CN107983413B - Fullerene composite photocatalyst for environmental pollution treatment - Google Patents
Fullerene composite photocatalyst for environmental pollution treatment Download PDFInfo
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- CN107983413B CN107983413B CN201711322953.XA CN201711322953A CN107983413B CN 107983413 B CN107983413 B CN 107983413B CN 201711322953 A CN201711322953 A CN 201711322953A CN 107983413 B CN107983413 B CN 107983413B
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 51
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000003912 environmental pollution Methods 0.000 title claims description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 105
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims abstract description 24
- -1 amino ferrocene Chemical compound 0.000 claims abstract description 20
- CTSLXHKWHWQRSH-UHFFFAOYSA-N oxalyl chloride Chemical compound ClC(=O)C(Cl)=O CTSLXHKWHWQRSH-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000001291 vacuum drying Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 14
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 11
- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 claims abstract description 10
- MSFXUHUYNSYIDR-UHFFFAOYSA-N 4-[4,6-bis(4-carboxyphenyl)-1,3,5-triazin-2-yl]benzoic acid Chemical compound C1=CC(C(=O)O)=CC=C1C1=NC(C=2C=CC(=CC=2)C(O)=O)=NC(C=2C=CC(=CC=2)C(O)=O)=N1 MSFXUHUYNSYIDR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 8
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 8
- 238000010025 steaming Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 230000004298 light response Effects 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- RBTKNAXYKSUFRK-UHFFFAOYSA-N heliogen blue Chemical compound [Cu].[N-]1C2=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=NC([N-]1)=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=N2 RBTKNAXYKSUFRK-UHFFFAOYSA-N 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
- B01J31/30—Halides
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a preparation method of a fullerene-based composite photocatalyst, which comprises the following steps: 1) dissolving 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine in dichloromethane, dropwise adding oxalyl chloride into the dichloromethane, stirring for 3-4h, dropwise adding a dichloromethane solution of amino ferrocene with the mass fraction of 20-30%, stirring and reacting for 30-36h at 40-50 ℃, washing the reaction product for 3-5 times by using a KOH solution with the mass fraction of 10-20%, and collecting a dichloromethane layer. Rotary steaming, washing and drying; 2) dissolving the product prepared in the step 1) in a solvent, adding amino modified fullerene and 1,3, 5-triglycidyl-S-triazine trione, stirring and reacting at 70-80 ℃ for 5-7 hours, adding copper chloride, performing rotary evaporation, and drying in a vacuum drying oven at 50-60 ℃ for 8-10 hours; the invention also discloses the fullerene-based composite photocatalyst prepared by the preparation method; the fullerene-based composite photocatalyst disclosed by the invention has the advantages of wide visible light response range, high photocatalytic activity and good stability.
Description
Technical Field
The invention belongs to the technical field of novel materials of environmental purification photocatalysts, relates to a photocatalyst and a preparation method thereof, and particularly relates to a fullerene-based composite photocatalyst with visible light response and a preparation method thereof.
Background
In recent years, with the rapid development of industry, the environmental pollution problem, which is one of the important factors restricting the development and progress of society, is becoming serious, and wastewater treatment becomes one of the problems to be solved urgently in the industry. The waste water contains a large amount of organic pollutants with complex components, high toxicity, high chromaticity and poor biochemical degradability, and how to treat the organic pollutants is always a difficult problem in waste water treatment. In order to solve the problem, various environment purification catalyst materials are produced, wherein the photocatalyst is used as a novel energy-saving green environment-friendly catalyst, has a wide application prospect in the field of environmental pollution treatment, and becomes an ideal environment pollution treatment catalyst.
Compared with the traditional catalyst, the photocatalyst can directly utilize sunlight to deeply mineralize pollutants without generating secondary pollution. Of the numerous semiconductor photocatalytic materials, titanium dioxide (TiO)2) Due to the advantages of strong light corrosion resistance, high stability, relatively low price, no toxicity to human bodies and the like, the method draws the attention of a plurality of experts and scholars. However, TiO is currently used in view of the utilization rate of solar energy2And the method cannot be popularized and applied in a large scale in actual industrial water treatment because the method only has response in an ultraviolet light range and has low utilization rate to visible light.
Therefore, the development of visible light-responsive photocatalysts and the search for novel highly efficient catalysts are gradually progressing
Become the hot spot of the current research.
Disclosure of Invention
The invention aims to solve the problems and provides the fullerene-based composite photocatalyst which is wide in visible light response range, high in photocatalytic activity, good in stability and low in manufacturing cost.
In order to achieve the above object, the present invention provides the following technical solution, a preparation method of a fullerene-based composite photocatalyst, comprising the following steps:
1) dissolving 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine in dichloromethane at room temperature, dropwise adding oxalyl chloride into the dichloromethane, stirring for 3-4h, dropwise adding a dichloromethane solution of amino ferrocene with the mass fraction of 20-30%, stirring and reacting for 30-36h at 40-50 ℃, washing the reaction product for 3-5 times by using a KOH solution with the mass fraction of 10-20%, and collecting a dichloromethane layer. Washing with ethyl acetate, ethanol and n-hexane for 5-8 times, rotary steaming, and drying in vacuum drying oven at 60-80 deg.C for 15-20 hr;
2) dissolving the product prepared in the step 1) in a solvent, adding amino modified fullerene and 1,3, 5-triglycidyl-S-triazine trione, stirring and reacting at 70-80 ℃ for 5-7 hours, adding copper chloride, removing the solvent by rotary evaporation, and drying in a vacuum drying oven at 50-60 ℃ for 8-10 hours;
wherein the mass ratio of the dichloromethane solution of the 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine, dichloromethane, oxalyl chloride and amino ferrocene in the step 1) is (1-2): (10-20):1: (5-8);
the solvent is selected from one or more of ethanol, n-butanol, dichloromethane and diethyl ether;
in the step 2), the mass ratio of the product prepared in the step 1), the solvent, the amino modified fullerene, the 1,3, 5-triglycidyl-S-triazine trione and the copper chloride is (1-2): (10-15): (3-5): (1-2): (0.1-0.2);
the fullerene-based composite photocatalyst is prepared by the preparation method of the fullerene-based composite photocatalyst.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
(1) the fullerene-based composite photocatalyst provided by the invention is simple and feasible in preparation method, low in equipment requirement, easily available in raw materials and low in price.
(2) The fullerene-based composite photocatalyst provided by the invention combines the advantages of fullerene, ferrocene and triazine photocatalysts, and has the excellent characteristics of wide visible light response range, high photocatalytic activity and good stability.
(3) According to the fullerene-based composite photocatalyst provided by the invention, fullerene and triazine conjugated compounds are adopted to pass through chemical bonds, and fullerene passes through host-guest interaction through ferrocene, so that the photocatalyst is high in stability, and has a more excellent photocatalytic effect through copper chloride doping.
(4) The fullerene-based composite photocatalyst provided by the invention provides more surface active sites, and is beneficial to separation of photo-generated electrons and holes.
(5) The fullerene-based composite photocatalyst provided by the invention can well adsorb organic dye, greatly enhance the utilization and capture capacity of light, reduce the forbidden bandwidth of the photocatalytic material due to the transmission of electrons between two phases, expand the spectrum range of sunlight utilized by the photocatalytic material, have good absorption and response in a visible light region, and enhance the photocatalytic effect.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the following provides a detailed description of the product of the present invention with reference to the examples.
Example 1
A preparation method of a fullerene-based composite photocatalyst comprises the following steps:
1) dissolving 100g of 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine in 1000g of dichloromethane at room temperature, dropwise adding 100g of oxalyl chloride, stirring for 3h, dropwise adding 500g of dichloromethane solution of amino ferrocene with the mass fraction of 20%, stirring at 40 ℃ for reaction for 30h, washing the reaction product for 3 times by KOH solution with the mass fraction of 10%, and collecting a dichloromethane layer. Washing with ethyl acetate, ethanol and n-hexane for 5 times, and drying in a vacuum drying oven at 60 deg.C for 15 hr;
2) dissolving 100g of the product prepared in the step 1) in 1000g of ether, adding 300g of amino modified fullerene and 100g of 1,3, 5-triglycidyl-S-triazine trione, stirring and reacting at 70 ℃ for 5 hours, adding 10g of copper chloride, removing the solvent by rotary evaporation, and drying in a vacuum drying oven at 50 ℃ for 8 hours;
the fullerene-based composite photocatalyst is prepared by the preparation method of the fullerene-based composite photocatalyst.
Example 2
A preparation method of a fullerene-based composite photocatalyst comprises the following steps:
1) dissolving 120g of 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine in 1400g of dichloromethane at room temperature, dropwise adding 100g of oxalyl chloride, stirring for 3.2h, dropwise adding 600g of dichloromethane solution of amino ferrocene with the mass fraction of 22%, stirring at 44 ℃ for reaction for 32h, washing the reaction product for 4 times by KOH solution with the mass fraction of 13%, and collecting a dichloromethane layer. Washing with ethyl acetate, ethanol and n-hexane for 6 times, and drying in a vacuum drying oven at 70 deg.C for 18 hr;
2) dissolving 100g of the product prepared in the step 1) in 1200g of dichloromethane, adding 380g of amino modified fullerene and 130g of 1,3, 5-triglycidyl-S-triazine trione, stirring and reacting at 76 ℃ for 6.5 hours, adding 15g of copper chloride, removing the solvent by rotary evaporation, and drying in a vacuum drying oven at 58 ℃ for 9 hours;
the fullerene-based composite photocatalyst is prepared by the preparation method of the fullerene-based composite photocatalyst.
Example 3
A preparation method of a fullerene-based composite photocatalyst comprises the following steps:
1) 160g of 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine is dissolved in 1700g of dichloromethane at room temperature, 100g of oxalyl chloride is dropwise added into the dichloromethane, after stirring for 3.6h, 700g of dichloromethane solution of amino ferrocene with the mass fraction of 26% is dropwise added, stirring reaction is carried out for 34h at the temperature of 48 ℃, the reaction product is washed for 5 times by KOH solution with the mass fraction of 16%, and a dichloromethane layer is collected. Washing with ethyl acetate, ethanol and n-hexane for 7 times, and drying in a vacuum drying oven at 72 deg.C for 18 hr;
2) dissolving 150g of the product prepared in the step 1) in 1400g of ethanol, adding 430g of amino modified fullerene and 170g of 1,3, 5-triglycidyl-S-triazine trione, stirring and reacting at 76 ℃ for 7 hours, adding 18g of copper chloride, removing the solvent by rotary evaporation, and drying in a vacuum drying oven at 58 ℃ for 10 hours;
the fullerene-based composite photocatalyst is prepared by the preparation method of the fullerene-based composite photocatalyst.
Example 4
A preparation method of a fullerene-based composite photocatalyst comprises the following steps:
1) dissolving 180g of 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine in 1800g of dichloromethane at room temperature, dropwise adding 100g of oxalyl chloride, stirring for 4h, dropwise adding 770g of a dichloromethane solution of 28% by mass of amino ferrocene, stirring at 50 ℃ for reaction for 34h, washing the reaction product for 5 times by using a KOH solution with the mass fraction of 18%, and collecting a dichloromethane layer. Washing with ethyl acetate, ethanol and n-hexane for 7 times, and drying in 80 deg.C vacuum drying oven for 19 hr;
2) dissolving 190g of the product prepared in the step 1) in 1400g of n-butanol, adding 450g of amino modified fullerene and 200g of 1,3, 5-triglycidyl-S-triazine trione, stirring and reacting at 77 ℃ for 7 hours, adding 20g of copper chloride, removing the solvent by rotary evaporation, and drying in a vacuum drying oven at 60 ℃ for 9.5 hours;
the fullerene-based composite photocatalyst is prepared by the preparation method of the fullerene-based composite photocatalyst.
Example 5
A preparation method of a fullerene-based composite photocatalyst comprises the following steps:
1) dissolving 200g of 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine in 2000g of dichloromethane at room temperature, dropwise adding 100g of oxalyl chloride, stirring for 4 hours, dropwise adding 800g of a dichloromethane solution of amino ferrocene with the mass fraction of 30%, stirring at 50 ℃ for reacting for 36 hours, washing the reaction product with a KOH solution with the mass fraction of 20% for 5 times, and collecting a dichloromethane layer. Washing with ethyl acetate, ethanol and n-hexane for 8 times, and drying in 80 deg.C vacuum drying oven for 20 hr;
2) dissolving 200g of the product prepared in the step 1) in 1500g of diethyl ether, adding 500g of amino modified fullerene and 200g of 1,3, 5-triglycidyl-S-triazine trione, stirring and reacting at 80 ℃ for 7 hours, adding 20g of copper chloride, removing the solvent by rotary evaporation, and drying in a vacuum drying oven at 60 ℃ for 10 hours;
the fullerene-based composite photocatalyst is prepared by the preparation method of the fullerene-based composite photocatalyst.
Comparative example 1
No photocatalyst is added;
comparative example 2
The photocatalyst is traditional titanium dioxide nano particles;
comparative example 3
The photocatalyst is a traditional copper phthalocyanine organic photocatalyst;
practical application of the photocatalyst prepared in the embodiment of the invention and the comparative example (degrading rhodamine): weighing 80mg of sample, adding 80mL of rhodamine solution (the concentration is 8mol/L), and stirring for 1 hour in the dark to ensure that the rhodamine solution achieves adsorption/desorption balance on the surface of the catalyst. Then, a light source is turned on for photocatalysis, 3mL of reaction solution is taken every 5 minutes, after centrifugal separation, the supernatant is detected by a Cary-500 spectrophotometer. The change of the rhodamine concentration in the degradation process is determined according to the absorbance value of the sample at 554 nm. The glow of the reaction was a 500W tungsten halogen lamp placed in a double glass jacket (through which condensed water was passed), and a filter was used to ensure that the incident light was visible light (wavelength range: 420-800nm), and the test results are shown in Table 1.
TABLE 1 results of photocatalytic rhodamine degradation test for examples and comparative examples
| Detecting items | After 5 minutes | After 10 minutes | After 15 minutes | After 20 minutes |
| Comparative example 1 | 1 | 1 | 1 | 1 |
| Comparative example 2 | 0.96 | 0.94 | 0.90 | 0.85 |
| Comparative example 3 | 0.54 | 0.45 | 0.38 | 0.29 |
| Example 1 | 0.2 | 0.02 | 0 | 0 |
| Example 2 | 0.17 | 0.02 | 0 | 0 |
| Example 3 | 0.11 | 0.01 | 0 | 0 |
| Example 4 | 0.06 | 0 | 0 | 0 |
| Example 5 | 0.01 | 0 | 0 | 0 |
Note: the data in the table are the ratio of the concentration of rhodamine to the initial concentration at different times
As can be seen from table 1, the doping of fullerene and copper chloride and the compounding with triazine and ferrocene are beneficial to improving the catalytic efficiency of the photocatalyst, and the two have synergistic effects, so that the photocatalyst prepared in the embodiment has very strong photocatalytic activity, and the photocatalyst disclosed in the embodiment of the invention has visible light response catalytic activity.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those of ordinary skill in the art can readily implement the present invention as described herein; however, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention; meanwhile, any changes, modifications, and evolutions of the equivalent changes of the above embodiments according to the actual techniques of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (5)
1. A preparation method of a fullerene composite photocatalyst for environmental pollution treatment is characterized by comprising the following steps:
1) dissolving 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine in dichloromethane at room temperature, dropwise adding oxalyl chloride into the dichloromethane, stirring for 3-4h, dropwise adding a dichloromethane solution of amino ferrocene with the mass fraction of 20-30%, stirring and reacting for 30-36h at 40-50 ℃, washing the reaction product for 3-5 times by using a KOH solution with the mass fraction of 10-20%, and collecting a dichloromethane layer; washing with ethyl acetate, ethanol and n-hexane for 5-8 times, rotary steaming, and drying in vacuum drying oven at 60-80 deg.C for 15-20 hr;
2) dissolving the product prepared in the step 1) in a solvent, adding amino modified fullerene and 1,3, 5-triglycidyl-S-triazine trione, stirring and reacting at 70-80 ℃ for 5-7 hours, adding copper chloride, removing the solvent by rotary evaporation, and drying in a vacuum drying oven at 50-60 ℃ for 8-10 hours.
2. The method for preparing a fullerene composite photocatalyst for environmental pollution treatment according to claim 1, wherein the mass ratio of the dichloromethane solution of 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine, dichloromethane, oxalyl chloride and amino ferrocene in step 1) is (1-2): (10-20):1: (5-8).
3. The method for preparing a fullerene composite photocatalyst for environmental pollution treatment according to claim 1, wherein the solvent is one or more selected from ethanol, n-butanol, dichloromethane and diethyl ether.
4. The method for preparing a fullerene composite photocatalyst for environmental pollution treatment according to claim 1, wherein the mass ratio of the product prepared in step 1) in step 2), the solvent, the amino-modified fullerene, 1,3, 5-triglycidyl-S-triazine trione and the copper chloride is (1-2): (10-15): (3-5): (1-2): (0.1-0.2).
5. A fullerene composite photocatalyst for environmental pollution abatement, which is characterized by being prepared by the preparation method of the fullerene composite photocatalyst for environmental pollution abatement according to any one of claims 1 to 4.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711322953.XA CN107983413B (en) | 2017-12-12 | 2017-12-12 | Fullerene composite photocatalyst for environmental pollution treatment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711322953.XA CN107983413B (en) | 2017-12-12 | 2017-12-12 | Fullerene composite photocatalyst for environmental pollution treatment |
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| Publication Number | Publication Date |
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| CN107983413A CN107983413A (en) | 2018-05-04 |
| CN107983413B true CN107983413B (en) | 2020-12-04 |
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| CN106925298A (en) * | 2017-03-02 | 2017-07-07 | 天津大学 | A kind of fullerene/cadmium sulfide nano composite photo-catalyst and preparation method thereof |
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