CN110743604B - Preparation method of organic sewage efficient photodegradation catalyst - Google Patents
Preparation method of organic sewage efficient photodegradation catalyst Download PDFInfo
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- CN110743604B CN110743604B CN201911147571.7A CN201911147571A CN110743604B CN 110743604 B CN110743604 B CN 110743604B CN 201911147571 A CN201911147571 A CN 201911147571A CN 110743604 B CN110743604 B CN 110743604B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 51
- 238000001782 photodegradation Methods 0.000 title claims abstract description 27
- 239000010865 sewage Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 52
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 26
- 238000000227 grinding Methods 0.000 claims abstract description 18
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 17
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 17
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 17
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 239000002002 slurry Substances 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 8
- 239000002351 wastewater Substances 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical group F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 abstract description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract description 4
- 238000011068 loading method Methods 0.000 abstract description 2
- 239000011787 zinc oxide Substances 0.000 abstract description 2
- 239000011941 photocatalyst Substances 0.000 description 5
- 239000003344 environmental pollutant Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000027756 respiratory electron transport chain Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000007704 transition Effects 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
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- B01J35/39—
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a preparation method of an organic sewage high-efficiency photodegradation catalyst, which comprises the steps of grinding fibrous light calcium carbonate to obtain a micron-sized calcium carbonate sheet template, then adding zinc sulfate, carbon nitride and a catalyst, carrying out hydrothermal reaction, drying, grinding to obtain precursor powder, and carrying out high-temperature calcination and natural cooling to obtain the organic sewage high-efficiency photodegradation catalyst. The catalyst is formed by loading nano-scale zinc oxide and carbon nitride on calcium carbonate in a mixed manner, has the characteristics of high efficiency and high speed, and can reach a removal rate of more than 98% for 30min for nitrobenzene under the condition that the use concentration is 0.05-0.2 mg/L.
Description
Technical Field
The invention relates to the technical field of photodegradation catalysts, in particular to a preparation method of an organic sewage high-efficiency photodegradation catalyst.
Background
The photocatalytic degradation is a process of degrading pollutants into inorganic substances completely by utilizing radicals with extremely strong activity generated in a reaction system by radiation and a photocatalyst through the processes of addition, substitution, electron transfer and the like between the radicals and organic pollutants.
The oxidation-reduction mechanism of the photocatalyst is mainly that the photocatalyst absorbs light energy to generate electron transition and generate electron-hole pairs under the action of light irradiation, and the pollutants adsorbed on the surface are directly subjected to oxidation-reduction or hydroxide radicals (OH-) adsorbed on the surface are oxidized to generate hydroxyl radicals (. OH) with strong oxidizing property so as to oxidize the pollutants.
The mechanism of photocatalytic degradation of Halogenated Organic Pollutants (HOPs) is generally characterized by electron transfer, i.e., active species generated by a photoexcited catalyst, such as eaq, eCB or OH, hVB and the like, respectively reduce HOPs into anionic radicals or oxidize HOPs into cationic radicals, and degradation is realized through C-X bond breakage.
In 2009, a new metal-free carbon nitride photocatalyst having a graphite phase was developed, and the oxidation efficiency of the catalyst was low. On the basis of the above, a great deal of related research is carried out at home and abroad, wherein, the Chinese invention patent CN105536846A discloses a titanium dioxide/carbon nitride composite photocatalyst, which effectively improves the capability of separating photo-generated electrons from positive charges and obviously improves the photocatalytic oxidation efficiency. The invention provides a preparation method of an organic sewage high-efficiency photodegradation catalyst, aiming at further improving the photocatalytic oxidation efficiency of the catalyst.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation method of an organic sewage high-efficiency photodegradation catalyst.
The technical scheme of the invention is as follows:
a preparation method of an organic sewage high-efficiency photodegradation catalyst comprises the following steps:
A. adding fibrous light calcium carbonate into ethanol;
B. adding a grinding aid into ethanol, and uniformly dispersing to obtain slurry;
C. repeatedly grinding the slurry, sieving with a 800-mesh sieve, and taking the slurry;
D. adding zinc sulfate, carbon nitride and a catalyst into the slurry, uniformly mixing, placing the mixture into a hydrothermal reactor with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 18-24h at the temperature of 220-250 ℃, evaporating and drying the solution, and grinding to obtain precursor powder;
E. the organic sewage high-efficiency photodegradation catalyst can be obtained after high-temperature calcination and natural cooling.
Preferably, in the step a, the fibrous light calcium carbonate has an aspect ratio of (60-120): 1.
preferably, in the step B, the grinding aid is glycerol.
Preferably, in the step C, the mass concentration of the light calcium carbonate in the slurry is 1-3%.
Preferably, in the step D, the catalyst is hydrogen fluoride.
Preferably, in the step D, the adding amount of the catalyst is 10-20% of the adding amount of zinc sulfate.
Preferably, in the step D, the mass ratio of the added zinc sulfate and the added carbon nitride to the light calcium carbonate in the slurry is (8-15): 100 and (1-2.5): 100.
preferably, in the step E, the temperature of the high-temperature calcination is 500-550 ℃, and the time is 1.5-2 h.
The invention has the advantages that: the preparation method of the organic sewage high-efficiency photodegradation catalyst comprises the steps of grinding fibrous light calcium carbonate to obtain a micron-sized calcium carbonate sheet template, adding zinc sulfate, carbon nitride and the catalyst, carrying out hydrothermal reaction, drying, grinding to obtain precursor powder, and carrying out high-temperature calcination and natural cooling to obtain the organic sewage high-efficiency photodegradation catalyst. The catalyst is formed by loading nano-scale zinc oxide and carbon nitride on calcium carbonate in a mixed manner, has the characteristics of high efficiency and high speed, and can reach a removal rate of more than 98% to 2mg/L nitrobenzene within 30min under the condition that the use concentration is 0.05-0.2 mg/L.
Detailed Description
Example 1
A preparation method of an organic sewage high-efficiency photodegradation catalyst comprises the following steps:
A. adding fibrous light calcium carbonate into ethanol;
B. adding 1.5% glycerol by volume into ethanol, and uniformly dispersing to obtain slurry;
C. repeatedly grinding the slurry, sieving with a 800-mesh sieve, and taking the slurry;
D. adding zinc sulfate, carbon nitride and a catalyst into the slurry, uniformly mixing, placing the mixture into a hydrothermal reactor with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 22 hours at the temperature of 230-240 ℃, evaporating and drying the solution, and grinding to obtain precursor powder;
E. the organic sewage high-efficiency photodegradation catalyst can be obtained after high-temperature calcination and natural cooling.
In the step A, the length-diameter ratio of the fibrous light calcium carbonate is (60-120): 1.
in the step C, the mass concentration of the light calcium carbonate in the slurry is 1.8%.
In the step D, the catalyst is hydrogen fluoride, and the addition amount of the catalyst is 15% of the addition amount of zinc sulfate.
The mass ratio of the added zinc sulfate and the carbon nitride to the light calcium carbonate in the slurry is respectively 12: 100 and 1.8: 100.
in the step E, the high-temperature calcination is carried out at 530 ℃ for 1.8 h.
Example 2
A preparation method of an organic sewage high-efficiency photodegradation catalyst comprises the following steps:
A. adding fibrous light calcium carbonate into ethanol;
B. adding glycerol with the volume ratio of 3.2% into ethanol, and uniformly dispersing to obtain slurry;
C. repeatedly grinding the slurry, sieving with a 800-mesh sieve, and taking the slurry;
D. adding zinc sulfate, carbon nitride and a catalyst into the slurry, uniformly mixing, placing the mixture into a hydrothermal reactor with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 18 hours at the temperature of 240 ℃ and 250 ℃, evaporating and drying the solution, and grinding to obtain precursor powder;
E. the organic sewage high-efficiency photodegradation catalyst can be obtained after high-temperature calcination and natural cooling.
In the step A, the length-diameter ratio of the fibrous light calcium carbonate is (60-120): 1.
in the step C, the mass concentration of the light calcium carbonate in the slurry is 3%.
In the step D, the catalyst is hydrogen fluoride, and the addition amount of the catalyst is 10% of the addition amount of zinc sulfate.
The mass ratio of the addition amount of zinc sulfate and carbon nitride to the light calcium carbonate in the slurry is respectively 15: 100 and 1: 100.
in the step E, the high-temperature calcination is carried out at 550 ℃ for 1.5 h.
Example 3
A preparation method of an organic sewage high-efficiency photodegradation catalyst comprises the following steps:
A. adding fibrous light calcium carbonate into ethanol;
B. adding 1.1% glycerol by volume into ethanol, and dispersing uniformly to obtain slurry;
C. repeatedly grinding the slurry, sieving with a 800-mesh sieve, and taking the slurry;
D. adding zinc sulfate, carbon nitride and a catalyst into the slurry, uniformly mixing, placing the mixture into a hydrothermal reactor with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 24 hours at the temperature of 220-225 ℃, evaporating and drying the solution, and grinding to obtain precursor powder;
E. the organic sewage high-efficiency photodegradation catalyst can be obtained after high-temperature calcination and natural cooling.
In the step A, the length-diameter ratio of the fibrous light calcium carbonate is (60-120): 1.
in the step C, the mass concentration of the light calcium carbonate in the slurry is 1%.
In the step D, the catalyst is hydrogen fluoride, and the addition amount of the catalyst is 20% of the addition amount of zinc sulfate.
The mass ratio of the addition amount of zinc sulfate and carbon nitride to the light calcium carbonate in the slurry is respectively 8: 100 and 2.5: 100.
in the step E, the high-temperature calcination is carried out at the temperature of 500 ℃ for 2 h.
0.5g of the catalyst powder of the above examples 1 to 3 was ball-milled and dispersed in 10L of water to prepare a dispersion, and the dispersion was added to 1L of an organic wastewater in which the contaminant was nitrobenzene. At the moment, the concentration of the catalyst in the water body is 0.1mg/L, the concentration of the nitrobenzene is 2mg/mL, and the sewage is placed at the illumination intensity of 0.51W/m2The Q-SUN aging box with a wavelength of @340nm is respectively tested for 30min, 60min and 120min to test the residual amount of nitrobenzene, and is compared with a comparative example (the catalyst prepared in the example 1 of the Chinese patent CN 105536846A) to obtain the following test data:
the test data show that the organic sewage high-efficiency photodegradation catalyst has a very good photodegradation effect on nitrobenzene, and has a very fast degradation speed.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A preparation method of an organic sewage high-efficiency photodegradation catalyst is characterized by comprising the following steps:
A. adding fibrous light calcium carbonate into ethanol;
B. adding a grinding aid into ethanol, and uniformly dispersing to obtain slurry;
C. repeatedly grinding the slurry, sieving with a 800-mesh sieve, and taking the slurry;
D. adding zinc sulfate, carbon nitride and a catalyst into the slurry, uniformly mixing, placing the mixture into a hydrothermal reactor with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 18-24h at the temperature of 220-250 ℃, evaporating and drying the solution, and grinding to obtain precursor powder;
E. the organic sewage high-efficiency photodegradation catalyst can be obtained after high-temperature calcination and natural cooling;
in the step E, the temperature of the high-temperature calcination is 500-550 ℃, and the time is 1.5-2 h.
2. The method for preparing the catalyst for high efficiency photodegradation of organic wastewater according to claim 1, wherein in the step A, the fibrous light calcium carbonate has an aspect ratio of (60-120): 1.
3. the method for preparing the catalyst for efficiently photodegradation of organic wastewater according to claim 1, wherein in the step B, the grinding aid is glycerol.
4. The method for preparing the catalyst for high efficiency photodegradation of organic wastewater according to claim 1, wherein in the step C, the slurry contains light calcium carbonate with a mass concentration of 1-3%.
5. The method according to claim 1, wherein in step D, the catalyst is hydrogen fluoride.
6. The method for preparing the catalyst for high efficiency photodegradation of organic wastewater according to claim 1, wherein in the step D, the addition amount of the catalyst is 10-20% of the addition amount of zinc sulfate.
7. The method for preparing the catalyst for high efficiency photodegradation of organic wastewater according to claim 1, wherein in the step D, the mass ratio of the zinc sulfate and the carbon nitride to the light calcium carbonate in the slurry is (8-15): 100 and (1-2.5): 100.
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CN105170170A (en) * | 2015-07-27 | 2015-12-23 | 江苏大学 | g-C3N4-ZnO/HNTs composite photocatalyst, preparation method therefor and application thereof |
CN105536846A (en) * | 2016-01-19 | 2016-05-04 | 南京工业大学 | Photodegradable catalyst for organic sewage treatment and preparation method of photodegradable catalyst |
CN106563485A (en) * | 2016-11-08 | 2017-04-19 | 江苏大学 | Carbon nitride/potassium calcium niobate composite material and preparing method and application thereof |
CN106964386A (en) * | 2017-02-23 | 2017-07-21 | 江苏大学 | A kind of preparation method of visible-light response type composite photo-catalyst |
CN108772095A (en) * | 2018-07-13 | 2018-11-09 | 中国计量大学 | A kind of preparation method of efficient degradation antibiotic visible light catalytic composite material |
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US10532939B2 (en) * | 2017-04-19 | 2020-01-14 | King Abdulaziz University | Composite, a method of making thereof, and a method for degrading a pollutant |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN105170170A (en) * | 2015-07-27 | 2015-12-23 | 江苏大学 | g-C3N4-ZnO/HNTs composite photocatalyst, preparation method therefor and application thereof |
CN105536846A (en) * | 2016-01-19 | 2016-05-04 | 南京工业大学 | Photodegradable catalyst for organic sewage treatment and preparation method of photodegradable catalyst |
CN106563485A (en) * | 2016-11-08 | 2017-04-19 | 江苏大学 | Carbon nitride/potassium calcium niobate composite material and preparing method and application thereof |
CN106964386A (en) * | 2017-02-23 | 2017-07-21 | 江苏大学 | A kind of preparation method of visible-light response type composite photo-catalyst |
CN108772095A (en) * | 2018-07-13 | 2018-11-09 | 中国计量大学 | A kind of preparation method of efficient degradation antibiotic visible light catalytic composite material |
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