CN107935103A - A kind for the treatment of process of silver-based composite photocatalyst for degrading dyeing waste water - Google Patents
A kind for the treatment of process of silver-based composite photocatalyst for degrading dyeing waste water Download PDFInfo
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- CN107935103A CN107935103A CN201711424981.2A CN201711424981A CN107935103A CN 107935103 A CN107935103 A CN 107935103A CN 201711424981 A CN201711424981 A CN 201711424981A CN 107935103 A CN107935103 A CN 107935103A
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- waste water
- dyeing waste
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- 239000002351 wastewater Substances 0.000 title claims abstract description 29
- 238000004043 dyeing Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 21
- 230000008569 process Effects 0.000 title claims abstract description 21
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052709 silver Inorganic materials 0.000 title claims description 13
- 239000004332 silver Substances 0.000 title claims description 13
- 230000000593 degrading effect Effects 0.000 title description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 49
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 47
- 230000001699 photocatalysis Effects 0.000 claims abstract description 23
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 28
- 235000013339 cereals Nutrition 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 11
- 239000004408 titanium dioxide Substances 0.000 claims description 11
- -1 Titanium oxide compound Chemical class 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 239000003643 water by type Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000005286 illumination Methods 0.000 claims description 7
- 239000002105 nanoparticle Substances 0.000 claims description 7
- PIEQFSVTZMAUJA-UHFFFAOYSA-N 7-hydroxy-8-{[4-(phenyldiazenyl)phenyl]diazenyl}naphthalene-1,3-disulfonic acid Chemical compound OC1=CC=C2C=C(S(O)(=O)=O)C=C(S(O)(=O)=O)C2=C1N=NC(C=C1)=CC=C1N=NC1=CC=CC=C1 PIEQFSVTZMAUJA-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical group CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 108010024636 Glutathione Proteins 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 235000013312 flour Nutrition 0.000 claims description 3
- 229960002163 hydrogen peroxide Drugs 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical class CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 230000003213 activating effect Effects 0.000 claims 1
- 230000031709 bromination Effects 0.000 claims 1
- 238000005893 bromination reaction Methods 0.000 claims 1
- 238000000502 dialysis Methods 0.000 claims 1
- 229960003180 glutathione Drugs 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 13
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 238000006731 degradation reaction Methods 0.000 abstract description 7
- 238000007540 photo-reduction reaction Methods 0.000 abstract description 6
- 239000000975 dye Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003426 co-catalyst Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- UXAMZEYKWGPDBI-UHFFFAOYSA-N C(CCCCCCCCCCCCCCC)Br(C)(C)C Chemical class C(CCCCCCCCCCCCCCC)Br(C)(C)C UXAMZEYKWGPDBI-UHFFFAOYSA-N 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical class [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- 229940126062 Compound A Drugs 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 230000007886 mutagenicity Effects 0.000 description 1
- 231100000299 mutagenicity Toxicity 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 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 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- B01J35/39—
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
-
- 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 for the treatment of process of photocatalytic degradation dyeing waste water, its photochemical catalyst used is ag nano-cluster Nano silver grain/TiO2/ graphene composite photocatalyst.Graphene oxide is made in the catalyst first, then TiO of the load with photocatalytic activity on its lamella2, then by ag nano-cluster modification to being loaded with TiO2Graphene sheet layer on, and photo-reduction is carried out to it, which has high catalytic degradation activity for dyeing waste water.The present invention solves the problems, such as that degradation of dye effluent efficiency is low in the prior art, the organic dyestuff suitable for degraded dyeing waste water.
Description
Technical field
The present invention relates to a kind for the treatment of process of photocatalytic degradation dyeing waste water, using ag nano-cluster-Nano silver grain/
TiO2/ graphene composite photocatalyst, the composition and special construction of the photochemical catalyst make it have efficient photocatalytic degradation and live
Property, which has the advantages that easy to operate, of low cost, degradation efficiency is high.
Background technology
In textile printing and dyeing process, largely use pollution environment and harmful auxiliary agent, these auxiliary agents big
Discharged more in the form of liquid, inevitably into water body environment, cause water pollution.If rhdamine B is with carcinogenic
And mutagenicity, the chroma in waste water containing rhodamine B is deep, organic pollution content is high, biological degradability is poor, with conventional method
Such as physisorphtion, Fenton process are difficult to administer, and cause to pollute water quality long-term degradation, seriously endanger the strong of water body environment and the mankind
Health, therefore seem particularly significant and urgent to the degradation treatment of this kind of waste water.
A large amount of Novel environment-friendlymaterial materials are come into being in recent years.Nano-TiO2Material be exactly it is this can environment purification and efficiently
Utilize the green functional material of solar energy.It not only has strong, the excellent chemical stability of oxidability, energy expenditure the, nothing
The advantages that follow-up secondary pollution, but also have the characteristics that it is cheap, nontoxic, can long-time service, it is therefore standby in recent years
By the favor and concern of photocatalysis researcher, and it is widely used in the quick magnificent solar-electricity of new energy field such as dyestuff
Pond, photodissociation aquatic products hydrogen, microwave absorption, light absorption, biological medicine processing, photovoltaic cell, photocatalysis, lithium ion battery etc..
But semiconductor TiO2Material there is also some it is serious the defects of, such as pure TiO2The photo-generate electron-hole of photochemical catalyst
To short life, light abstraction width is narrow low with light conversion efficiency, limits the application of solid powder th-1 catalyst.So need to receiving
The pattern of rice titanium dioxide is modified and study on the modification, and it is extremely urgent to sun efficiency of light absorption to improve it.Therefore, close
Reason ground prepares Hydrogen Energy with solar energy and conductor oxidate and effectively Environment control will be subject to people more and more to pay attention to.
Noble metal nano particles can provide the avtive spot of catalytic reaction, meanwhile, relatively low Fermi can be quick
Light induced electron is captured, the interfacial migration of accelerated charge extends the service life of photo-generated carrier, thus co-catalyst can be used as to improve light
It is catalyzed the transformation efficiency of solar energy.In addition, some special noble metals such as gold, silver nano-particle has plasma in visible region
RESONANCE ABSORPTION, can effectively expand the light abstraction width of photochemical catalyst.In recent years, there is the super of specific structure and atom number
Small-sized noble metal nano cluster because it is different from unique photoelectric property of common nano-particle and by people's extensive concern.Due to receiving
The particle diameter of rice cluster is close with the de Broglie wavelength of Fermi's wavelength or conduction band electron, and quantum effect, which makes it have metalloid, to be had
Machine molecular energy level property.So that there are noble metal nano cluster stepped light absorbs, fluorescence to send out before this discrete electronics moon
The property such as penetrate, thus there is good prospect in photocatalytic applications as photosensitizer or co-catalyst.
Graphene is the semimetal that a kind of energy gap is zero, in photocatalysis field, since graphene has unique electronics special
Property, great specific surface area and higher transparency become the ideal carrier for synthesizing composite photo-catalyst, the electricity of graphene
Transport factor is very high, and photochemical catalyst is modified using graphene, can not only realize broadband light absorbs, but also
Electric charge can be made more to be matched with catalyst in transfer process, improve its photocatalysis performance；Secondly graphene has uniqueness
Two-dimensional surface structure and there is larger specific surface area, can be induced when forming compound and produce the absorption strong to pollutant and make
With being conducive to the further progress of photocatalytic degradation.
The content of the invention
The shortcomings that in order to overcome the above-mentioned prior art, it is an object of the invention to provide a kind of photocatalytic degradation dyeing waste water
Treatment process, it uses light-catalysed mode to degrade dyestuff therein, and used photochemical catalyst is ag nano-cluster-Yin Na
Rice corpuscles/TiO2/ graphene composite photocatalyst.
Realize technical scheme：Dyeing waste water is handled by the way of a kind of Visible Light Induced Photocatalytic, and is prepared for one
Ag nano-cluster-Nano silver grain/TiO of the kind with excellent Photocatalytic activity2/ graphene composite photocatalyst.
The treatment process of the Visible Light Induced Photocatalytic dyeing waste water, includes the following steps：
By ag nano-cluster-Nano silver grain/TiO2/ graphene composite photocatalyst is added to certain density dyeing waste water
In, it is sufficiently stirred and adjusts pH value of solution=3.5~4.5, mixed solution is transferred in vial, dark reaction 0.5 in dark surrounds~
1h, then carries out room temperature, stirring visible light photocatalytic degradation reacts 0.5~2.5h under the xenon lamp of 500W~600W.
Ag nano-cluster-Nano silver grain/the TiO2The preparation method of/graphene composite photocatalyst, specifically press with
What lower step was completed：
First, the preparation of graphene oxide：
250~350mg graphite powders, 1.5~2.5g sodium nitrate mixed solution in, add the dense sulphur of 15~25mL 98wt%
Acid, is stirred at a temperature of 5 DEG C of ＜, allows it to react 1.5~2.0 h in beaker；By potassium permanganate grind into powder, Ran Hou
In 0.5h, 1.5~2.0g powder is added in beaker, 1.5~2.0h is reacted in 5 DEG C of ＜；Beaker is placed in insulating box and is risen
Temperature is to 45~50 DEG C, then 1.5~2h of constant temperature, and constant temperature terminates to add 40~50mL deionized waters in backward beaker, then by temperature
80~90 DEG C are risen to, 10~20min of constant temperature；Then the solution in beaker is cooled to indoor temperature, add 80~120mL go from
Sub- water dilution, solution are changed into glassy yellow, add the hydrogenperoxide steam generator of 10~15mL 35wt% afterwards；Then filtered,
By the salt acid elution of filter residue 300~400mL 5wt%, drain repeated washing three times with aspiration pump, be then washed with deionized water again
Wash three times, finally dialysed two days with bag filter, be put into vacuum drying chamber dry 20h, last abrasive flour at 80 DEG C afterwards
Obtain graphene oxide；
2nd, the preparation of graphene-nanometer titanium dioxide compound：
20~30mg of graphene oxide obtained above is taken, 20~30mL deionized waters is added, is existed using processor for ultrasonic wave
30~60min is ultrasonically treated under 60W power, the graphene oxide solution that mass concentration is 1mg/mL can be obtained；By 5.0~
6.0g cetyl trimethylammonium bromides are dissolved in the mixed solution of 5~20mL n-amyl alcohols and 50~65mL n-hexanes, are obtained
Hexadecyltrimethylammonium chloride solution；Hexadecyltrimethylammonium chloride solution is added to the same of graphene oxide solution
When, after 30min is stirred at room temperature, pour into autoclave, place in an oven, 200 DEG C of constant temperature 6h；By the production after constant temperature
Thing is put into reduced pressure treatment in rotary evaporator and precipitates, and removes organic solvent, obtained precipitation is repeatedly with deionized water and anhydrous
Ethanol washs 2~5 times, removes surfactant and other impurities, and obtained final product is dry 1 under the conditions of being placed on 80 DEG C~
4h, that is, obtain graphene-nanometer titanium dioxide compound；
3rd, ag nano-cluster-Nano silver grain/TiO2The preparation of/graphene composite photocatalyst：
Silver nitrate is soluble in water, add reduced glutathione to stir to colourless, then flow back 24h at 70 DEG C, adds acetonitrile
After purification, centrifuge, wash, is dry, obtaining solid silver nano cluster, obtained solid ag nano-cluster is re-dispersed into water,
Obtain ag nano-cluster solution；By graphene-nanometer titanium dioxide compound and ag nano-cluster solution under mildly acidic conditions
4h is mixed, centrifugation, washing, drying, obtain ag nano-cluster/TiO2/ graphene；It is placed in vacuum environment, sacrifices
Illumination is carried out under the conditions of agent is existing, obtains the ag nano-cluster-Nano silver grain/TiO2/ graphene composite photocatalyst.
The weight ratio of silver nitrate and reduced glutathione used is 1 in step 3:1；Mild acid conditions are that pH value is 4；Institute
The weight ratio for stating graphene-nanometer titanium dioxide compound and solid silver nano cluster is 100:2~100:8；The illumination
Wavelength is 300nm~800nm, and irradiation time is 3~60h, makes ag nano-cluster through different journeys with the difference using illumination condition
The converted in-situ of degree, obtains the Nano silver grain with different-grain diameter, and the sacrifice agent is lactic acid.
Acid Brilliant Scarlet GR, chemical formula C22H14N4Na2O7S2, red powder, belongs to hazardous chemical, if existed in water
Water pollution can be caused, therefore selects Acid Brilliant Scarlet GR as target contaminant to simulate the catalytic efficiency of assessment catalysis material.
Compared with prior art, the present invention has the following advantages：
1st, compared with prior art, the method for photocatalysis treatment dyeing waste water of the present invention is easy to operate, easy control of reaction conditions,
It is of low cost, there is potential industrial applications prospect；
2nd, in photochemical catalyst of the invention, by ag nano-cluster-Nano silver grain/TiO2Embedded in very big specific surface area and excellent
The surface of the graphene of different electric conductivity, promotes photochemical catalyst to realize broadband light absorbs, and excellent using graphene sheet layer
Electric conductivity light induced electron is spread in time, slow down light induced electron and hole it is compound, and electric charge is in transfer process
In more matched with active component, improve photocatalytic activity, and then improve the degradation efficiency of pollutant in dyeing waste water；
3rd, the present invention can control silver nanoparticle group by controlling the conditions such as atmosphere, addition sacrifice agent, illumination wavelength and light application time
Cluster makes gained ag nano-cluster-Nano silver grain/TiO to the converted in-situ degree of Nano silver grain2/ graphene complex light is urged
Agent has different nano silver particle diameters, so as to fulfill the tune to catalyst photocatalytic activity and the degradation efficiency of dyeing waste water
Control；
4th, composite photo-catalyst preparation method of the present invention is simple, green, without high temperature and pressure, and can be using solar energy as energy
Source, is conducive to the sustainable development of environment and the energy.
Embodiment
With reference to specific embodiment the present invention is further elaborated the solution of the present invention.
Embodiment 1
First, the preparation of graphene oxide：
350mg graphite powders, 2.4g sodium nitrate mixed solution in, the concentrated sulfuric acid of 21mL 98wt% is added, in 5 DEG C of temperature of ＜
Lower stirring, allows it to react 1.8h in beaker；By potassium permanganate grind into powder, then in 0.5h, added in beaker
2.0g powder, reacts 1.8h in 5 DEG C of ＜；Beaker is placed in insulating box and is warming up to 48 DEG C, then constant temperature 2.2h, constant temperature terminates
45mL deionized waters are added in backward beaker, then temperature is risen to 85 DEG C, constant temperature 15min；Then the solution in beaker is cooled down
To indoor temperature, the dilution of 80mL deionized waters is added, solution is changed into glassy yellow, adds the hydrogen peroxide of 13mL 35wt% afterwards
Solution；Then filtered, by the salt acid elution of filter residue 400mL 5wt%, drain repeated washing 3 times with aspiration pump, Ran Houzai
It is washed with deionized 3 times, is finally dialysed 2 days with bag filter, is put into vacuum drying chamber the dry 20h at 80 DEG C afterwards, most
Abrasive flour obtains graphene oxide afterwards；
2nd, the preparation of graphene-nanometer titanium dioxide compound：
Graphene oxide 25mg obtained above is taken, adds 25mL deionized waters, using processor for ultrasonic wave under 60W power
40min is ultrasonically treated, the graphene oxide solution that mass concentration is 1mg/mL can be obtained；By 6.0g cetyl trimethyl bromines
Change ammonium to be dissolved in the mixed solution of 15mL n-amyl alcohols and 55mL n-hexanes, obtain hexadecyltrimethylammonium chloride solution；Will
While hexadecyltrimethylammonium chloride solution is added to graphene oxide solution, after 30min is stirred at room temperature, height is poured into
Press in reaction kettle, place in an oven, 200 DEG C of constant temperature 6h；Product after constant temperature is put into rotary evaporator reduced pressure treatment simultaneously
Precipitation, removes organic solvent, and obtained precipitation wash 3 times with deionized water and absolute ethyl alcohol repeatedly, removing surfactant with
Other impurities, obtained final product dry 1.5h under the conditions of being placed on 80 DEG C, that is, it is compound to obtain graphene-nano-titanium dioxide
Thing, is denoted as sample A；
3rd, ag nano-cluster-Nano silver grain/TiO2The preparation of/graphene composite photocatalyst：
Silver nitrate is soluble in water, add reduced glutathione to stir to colourless, then flow back 24h at 70 DEG C, adds acetonitrile
After purification, centrifuge, wash, is dry, obtaining solid silver nano cluster, obtained solid ag nano-cluster is re-dispersed into water,
Obtain ag nano-cluster solution；By graphene-nanometer titanium dioxide compound A and the mass ratio 100 of ag nano-cluster:5 by stone
4h is mixed under conditions of being 4 in pH value in black alkene-nanometer titanium dioxide compound and ag nano-cluster solution, centrifuge, wash,
It is dry, obtain ag nano-cluster/TiO2/ graphene, is denoted as sample B；It is placed in vacuum environment, under the conditions of lactic acid is existing
The photoreduction of 5h is carried out, obtains the ag nano-cluster-Nano silver grain/TiO2/ graphene composite photocatalyst, is denoted as sample
Product C.
Specific test method is as follows：Prepare the Acid Brilliant Scarlet GR solution that three parts of 200mL concentration are 8mg/mL and be used as print
The model of waste water is contaminated, adds in 0.01g embodiments 1 graphene-nanometer titanium dioxide compound the A, not prepared thereto respectively
Ag nano-cluster/TiO through photoreduction2/ graphene B and ag nano-cluster-Nano silver grain/TiO by photoreduction2/
Graphene composite photocatalyst C, it is 4.0 to be sufficiently stirred and adjust solution ph respectively, and mixed solution then is respectively charged into glass
In glass bottle, respective dark reaction 0.5h in dark surrounds, then under the xenon lamp irradiation of 500W, investigates different time catalyst to dirt
The degree of purification of waste water is contaminated, specific data are referring to table 1 below：
Degrading activity of the different samples of table 1. to Acid Brilliant Scarlet GR
It is compound compared to the graphene-nano-titanium dioxide modified without ag nano-cluster from the data analysis in table 1
Thing, by ag nano-cluster modification but ag nano-cluster/TiO without photoreduction2Degraded of/the graphene to Acid Brilliant Scarlet GR
Activity, which has, to be substantially improved, this is because ag nano-cluster is dispersed in the graphene sheet layer for being loaded with nano-titanium dioxide
On, add conduction and the separative efficiency in light induced electron and hole of light induced electron, and ag nano-cluster-silver Jing Guo photo-reduction
Nano-particle/TiO2The photocatalytic activity of/graphene composite photocatalyst under equal conditions has further lifting, can
Efficiently complete the efficient process to the dyeing waste water containing dyestuff.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind for the treatment of process of Visible Light Induced Photocatalytic dyeing waste water, it is characterised in that include the following steps：By ag nano-cluster-
Nano silver grain/TiO2/ graphene composite photocatalyst is added in certain density dyeing waste water, is sufficiently stirred and is adjusted molten
Liquid pH=3.5~4.5, mixed solution is transferred in vial, 0.5~1h of dark reaction in dark surrounds, then in 500W~600W
Xenon lamp under carry out room temperature, stirring visible light photocatalytic degradation react 0.5~2.5h.
2. the treatment process of Visible Light Induced Photocatalytic dyeing waste water as claimed in claim 1, it is characterised in that in the dyeing waste water
Contain Acid Brilliant Scarlet GR.
3. the treatment process of Visible Light Induced Photocatalytic dyeing waste water as claimed in claim 1, it is characterised in that the silver nanoparticle group
Cluster-Nano silver grain/TiO2The preparation method of/graphene composite photocatalyst includes the following steps：In 250~350mg graphite
Powder, 1.5~2.5g sodium nitrate mixed solution in, add the concentrated sulfuric acid of 15~25mL 98wt%, stirred at a temperature of 5 DEG C of ＜
Mix, allow it to react 1.5~2.0 h in beaker；By potassium permanganate grind into powder, then in 0.5h, added in beaker
1.5~2.0g powder, reacts 1.5~2.0h in 5 DEG C of ＜；Beaker is placed in insulating box and is warming up to 45~50 DEG C, Ran Houheng
1.5~2h of temperature, constant temperature terminates to add 40~50mL deionized waters in backward beaker, then temperature is risen to 80~90 DEG C, constant temperature 10
~20min；Then the solution in beaker is cooled to indoor temperature, adds the dilution of 80~120mL deionized waters, solution is changed into bright
Yellow, adds the hydrogenperoxide steam generator of 10~15mL 35wt% afterwards；Then filtered, by filter residue with 300~400mL
The salt acid elution of 5wt%, drains repeated washing three times with aspiration pump, is then washed with deionized again three times, finally uses bag filter
Dialysis two days, is put into vacuum drying chamber dry 20h, last abrasive flour at 80 DEG C and obtains graphene oxide afterwards.
4. the treatment process of Visible Light Induced Photocatalytic dyeing waste water as claimed in claim 1, it is characterised in that the silver nanoparticle group
Cluster-Nano silver grain/TiO2The preparation method of/graphene composite photocatalyst includes the following steps：Take oxidation obtained above
20~30mg of graphene, adds 20~30mL deionized waters, it is ultrasonically treated under 60W power 30 using processor for ultrasonic wave~
60min, can obtain the graphene oxide solution that mass concentration is 1mg/mL；By 5.0~6.0g cetyl trimethyl brominations
Ammonium is dissolved in the mixed solution of 5~20mL n-amyl alcohols and 50~65mL n-hexanes, and it is molten to obtain hexadecyltrimethylammonium chloride
Liquid；While hexadecyltrimethylammonium chloride solution is added to graphene oxide solution, after 30min is stirred at room temperature,
Pour into autoclave, place in an oven, 200 DEG C of constant temperature 6h；Product after constant temperature is put into rotary evaporator and is depressurized
Handle and precipitate, remove organic solvent, obtained precipitation is washed 2~5 times with deionized water and absolute ethyl alcohol repeatedly, removes surface
Activating agent and other impurities, obtained final product dry 1~4h under the conditions of being placed on 80 DEG C, that is, obtain graphene-nanometer two
Titanium oxide compound.
5. the treatment process of Visible Light Induced Photocatalytic dyeing waste water as claimed in claim 1, it is characterised in that the silver nanoparticle group
Cluster-Nano silver grain/TiO2The preparation method of/graphene composite photocatalyst includes the following steps：Silver nitrate is soluble in water,
Reduced glutathione is added to stir to colourless, then flow back 24h at 70 DEG C, adds acetonitrile after purification, centrifugation, washing, dry,
Solid silver nano cluster is obtained, obtained solid ag nano-cluster is re-dispersed into water, obtains ag nano-cluster solution；By stone
4h is mixed in black alkene-nanometer titanium dioxide compound and ag nano-cluster solution under mildly acidic conditions, and centrifugation, washing, do
It is dry, obtain ag nano-cluster/TiO2/ graphene；It is placed in vacuum environment, carries out illumination under the conditions of sacrifice agent is existing,
Obtain the ag nano-cluster-Nano silver grain/TiO2/ graphene composite photocatalyst.
6. the treatment process of Visible Light Induced Photocatalytic dyeing waste water as claimed in claim 5, it is characterised in that silver nitrate and reduced form
The weight ratio of glutathione is 1:1.
7. the treatment process of Visible Light Induced Photocatalytic dyeing waste water as claimed in claim 5, it is characterised in that mild acid conditions are pH value
For 4.
8. the treatment process of Visible Light Induced Photocatalytic dyeing waste water as claimed in claim 5, it is characterised in that the graphene-receive
The weight ratio of rice titanium dioxide compound and solid silver nano cluster is 100:2~100:8.
9. the treatment process of Visible Light Induced Photocatalytic dyeing waste water as claimed in claim 5, it is characterised in that the wavelength of the illumination
For 300nm~800nm, irradiation time is 3~60h, ag nano-cluster is passed through in various degree with the difference using illumination condition
Converted in-situ, obtains the Nano silver grain with different-grain diameter.
10. the treatment process of Visible Light Induced Photocatalytic dyeing waste water as claimed in claim 5, it is characterised in that the sacrifice agent is
Lactic acid.
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