nano-layered g-C by one-step calcination of urea3N4The preparation method has the advantages that the specific surface area is higher, the integral photocatalytic activity is improved, the introduction of ppy is realized through sodium dodecyl benzene sulfonate and ferric trichloride subsequently, the preparation method is simple, the cost of raw materials is low, and the purity of the finished product obtained subsequently is high.
Detailed Description
The following is further described with reference to specific embodiments, which are not intended to limit the invention.
Example 1
A method for preparing a semiconductor coupled composite photocatalyst for treating refractory wastewater is characterized in that the semiconductor coupled composite photocatalyst is PPy/Ag/g-C3N4The preparation method comprises the following steps:
(1) nano-layered g-C3N4The preparation of (1): weighing urea, pre-drying at 80 deg.C for 16 hr, and dryingGrinding, namely putting the ground urea into an alumina crucible for calcination, wherein the calcination temperature is 490 ℃, the heating rate is 2.5 ℃/min, the heat preservation time is 2h, naturally cooling the alumina crucible to room temperature after the reaction is finished, putting the calcined blocky product into absolute ethyl alcohol for ultrasonic dispersion, the ultrasonic dispersion time is 12h, then carrying out centrifugal separation and drying to obtain the nano-layered g-C3N4The centrifugal speed was controlled at 3500 rmp.
（2）Ag/g-C3N4The preparation of (1): taking 5g of nano-layered g-C prepared in the step (1)3N4Adding anhydrous ethanol, stirring, and ultrasonically dispersing to obtain 0.045g AgNO3The same organic solvent is adopted to prepare AgNO3The solution is again AgNO3The solution is dropwise added into the nano-layered g-C3N4In the dispersion liquid, the total volume of an organic solvent is 500mL, stirring is carried out at room temperature, then the mixed solution is poured into a reaction kettle for reaction, nitrogen is filled into the reaction kettle for protection, the reaction temperature is 550 ℃, the reaction time is 2 hours, the mixed solution is cooled to room temperature after the reaction is finished, a product obtained after the reaction is washed for a plurality of times by deionized water and absolute ethyl alcohol and then is freeze-dried, and the product Ag/g-C is obtained3N4。
(3) Semiconductor coupling composite photocatalyst PPy/Ag/g-C3N4The preparation of (1): taking the Ag/g-C prepared in the step (2) of 8g3N4Dissolving 0.02g of sodium dodecyl benzene sulfonate in ultrapure water, performing ultrasonic dispersion for 30min, then dripping 20 mu L of pyrrole in an ice-water bath condition, slowly stirring for reaction, then dropwise adding a ferric trichloride solution, wherein the weight of ferric trichloride is 0.13g, standing for reaction for 1h after the dropwise adding is finished, performing suction filtration to obtain a product, washing the product for several times by using deionized water and absolute ethyl alcohol, and drying to obtain the semiconductor coupled composite photocatalyst PPy/Ag/g-C3N4The purity was 97.8%.
Example 2
A method for preparing a semiconductor coupled composite photocatalyst for treating refractory wastewater is characterized in that the semiconductor coupled composite photocatalyst is PPy/Ag/g-C3N4The preparation method comprises the following steps:
(1) nano-layered g-C3N4The preparation of (1): weighing urea, pre-drying at 77 ℃ for 17h, grinding, calcining in an alumina crucible at 500 ℃ at 3.0 ℃/min for 2.5h, naturally cooling to room temperature, ultrasonically dispersing the calcined massive product in absolute ethyl alcohol for 14h, centrifuging, and drying to obtain the nano-layered g-C3N4The centrifugal speed was controlled at 4000 rmp.
（2）Ag/g-C3N4The preparation of (1): taking 5g of nano-layered g-C prepared in the step (1)3N4Adding acetone, stirring, and ultrasonically dispersing to obtain 0.01g AgNO3The same organic solvent is adopted to prepare AgNO3The solution is again AgNO3The solution is dropwise added into the nano-layered g-C3N4In the dispersion liquid, the total volume of an organic solvent is 400mL, stirring is carried out at room temperature, then the mixed solution is poured into a reaction kettle for reaction, nitrogen is filled into the reaction kettle for protection, the reaction temperature is 520 ℃, the reaction time is 3 hours, the mixed solution is cooled to room temperature after the reaction is finished, a product obtained after the reaction is washed for a plurality of times by deionized water and absolute ethyl alcohol and then is freeze-dried, and the product Ag/g-C is obtained3N4。
(3) Semiconductor coupling composite photocatalyst PPy/Ag/g-C3N4The preparation of (1): taking the Ag/g-C prepared in the step (2) of 8g3N4Dissolving the semiconductor coupling composite photocatalyst and 0.0195g of sodium dodecyl benzene sulfonate in ultrapure water, performing ultrasonic dispersion for 40min, then dripping 24 mu L of pyrrole in ice-water bath, slowly stirring for reaction, then dropwise adding ferric trichloride solution, wherein the weight of ferric trichloride is 0.15g, standing for reaction for 1h after the dropwise adding is finished, performing suction filtration to obtain a product, washing the product for a plurality of times by using deionized water and absolute ethyl alcohol, and drying to obtain the semiconductor coupling composite photocatalyst PPy/Ag/g-C3N4The purity was 98.1%.
Example 3
Semiconductor coupling composite photocatalyst for treating refractory wastewaterThe method of the agent is characterized in that the semiconductor coupling composite photocatalyst is PPy/Ag/g-C3N4The preparation method comprises the following steps:
(1) nano-layered g-C3N4The preparation of (1): weighing urea, pre-drying at 82 ℃ for 17h, grinding, calcining in an alumina crucible at 480 ℃, heating at 3.2 ℃/min for 2.5h, naturally cooling to room temperature after the reaction is finished, ultrasonically dispersing the calcined massive product in absolute ethyl alcohol for 16h, centrifuging, and drying to obtain the nano-layered g-C3N4The centrifugal speed was controlled at 3800 rmp.
（2）Ag/g-C3N4The preparation of (1): taking 5g of nano-layered g-C prepared in the step (1)3N4Adding isopropanol, stirring, ultrasonically dispersing, and collecting 0.45g AgNO3The same organic solvent is adopted to prepare AgNO3The solution is again AgNO3The solution is dropwise added into the nano-layered g-C3N4In the dispersion liquid, the total volume of an organic solvent is 700mL, stirring is carried out at room temperature, then the mixed solution is poured into a reaction kettle for reaction, nitrogen is filled into the reaction kettle for protection, the reaction temperature is 550 ℃, the reaction time is 2 hours, the mixed solution is cooled to room temperature after the reaction is finished, a product obtained after the reaction is washed for a plurality of times by deionized water and absolute ethyl alcohol and then is freeze-dried, and the product Ag/g-C is obtained3N4。
(3) Semiconductor coupling composite photocatalyst PPy/Ag/g-C3N4The preparation of (1): taking the Ag/g-C prepared in the step (2) of 8g3N4Dissolving the semiconductor coupling composite photocatalyst and 0.0191g of sodium dodecyl benzene sulfonate in ultrapure water, performing ultrasonic dispersion for 45min, then dripping 16 mu L of pyrrole in ice-water bath, slowly stirring for reaction, then dropwise adding ferric trichloride solution, wherein the weight of ferric trichloride is 0.16g, standing for reaction for 1h after the dropwise adding is finished, performing suction filtration to obtain a product, washing the product for a plurality of times by using deionized water and absolute ethyl alcohol, and drying to obtain the semiconductor coupling composite photocatalyst PPy/Ag/g-C3N4，The purity was 97.5%.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention.
Claims (9)
1. A method for preparing a semiconductor coupled composite photocatalyst for treating refractory wastewater is characterized in that the semiconductor coupled composite photocatalyst is PPy/Ag/g-C3N4The preparation method comprises the following steps:
(1) nano-layered g-C3N4The preparation of (1): weighing urea, grinding, placing the ground urea in an alumina crucible for calcination, keeping the temperature for reaction for a period of time, finishing the reaction, naturally cooling the alumina crucible to room temperature, placing the calcined blocky product in absolute ethyl alcohol for ultrasonic dispersion, then performing centrifugal separation and drying to obtain the nano-layered g-C3N4；
（2）Ag/g-C3N4The preparation of (1): taking the nano-layered g-C prepared in the step (1)3N4Adding organic solvent, stirring, ultrasonic dispersing, and collecting AgNO3The same organic solvent is adopted to prepare AgNO3The solution is again AgNO3The solution is dropwise added into the nano-layered g-C3N4Stirring the dispersion liquid at room temperature, pouring the mixed solution into a reaction kettle for reaction, cooling the reaction product to the room temperature after the reaction is finished, washing the product obtained by the reaction for a plurality of times by using deionized water and absolute ethyl alcohol, and freeze-drying the product to obtain the product Ag/g-C3N4；
(3) Semiconductor coupling composite photocatalyst PPy/Ag/g-C3N4The preparation of (1): taking Ag/g-C prepared in the step (2)3N4Dissolving with sodium dodecyl benzene sulfonate in ultrapure water, ultrasonically dispersing, dripping pyrrole in ice water bath, slowly stirring for reaction, dripping ferric trichloride solution, and drippingStanding for reaction for 1h after the reaction is finished, performing suction filtration to obtain a product, washing the product for a plurality of times by using deionized water and absolute ethyl alcohol, and drying the product to obtain the semiconductor coupled composite photocatalyst PPy/Ag/g-C3N4。
2. The method for preparing the semiconductor-coupled composite photocatalyst for treating refractory wastewater as claimed in claim 1, wherein the method comprises the following steps: the urea in the step (1) needs to be pre-dried before grinding, the drying temperature is 75-82 ℃, and the drying time is 16-18 h.
3. The method for preparing the semiconductor-coupled composite photocatalyst for treating refractory wastewater as claimed in claim 1, wherein the method comprises the following steps: the calcination temperature in the step (1) is 480-520 ℃, the temperature rising speed is 2.5-3.2 ℃/min, and the heat preservation time is 2-2.5 h.
4. The method for preparing the semiconductor-coupled composite photocatalyst for treating refractory wastewater as claimed in claim 1, wherein the method comprises the following steps: the ultrasonic dispersion time in the step (1) is 12-16h, and the centrifugal rotation speed is controlled at 3500-4000 rmp.
5. The method for preparing the semiconductor-coupled composite photocatalyst for treating refractory wastewater as claimed in claim 1, wherein the method comprises the following steps: the organic solvent in (2) is selected from one of absolute ethyl alcohol, acetone or isopropanol.
6. The method for preparing the semiconductor-coupled composite photocatalyst for treating refractory wastewater as claimed in claim 1, wherein the method comprises the following steps: AgNO in the (2)3、g-C3N4The dosage ratio of the organic solvent to the total organic solvent is as follows: 0.009-0.099g of 1g and 80-140mL of the total weight.
7. The method for preparing the semiconductor-coupled composite photocatalyst for treating refractory wastewater as claimed in claim 1, wherein the method comprises the following steps: and (3) filling nitrogen into the reaction kettle in the step (2) for protection, wherein the reaction temperature is 500-550 ℃, and the reaction time is 2-3 h.
8. The method for preparing the semiconductor-coupled composite photocatalyst for treating refractory wastewater as claimed in claim 1, wherein the method comprises the following steps: Ag/g-C in the above (3)3N4The mass ratio of the sodium dodecyl benzene sulfonate and the sodium dodecyl benzene sulfonate is 400-420:1, and the ultrasonic dispersion time is 30-45 min.
9. The method for preparing the semiconductor-coupled composite photocatalyst for treating refractory wastewater as claimed in claim 1, wherein the method comprises the following steps: Ag/g-C in the above (3)3N4The dosage ratio of pyrrole to ferric trichloride is: 1g of 2-3 mu L of 0.015-0.02 g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110822107.4A CN113559906A (en) | 2021-07-21 | 2021-07-21 | Method for preparing semiconductor coupling composite photocatalyst for treating refractory wastewater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110822107.4A CN113559906A (en) | 2021-07-21 | 2021-07-21 | Method for preparing semiconductor coupling composite photocatalyst for treating refractory wastewater |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113559906A true CN113559906A (en) | 2021-10-29 |
Family
ID=78165856
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110822107.4A Pending CN113559906A (en) | 2021-07-21 | 2021-07-21 | Method for preparing semiconductor coupling composite photocatalyst for treating refractory wastewater |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113559906A (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103623855A (en) * | 2013-11-12 | 2014-03-12 | 江苏大学 | Method for preparing carbon nitride/silver nano composite material by reduction with chemical reducer |
| CN106076384A (en) * | 2016-06-12 | 2016-11-09 | 江苏大学 | A kind of tri compound catalysis material and its production and use |
| CN108059230A (en) * | 2017-12-22 | 2018-05-22 | 南京工业大学 | Deep catalytic oxidation device for high-organic-matter wastewater treatment |
| US20180194620A1 (en) * | 2017-01-11 | 2018-07-12 | Baker Hughes, A Ge Company, Llc | Thin film substrates including crosslinked carbon nanostructures and related methods |
| CN108499587A (en) * | 2017-02-25 | 2018-09-07 | 北京化工大学 | Ag/g-C3N4The preparation of composite visible light catalyst |
| CN111018041A (en) * | 2019-12-19 | 2020-04-17 | 南华大学 | Preparation method and application of polypyrrole graphite phase carbon nitride composite material for treating uranium-containing wastewater through photocatalytic reduction |
| CN112547108A (en) * | 2020-12-11 | 2021-03-26 | 江南大学 | Ternary composite photocatalyst for antibiotic pollution degradation and preparation method thereof |
| CN112973750A (en) * | 2021-01-29 | 2021-06-18 | 南京工业大学 | Carbon quantum dot coated metal monoatomic-carbon nitride composite material and preparation method thereof |
-
2021
- 2021-07-21 CN CN202110822107.4A patent/CN113559906A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103623855A (en) * | 2013-11-12 | 2014-03-12 | 江苏大学 | Method for preparing carbon nitride/silver nano composite material by reduction with chemical reducer |
| CN106076384A (en) * | 2016-06-12 | 2016-11-09 | 江苏大学 | A kind of tri compound catalysis material and its production and use |
| US20180194620A1 (en) * | 2017-01-11 | 2018-07-12 | Baker Hughes, A Ge Company, Llc | Thin film substrates including crosslinked carbon nanostructures and related methods |
| CN108499587A (en) * | 2017-02-25 | 2018-09-07 | 北京化工大学 | Ag/g-C3N4The preparation of composite visible light catalyst |
| CN108059230A (en) * | 2017-12-22 | 2018-05-22 | 南京工业大学 | Deep catalytic oxidation device for high-organic-matter wastewater treatment |
| CN111018041A (en) * | 2019-12-19 | 2020-04-17 | 南华大学 | Preparation method and application of polypyrrole graphite phase carbon nitride composite material for treating uranium-containing wastewater through photocatalytic reduction |
| CN112547108A (en) * | 2020-12-11 | 2021-03-26 | 江南大学 | Ternary composite photocatalyst for antibiotic pollution degradation and preparation method thereof |
| CN112973750A (en) * | 2021-01-29 | 2021-06-18 | 南京工业大学 | Carbon quantum dot coated metal monoatomic-carbon nitride composite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| ZHU, ZHI ET AL. * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105080528A (en) | Preparation method of preformed diatomite loaded TiO2 and rare earth doped TiO2 photocatalyst | |
| CN105148975B (en) | Application of a Potassium-doped Mesoporous g‑C3N4 Photocatalytic Material in the Degradation of Organic Dye Wastewater | |
| CN1319640C (en) | Method for preparing active fly ash phosphorus adsorbent | |
| CN105664835A (en) | Batch preparation method of porous carbon nitride material under assistance of organic carboxylic acid | |
| CN101549895A (en) | Preparation method of carbon aerogel load titanium dioxide electrodes and application thereof | |
| CN103991945B (en) | A kind of method of PVA in fast degradation water | |
| CN102532045B (en) | A kind of method that is raw material production cyanuric acid with urea | |
| CN104909427A (en) | Construction and application method of photoassisted porous copper bismuthate activated persulfate water treatment high-grade oxidation technology | |
| CN107617393B (en) | A phosgene reactor for carbon tetrachloride treatment equipment | |
| CN103041795A (en) | Preparation method of titanium dioxide photocatalyst | |
| CN108097310B (en) | C for effectively degrading methylene blue dye wastewater3N4Preparation method of/agar composite aerogel photocatalytic material | |
| CN104607214B (en) | A kind of visible light-responded AgBr/TiO2The preparation method of catalyst | |
| CN102583636B (en) | Mixed nanometer cobalt titanium dioxide/chitosan compound microsphere photodissociation organophosphorus pesticide wastewater | |
| CN105944710A (en) | A kind of quartz sand supported lanthanum titanate photocatalyst and preparation method thereof | |
| CN105883804A (en) | Preparation method of porous carbon nanomaterial for adsorbing methylene blue | |
| CN100594976C (en) | Preparation method of nano-titanium dioxide photocatalytic indoor purifier | |
| CN106391043A (en) | Preparation method and application of Fe-Mn bi-component catalyst supported by modified attapulgite | |
| CN106185923A (en) | A kind of inorganic salt template auxiliary method preparing porous carbon nano material and application thereof | |
| CN113559906A (en) | Method for preparing semiconductor coupling composite photocatalyst for treating refractory wastewater | |
| CN112473733B (en) | Mo-Eu co-doped titanium dioxide/aluminum phosphate molecular sieve composite photocatalyst and application thereof | |
| CN107096497A (en) | A kind of preparation method of high activity attapulgite | |
| CN102274727B (en) | A kind of drinking water purification agent and preparation method thereof | |
| CN109351329A (en) | Zeolite modified activated coke adsorption material and preparation method and application thereof | |
| CN107739049A (en) | A kind of black Bi4Ti3O12The preparation method and applications of material | |
| CN118221128A (en) | Nuclear grade boron-10 acid purification process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211029 |