CN107983413A - A kind of fullerene composite photo-catalyst for environmental pollution improvement - Google Patents
A kind of fullerene composite photo-catalyst for environmental pollution improvement Download PDFInfo
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- CN107983413A CN107983413A CN201711322953.XA CN201711322953A CN107983413A CN 107983413 A CN107983413 A CN 107983413A CN 201711322953 A CN201711322953 A CN 201711322953A CN 107983413 A CN107983413 A CN 107983413A
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- catalyst
- composite photo
- fullerene
- dichloromethane
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- 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 40
- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 40
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000003912 environmental pollution Methods 0.000 title claims description 10
- 230000006872 improvement Effects 0.000 title claims description 9
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 93
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- CTSLXHKWHWQRSH-UHFFFAOYSA-N oxalyl chloride Chemical compound ClC(=O)C(Cl)=O CTSLXHKWHWQRSH-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001291 vacuum drying Methods 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 239000000047 product Substances 0.000 claims abstract description 11
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 10
- -1 amino modified fullerene Chemical class 0.000 claims abstract description 8
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 8
- MYCZBBOLTYBTCX-UHFFFAOYSA-N cyclopenta-2,4-dien-1-amine;cyclopenta-1,3-diene;iron(2+) Chemical compound [Fe+2].C=1C=C[CH-]C=1.NC1=CC=C[CH-]1 MYCZBBOLTYBTCX-UHFFFAOYSA-N 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 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 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 125000003431 oxalo group Chemical group 0.000 claims description 2
- ZHPQBIDORRABIG-UHFFFAOYSA-N N1C(NC(NC1=O)=O)=O.OCC(O)CO Chemical class N1C(NC(NC1=O)=O)=O.OCC(O)CO ZHPQBIDORRABIG-UHFFFAOYSA-N 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 150000000182 1,3,5-triazines Chemical class 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000463 material Substances 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
- 238000007146 photocatalysis Methods 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction 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
- 150000003918 triazines Chemical class 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003287 optical effect Effects 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
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 1
- 230000002708 enhancing 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
- 150000002367 halogens Chemical class 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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 kind of preparation method based on fullerene composite photo-catalyst, include the following steps：1）By 2,4,6 three (4 carboxyl phenyls) 1,3,5 triazines are dissolved in dichloromethane, and oxalyl chloride is added dropwise thereto, after stirring 3 4h, the dichloromethane solution for the Aminoferrocene that mass fraction is 20 30% is added dropwise, 30 36h of reaction are stirred at 40 50 DEG C, reaction product washes 35 times as 10 20% KOH solution using mass fraction and collects dichloromethane layer.Revolving, washing, drying；2）By step 1）The product being prepared is dissolved in solvent, then adds amino modified fullerene, 1,3 thereto, 5 three-glycidyl S triazinetriones, at 70 80 DEG C stirring reaction 57 it is small when, after add copper chloride thereto, then rotate, after in 50 60 DEG C of vacuum drying chamber it is dry 8 10 it is small when；The invention also discloses according to the preparation method be prepared based on fullerene composite photo-catalyst；It is disclosed by the invention based on the visible light-responded scope of fullerene composite photo-catalyst is wide, photocatalytic activity is high, stability is good.
Description
Technical field
The invention belongs to depollution of environment photochemical catalyst new material technology field, it is related to a kind of photochemical catalyst and its preparation side
Method, and in particular to a kind of with visible light-responded based on fullerene composite photo-catalyst and preparation method thereof.
Background technology
In recent years, with the fast development of industry, restriction social development and progress the environmental pollution of one of an important factor for
Problem getting worse, wastewater treatment become one of urgent problem to be solved in the industry.Contain substantial amounts of complicated component, toxicity in waste water
Greatly, colourity height, the organic pollution of bio-degradable difference, how to handle these organic pollutions is always in wastewater treatment
Problem.In order to solve this problem, various depollution of environment catalyst materials come into being, wherein, photochemical catalyst is as a kind of new
Emerging energy saving environmentally protective catalyst, wide application prospect is shown in field of environment pollution control, becomes a kind of reason
The environmental pollution improvement's catalyst thought.
Compared with traditional catalyst, photochemical catalyst can directly utilize sunlight, by pollutant depth mineralising, not produce two
Secondary pollution.In numerous conductor photocatalysis materials, titanium dioxide (TiO2) due to fast light corrosive power is strong, degree of stability is high,
Relative low price and to human body it is non-toxic the advantages that, cause the concern of numerous experts and scholars.But from the profit of solar energy
From the point of view of rate, TiO at present2It can not also be promoted and applied on a large scale in actual industrial water process, because it is only ultraviolet
There is response in optical range, it is low to visible light utilization efficiency.
Therefore, develop visible-light-responsive photocatalyst and find efficient catalyst and be increasingly becoming what is studied at present
Hot spot.
The content of the invention
Present invention seek to address that the above problem, there is provided one kind is based on fullerene composite photo-catalyst, and the catalyst is visible
Photoresponse scope is wide, photocatalytic activity is high, stability is good, and manufacture is of low cost.
To achieve the above object, the present invention provides following technical solution, a kind of based on fullerene composite photo-catalyst
Preparation method, includes the following steps：
1）At room temperature, by 2,4,6- tri- (4- carboxyl phenyls), -1,3,5-triazines is dissolved in dichloromethane, and oxalyl is added dropwise thereto
Chlorine, after stirring 3-4h, adds dropwise the dichloromethane solution for the Aminoferrocene that mass fraction is 20-30%, at 40-50 DEG C
Stirring reaction 30-36h, KOH solution of the reaction product using mass fraction as 10-20 % are washed 3-5 times and collect dichloromethane layer.
Washed 5-8 times with ethyl acetate, ethanol, n-hexane after revolving, done after revolving in 60-80 DEG C of vacuum drying chamber respectively successively
When dry 15-20 is small；
2）By step 1）The product being prepared is dissolved in solvent, then adds amino modified fullerene, 1 thereto, and 3,5- tri-
Glycidol-S- triazinetriones, at 70-80 DEG C stirring reaction 5-7 it is small when, after add copper chloride thereto, then revolving remove
Remove solvent, after when dry 8-10 is small in 50-60 DEG C of vacuum drying chamber；
Wherein, step 1）Described in 2,4,6- tri- (4- carboxyl phenyls) -1,3,5- triazines, dichloromethane, oxalyl chloride, the cyclopentadienyl of amino two
The mass ratio of the dichloromethane solution of iron is（1-2）：（10-20）:1：（5-8）；
One or more of the solvent in ethanol, n-butanol, dichloromethane, ether；
Step 2）Described in step 1）Product, solvent, amino modified fullerene, the 1,3,5- three-glycidyls-S- being prepared
Triazinetrione, the mass ratio of copper chloride are（1-2）：（10-15）：（3-5）：（1-2）：（0.1-0.2）；
One kind is based on fullerene composite photo-catalyst, using a kind of preparation method system based on fullerene composite photo-catalyst
It is standby to obtain.
Since above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
（1）Provided by the invention to be based on fullerene composite photo-catalyst, preparation method is simple and practicable, not high to equipment requirement, former
Material is easy to get, cheap.
（2）It is provided by the invention to be based on fullerene composite photo-catalyst, combine fullerene, ferrocene and triazines light and urge
The advantages of agent, have the advantageous feature that visible light-responded scope is wide, photocatalytic activity is high, stability is good.
（3）It is provided by the invention to be based on fullerene composite photo-catalyst, led to using fullerene and triazines conjugated compound
Chemical bond is crossed, and fullerene passes through host-guest interaction by ferrocene so that photochemical catalyst stability is strong, passes through copper chloride
Doping so that it has more excellent photocatalysis effect.
（4）It is provided by the invention to be based on fullerene composite photo-catalyst, there is provided more surface-active site, is conducive to
Light induced electron and the separation in hole.
（5）It is provided by the invention to be based on fullerene composite photo-catalyst, organic dyestuff can not only be adsorbed well, significantly
Strengthen the utilization to light and capture ability, and the transmission due to electronics between the two phases, the taboo of catalysis material can be reduced
Bandwidth, expands the spectral range that catalysis material utilizes sunlight, has in visible region and absorbs and respond well, enhancing
Photocatalysis effect.
Embodiment
In order that those skilled in the art will better understand the technical solution of the present invention, with reference to embodiment to this
Invention product is described in further detail.
Embodiment 1
A kind of preparation method based on fullerene composite photo-catalyst, includes the following steps：
1）At room temperature, 2,4,6- tri- (4- carboxyl phenyls) -1,3,5-triazines 100g are dissolved in dichloromethane 1000g, and to its
Middle dropwise addition oxalyl chloride 100g, after stirring 3h, adds dropwise the dichloromethane solution for the Aminoferrocene that mass fraction is 20%
500g, stirring reaction 30h, reaction product wash 3 times as 10% KOH solution using mass fraction and collect dichloromethane at 40 DEG C
Layer.Washed respectively 5 times with ethyl acetate, ethanol, n-hexane successively after revolving, it is dry in 60 DEG C of vacuum drying chamber after revolving
15 it is small when；
2）By step 1）The product 100g being prepared is dissolved in ether 1000g, then adds amino modified fullerene thereto
300g, 1,3,5- three-glycidyl-S- triazinetrione 100g, at 70 DEG C stirring reaction 5 it is small when, after add copper chloride thereto
10g, then revolving remove solvent, after in 50 DEG C of vacuum drying chamber it is dry 8 it is small when；
One kind is based on fullerene composite photo-catalyst, using a kind of preparation method system based on fullerene composite photo-catalyst
It is standby to obtain.
Embodiment 2
A kind of preparation method based on fullerene composite photo-catalyst, includes the following steps：
1）At room temperature, 2,4,6- tri- (4- carboxyl phenyls) -1,3,5-triazines 120g are dissolved in dichloromethane 1400g, and to its
Middle dropwise addition oxalyl chloride 100g, after stirring 3.2h, adds dropwise the dichloromethane solution for the Aminoferrocene that mass fraction is 22%
600g, stirring reaction 32h, reaction product wash 4 times as 13% KOH solution using mass fraction and collect dichloromethane at 44 DEG C
Layer.Washed respectively 6 times with ethyl acetate, ethanol, n-hexane successively after revolving, it is dry in 70 DEG C of vacuum drying chamber after revolving
18 it is small when；
2）By step 1）The product 100g being prepared is dissolved in dichloromethane 1200g, then adds amino modified richness thereto
Strangle alkene 380g, 1,3,5- three-glycidyl-S- triazinetrione 130g, when stirring reaction 6.5 is small at 76 DEG C, after add thereto
Copper chloride 15g, then revolving remove solvent, after in 58 DEG C of vacuum drying chamber it is dry 9 it is small when；
One kind is based on fullerene composite photo-catalyst, using a kind of preparation method system based on fullerene composite photo-catalyst
It is standby to obtain.
Embodiment 3
A kind of preparation method based on fullerene composite photo-catalyst, includes the following steps：
1）At room temperature, 2,4,6- tri- (4- carboxyl phenyls) -1,3,5-triazines 160g are dissolved in dichloromethane 1700g, and to its
Middle dropwise addition oxalyl chloride 100g, after stirring 3.6h, adds dropwise the dichloromethane solution for the Aminoferrocene that mass fraction is 26%
700g, stirring reaction 34h, KOH solution of the reaction product using mass fraction as 16 % are washed 5 times and collect dichloromethane at 48 DEG C
Layer.Washed respectively 7 times with ethyl acetate, ethanol, n-hexane successively after revolving, it is dry in 72 DEG C of vacuum drying chamber after revolving
18 it is small when；
2）By step 1）The product 150g being prepared is dissolved in ethanol 1400g, then adds amino modified fullerene thereto
430g, 1,3,5- three-glycidyl-S- triazinetrione 170g, at 76 DEG C stirring reaction 7 it is small when, after add copper chloride thereto
18g, then revolving remove solvent, after in 58 DEG C of vacuum drying chamber it is dry 10 it is small when；
One kind is based on fullerene composite photo-catalyst, using a kind of preparation method system based on fullerene composite photo-catalyst
It is standby to obtain.
Embodiment 4
A kind of preparation method based on fullerene composite photo-catalyst, includes the following steps：
1）At room temperature, 2,4,6- tri- (4- carboxyl phenyls) -1,3,5-triazines 180g are dissolved in dichloromethane 1800g, and to its
Middle dropwise addition oxalyl chloride 100g, after stirring 4h, adds dropwise the dichloromethane solution for the Aminoferrocene that mass fraction is 28%
770g, stirring reaction 34h, reaction product wash 5 times as 18% KOH solution using mass fraction and collect dichloromethane at 50 DEG C
Layer.Washed respectively 7 times with ethyl acetate, ethanol, n-hexane successively after revolving, it is dry in 80 DEG C of vacuum drying chamber after revolving
19 it is small when；
2）By step 1）The product 190g being prepared is dissolved in n-butanol 1400g, then adds amino modified fowler thereto
Alkene 450g, 1,3,5- three-glycidyl-S- triazinetrione 200g, at 77 DEG C stirring reaction 7 it is small when, after add chlorination thereto
Copper 20g, then revolving remove solvent, after in 60 DEG C of vacuum drying chamber it is dry 9.5 it is small when；
One kind is based on fullerene composite photo-catalyst, using a kind of preparation method system based on fullerene composite photo-catalyst
It is standby to obtain.
Embodiment 5
A kind of preparation method based on fullerene composite photo-catalyst, includes the following steps：
1）At room temperature, 2,4,6- tri- (4- carboxyl phenyls) -1,3,5-triazines 200g are dissolved in dichloromethane 2000g, and to its
Middle dropwise addition oxalyl chloride 100g, after stirring 4h, adds dropwise the dichloromethane solution for the Aminoferrocene that mass fraction is 30%
800g, stirring reaction 36h, KOH solution of the reaction product using mass fraction as 20 % are washed 5 times and collect dichloromethane at 50 DEG C
Layer.Washed respectively 8 times with ethyl acetate, ethanol, n-hexane successively after revolving, it is dry in 80 DEG C of vacuum drying chamber after revolving
20 it is small when；
2）By step 1）The product 200g being prepared is dissolved in ether 1500g, then adds amino modified fullerene thereto
500g, 1,3,5- three-glycidyl-S- triazinetrione 200g, at 80 DEG C stirring reaction 7 it is small when, after add copper chloride thereto
20g, then revolving remove solvent, after in 60 DEG C of vacuum drying chamber it is dry 10 it is small when；
One kind is based on fullerene composite photo-catalyst, using a kind of preparation method system based on fullerene composite photo-catalyst
It is standby to obtain.
Comparative example 1
It is not added with any photochemical catalyst；
Comparative example 2
The photochemical catalyst is traditional titanium dioxide nano-particle；
Comparative example 3
The photochemical catalyst is the organic photochemical catalyst of traditional phthalein mountain valley with clumps of trees and bamboo copper；
The practical application of photochemical catalyst prepared by the embodiment of the present invention and comparative example（Degraded rhodamine）：Weigh the addition of 80mg samples
80mL rhodamine liquors（Concentration 8mol/L）, lucifuge stirring 1 it is small when so that rhodamine liquor catalyst surface reach absorption/
Desorption equilibrium.It is then turned on light source and carries out photocatalysis, 3mL reaction solutions were taken every 5 minutes, after being centrifuged, supernatant is used
Cary-500 spectrophotometers detect.Determine that rhodamine concentration changes in degradation process according to light absorption value at sample 554nm.Instead
The radiance answered is to be placed in double glass jackets（Logical condensed water）In 500W halogen tungsten lamps, using optical filter to ensure incident light to be visible
Light（Wave-length coverage：420-800nm）, test result is shown in Table 1.
1 embodiment of table and comparative example photochemical catalyst catalysis rhodamine degraded test result
| Detection project | After five minutes | After ten minutes | After 15 minutes | After twenty 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 |
| Embodiment 1 | 0.2 | 0.02 | 0 | 0 |
| Embodiment 2 | 0.17 | 0.02 | 0 | 0 |
| Embodiment 3 | 0.11 | 0.01 | 0 | 0 |
| Embodiment 4 | 0.06 | 0 | 0 | 0 |
| Embodiment 5 | 0.01 | 0 | 0 | 0 |
Note：Data are different time rhodamine concentration and the ratio of initial concentration in table
As seen from Table 1, fullerene, chlorination Copper-cladding Aluminum Bar and with the compound catalytic efficiency to improving photochemical catalyst of triazines, ferrocene
All beneficial, both act synergistically so that the photochemical catalyst prepared in the present embodiment has very strong photocatalytic activity, and the present invention is real
Applying photochemical catalyst disclosed in example has visible light-responded catalytic activity.
The foregoing is only a preferred embodiment of the present invention, not makees limitation in any form to the present invention；
The those of ordinary skill of all industry can swimmingly implement the present invention described in by specification；But all it is familiar with this specialty
Technical staff without departing from the scope of the present invention, makes a little using disclosed above technology contents
The equivalent variations of variation, modification and evolution, are the equivalent embodiment of the present invention；Meanwhile all substantial technologicals according to the present invention
Variation, modification and evolution of any equivalent variations made to above example etc., still fall within technical scheme
Protection domain within.
Claims (5)
1. the preparation method of a kind of fullerene composite photo-catalyst for environmental pollution improvement, it is characterised in that including as follows
Step：
1）At room temperature, by 2,4,6- tri- (4- carboxyl phenyls), -1,3,5-triazines is dissolved in dichloromethane, and oxalyl is added dropwise thereto
Chlorine, after stirring 3-4h, adds dropwise the dichloromethane solution for the Aminoferrocene that mass fraction is 20-30%, at 40-50 DEG C
Stirring reaction 30-36h, KOH solution of the reaction product using mass fraction as 10-20 % are washed 3-5 times and collect dichloromethane layer；
Washed 5-8 times with ethyl acetate, ethanol, n-hexane after revolving, done after revolving in 60-80 DEG C of vacuum drying chamber respectively successively
When dry 15-20 is small；
2）By step 1）The product being prepared is dissolved in solvent, then adds amino modified fullerene, 1 thereto, and 3,5- tri-
Glycidol-S- triazinetriones, at 70-80 DEG C stirring reaction 5-7 it is small when, after add copper chloride thereto, then revolving remove
Remove solvent, after when dry 8-10 is small in 50-60 DEG C of vacuum drying chamber.
2. a kind of preparation method of fullerene composite photo-catalyst for environmental pollution improvement according to claim 1,
It is characterized in that, step 1）Described in 2,4,6- tri- (4- carboxyl phenyls) -1,3,5- triazines, dichloromethane, oxalyl chloride, amino two
The mass ratio of the dichloromethane solution of luxuriant iron is（1-2）：（10-20）:1：（5-8）.
3. a kind of preparation method of fullerene composite photo-catalyst for environmental pollution improvement according to claim 1,
It is characterized in that, one or more of the solvent in ethanol, n-butanol, dichloromethane, ether.
4. a kind of preparation method of fullerene composite photo-catalyst for environmental pollution improvement according to claim 1,
It is characterized in that, step 2）Described in step 1）Product, solvent, amino modified fullerene, the 1,3,5- tri- being prepared shrink
Glycerine-S- triazinetriones, the mass ratio of copper chloride are（1-2）：（10-15）：（3-5）：（1-2）：（0.1-0.2）.
5. the preparation method of a kind of fullerene composite photo-catalyst for environmental pollution improvement, it is characterised in that using right
It is required that a kind of preparation method of any one of 1-4 fullerene composite photo-catalysts for environmental pollution improvement is prepared.
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| CN111154361A (en) * | 2020-01-10 | 2020-05-15 | 林才珏 | Corrosion-resistant water-based paint and preparation process thereof |
| CN113519552A (en) * | 2021-07-28 | 2021-10-22 | 安徽江淮汽车集团股份有限公司 | Preparation method of antibacterial agent, thermoplastic resin composite material and preparation method thereof |
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| CN105964296A (en) * | 2016-04-22 | 2016-09-28 | 宁波高新区夏远科技有限公司 | Organic photocatalyst and preparation method thereof |
| 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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| CN105964296A (en) * | 2016-04-22 | 2016-09-28 | 宁波高新区夏远科技有限公司 | Organic photocatalyst and preparation method thereof |
| 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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| CN111154361A (en) * | 2020-01-10 | 2020-05-15 | 林才珏 | Corrosion-resistant water-based paint and preparation process thereof |
| CN113519552A (en) * | 2021-07-28 | 2021-10-22 | 安徽江淮汽车集团股份有限公司 | Preparation method of antibacterial agent, thermoplastic resin composite material and preparation method thereof |
| CN113519552B (en) * | 2021-07-28 | 2021-12-07 | 安徽江淮汽车集团股份有限公司 | Preparation method of antibacterial agent, thermoplastic resin composite material and preparation method thereof |
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