CN108970641A - A kind of pulping wastewater treatment catalyst and preparation method thereof based on aluminium base quantum dot - Google Patents
A kind of pulping wastewater treatment catalyst and preparation method thereof based on aluminium base quantum dot Download PDFInfo
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- CN108970641A CN108970641A CN201810963689.6A CN201810963689A CN108970641A CN 108970641 A CN108970641 A CN 108970641A CN 201810963689 A CN201810963689 A CN 201810963689A CN 108970641 A CN108970641 A CN 108970641A
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- quantum dot
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- 239000004411 aluminium Substances 0.000 title claims abstract description 107
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 107
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000002096 quantum dot Substances 0.000 title claims abstract description 104
- 239000003054 catalyst Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 48
- 238000004065 wastewater treatment Methods 0.000 title claims abstract description 47
- 238000004537 pulping Methods 0.000 title claims abstract description 46
- 239000011248 coating agent Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000576 coating method Methods 0.000 claims abstract description 25
- 230000004048 modification Effects 0.000 claims abstract description 25
- 238000012986 modification Methods 0.000 claims abstract description 25
- 239000002131 composite material Substances 0.000 claims abstract description 9
- 238000005342 ion exchange Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 43
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 35
- 150000001875 compounds Chemical class 0.000 claims description 32
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 27
- 229960004756 ethanol Drugs 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 12
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 12
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 11
- 239000005977 Ethylene Substances 0.000 claims description 11
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- LMBWSYZSUOEYSN-UHFFFAOYSA-N diethyldithiocarbamic acid Chemical compound CCN(CC)C(S)=S LMBWSYZSUOEYSN-UHFFFAOYSA-N 0.000 claims description 9
- 229950004394 ditiocarb Drugs 0.000 claims description 9
- 239000001509 sodium citrate Substances 0.000 claims description 9
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000003999 initiator Substances 0.000 claims description 8
- 229910052746 lanthanum Inorganic materials 0.000 claims description 8
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 8
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 8
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 6
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 5
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910017569 La2(CO3)3 Inorganic materials 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 claims description 3
- 229960001633 lanthanum carbonate Drugs 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- -1 feature Be Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 229960001790 sodium citrate Drugs 0.000 claims description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims 1
- 229910052731 fluorine Inorganic materials 0.000 claims 1
- 239000011737 fluorine Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 239000002585 base Substances 0.000 description 85
- 230000001699 photocatalysis Effects 0.000 description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 9
- 238000007146 photocatalysis Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 7
- 238000012545 processing Methods 0.000 description 7
- 229920002620 polyvinyl fluoride Polymers 0.000 description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 5
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 5
- 229910000077 silane Inorganic materials 0.000 description 5
- 239000010893 paper waste Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 2
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- 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
-
- 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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/26—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof
- C02F2103/28—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof from the paper or cellulose industry
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The present invention provides a kind of preparation method of pulping wastewater treatment catalyst based on aluminium base quantum dot, includes the following steps: the preparation of I mesoporous La-Ti-O-S, II mesoporous La-Ti-O-S/ aluminium base quantum dot composite surface modification, III surface-coating, IV ion exchange.The invention also discloses the pulping wastewater treatment catalyst based on aluminium base quantum dot being prepared according to the preparation method of the pulping wastewater treatment catalyst based on aluminium base quantum dot.It is of the present invention that preparation method is simple, it is not high to device dependence, preparation condition is required not harsh, raw material is easy to get, it is cheap, it is suitble to large-scale production, the pulping wastewater treatment catalyst based on aluminium base quantum dot being prepared is with performance is more stable, price is cheaper, catalytic effect is more preferable, catalytic efficiency is higher, visible light-responded range is wider, water treatment effect more preferably, the more diversified advantage of function.
Description
Technical field
The present invention relates at pulping wastewater treatment technical field more particularly to a kind of paper waste based on aluminium base quantum dot
Manage catalyst and preparation method thereof.
Background technique
In recent years, with the propulsion of global industry process, paper-making industry is rapidly developed, and is contributed to economic growth huge
Strength also brings to environment and seriously threatens at the same time.Paper waste discharge amount is big, and the organism kinds contained are more, processing
Difficulty injures huge to the health bring of ecological environment and people.With countries in the world discharge of wastewater is required it is tight
It formats and people gos deep into in environmental problem and own bodies health understanding, carrying out processing to paper waste is that numerous papermaking are looked forward to
Industry is had to a difficult problem faced, is to hinder one of paper-making industry or even the principal element of economic development.
Currently, specifically include that biologic treating technique to the processing technique of paper waste, chemical treatment method and adsorbed
The physical processing techniques such as filter.The new technology of photocatalytic oxidation processing Organic Pollutants In Water has been developed in recent years.Light is urged
Organic pollutant can be effectively removed by changing degradation, and avoid the secondary pollution to water body.In order to improve photocatalytic degradation efficiency, open up
Wide spectrum absorption band, transition metal and precious metal doping conductor oxidate are used for visible light photocatalysis research, but its cost
It is higher.And visible light is not responding to by the photochemical catalyst of representative of titanium dioxide, so that photocatalysis efficiency is low.The prior art
In disclose various method of modifying and carry out modifying titanium dioxide, these methods can expand visible light-responded range to a certain extent,
To improve photocatalysis sewage treatment effect, but its more or less there is also structural instability, can outflow with water and use
The deficiencies of service life is short.
Application publication number is that the Chinese invention patent of CN105344377A discloses a kind of sewage treatment nanometer titanium dioxide
The preparation method of titanium modified light catalyst belongs to the technical field of photochemical catalyst, the preparation including γ-Fe2O3 powder, then will
γ-the Fe of preparation2O3Powder, nano-TiO2Powder carries out coating processing with coating agent, obtains modified light catalyst, by γ-Fe2O3
Powder, nano-TiO2Powder is (6-8) in mass ratio: the ratio of (4-6) is sent into airslide disintegrating mill and is crushed, when charging with plus packet
Film has following methods to be prepared powder coating, the coating agent: polyacrylamide is molten under the stirring of 120rpm
Solution is configured to the solution that concentration is 1% in 50~60 DEG C of deionized water, adds that be kept stirring 5-7 after polyacrylamide small
When to get coating agent.Method of the invention is simple, easy to operate, by nano-TiO2It handled, be modified, so that modified light
The separation and recovery rate of catalyst can achieve 99.5% or more, however this modified light catalyst is due between coating agent and powder
Compatibility is bad, and film is easy to fall off, and can not also solve the problems, such as that visible light is not responding to, using with biggish limitation.
Therefore, develop that a kind of performance is more stable, price is cheaper, catalytic effect is more preferable, catalytic efficiency is higher, visible
Optical response range is wider, and more preferably, the more diversified pulping wastewater treatment catalyst of function meets market to be needed water treatment effect
It asks, there is extensive market value and application prospect.
Summary of the invention
The main purpose of the present invention is to provide a kind of pulping wastewater treatment catalyst and its system based on aluminium base quantum dot
Preparation Method, preparation method is simple for this, not high to device dependence, not harsh to preparation condition requirement, and raw material is easy to get, price
It is cheap, it is suitble to large-scale production.The pulping wastewater treatment catalyst based on aluminium base quantum dot being prepared overcomes existing skill
In art wastewater treatment catalyst more or less existing expensive, structural instability, easily outflow with water, service life it is short not
Foot, catalytic effect is poor, catalytic efficiency is low technical problem, with performance is more stable, price is cheaper, catalytic effect more
It is good, catalytic efficiency is higher, visible light-responded range is wider, water treatment effect more preferably, the more diversified advantage of function.
To achieve the above objectives, the present invention provides a kind of preparation of pulping wastewater treatment catalyst based on aluminium base quantum dot
Method includes the following steps:
The preparation of I mesoporous La-Ti-O-S: titanium source, lanthanum source, sodium diethyldithiocarbamate are added to equipped with ethyl alcohol
Beaker in, stirring 1.5-2.5 hours after, be slowly added to sodium citrate, after being vigorously agitated again 2-3 hours, transfer the solution into
In the hydrothermal reaction kettle of polyvinyl fluoride liner, 200-220 DEG C reaction 15-20 hours.Reaction kettle is taken out, it is cooling to reaction system
It is successively washed 4-6 times with deionized water and dehydrated alcohol respectively afterwards, finally the dry 15-20 in 85-95 DEG C of vacuum oven
Hour, obtain mesoporous La-Ti-O-S；
II mesoporous La-Ti-O-S/ aluminium base quantum dot composite surface modification: the mesoporous La- that will be prepared by step I
Ti-O-S, aluminium base quantum dot are uniformly mixed, and are redispersed in ethyl alcohol, and 9- [3- (triethoxysilicane alkyl) is then added thereto
Propyl] -9H- carbazole, it is stirred to react at 30-40 DEG C 3-5 hours, then quaternary ammonium salt -15 and basic catalyst are added thereto, after
It is continuous to be stirred to react 6-8 hours, it is rear to filter, and successively washed 3-5 times with water and methylene chloride respectively, then rotate removing dichloromethane
Alkane obtains the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface modification；
III surface-coating: the mesoporous La-Ti-O-S/ aluminium base quantum dot of surface modification being prepared by step II is compound
Object is scattered in high boiling solvent, then acrylamide, initiator are added thereto, in nitrogen or 65-75 DEG C of atmosphere of inert gases
Under be stirred to react 3-5 hours, after settle out in acetone, be placed at 70-80 DEG C of vacuum oven 10-15 hours dry, obtain
The mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface-coating；
IV ion exchange: the mesoporous La-Ti-O-S/ aluminium base quantum dot of surface-coating being prepared by step III is compound
Object, four [4- (4'- carboxyl phenyl) phenyl] ethylene are added in toluene, are stirred to react at 50-60 DEG C 3-5 hours, rear to rotate
Solvent is removed, then is washed 3-5 times with tetrahydrofuran, drying 15-20 hours at 75-85 DEG C of vacuum oven is placed in, obtains base
In the pulping wastewater treatment catalyst of aluminium base quantum dot.
Preferably, titanium source described in step I, lanthanum source, sodium diethyldithiocarbamate, ethyl alcohol, sodium citrate matter
Amount is than being 2:1:0.2:(10-15): 9.
Preferably, the titanium source is selected from one of titanium tetrachloride, butyl titanate；The lanthanum source is selected from lanthanum chloride, carbon
One of sour lanthanum.
Preferably, mesoporous La-Ti-O-S described in step II, aluminium base quantum dot, ethyl alcohol, 9- [3- (triethoxysilane
Base) propyl] -9H- carbazole, quaternary ammonium salt -15, basic catalyst mass ratio be 2:1:(10-15): 0.8:0.5:(0.2-0.4).
Preferably, the aluminium base quantum dot is that aluminium adulterates cadmium selenide/cadmium sulfide nuclear shell structure quantum point, to be previously prepared,
Preparation method referenced patent application number is the Chinese invention patent of CN105670631A.
Preferably, the basic catalyst is selected from one of sodium carbonate, potassium carbonate, sodium hydroxide, potassium hydroxide or several
Kind.
Further, the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface modification described in step III, higher boiling are molten
Agent, acrylamide, initiator mass ratio be 3:(10-15): 1:(0.02-0.04).
Preferably, the high boiling solvent is in dimethyl sulfoxide, n,N-Dimethylformamide, N-Methyl pyrrolidone
It is one or more of.
Preferably, the initiator is selected from least one of azodiisobutyronitrile, azobisisoheptonitrile；The indifferent gas
Body is selected from one or more of helium, neon, argon gas.
Preferably, the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface-coating described in step IV, four [4- (4'- carboxylics
Base phenyl) phenyl] ethylene, toluene mass ratio be (3-5): 1:(10-15).
A kind of pulping wastewater treatment catalyst based on aluminium base quantum dot, it is useless using the above-mentioned papermaking based on aluminium base quantum dot
The preparation method for the treatment of catalyst is prepared.
Due to the application of the above technical scheme, the invention has the following advantages:
(1) the pulping wastewater treatment catalyst disclosed by the invention based on aluminium base quantum dot, preparation method is simple, right
Device dependence is not high, not harsh to preparation condition requirement, and raw material is easy to get, cheap, is suitble to large-scale production.
(2) the pulping wastewater treatment catalyst disclosed by the invention based on aluminium base quantum dot, overcomes and gives up in the prior art
The more or less existing expensive, structural instability for the treatment of catalyst easily outflows with water, the short insufficient, catalysis of service life
The technical problem that effect is poor, catalytic efficiency is low, with performance is more stable, price is cheaper, catalytic effect is more preferable, catalysis effect
Rate is higher, visible light-responded range is wider, water treatment effect more preferably, the more diversified advantage of function.
(3) the pulping wastewater treatment catalyst disclosed by the invention based on aluminium base quantum dot, by adding mesoporous La-Ti-
O-S enhances photocatalysis effect, improves photocatalysis efficiency, has broader visible light-responded range, assists with aluminium base quantum dot
Photocatalysis efficiency not only can be improved in same-action, also have preferable adsorption function, can have to the heavy metal ion in waste water compared with
Good suction-operated.It is modified by surface, improve the stability and water resistance of catalyst, extend service life, have compared with
Good economic value.
(4) the pulping wastewater treatment catalyst disclosed by the invention based on aluminium base quantum dot, in mesoporous La-Ti-O-S/ aluminium
It is polymer that based quantum dot composite surface, which modifies acrylamide and the copolymerization formation of quaternary ammonium salt 15, due to amide groups, quaternary ammonium salt, aluminium
Presence, synergistic effect form better flocculating effect, pass through ion exchange introduce four [4- (4'- carboxyl phenyl) phenyl] ethylene
Structure introduces conjugated structure, further increases visible light-responded range, on the other hand improving photocatalysis efficiency may be incorporated into
More carboxyl and benzene ring structure, carboxyl can improve the absorption complexing power of catalyst towards heavy metal ion, and phenyl ring can improve catalysis
The salt resistance stain resistance of agent, extends the service life of catalyst, and quaternary ammonium salt can play the role of improving antibiotic property again.
Specific embodiment
It is described below for disclosing the present invention so that those skilled in the art can be realized the present invention.It is excellent in being described below
Embodiment is selected to be only used as illustrating, it may occur to persons skilled in the art that other obvious modifications.
The aluminium base quantum dot used in the embodiment of the present invention is that aluminium adulterates cadmium selenide/cadmium sulfide core-shell structure quantum
Point, to be previously prepared, preparation method referenced patent application number is the Chinese invention patent of CN105670631A；Other raw materials are purchased from
Mo Bei (Shanghai) Biotechnology Co., Ltd.
Embodiment 1
A kind of preparation method of the pulping wastewater treatment catalyst based on aluminium base quantum dot, includes the following steps:
The preparation of I mesoporous La-Ti-O-S: by titanium tetrachloride 20g, lanthanum chloride 10g, sodium diethyldithiocarbamate 2g
It is added in the beaker equipped with ethyl alcohol 100g, after stirring 1.5 hours, is slowly added to sodium citrate 90g, is vigorously agitated again 2 hours
Afterwards, it transfers the solution into the hydrothermal reaction kettle of polyvinyl fluoride liner, is reacted 15 hours at 200 DEG C.Reaction kettle is taken out, wait react
It is successively washed 4 times with deionized water and dehydrated alcohol respectively after system is cooling, finally dry 15 in 85 DEG C of vacuum oven
Hour, obtain mesoporous La-Ti-O-S；
II mesoporous La-Ti-O-S/ aluminium base quantum dot composite surface modification: the mesoporous La- that will be prepared by step I
Ti-O-S20g, aluminium base quantum dot 10g are uniformly mixed, and are redispersed in ethyl alcohol 100g, and 9- [3- (three ethoxies are then added thereto
Base silane base) propyl] -9H- carbazole 8g, it is stirred to react at 30 DEG C 3 hours, then quaternary ammonium salt -155g and carbonic acid are added thereto
Sodium 2g continues to be stirred to react 6 hours, rear to filter, and is successively washed 3 times with water and methylene chloride respectively, then rotate removing dichloro
Methane obtains the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface modification；
III surface-coating: the mesoporous La-Ti-O-S/ aluminium base quantum dot of surface modification being prepared by step II is compound
Object 30g is scattered in dimethyl sulfoxide 100g, then acrylamide 10g, azodiisobutyronitrile 0.2g are added thereto, in nitrogen atmosphere
Be stirred to react at 65 DEG C 3 hours, after settle out in acetone, be placed at 70 DEG C of vacuum oven 10 hours dry, obtain surface
The mesoporous La-Ti-O-S/ aluminium base quantum dot compound of coating；
IV ion exchange: the mesoporous La-Ti-O-S/ aluminium base quantum dot of surface-coating being prepared by step III is compound
Object 30g, four [4- (4'- carboxyl phenyl) phenyl] ethylene 10g are added in toluene 100g, are stirred to react at 50 DEG C 3 hours, after
Revolving removes solvent, then is washed 3 times with tetrahydrofuran, is placed in drying 15 hours at 75 DEG C of vacuum oven, obtains based on aluminium
The pulping wastewater treatment catalyst of based quantum dot.
A kind of pulping wastewater treatment catalyst based on aluminium base quantum dot, it is useless using the above-mentioned papermaking based on aluminium base quantum dot
The preparation method for the treatment of catalyst is prepared.
Embodiment 2
A kind of preparation method of the pulping wastewater treatment catalyst based on aluminium base quantum dot, includes the following steps:
The preparation of I mesoporous La-Ti-O-S: by butyl titanate 20g, lanthanum carbonate 10g, sodium diethyldithiocarbamate
2g is added in the beaker equipped with ethyl alcohol 110g, after stirring 1.7 hours, is slowly added to sodium citrate 90g, is vigorously agitated again 2.3
It after hour, transfers the solution into the hydrothermal reaction kettle of polyvinyl fluoride liner, is reacted 16 hours at 205 DEG C.Reaction kettle is taken out, to
It is successively washed 5 times with deionized water and dehydrated alcohol after reaction system is cooling, is finally done in 87 DEG C of vacuum oven respectively
Dry 17 hours, obtain mesoporous La-Ti-O-S；
II mesoporous La-Ti-O-S/ aluminium base quantum dot composite surface modification: the mesoporous La- that will be prepared by step I
Ti-O-S20g, aluminium base quantum dot 10g are uniformly mixed, and are redispersed in ethyl alcohol 110g, and 9- [3- (three ethoxies are then added thereto
Base silane base) propyl] -9H- carbazole 8g, it is stirred to react at 33 DEG C 3.5 hours, then quaternary ammonium salt -155g and carbon are added thereto
Sour potassium 2.5g continues to be stirred to react 6.5 hours, rear to filter, and is successively washed 4 times with water and methylene chloride respectively, then rotate and remove
Methylene chloride is removed, the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface modification is obtained；
III surface-coating: the mesoporous La-Ti-O-S/ aluminium base quantum dot of surface modification being prepared by step II is compound
Object 30g is scattered in n,N-Dimethylformamide 115g, then acrylamide 10g, azobisisoheptonitrile 0.25g are added thereto,
Be stirred to react at 67 DEG C of helium atmosphere 3.5 hours, after settle out in acetone, it is small to be placed at 73 DEG C of vacuum oven dry 12
When, obtain the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface-coating；
IV ion exchange: the mesoporous La-Ti-O-S/ aluminium base quantum dot of surface-coating being prepared by step III is compound
Object 14g, four [4- (4'- carboxyl phenyl) phenyl] ethylene 4g are added in toluene 45g, are stirred to react at 53 DEG C 3.5 hours, after
Revolving removes solvent, then is washed 4 times with tetrahydrofuran, is placed in drying 16 hours at 78 DEG C of vacuum oven, obtains based on aluminium
The pulping wastewater treatment catalyst of based quantum dot.
A kind of pulping wastewater treatment catalyst based on aluminium base quantum dot, it is useless using the above-mentioned papermaking based on aluminium base quantum dot
The preparation method for the treatment of catalyst is prepared.
Embodiment 3
A kind of preparation method of the pulping wastewater treatment catalyst based on aluminium base quantum dot, includes the following steps:
The preparation of I mesoporous La-Ti-O-S: by titanium tetrachloride 20g, lanthanum carbonate 10g, sodium diethyldithiocarbamate 2g
It is added in the beaker equipped with ethyl alcohol 125g, after stirring 1.9 hours, is slowly added to sodium citrate 90g, it is small to be vigorously agitated again 2.5
Shi Hou is transferred the solution into the hydrothermal reaction kettle of polyvinyl fluoride liner, is reacted 18 hours at 210 DEG C.Reaction kettle is taken out, to anti-
It is successively washed 6 times with deionized water and dehydrated alcohol respectively after answering system cooling, it is finally dry in 89 DEG C of vacuum oven
17.5 hours, obtain mesoporous La-Ti-O-S；
II mesoporous La-Ti-O-S/ aluminium base quantum dot composite surface modification: the mesoporous La- that will be prepared by step I
Ti-O-S20g, aluminium base quantum dot 10g are uniformly mixed, and are redispersed in ethyl alcohol 125g, and 9- [3- (three ethoxies are then added thereto
Base silane base) propyl] -9H- carbazole 8g, it is stirred to react at 35 DEG C 4 hours, then quaternary ammonium salt -155g and hydrogen-oxygen are added thereto
Change sodium 3g, continues to be stirred to react 7 hours, it is rear to filter, and successively washed 5 times with water and methylene chloride respectively, then rotate removing two
Chloromethanes obtains the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface modification；
III surface-coating: the mesoporous La-Ti-O-S/ aluminium base quantum dot of surface modification being prepared by step II is compound
Object 30g is scattered in N-Methyl pyrrolidone 130g, then acrylamide 10g, azodiisobutyronitrile 0.3g are added thereto, in neon
Atmosphere is enclosed to be stirred to react 4.1 hours at 70 DEG C, after settle out in acetone, be placed at 75 DEG C of vacuum oven it is 13 hours dry,
Obtain the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface-coating；
IV ion exchange: the mesoporous La-Ti-O-S/ aluminium base quantum dot of surface-coating being prepared by step III is compound
Object 16g, four [4- (4'- carboxyl phenyl) phenyl] ethylene 4g are added in toluene 52g, are stirred to react at 57 DEG C 4.2 hours, after
Revolving removes solvent, then is washed 5 times with tetrahydrofuran, is placed in drying 18 hours at 81 DEG C of vacuum oven, obtains based on aluminium
The pulping wastewater treatment catalyst of based quantum dot.
A kind of pulping wastewater treatment catalyst based on aluminium base quantum dot, it is useless using the above-mentioned papermaking based on aluminium base quantum dot
The preparation method for the treatment of catalyst is prepared.
Embodiment 4
A kind of preparation method of the pulping wastewater treatment catalyst based on aluminium base quantum dot, includes the following steps:
The preparation of I mesoporous La-Ti-O-S: by butyl titanate 20g, lanthanum chloride 10g, sodium diethyldithiocarbamate
2g is added in the beaker equipped with ethyl alcohol 145g, after stirring 2.3 hours, is slowly added to sodium citrate, is vigorously agitated again 2.8 hours
Afterwards, it transfers the solution into the hydrothermal reaction kettle of polyvinyl fluoride liner, is reacted 19 hours at 215 DEG C.Reaction kettle is taken out, wait react
It is successively washed 5 times with deionized water and dehydrated alcohol respectively after system is cooling, finally dry 19 in 93 DEG C of vacuum oven
Hour, obtain mesoporous La-Ti-O-S；
II mesoporous La-Ti-O-S/ aluminium base quantum dot composite surface modification: the mesoporous La- that will be prepared by step I
Ti-O-S20g, aluminium base quantum dot 10g are uniformly mixed, and are redispersed in ethyl alcohol 145g, and 9- [3- (three ethoxies are then added thereto
Base silane base) propyl] -9H- carbazole 8g, it is stirred to react at 38 DEG C 4.5 hours, then quaternary ammonium salt -155g and alkali are added thereto
Property catalyst 3.5g, continue to be stirred to react 7.5 hours, it is rear to filter, and successively washed 5 times with water and methylene chloride respectively, then revolve
Methylene chloride is evaporated off, obtains the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface modification；The basic catalyst is carbon
The mixture that sour sodium, potassium carbonate, sodium hydroxide, potassium hydroxide 1:2:1:5 in mass ratio are mixed；
III surface-coating: the mesoporous La-Ti-O-S/ aluminium base quantum dot of surface modification being prepared by step II is compound
Object 30g is scattered in high boiling solvent 145g, then acrylamide 10g, initiator 0.35g are added thereto, in argon atmosphere 73
Be stirred to react at DEG C 4.5 hours, after settle out in acetone, be placed at 78 DEG C of vacuum oven 14.5 hours dry, obtain table
The mesoporous La-Ti-O-S/ aluminium base quantum dot compound of bread film；The high boiling solvent is dimethyl sulfoxide, N, N- dimethyl formyl
The mixture that amine, N-Methyl pyrrolidone 1:3:2 in mass ratio are mixed；The initiator is azodiisobutyronitrile, azo
The mixture that two different heptonitrile 3:5 in mass ratio are mixed；
IV ion exchange: the mesoporous La-Ti-O-S/ aluminium base quantum dot of surface-coating being prepared by step III is compound
Object 18g, four [4- (4'- carboxyl phenyl) phenyl] ethylene 4g are added in toluene 58g, are stirred to react at 58 DEG C 4.5 hours, after
Revolving removes solvent, then is washed 5 times with tetrahydrofuran, is placed in drying 19 hours at 84 DEG C of vacuum oven, obtains based on aluminium
The pulping wastewater treatment catalyst of based quantum dot.
A kind of pulping wastewater treatment catalyst based on aluminium base quantum dot, it is useless using the above-mentioned papermaking based on aluminium base quantum dot
The preparation method for the treatment of catalyst is prepared.
Embodiment 5
A kind of preparation method of the pulping wastewater treatment catalyst based on aluminium base quantum dot, includes the following steps:
The preparation of I mesoporous La-Ti-O-S: titanium tetrachloride 20g, lanthanum source 10g, sodium diethyldithiocarbamate 2g are added
Enter into the beaker equipped with ethyl alcohol 150g, after stirring 2.5 hours, is slowly added to sodium citrate 90g, after being vigorously agitated again 3 hours,
It transfers the solution into the hydrothermal reaction kettle of polyvinyl fluoride liner, is reacted 20 hours at 220 DEG C.Reaction kettle is taken out, to reactant
It is successively washed 6 times with deionized water and dehydrated alcohol respectively after system is cooling, finally drying 20 is small in 95 DEG C of vacuum oven
When, obtain mesoporous La-Ti-O-S；
II mesoporous La-Ti-O-S/ aluminium base quantum dot composite surface modification: the mesoporous La- that will be prepared by step I
Ti-O-S20g, aluminium base quantum dot 10g are uniformly mixed, and are redispersed in ethyl alcohol 150g, and 9- [3- (three ethoxies are then added thereto
Base silane base) propyl] -9H- carbazole 8g, it is stirred to react at 40 DEG C 5 hours, then quaternary ammonium salt -155g and hydrogen-oxygen are added thereto
Change potassium 4g, continues to be stirred to react 8 hours, it is rear to filter, and successively washed 5 times with water and methylene chloride respectively, then rotate removing two
Chloromethanes obtains the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface modification；
III surface-coating: the mesoporous La-Ti-O-S/ aluminium base quantum dot of surface modification being prepared by step II is compound
Object 30g is scattered in n,N-Dimethylformamide 150g, then acrylamide 10g, azobisisoheptonitrile 0.4g are added thereto,
Be stirred to react at 75 DEG C of nitrogen atmosphere 5 hours, after settle out in acetone, be placed at 80 DEG C of vacuum oven it is 15 hours dry,
Obtain the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface-coating；
IV ion exchange: the mesoporous La-Ti-O-S/ aluminium base quantum dot of surface-coating being prepared by step III is compound
Object 20g, four [4- (4'- carboxyl phenyl) phenyl] ethylene 4g are added in toluene 60g, 5 hours are stirred to react at 60 DEG C, back spin
Solvent is evaporated off, then is washed 5 times with tetrahydrofuran, is placed in drying 20 hours at 85 DEG C of vacuum oven, obtains based on aluminium base
The pulping wastewater treatment catalyst of quantum dot.
A kind of pulping wastewater treatment catalyst based on aluminium base quantum dot, it is useless using the above-mentioned papermaking based on aluminium base quantum dot
The preparation method for the treatment of catalyst is prepared.
Comparative example
This example provides a kind of Photodegradation catalyst for organic sewage processing, formula and the same Chinese invention of preparation method
105536846 A embodiment 1 of patent CN.
By the above embodiments 1-5 pulping wastewater treatment catalyst based on aluminium base quantum dot prepared and comparative example photocatalysis
Agent is tested for the property, and test method refers to 107185515 A performance test methods of Chinese invention patent CN, and test result is shown in
Table 1.
Table 1
| Performance detection project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example |
| Rate of photocatalytic oxidation (g/30min) | 95.23 | 95.45 | 95.61 | 95.85 | 96.04 | 90.10 |
| Stability (%) | 99.96 | 99.98 | 99.99 | 100 | 100 | 98.98 |
| Service life (year) | ≥3 | ≥3 | ≥3 | ≥3 | ≥3 | ≥3 |
| Light transmittance (%) | 95.8 | 96.3 | 96.6 | 96.8 | 97.2 | 90 |
| Rate of weight loss (%) | 0.85 | 0.81 | 0.78 | 0.75 | 0.73 | 1 |
As seen from Table 1, the pulping wastewater treatment catalyst disclosed by the embodiments of the present invention based on aluminium base quantum dot, and it is existing
Photochemical catalyst is compared in technology, has more excellent rate of photocatalytic oxidation, stability, light transmittance and water resistance.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection scope by appended claims and its
Equivalent defines.
Claims (10)
1. a kind of preparation method of the pulping wastewater treatment catalyst based on aluminium base quantum dot, which is characterized in that including walking as follows
It is rapid:
The preparation of I mesoporous La-Ti-O-S: titanium source, lanthanum source, sodium diethyldithiocarbamate are added to the burning equipped with ethyl alcohol
In cup, after stirring 1.5-2.5 hours, it is slowly added to sodium citrate, after being vigorously agitated again 2-3 hours, transfers the solution into poly- fluorine
In the hydrothermal reaction kettle of ethylene liner, 200-220 DEG C reaction 15-20 hours.Reaction kettle is taken out, is divided after reaction system is cooling
It is not washed 4-6 times with deionized water and dehydrated alcohol successively, it is finally 15-20 hours dry in 85-95 DEG C of vacuum oven,
Obtain mesoporous La-Ti-O-S；
II mesoporous La-Ti-O-S/ aluminium base quantum dot composite surface modification: the mesoporous La-Ti- that will be prepared by step I
O-S, aluminium base quantum dot are uniformly mixed, and are redispersed in ethyl alcohol, and 9- [3- (triethoxysilicane alkyl) third is then added thereto
Base] -9H- carbazole, it is stirred to react 3-5 hours, then quaternary ammonium salt -15 and basic catalyst are added thereto, continues at 30-40 DEG C
It is stirred to react 6-8 hours, it is rear to filter, and successively washed 3-5 times with water and methylene chloride respectively, then rotate removing methylene chloride,
Obtain the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface modification；
III surface-coating: the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface modification point that will be prepared by step II
It dissipates in high boiling solvent, then acrylamide, initiator is added thereto, stirred at nitrogen or 65-75 DEG C of atmosphere of inert gases
Mix reaction 3-5 hour, after settle out in acetone, be placed at 70-80 DEG C of vacuum oven dry 10-15 hours, obtain surface
The mesoporous La-Ti-O-S/ aluminium base quantum dot compound of coating；
IV ion exchange: by the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface-coating being prepared by step III,
Four [4- (4'- carboxyl phenyl) phenyl] ethylene are added in toluene, are stirred to react at 50-60 DEG C 3-5 hours, back spin is evaporated off
Solvent, then washed 3-5 times with tetrahydrofuran, drying 15-20 hours at 75-85 DEG C of vacuum oven are placed in, are obtained based on aluminium
The pulping wastewater treatment catalyst of based quantum dot.
2. the preparation method of the pulping wastewater treatment catalyst according to claim 1 based on aluminium base quantum dot, feature
Be, titanium source described in step I, lanthanum source, sodium diethyldithiocarbamate, ethyl alcohol, sodium citrate mass ratio be 2:1:
0.2:(10-15):9。
3. the preparation method of the pulping wastewater treatment catalyst according to claim 1 based on aluminium base quantum dot, feature
It is, the titanium source is selected from one of titanium tetrachloride, butyl titanate；The lanthanum source in lanthanum chloride, lanthanum carbonate one
Kind.
4. the preparation method of the pulping wastewater treatment catalyst according to claim 1 based on aluminium base quantum dot, feature
It is, mesoporous La-Ti-O-S described in step II, aluminium base quantum dot, ethyl alcohol, 9- [3- (triethoxysilicane alkyl) propyl] -9H-
Carbazole, quaternary ammonium salt -15, basic catalyst mass ratio be 2:1:(10-15): 0.8:0.5:(0.2-0.4).
5. the preparation method of the pulping wastewater treatment catalyst according to claim 1 based on aluminium base quantum dot, feature
It is, the basic catalyst is selected from one or more of sodium carbonate, potassium carbonate, sodium hydroxide, potassium hydroxide.
6. the preparation method of the pulping wastewater treatment catalyst according to claim 1 based on aluminium base quantum dot, feature
Be, the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface modification described in step III, high boiling solvent, acrylamide,
The mass ratio of initiator is 3:(10-15): 1:(0.02-0.04).
7. the preparation method of the pulping wastewater treatment catalyst according to claim 1 based on aluminium base quantum dot, feature
It is, the high boiling solvent is selected from one of dimethyl sulfoxide, n,N-Dimethylformamide, N-Methyl pyrrolidone or several
Kind.
8. the preparation method of the pulping wastewater treatment catalyst according to claim 1 based on aluminium base quantum dot, feature
It is, the initiator is selected from least one of azodiisobutyronitrile, azobisisoheptonitrile；The inert gas is selected from helium
One or more of gas, neon, argon gas.
9. the preparation method of the pulping wastewater treatment catalyst according to claim 1 based on aluminium base quantum dot, feature
It is, the mesoporous La-Ti-O-S/ aluminium base quantum dot compound of surface-coating described in step IV, four [4- (4'- carboxyl phenyl) benzene
Base] ethylene, toluene mass ratio be (3-5): 1:(10-15).
10. a kind of preparation using the pulping wastewater treatment catalyst described in claim any one of 1-9 based on aluminium base quantum dot
The pulping wastewater treatment catalyst based on aluminium base quantum dot that method is prepared.
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| CN111393085A (en) * | 2020-03-26 | 2020-07-10 | 闫明亮 | Environment-friendly diatom ooze and preparation method thereof |
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Application publication date: 20181211 |