CN106563500A - Preparation method of photocatalyst used for degrading organic pollutants - Google Patents
Preparation method of photocatalyst used for degrading organic pollutants Download PDFInfo
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- CN106563500A CN106563500A CN201610945900.2A CN201610945900A CN106563500A CN 106563500 A CN106563500 A CN 106563500A CN 201610945900 A CN201610945900 A CN 201610945900A CN 106563500 A CN106563500 A CN 106563500A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000002957 persistent organic pollutant Substances 0.000 title claims abstract description 15
- 230000000593 degrading effect Effects 0.000 title abstract 3
- 238000000034 method Methods 0.000 claims abstract description 59
- 239000000463 material Substances 0.000 claims abstract description 32
- 239000002114 nanocomposite Substances 0.000 claims abstract description 23
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 22
- 239000012298 atmosphere Substances 0.000 claims abstract description 21
- 239000010409 thin film Substances 0.000 claims abstract description 21
- 238000000137 annealing Methods 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 160
- 229910052757 nitrogen Inorganic materials 0.000 claims description 80
- 238000010926 purge Methods 0.000 claims description 68
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 66
- 238000006243 chemical reaction Methods 0.000 claims description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 59
- 239000008367 deionised water Substances 0.000 claims description 58
- 229910021641 deionized water Inorganic materials 0.000 claims description 58
- 238000000151 deposition Methods 0.000 claims description 42
- 230000001699 photocatalysis Effects 0.000 claims description 37
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 230000008021 deposition Effects 0.000 claims description 28
- 230000008569 process Effects 0.000 claims description 25
- 230000015556 catabolic process Effects 0.000 claims description 23
- 238000006731 degradation reaction Methods 0.000 claims description 23
- 229910052719 titanium Inorganic materials 0.000 claims description 23
- 239000010936 titanium Substances 0.000 claims description 23
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 21
- 239000011159 matrix material Substances 0.000 claims description 21
- 229910052760 oxygen Inorganic materials 0.000 claims description 21
- 239000001301 oxygen Substances 0.000 claims description 21
- 238000007146 photocatalysis Methods 0.000 claims description 21
- 241000292525 Titanio Species 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims description 20
- 230000005855 radiation Effects 0.000 claims description 19
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 18
- 230000015572 biosynthetic process Effects 0.000 claims description 17
- 238000007654 immersion Methods 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000000356 contaminant Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- 229910003074 TiCl4 Inorganic materials 0.000 claims description 12
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 230000003213 activating effect Effects 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 6
- 229920002521 macromolecule Polymers 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 5
- 239000004065 semiconductor Substances 0.000 claims description 5
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 239000013557 residual solvent Substances 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 22
- 230000004913 activation Effects 0.000 abstract description 19
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
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- 239000004744 fabric Substances 0.000 description 117
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 26
- 239000000243 solution Substances 0.000 description 17
- WXLFIFHRGFOVCD-UHFFFAOYSA-L azophloxine Chemical compound [Na+].[Na+].OC1=C2C(NC(=O)C)=CC(S([O-])(=O)=O)=CC2=CC(S([O-])(=O)=O)=C1N=NC1=CC=CC=C1 WXLFIFHRGFOVCD-UHFFFAOYSA-L 0.000 description 10
- CRPUJAZIXJMDBK-UHFFFAOYSA-N camphene Chemical compound C1CC2C(=C)C(C)(C)C1C2 CRPUJAZIXJMDBK-UHFFFAOYSA-N 0.000 description 10
- 238000005660 chlorination reaction Methods 0.000 description 10
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- 229920006221 acetate fiber Polymers 0.000 description 7
- GTRGJJDVSJFNTE-UHFFFAOYSA-N chembl2009633 Chemical compound OC1=CC=C2C=C(S(O)(=O)=O)C=CC2=C1N=NC1=CC=CC=C1 GTRGJJDVSJFNTE-UHFFFAOYSA-N 0.000 description 7
- 229910052717 sulfur Inorganic materials 0.000 description 7
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- -1 wherein Substances 0.000 description 6
- QPQKUYVSJWQSDY-UHFFFAOYSA-N 4-phenyldiazenylaniline Chemical compound C1=CC(N)=CC=C1N=NC1=CC=CC=C1 QPQKUYVSJWQSDY-UHFFFAOYSA-N 0.000 description 5
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 5
- PXRCIOIWVGAZEP-UHFFFAOYSA-N Primaeres Camphenhydrat Natural products C1CC2C(O)(C)C(C)(C)C1C2 PXRCIOIWVGAZEP-UHFFFAOYSA-N 0.000 description 5
- XCPQUQHBVVXMRQ-UHFFFAOYSA-N alpha-Fenchene Natural products C1CC2C(=C)CC1C2(C)C XCPQUQHBVVXMRQ-UHFFFAOYSA-N 0.000 description 5
- 229930006739 camphene Natural products 0.000 description 5
- ZYPYEBYNXWUCEA-UHFFFAOYSA-N camphenilone Natural products C1CC2C(=O)C(C)(C)C1C2 ZYPYEBYNXWUCEA-UHFFFAOYSA-N 0.000 description 5
- 150000002469 indenes Chemical class 0.000 description 5
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 5
- 239000004180 red 2G Substances 0.000 description 5
- 235000012739 red 2G Nutrition 0.000 description 5
- KKAJSJJFBSOMGS-UHFFFAOYSA-N 3,6-diamino-10-methylacridinium chloride Chemical compound [Cl-].C1=C(N)C=C2[N+](C)=C(C=C(N)C=C3)C3=CC2=C1 KKAJSJJFBSOMGS-UHFFFAOYSA-N 0.000 description 4
- 230000008878 coupling Effects 0.000 description 4
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- 239000006185 dispersion Substances 0.000 description 4
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- 239000002245 particle Substances 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- CKAPSXZOOQJIBF-UHFFFAOYSA-N hexachlorobenzene Chemical compound ClC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl CKAPSXZOOQJIBF-UHFFFAOYSA-N 0.000 description 3
- 150000002894 organic compounds Chemical class 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 108010073771 Soybean Proteins Proteins 0.000 description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 2
- XCJXQCUJXDUNDN-UHFFFAOYSA-N chlordene Chemical compound C12C=CCC2C2(Cl)C(Cl)=C(Cl)C1(Cl)C2(Cl)Cl XCJXQCUJXDUNDN-UHFFFAOYSA-N 0.000 description 2
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- 239000000992 solvent dye Substances 0.000 description 2
- 235000019710 soybean protein Nutrition 0.000 description 2
- 239000000988 sulfur dye Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 235000021419 vinegar Nutrition 0.000 description 2
- 239000000052 vinegar Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- KVGZZAHHUNAVKZ-UHFFFAOYSA-N 1,4-Dioxin Chemical compound O1C=COC=C1 KVGZZAHHUNAVKZ-UHFFFAOYSA-N 0.000 description 1
- HPARLNRMYDSBNO-UHFFFAOYSA-N 1,4-benzodioxine Chemical compound C1=CC=C2OC=COC2=C1 HPARLNRMYDSBNO-UHFFFAOYSA-N 0.000 description 1
- 241000283690 Bos taurus Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
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- 238000006065 biodegradation reaction Methods 0.000 description 1
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- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
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- 238000012851 eutrophication Methods 0.000 description 1
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- 231100000252 nontoxic Toxicity 0.000 description 1
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- 238000003980 solgel method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
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- 210000003462 vein Anatomy 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 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
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
-
- 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
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
- B01J35/59—Membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/06—Washing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Optics & Photonics (AREA)
- Electromagnetism (AREA)
- Plasma & Fusion (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention relates to a preparation method of a photocatalyst used for degrading organic pollutants and belongs to the technical field of catalyst preparation. The method is executed according to the following steps that a, a base material is cleaned and dried so that attachments on the surface of the base material can be removed, and then the surface of the base material is embellished through corona activation treatment; b, a functional nanometer TiO2 thin film is deposited on the surface of the activated base material by means of the atomic layer deposition technology, and a TiO2 functional nanocomposite is obtained; and c, the TiO2 functional nanocomposite is subjected to annealing treatment in the air atmosphere at 500-600 DEG C, and the photocatalyst used for degrading the organic pollutants is obtained. The preparation method aims at providing the photocatalyst which is large in specific surface area, high in catalytic activity, good in light transmission performance, capable of being recycled and wide in light response range, the preparation process is highly controllable, cost and the energy consumption are low, repeated use can be achieved, and pollution to the ecological environment is avoided.
Description
Technical field
The present invention relates to a kind of preparation method for degradable organic pollutant photocatalyst, belongs to catalyst preparation technology
Field.
Background technology
With national continuous development and progress, the life of generation and trade effluent are also gradually increasing, and especially industry is arranged
The waste water put has the features such as complicated component, organic compound content height, big Biochemical oxygen demand, difficult degradation, therefore, purified treatment
Technology has very important realistic meaning.Organic compound belongs to Recalcitrant chemicals, easily causes body eutrophication, environment
The problems such as pollution, wherein oxidation-reduction method, physisorphtion, biodegradation etc. method become solve life and trade effluent weight
Want one of approach, although these methods can to a certain extent solve the pollution problems such as waste water and waste gas, but not adapt to future
The requirement of environmental improvement, high efficiency, low cost and low energy consumption.The method of the photochemical catalysis for developing in recent years is in Environment control
The process of poisonous and hazardous difficult degradation persistent organism provides good approach, wherein the TiO with Detitanium-ore-type2
Become the object that photocatalyst is widely studied, TiO2It is typical N-type semiconductor, Detitanium-ore-type TiO2Bandgap value is
3.2eV, has the advantages that with low cost, nontoxic, catalysis activity is high and photochemical stability is good.Therefore, prepare specific surface area it is big,
Catalysis activity is high, the Detitanium-ore-type TiO that chemical stability is good2Become the focus of current photocatalyst research.China Patent No.
CN105032479A, publication date is on November 11st, 2015, a kind of entitled " TiO2The preparation method of photocatalyst ", the method
With natural zeolite as carrier, with butyl titanate as predecessor, natural zeolite support type light is prepared using sol-gel process
Catalyst, the photocatalyst that the technique is obtained not only has photocatalytic effect, while with certain adsorption function.But prepare
TiO2Particle diameter is larger, and photocatalysis efficiency is low, and TiO2Particle is poor in natural zeolite surface adhesion force, easily occurs peeling off or coming off,
So as to affect photocatalytic effect.China Patent Publication No. CN105107538A, publication date is on December 2nd, 2015, entitled " one
Plant sulfur N doping TiO2Nitric acid is added butyl titanate to form mixed solution by the preparation method of photocatalyst ", the method first,
Then press element proportioning and add thioacetamide, through hydro-thermal reaction, washing and dry prepared sulfur N doping TiO2Photocatalyst,
Catalysis activity is high during Cr (VI) catalytic degradation.But the method preparation efficiency is low, catalysis scope is little, strong for Cr (VI) etc.
Oxidant can just highlight catalytic efficiency.China Patent Publication No. CN105536765A, publication date is on May 4th, 2016, entitled
" a kind of shell base boron-doped titanium dioxide composite photo-catalyst and preparation method thereof ", the technique with titanate esters as presoma, boric acid
Primary response liquid is prepared for additive with conch meal, then through the operations such as hydro-thermal reaction, grinding and calcining, the shell base for obtaining
The active height of boron-doped titanium dioxide composite photo-catalyst, the advantages of recycling, but complicated process of preparation, efficiency is low, and
Secondary pollution may be brought.
The content of the invention
For the problems referred to above, it is an object of the invention to provide a kind of preparation for degradable organic pollutant photocatalyst
Method.
To achieve these goals, technical solution of the invention is that one kind is used for degradable organic pollutant photocatalysis
The preparation method of agent, described method is carried out according to the following steps:
A. matrix material is placed in into organic solvent for ultrasonic cleaning 30-60min, then deionized water carries out immersion 20min,
To remove the residual solvent of substrate material surface, the matrix material after process is dried up with nitrogen, standby;Organic solvent used is
Methanol or ethanol or propanol or isopropanol or n-butyl alcohol or ether or acetone or butanone or the one kind in chloroform.
B. the matrix material Jing after the cleaning that step a is obtained is adopted into low temperature corona radiation treatment 5-10min, is activated
Matrix material, wherein, the temperature of low temperature corona irradiation is 10-45 DEG C, and the voltage of low temperature corona irradiation is 6-15KV, low temp. electric
The distance of dizzy irradiation is 0.5-3cm, and matrix material used is porous material of the decomposition temperature less than 280 DEG C or quasiconductor material
Material or natural macromolecular material or synthesising macromolecule copolymer class material, wherein, porous material includes carbon fiber, microsphere, silicon
Glue, natural macromolecular material includes paper, cotton fiber and its fabric, bamboo fibre and its fabric, flaxen fiber and its fabric, silk fiber
And its fabric, wool fiber and its fabric, down fiber and its fabric, soybean fiber and its fabric, milk protein fiber
And its fabric, semi-conducting material include monocrystalline silicon piece, monocrystalline germanium wafer, synthesising macromolecule copolymer class material include viscose rayon or
Fabric, acetate fiber or fabric, polyster fibre or fabric, vinylon fibre or fabric, acrylic fiber or fabric, CUP are knitted
Thing.
C. the activated matrix material Jing after the process of step b is placed in the reaction cavity of atomic layer deposition apparatus, and with pure
The nitrogen purging 3-10min for 99.9999% is spent, at 120-200 DEG C, chamber pressure is controlled in 50Pa- for cavity temperature control
80Pa, is then more than 97% TiCl with purity4Or titanium tetraisopropylate is titanium source, deionized water is oxygen source, by TiCl during deposition4
Or titanium tetraisopropylate is heated to 60-120 DEG C of formation TiCl4Or titanium tetraisopropylate steam, then pulse to reaction cavity, pulse
Time is 0.05-0.5s, and open-assembly time is 8-25s, then is purged with the nitrogen that purity is 99.9999%, and purge time is 15-
30s, then by deionized water pulse to reaction cavity, the burst length is 0.01-0.2s, and open-assembly time is 8-25s, then with pure
Spend the nitrogen purging for 99.9999%, purge time is 15-30s, complete primary depositing circulation, i.e., it is heavy in substrate material surface
One layer of titanio function nano thin film is accumulated.
D. the deposition cycle of repeat step c 100-10000 time, obtains titanio functional nanocomposite.
E. the titanio functional nanocomposite for Jing steps d being obtained 500-600 DEG C of annealing 0.5-4h in air atmosphere,
Obtain the photocatalyst for degradable organic pollutant.
The Detitanium-ore-type TiO of preparation2The organic pollution that can be degraded is chlorination indenes, heptachlor indenes, chlorination camphene, chlordene
Benzene, Polychlorinated biphenyls, polychlorinated dibenzo-2 dislike English, polychlorinated dibenzo, acid stain (acid bright red E-B), azoic dyes (color
Phenol AS), the dye of positive ion (basic flavine O), direct dyess (directly black OB), disperse dyes (the gorgeous Huang of dispersion), reactive dye it is (living
The gorgeous orange X-2R of property), sulfur dye (sulfur blue CV), reducing dye (vat red 2G), the one kind in solvent dye (solvent yellow BL)
Or it is several.
Due to a kind of preparation for degradable organic pollutant photocatalyst provided using above technical scheme, the present invention
The beneficial effect of method is:
(1) present invention prepares Detitanium-ore-type TiO using technique for atomic layer deposition2, it is preparation process is simple, easy to operate, raw
Produce efficiency high, cost and energy consumption low, the TiO of preparation2Substrate material surface is formed in by way of chemical bonding, and is distributed
Uniformly, the conformality of particle is good, can effectively prevent TiO2Reuniting and reducing specific surface area occur in preparation process in particle so that
Photocatalysis efficiency is reduced.
(2) present invention is preparing Detitanium-ore-type TiO2During, matrix material used is various in style, applied widely,
Residue does not affect TiO after calcining2The functionalization characteristic of itself, it is also possible to utilize to waste and old matrix material, carries
The utilization rate of high matrix material.
(3) Detitanium-ore-type TiO prepared by the present invention2With good light transmission, catalysis activity height, can recycle and light
Response range is big, preferable for the photocatalytic degradation effect of the organic compound of various difficult degradations, either the also right and wrong of azo
Azo, acid still alkalescence, all effect with fast degradation.
Description of the drawings
Fig. 1 is calcined product Detitanium-ore-type TiO2XRD figure.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
A kind of preparation method for degradable organic pollutant photocatalyst, methods described is carried out according to the following steps:
A. matrix material is placed in into organic solvent for ultrasonic cleaning 30-60min, then deionized water carries out immersion 20min,
To remove the residual solvent of substrate material surface, the matrix material after process is dried up with nitrogen, standby;Organic solvent used is
Methanol or ethanol or propanol or isopropanol or n-butyl alcohol or ether or acetone or butanone or the one kind in chloroform.
B. the matrix material Jing after the cleaning that step a is obtained is adopted into low temperature corona radiation treatment 5-10min, is activated
Matrix material, wherein, the temperature of low temperature corona irradiation is 10-45 DEG C, and the voltage of low temperature corona irradiation is 6-15KV, low temp. electric
The distance of dizzy irradiation is 0.5-3cm, and matrix material used is porous material of the decomposition temperature less than 280 DEG C or quasiconductor material
Material or natural macromolecular material or synthesising macromolecule copolymer class material.Wherein, porous material includes carbon fiber, microsphere, silicon
Glue, natural macromolecular material includes paper, cotton fiber and its fabric, bamboo fibre and its fabric, flaxen fiber and its fabric, silk fiber
And its fabric, wool fiber and its fabric, down fiber and its fabric, soybean fiber and its fabric, milk protein fiber
And its fabric, semi-conducting material include monocrystalline silicon piece, monocrystalline germanium wafer, synthesising macromolecule copolymer class material include viscose rayon or
Fabric, acetate fiber or fabric, polyster fibre or fabric, vinylon fibre or fabric, acrylic fiber or fabric, CUP are knitted
Thing.
C. the activated matrix material Jing after the process of step b is placed in the reaction cavity of atomic layer deposition apparatus, and with pure
The nitrogen purging 3-10min for 99.9999% is spent, at 120-200 DEG C, chamber pressure is controlled in 50Pa- for cavity temperature control
80Pa, is then more than 97% TiCl with purity4Or titanium tetraisopropylate is titanium source, deionized water is oxygen source, by TiCl during deposition4
Or titanium tetraisopropylate is heated to 60-120 DEG C of formation TiCl4Or titanium tetraisopropylate steam, then pulse to reaction cavity, pulse
Time is 0.05-0.5s, and open-assembly time is 8-25s, then is purged with the nitrogen that purity is 99.9999%, and purge time is 15-
30s, then by deionized water pulse to reaction cavity, the burst length is 0.01-0.2s, and open-assembly time is 8-25s, then with pure
Spend the nitrogen purging for 99.9999%, purge time is 15-30s, complete primary depositing circulation, i.e., it is heavy in substrate material surface
One layer of titanio function nano thin film is accumulated;
D. the deposition cycle of repeat step c 100-10000 time, obtains titanio functional nanocomposite;
E. the titanio functional nanocomposite for Jing steps d being obtained 500-600 DEG C of annealing 0.5-4h in air atmosphere,
Obtain the photocatalyst for degradable organic pollutant, described Detitanium-ore-type TiO2For typical N-type semiconductor, and bandgap
Value is 3.2eV, electron transition can occur under visible light conditions and have catalytic effect.
The Detitanium-ore-type TiO prepared using the method2Size tunable, conformality is good, mainly by the side of chemical bonding
Formula is formed in substrate material surface, and matrix material is to TiO after calcining2Photo-catalysis function do not produce impact, what is prepared is sharp
Titanium ore type TiO2It is high with catalysis activity, can recycle, photoresponse scope is big, especially to following various difficult degradation organic contaminations
The photocatalytic degradation effect of thing is preferable, such as chlorination indenes, heptachlor indenes, chlorination camphene, Perchlorobenzene, Polychlorinated biphenyls, many chlorodiphenyls simultaneously
Dioxin, polychlorinated dibenzo, acid stain (acid bright red E-B), azoic dyes (azoic coupling component AS), the dye of positive ion (alkalescence
Light yellow O), direct dyess (directly black OB), disperse dyes (the gorgeous Huang of dispersion), reactive dye (reactive brilliant orange X-2R), sulfur dye
One or more in (sulfur blue CV), reducing dye (vat red 2G), solvent dye (solvent yellow BL).
Embodiment 1
Carbon fiber is placed in methanol and is cleaned by ultrasonic 30min, then deionized water carries out immersion 20min, with except carbon elimination fibre
The residual methanol in dimension table face, the carbon fiber after process is dried up with nitrogen, standby;Carbon fiber after cleaning adopts low temperature corona irradiation
5min is processed, the carbon fiber for activating is obtained, wherein, the temperature of low temperature corona irradiation is 10 DEG C, and the voltage of low temperature corona irradiation is
6KV, the distance of low temperature corona irradiation is 0.5cm, and the carbon fiber after activation is placed in the reaction cavity of atomic layer deposition apparatus, and
With nitrogen that purity is 99.9999% purging 3min, cavity temperature control at 120 DEG C, chamber pressure control in 50Pa, then with
TiCl of the purity more than 97%4For titanium source, deionized water is oxygen source, by TiCl during deposition4It is heated to 60 DEG C of formation TiCl4Steam,
Then to reaction cavity, the burst length is 0.05s for pulse, and open-assembly time is 8s, then is blown with the nitrogen that purity is 99.9999%
Sweep, purge time is 15s, then by deionized water pulse to reaction cavity, the burst length is 0.01s, and open-assembly time is 8s,
Again with the nitrogen purging that purity is 99.9999%, purge time is 15s, i.e., deposited one layer of titanio function in carbon fiber surface
Nano thin-film, repeats this deposition cycle 100 times, by titanio functional nanocomposite in air atmosphere 500 DEG C of annealing 0.5h,
Obtain the photocatalyst for photocatalysis degradation organic contaminant
The Detitanium-ore-type TiO obtained using said method2Quality is 0.07-0.1mg, in adding chlorination indenes solution, wherein
Chlorination indenes concentration is 20mg/L, and volume is 50mL, and 30min is stood in visible ray, and chlorination indenes photocatalytic activity is 23.2%.
Embodiment 2
Microsphere is placed in ethanol and is cleaned by ultrasonic 40min, then deionized water carries out immersion 20min, to remove microsphere table
The residual ethanol in face, the microsphere after process is dried up with nitrogen, standby;Microsphere after cleaning adopts low temperature corona radiation treatment
6min, obtains the microsphere for activating, wherein, the temperature of low temperature corona irradiation is 15 DEG C, and the voltage of low temperature corona irradiation is 8KV, low
The distance of warm corona irradiation is 0.8cm, and the microsphere after activation is placed in the reaction cavity of atomic layer deposition apparatus, and is with purity
99.9999% nitrogen purging 5min, at 140 DEG C, chamber pressure is controlled in 60Pa, is then more than with purity for cavity temperature control
97% titanium tetraisopropylate is titanium source, and deionized water is oxygen source, and titanium tetraisopropylate is heated to into 60 DEG C of four isopropyls of formation during deposition
Alcohol titanium tetrachloride vapor, then to reaction cavity, the burst length is 0.1s, and open-assembly time is 10s, then is with purity for pulse
99.9999% nitrogen purging, purge time is 18s, and then by deionized water pulse to reaction cavity, the burst length is
0.02s, open-assembly time is 10s, then is purged with the nitrogen that purity is 99.9999%, and purge time is 16s, i.e., in microsphere surface
One layer of titanio function nano thin film is deposited, repeats this deposition cycle 500 times, by titanio functional nanocomposite in air atmosphere
550 DEG C of annealing 1h, obtain the photocatalyst for photocatalysis degradation organic contaminant in enclosing
The Detitanium-ore-type TiO obtained using said method2Quality be 0.2-0.3mg, add heptachlor indenes solution in, its
The concentration of middle heptachlor indenes is 20mg/L, and volume is 50mL, and 30min, heptachlor indenes photocatalytic activity are stood in visible ray
For 37.3%.
Embodiment 3
Cotton fiber and its fabric are placed in ethanol and are cleaned by ultrasonic 45min, then deionized water carries out immersion 20min, with
The residual ethanol of cotton fiber and its fabric face is removed, the cotton fiber and its fabric after process is dried up with nitrogen, standby;After cleaning
Cotton fiber and its fabric adopt low temperature corona radiation treatment 7min, obtain activate cotton fiber and its fabric, wherein, low temp. electric
The temperature of dizzy irradiation is 18 DEG C, and the voltage of low temperature corona irradiation is 10KV, and the distance of low temperature corona irradiation is 1.0cm, after activation
Cotton fiber and its fabric be placed in the reaction cavity of atomic layer deposition apparatus, and with nitrogen that purity is 99.9999% purging
6min, at 150 DEG C, chamber pressure is controlled in 65Pa for cavity temperature control, and then the titanium tetraisopropylate with purity more than 97% is
Titanium source, deionized water is oxygen source, and titanium tetraisopropylate is heated to into 80 DEG C of formation titanium tetraisopropylate steams during deposition, and then pulse is extremely
In reaction cavity, the burst length is 0.15s, and open-assembly time is 12s, then is purged with the nitrogen that purity is 99.9999%, during purging
Between be 20s, then by deionized water pulse to reaction cavity, the burst length is 0.05s, and open-assembly time is 10s, then uses purity
Nitrogen for 99.9999% is purged, and purge time is 18s, i.e., deposited one layer of titanio function in cotton fiber and its fabric face
Nano thin-film, repeats this deposition cycle 1000 times, by titanio functional nanocomposite in air atmosphere 550 DEG C of annealing 1h,
Obtain the photocatalyst for photocatalysis degradation organic contaminant.
The Detitanium-ore-type TiO obtained using said method2Quality be 0.6-0.7mg, add chlorination camphene solution in, its
The concentration of middle chlorination camphene is 20mg/L, and volume is 50mL, and 30min, chlorination camphene photocatalytic activity are stood in visible ray
For 42.1%.
Embodiment 4
Bamboo fibre and its fabric are placed in propanol and are cleaned by ultrasonic 50min, then deionized water carries out immersion 20min, with
The residual propanol of bamboo fibre and its fabric face is removed, the bamboo fibre and its fabric after process is dried up with nitrogen, standby;After cleaning
Bamboo fibre and its fabric adopt low temperature corona radiation treatment 8min, obtain activate bamboo fibre and its fabric, wherein, low temp. electric
The temperature of dizzy irradiation is 20 DEG C, and the voltage of low temperature corona irradiation is 10KV, and the distance of low temperature corona irradiation is 1.2cm, after activation
Bamboo fibre and its fabric be placed in the reaction cavity of atomic layer deposition apparatus, and with nitrogen that purity is 99.9999% purging
8min, at 160 DEG C, chamber pressure is controlled in 70Pa for cavity temperature control, and then the titanium tetraisopropylate with purity more than 97% is
Titanium source, deionized water is oxygen source, and titanium tetraisopropylate is heated to into 85 DEG C of formation titanium tetraisopropylate steams during deposition, and then pulse is extremely
In reaction cavity, the burst length is 0.2s, and open-assembly time is 14s, then is purged with the nitrogen that purity is 99.9999%, during purging
Between be 22s, then by deionized water pulse to reaction cavity, the burst length is 0.08s, and open-assembly time is 12s, then uses purity
Nitrogen for 99.9999% is purged, and purge time is 20s, i.e., deposited one layer of titanio function in bamboo fibre and its fabric face
Nano thin-film, repeats this deposition cycle 1500 times, by titanio functional nanocomposite in air atmosphere 580 DEG C of annealing 1h,
Obtain the photocatalyst for photocatalysis degradation organic contaminant.
The Detitanium-ore-type TiO obtained using said method2Quality be 0.9-1.0mg, add chlordene benzole soln in, wherein
The concentration of Perchlorobenzene is 20mg/L, and volume is 50mL, and 30min is stood in visible ray, and Perchlorobenzene photocatalytic activity is
48.1%.
Embodiment 5
Flaxen fiber and its fabric are placed in isopropanol and are cleaned by ultrasonic 50min, then deionized water carries out immersion 20min,
To remove the residual isopropanol of flaxen fiber and its fabric, the flaxen fiber and its fabric after process is dried up with nitrogen, standby;After cleaning
Flaxen fiber and its fabric adopt low temperature corona radiation treatment 8min, obtain activate flaxen fiber and its fabric, wherein, low temp. electric
The temperature of dizzy irradiation is 18 DEG C, and the voltage of low temperature corona irradiation is 15KV, and the distance of low temperature corona irradiation is 1.5cm, after activation
Flaxen fiber and its fabric be placed in the reaction cavity of atomic layer deposition apparatus, and with nitrogen that purity is 99.9999% purging
8min, at 180 DEG C, then chamber pressure control be more than 97% TiCl in 80Pa with purity for cavity temperature control4For titanium source,
Deionized water is oxygen source, by TiCl during deposition4It is heated to 75 DEG C of formation TiCl4Steam, then pulse to reaction cavity, pulse
Time is 0.2s, and open-assembly time is 14s, then is purged with the nitrogen that purity is 99.9999%, and purge time is 22s, then will be gone
To reaction cavity, the burst length is 0.1s to ion aquapulse, and open-assembly time is 16s, then with the nitrogen that purity is 99.9999%
Purging, purge time is 25s, i.e., deposited one layer of titanio function nano thin film in flaxen fiber and its fabric face, repeats this and sinks
Product circulation 2000 times, by titanio functional nanocomposite in air atmosphere 550 DEG C annealing 1.5h, obtain for photocatalysis drop
The photocatalyst of solution organic pollution.
The Detitanium-ore-type TiO obtained using said method2Quality be 1.15-1.2mg, add Polychlorinated biphenyls solution in,
Wherein Polychlorinated biphenyls concentration is 20mg/L, and volume is 50mL, and 30min, Polychlorinated biphenyls photocatalytic activity are stood in visible ray
For 53.6%.
Embodiment 6
Silk fiber and its fabric are placed in n-butyl alcohol and are cleaned by ultrasonic 60min, then deionized water is soaked
20min, to remove the residual n-butyl alcohol of silk fiber and its fabric, the silk fiber and its fabric after process is dried up with nitrogen,
It is standby;Silk fiber and its fabric after cleaning adopt low temperature corona radiation treatment 8min, obtain activate silk fiber and its
Fabric, wherein, the temperature of low temperature corona irradiation is 25 DEG C, and the voltage of low temperature corona irradiation is 12KV, low temperature corona irradiation away from
From for 1.8cm, the silk fiber and its fabric after activation is placed in the reaction cavity of atomic layer deposition apparatus, and is with purity
99.9999% nitrogen purging 10min, cavity temperature control is at 180 DEG C, and chamber pressure is controlled in 55Pa, then big with purity
In 97% TiCl4For titanium source, deionized water is oxygen source, by TiCl during deposition4It is heated to 80 DEG C of formation TiCl4Steam, then arteries and veins
Rush to reaction cavity, the burst length is 0.25s, open-assembly time is 18s, then with the nitrogen purging that purity is 99.9999%, blow
Flyback time is 25s, and then by deionized water pulse to reaction cavity, the burst length is 0.12s, and open-assembly time is 18s, then is used
Purity is 99.9999% nitrogen purging, and purge time is 25s, i.e., deposited one layer of titanium in silk fiber and its fabric face
Base function nano thin film, repeats this deposition cycle 2500 times, and titanio functional nanocomposite is moved back for 600 DEG C in air atmosphere
Fiery 1.5h, obtains the photocatalyst for photocatalysis degradation organic contaminant.
The Detitanium-ore-type TiO obtained using said method2Quality be 1.4-1.6mg, add polychlorinated dibenzo-2 dislike English
In solution, it is 20mg/L that wherein polychlorinated dibenzo-2 dislikes English concentration, and volume is 50mL, and 30min, many chlorine two are stood in visible ray
Benzo dioxin photocatalytic activity is 58.4%.
Embodiment 7
Wool fiber and its fabric are placed in ether and are cleaned by ultrasonic 60min, then deionized water carries out immersion 20min,
To remove the residual ether of wool fiber and its fabric face, the wool fiber and its fabric after process is dried up with nitrogen, standby;
Wool fiber and its fabric after cleaning adopts low temperature corona radiation treatment 8min, obtains wool fiber and its fabric for activating,
Wherein, the temperature of low temperature corona irradiation is 20 DEG C, and the voltage of low temperature corona irradiation is 10KV, and the distance of low temperature corona irradiation is
1.2cm, the wool fiber and its fabric after activation is placed in the reaction cavity of atomic layer deposition apparatus, and is with purity
99.9999% nitrogen purging 8min, at 160 DEG C, chamber pressure is controlled in 70Pa, is then more than with purity for cavity temperature control
97% titanium tetraisopropylate is titanium source, and deionized water is oxygen source, and titanium tetraisopropylate is heated to into 85 DEG C of four isopropyls of formation during deposition
Alcohol titanium tetrachloride vapor, then to reaction cavity, the burst length is 0.2s, and open-assembly time is 14s, then is with purity for pulse
99.9999% nitrogen purging, purge time is 22s, and then by deionized water pulse to reaction cavity, the burst length is
0.08s, open-assembly time is 12s, then is purged with the nitrogen that purity is 99.9999%, and purge time is 20s, i.e., in wool fiber
And its fabric face deposited one layer of titanio function nano thin film, repeat this deposition cycle 3000 times, titanio function nano is answered
Condensation material 580 DEG C of annealing 2h in air atmosphere, obtain the photocatalyst for photocatalysis degradation organic contaminant.
The Detitanium-ore-type TiO obtained using said method2Quality be 1.7-1.9mg, add polychlorinated dibenzo it is molten
In liquid, wherein the concentration of polychlorinated dibenzo is 20mg/L, and volume is 50mL, and in visible ray 30min is stood, and many chlorodiphenyls are simultaneously
Furan photocatalytic activity is 63.5%.
Embodiment 8
Down fiber and its fabric are placed in acetone and are cleaned by ultrasonic 60min, then deionized water carries out immersion 20min,
To remove the residual acetone of down fiber and its fabric face, the down fiber and its fabric after process is dried up with nitrogen, standby;
Down fiber and its fabric after cleaning adopts low temperature corona radiation treatment 10min, obtains down fiber and its fabric for activating,
Wherein, the temperature of low temperature corona irradiation is 30 DEG C, and the voltage of low temperature corona irradiation is 12KV, and the distance of low temperature corona irradiation is
2.0cm, the down fiber and its fabric after activation is placed in the reaction cavity of atomic layer deposition apparatus, and is with purity
99.9999% nitrogen purging 8min, at 200 DEG C, chamber pressure is controlled in 70Pa, is then more than with purity for cavity temperature control
97% titanium tetraisopropylate is titanium source, and deionized water is oxygen source, and titanium tetraisopropylate is heated to into 85 DEG C of four isopropyls of formation during deposition
Alcohol titanium tetrachloride vapor, then to reaction cavity, the burst length is 0.3s, and open-assembly time is 25s, then is with purity for pulse
99.9999% nitrogen purging, purge time is 28s, and then by deionized water pulse to reaction cavity, the burst length is
0.12s, open-assembly time is 25s, then is purged with the nitrogen that purity is 99.9999%, and purge time is 26s, i.e., in down fiber
And its fabric face deposited one layer of titanio function nano thin film, repeat this deposition cycle 3500 times, titanio function nano is answered
Condensation material 580 DEG C of annealing 2.5h in air atmosphere, obtain the photocatalyst for photocatalysis degradation organic contaminant.
The Detitanium-ore-type TiO obtained using said method2Quality be 2.0-2.2mg, add acid bright red E-B solution
In, wherein the concentration of acid bright red E-B is 20mg/L, volume is 50mL, and 30min, acid bright red E-B light are stood in visible ray
Catalysis degradation modulus are 68.8%.
Embodiment 9
Milk protein fiber and its fabric are placed in butanone and are cleaned by ultrasonic 45min, then deionized water is soaked
20min, the milk protein fiber and its fabric nitrogen to remove the residual butanone of milk protein fiber and its fabric, after process
Dry up, it is standby;Milk protein fiber and its fabric after cleaning adopts low temperature corona radiation treatment 10min, obtains the cattle for activating
Milk proem fiber and its fabric, wherein, the temperature of low temperature corona irradiation is 30 DEG C, and the voltage of low temperature corona irradiation is 8KV, low temperature
The distance of corona irradiation is 2.4cm, and the milk protein fiber and its fabric after activation is placed in the reaction chamber of atomic layer deposition apparatus
In vivo, and with the nitrogen that purity is 99.9999% 10min is purged, at 200 DEG C, chamber pressure control exists for cavity temperature control
60Pa, is then more than 97% TiCl with purity4For titanium source, deionized water is oxygen source, by TiCl during deposition4It is heated to 100 DEG C of shapes
Into TiCl4Steam, then to reaction cavity, the burst length is 0.3s, and open-assembly time is 18s, then is with purity for pulse
99.9999% nitrogen purging, purge time is 20s, and then by deionized water pulse to reaction cavity, the burst length is
0.15s, open-assembly time is 20s, then is purged with the nitrogen that purity is 99.9999%, and purge time is 25s, i.e., in milk protein
Fiber and its fabric face deposited one layer of titanio function nano thin film, repeat this deposition cycle 4000 times, and titanio function is received
Nano composite material 600 DEG C of annealing 3.5h in air atmosphere, obtain the photocatalyst for photocatalysis degradation organic contaminant.
The Detitanium-ore-type TiO obtained using said method2Quality be 2.3-2.4mg, add azoic coupling component AS solution in, wherein
Azoic coupling component AS concentration is 20mg/L, and volume is 50mL, and 30min is stood in visible ray, and azoic coupling component AS photocatalytic activities are 74.4%.
Embodiment 10
Soybean fiber and its fabric are placed in chloroform and are cleaned by ultrasonic 45min, then deionized water is soaked
20min, the soybean fiber and its fabric nitrogen to remove the residual chloroform of soybean fiber and its fabric, after process
Dry up, it is standby;Soybean fiber and its fabric after cleaning adopts low temperature corona radiation treatment 10min, obtains the big of activation
Soybean protein fiber and its fabric, wherein, the temperature of low temperature corona irradiation is 30 DEG C, and the voltage of low temperature corona irradiation is 8KV, low temperature
The distance of corona irradiation is 2.8cm, and the soybean fiber and its fabric after activation is placed in the reaction chamber of atomic layer deposition apparatus
In vivo, and with the nitrogen that purity is 99.9999% 10min is purged, at 200 DEG C, chamber pressure control exists for cavity temperature control
64Pa, is then more than 97% TiCl with purity4For titanium source, deionized water is oxygen source, by TiCl during deposition4It is heated to 100 DEG C of shapes
Into TiCl4Steam, then to reaction cavity, the burst length is 0.3s, and open-assembly time is 25s, then is with purity for pulse
99.9999% nitrogen purging, purge time is 30s, and then by deionized water pulse to reaction cavity, the burst length is
0.15s, open-assembly time is 20s, then is purged with the nitrogen that purity is 99.9999%, and purge time is 28s, i.e., in soybean protein
Fiber and its fabric face deposited one layer of titanio function nano thin film, repeat this deposition cycle 4500 times, and titanio function is received
Nano composite material 600 DEG C of annealing 3.5h in air atmosphere, obtain the photocatalyst for photocatalysis degradation organic contaminant.
The Detitanium-ore-type TiO obtained using said method2Quality be 2.6-2.75mg, add basic flavine O solution in,
Wherein basic flavine O concentration is 20mg/L, and volume is 50mL, and 30min, basic flavine O photocatalytic degradation are stood in visible ray
Rate is 79.1%.
Embodiment 11
Monocrystalline silicon piece is placed in acetone and is cleaned by ultrasonic 40min, then deionized water carries out immersion 20min, to remove list
The residual acetone on crystal silicon chip surface, the monocrystalline silicon piece after process is dried up with nitrogen, standby;Monocrystalline silicon piece after cleaning adopts low temperature
Corona radiation treatment 6min, obtains the monocrystalline silicon piece for activating, wherein, the temperature of low temperature corona irradiation is 45 DEG C, low temperature corona spoke
According to voltage be 6KV, the distance of low temperature corona irradiation is 2.5cm, and the monocrystalline silicon piece after activation is placed in atomic layer deposition apparatus
In reaction cavity, and 8min is purged with the nitrogen that purity is 99.9999%, at 190 DEG C, chamber pressure is controlled for cavity temperature control
In 60Pa, then as titanium source, deionized water is oxygen source to the titanium tetraisopropylate with purity more than 97%, by titanium tetraisopropylate during deposition
110 DEG C of formation titanium tetraisopropylate steams are heated to, then to reaction cavity, the burst length is 0.35s for pulse, and open-assembly time is
20s, then purged with the nitrogen that purity is 99.9999%, purge time is 28s, then by deionized water pulse to reaction cavity
Interior, the burst length is 0.15s, and open-assembly time is 20s, then is purged with the nitrogen that purity is 99.9999%, and purge time is 26s,
One layer of titanio function nano thin film is deposited in monocrystalline silicon sheet surface, repeat this deposition cycle 5000 times, titanio function is received
Nano composite material 550 DEG C of annealing 2.5h in air atmosphere, obtain the photocatalyst for photocatalysis degradation organic contaminant.
The Detitanium-ore-type TiO obtained using said method2Quality be 2.9-3.1mg, in adding directly black OB solution, its
In the concentration of direct black OB be 20mg/L, volume is 50mL, and 30min is stood in visible ray, directly black OB photocatalytic activities
For 84.6%.
Embodiment 12
Monocrystalline germanium wafer is placed in chloroform and is cleaned by ultrasonic 50min, then deionized water carries out immersion 20min, to remove list
The residual chloroform of brilliant germanium wafer, the monocrystalline germanium wafer after process is dried up with nitrogen, standby;Monocrystalline germanium wafer after cleaning adopts low temperature corona
Radiation treatment 8min, obtains the monocrystalline germanium wafer for activating, wherein, the temperature of low temperature corona irradiation is 45 DEG C, low temperature corona irradiation
Voltage is 8KV, and the distance of low temperature corona irradiation is 3.0cm, and the monocrystalline germanium wafer after activation is placed in the reaction of atomic layer deposition apparatus
In cavity, and 5min is purged with the nitrogen that purity is 99.9999%, at 150 DEG C, chamber pressure control exists for cavity temperature control
55Pa, is then more than 97% TiCl with purity4For titanium source, deionized water is oxygen source, by TiCl during deposition4It is heated to 100 DEG C of shapes
Into TiCl4Steam, then to reaction cavity, the burst length is 0.4s, and open-assembly time is 18s, then is with purity for pulse
99.9999% nitrogen purging, purge time is 25s, and then by deionized water pulse to reaction cavity, the burst length is
0.2s, open-assembly time is 18s, then is purged with the nitrogen that purity is 99.9999%, and purge time is 30s, i.e., in monocrystalline germanium wafer table
Face deposited one layer of titanio function nano thin film, repeat this deposition cycle 5500 times, by titanio functional nanocomposite in sky
Atmosphere enclose in 600 DEG C annealing 4.0h, obtain the photocatalyst for photocatalysis degradation organic contaminant.
The Detitanium-ore-type TiO obtained using said method2Quality be 3.3-3.4mg, in adding the gorgeous yellow solution of dispersion, its
Middle to disperse gorgeous yellow concentration to be 20mg/L, volume is 50mL, and 30min is stood in visible ray, and the gorgeous gold-tinted catalysis degradation modulus of dispersion are
89.1%.
Embodiment 13
Viscose rayon or fabric are placed in ethanol and are cleaned by ultrasonic 30min, then deionized water carries out immersion 20min, with
The residual ethanol of viscose rayon or fabric face is removed, the viscose rayon or fabric after process is dried up with nitrogen, standby;After cleaning
Viscose rayon or fabric adopt low temperature corona radiation treatment 6min, obtain activate viscose rayon or fabric, wherein, low temp. electric
The temperature of dizzy irradiation is 35 DEG C, and the voltage of low temperature corona irradiation is 8KV, and the distance of low temperature corona irradiation is 2.5cm, after activation
Viscose rayon or fabric are placed in the reaction cavity of atomic layer deposition apparatus, and are purged with the nitrogen that purity is 99.9999%
8min, at 160 DEG C, chamber pressure is controlled in 65Pa for cavity temperature control, and then the titanium tetraisopropylate with purity more than 97% is
Titanium source, deionized water is oxygen source, and titanium tetraisopropylate is heated to into 110 DEG C of formation titanium tetraisopropylate steams, then pulse during deposition
To reaction cavity, the burst length is 0.4s, and open-assembly time is 20s, then with the nitrogen purging that purity is 99.9999%, is purged
Time is 30s, and then by deionized water pulse to reaction cavity, the burst length is 0.15s, and open-assembly time is 30s, then with pure
The nitrogen purging for 99.9999% is spent, purge time is 26s, i.e., deposited one layer of titanio work(in viscose rayon or fabric face
Energy nano thin-film, repeats this deposition cycle 6000 times, 550 DEG C of annealing in air atmosphere by titanio functional nanocomposite
2.5h, obtains the photocatalyst for photocatalysis degradation organic contaminant.
The Detitanium-ore-type TiO obtained using said method2Quality be 3.8-4.0mg, add reactive brilliant orange X-2R solution
In, wherein the concentration of reactive brilliant orange X-2R is 20mg/L, and volume is 50mL, and 30min, reactive brilliant orange X-2R are stood in visible ray
Photocatalytic activity is 92.9%.
Embodiment 14
Acetate fiber or fabric are placed in chloroform and are cleaned by ultrasonic 50min, then deionized water carries out immersion 20min, with
The residual chloroform of acetate fiber or fabric is removed, the acetate fiber or fabric after process is dried up with nitrogen, standby;Vinegar after cleaning
Ester fiber or fabric adopt low temperature corona radiation treatment 8min, obtain acetate fiber or the fabric for activating, wherein, low temperature corona spoke
According to temperature be 45 DEG C, the voltage of low temperature corona irradiation is 8KV, and the distance of low temperature corona irradiation is 2.0cm, the vinegar ester after activation
Fiber or fabric are placed in the reaction cavity of atomic layer deposition apparatus, and purge 5min, chamber with the nitrogen that purity is 99.9999%
At 150 DEG C, then chamber pressure control be more than 97% TiCl in 65Pa with purity for temperature control4For titanium source, deionized water
For oxygen source, by TiCl during deposition4It is heated to 120 DEG C of formation TiCl4Steam, then to reaction cavity, the burst length is for pulse
0.5s, open-assembly time is 25s, then is purged with the nitrogen that purity is 99.9999%, and purge time is 30s, then by deionized water
To reaction cavity, the burst length is 0.2s for pulse, and open-assembly time is 18s, then is purged with the nitrogen that purity is 99.9999%,
Purge time is 30s, i.e., deposited one layer of titanio function nano thin film in acetate fiber or fabric face, repeats this deposition cycle
7000 times, by titanio functional nanocomposite in air atmosphere 600 DEG C annealing 4.0h, obtain organic for photocatalytic degradation
The photocatalyst of pollutant.
The Detitanium-ore-type TiO obtained using said method2Quality be 4.2-4.4mg, add sulfur blue CV solution in, its
Middle sulfur blue CV concentration is 20mg/L, and volume is 50mL, and 30min is stood in visible ray, and sulfur blue CV photocatalytic activities are
98.7%.
Embodiment 15
Vinylon fibre or fabric are placed in ethanol and are cleaned by ultrasonic 35min, then deionized water carries out immersion 20min, with
The residual ethanol of vinylon fibre or fabric face is removed, the vinylon fibre or fabric after process is dried up with nitrogen, standby;After cleaning
Vinylon fibre or fabric adopt low temperature corona radiation treatment 6min, obtain activate vinylon fibre or fabric, wherein, low temp. electric
The temperature of dizzy irradiation is 35 DEG C, and the voltage of low temperature corona irradiation is 14KV, and the distance of low temperature corona irradiation is 1.5cm, after activation
Vinylon fibre or fabric be placed in the reaction cavity of atomic layer deposition apparatus, and with nitrogen that purity is 99.9999% purging
7min, at 160 DEG C, chamber pressure is controlled in 70Pa for cavity temperature control, and then the titanium tetraisopropylate with purity more than 97% is
Titanium source, deionized water is oxygen source, and titanium tetraisopropylate is heated to into 110 DEG C of formation titanium tetraisopropylate steams, then pulse during deposition
To reaction cavity, the burst length is 0.2s, and open-assembly time is 15s, then with the nitrogen purging that purity is 99.9999%, is purged
Time is 20s, and then by deionized water pulse to reaction cavity, the burst length is 0.15s, and open-assembly time is 15s, then with pure
The nitrogen purging for 99.9999% is spent, purge time is 20s, i.e., deposited one layer of titanio work(in vinylon fibre or fabric face
Energy nano thin-film, repeats this deposition cycle 8000 times, 550 DEG C of annealing in air atmosphere by titanio functional nanocomposite
3.5h, obtains the photocatalyst for photocatalysis degradation organic contaminant.
The Detitanium-ore-type TiO obtained using said method2Quality be 4.6-4.7mg, add reactive brilliant orange X-2R solution
In, wherein the concentration of reactive brilliant orange X-2R is 20mg/L, and volume is 50mL, and 15min, reactive brilliant orange X-2R are stood in visible ray
Photocatalytic activity is 94.9%.
Embodiment 16
Acrylic fiber or fabric are placed in n-butyl alcohol and are cleaned by ultrasonic 50min, then deionized water carries out immersion 20min,
To remove the residual n-butyl alcohol of acrylic fiber or fabric, the acrylic fiber or fabric after process is dried up with nitrogen, standby;After cleaning
Acrylic fiber or fabric adopt low temperature corona radiation treatment 8min, obtain activate acrylic fiber or fabric, wherein, low temp. electric
The temperature of dizzy irradiation is 15 DEG C, and the voltage of low temperature corona irradiation is 8KV, and the distance of low temperature corona irradiation is 1.8cm, after activation
Acrylic fiber or fabric are placed in the reaction cavity of atomic layer deposition apparatus, and are purged with the nitrogen that purity is 99.9999%
5min, at 150 DEG C, then chamber pressure control be more than 97% TiCl in 55Pa with purity for cavity temperature control4For titanium source,
Deionized water is oxygen source, by TiCl during deposition4It is heated to 100 DEG C of formation TiCl4Steam, then pulse to reaction cavity, pulse
Time is 0.5s, and open-assembly time is 10s, then is purged with the nitrogen that purity is 99.9999%, and purge time is 20s, then will be gone
To reaction cavity, the burst length is 0.12s to ion aquapulse, and open-assembly time is 12s, then with the nitrogen that purity is 99.9999%
Air-blowing is swept, and purge time is 25s, i.e., deposited one layer of titanio function nano thin film in acrylic fiber or fabric face, repeats this
Deposition cycle 9000 times, by titanio functional nanocomposite in air atmosphere 600 DEG C annealing 4.0h, obtain for photocatalysis
The photocatalyst of degradable organic pollutant.
The Detitanium-ore-type TiO obtained using said method2Quality be 5.0-5.2mg, add vat red 2G solution in, its
Middle vat red 2G concentration is 20mg/L, and volume is 50mL, and 10min is stood in visible ray, and vat red 2G photocatalytic activities are
96.8%.
Embodiment 17
CUP or fabric are placed in ethanol and are cleaned by ultrasonic 35min, then deionized water carries out immersion 20min, with
The residual ethanol of CUP or fabric face is removed, the CUP or fabric after process is dried up with nitrogen, standby;After cleaning
CUP or fabric adopt low temperature corona radiation treatment 6min, obtain activate CUP or fabric, wherein, low temp. electric
The temperature of dizzy irradiation is 35 DEG C, and the voltage of low temperature corona irradiation is 15KV, and the distance of low temperature corona irradiation is 1.5cm, after activation
CUP or fabric be placed in the reaction cavity of atomic layer deposition apparatus, and with nitrogen that purity is 99.9999% purging
7min, at 180 DEG C, chamber pressure is controlled in 60Pa for cavity temperature control, and then the titanium tetraisopropylate with purity more than 97% is
Titanium source, deionized water is oxygen source, and titanium tetraisopropylate is heated to into 90 DEG C of formation titanium tetraisopropylate steams during deposition, and then pulse is extremely
In reaction cavity, the burst length is 0.2s, and open-assembly time is 15s, then is purged with the nitrogen that purity is 99.9999%, during purging
Between be 20s, then by deionized water pulse to reaction cavity, the burst length is 0.05s, and open-assembly time is 28s, then uses purity
Nitrogen for 99.9999% is purged, and purge time is 20s, i.e., deposited one layer of titanio function in CUP or fabric face
Nano thin-film, repeats this deposition cycle 10000 times, 550 DEG C of annealing in air atmosphere by titanio functional nanocomposite
3.5h, obtains the photocatalyst for photocatalysis degradation organic contaminant.
By the Detitanium-ore-type TiO obtained using said method2Quality be 5.6-5.8mg, add solvent yellow BL solution in,
Wherein the concentration of solvent yellow BL is 20mg/L, and volume is 50mL, and 5min, solvent yellow BL photocatalytic activities are stood in visible ray
For 98.9%.
Claims (3)
1. a kind of preparation method for degradable organic pollutant photocatalyst, it is characterised in that the preparation method is by following
Step is carried out:
A. matrix material is placed in into organic solvent for ultrasonic cleaning 30-60min, then deionized water carries out immersion 20min, to remove
The residual solvent of substrate material surface is removed, the matrix material after process is dried up with nitrogen, standby;
B. the matrix material Jing after the cleaning that step a is obtained is adopted into low temperature corona radiation treatment 5-10min, obtains the base for activating
Body material, wherein, the temperature of low temperature corona irradiation is 10-45 DEG C, and the voltage of low temperature corona irradiation is 6-15KV, low temperature corona spoke
According to distance be 0.5-3cm;
C. the activated matrix material Jing after the process of step b is placed in the reaction cavity of atomic layer deposition apparatus, and is with purity
99.9999% nitrogen purging 3-10min, at 120-200 DEG C, chamber pressure is controlled in 50Pa-80Pa, so for cavity temperature control
It is more than 97% TiCl with purity afterwards4Or titanium tetraisopropylate is titanium source, deionized water is oxygen source, by TiCl during deposition4Or four isopropyls
Alcohol titanium is heated to 60-120 DEG C of formation TiCl4Or titanium tetraisopropylate steam, then to reaction cavity, the burst length is for pulse
0.05-0.5s, open-assembly time is 8-25s, then is purged with the nitrogen that purity is 99.9999%, and purge time is 15-30s, then
By in deionized water pulse to reaction cavity, the burst length is 0.01-0.2s, and open-assembly time is 8-25s, then is with purity
99.9999% nitrogen purging, purge time is 15-30s, completes primary depositing circulation, i.e., deposited in substrate material surface
One layer of titanio function nano thin film;
D. the deposition cycle of repeat step c 100-10000 time, obtains titanio functional nanocomposite;
E. the titanio functional nanocomposite for Jing steps d being obtained 500-600 DEG C of annealing 0.5-4h in air atmosphere, obtains
For the photocatalyst of degradable organic pollutant.
2. prepared by a kind of photocatalyst for photocatalysis degradation organic contaminant and photocatalytic water according to claims 1
Method, it is characterised in that:Described organic solvent is methanol or ethanol or propanol or isopropanol or n-butyl alcohol or ether or acetone
Or butanone or the one kind in chloroform.
3. a kind of preparation method for degradable organic pollutant photocatalyst according to claims 1, its feature exists
In:Described matrix material is porous material of the decomposition temperature less than 280 DEG C or semi-conducting material or natural macromolecular material
Or synthesising macromolecule copolymer class material.
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