CN108940339A - A kind of N-TiO2/ calcium system bentonite composite adsorption catalyst and application - Google Patents
A kind of N-TiO2/ calcium system bentonite composite adsorption catalyst and application Download PDFInfo
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- CN108940339A CN108940339A CN201810763908.6A CN201810763908A CN108940339A CN 108940339 A CN108940339 A CN 108940339A CN 201810763908 A CN201810763908 A CN 201810763908A CN 108940339 A CN108940339 A CN 108940339A
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- 239000000440 bentonite Substances 0.000 title claims abstract description 96
- 229910000278 bentonite Inorganic materials 0.000 title claims abstract description 96
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 title claims abstract description 96
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000011575 calcium Substances 0.000 title claims abstract description 78
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 78
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 43
- 239000003054 catalyst Substances 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000002351 wastewater Substances 0.000 claims abstract description 58
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000725 suspension Substances 0.000 claims abstract description 25
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 23
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 7
- 238000012805 post-processing Methods 0.000 claims abstract description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 44
- 229910052698 phosphorus Inorganic materials 0.000 claims description 44
- 239000011574 phosphorus Substances 0.000 claims description 44
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 40
- 238000006243 chemical reaction Methods 0.000 claims description 40
- 239000000047 product Substances 0.000 claims description 28
- 238000009713 electroplating Methods 0.000 claims description 23
- 230000015556 catabolic process Effects 0.000 claims description 18
- 238000006731 degradation reaction Methods 0.000 claims description 18
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 12
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 11
- 239000001110 calcium chloride Substances 0.000 claims description 11
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 11
- 238000005286 illumination Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000013019 agitation Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 230000003287 optical effect Effects 0.000 claims description 9
- 229910052724 xenon Inorganic materials 0.000 claims description 9
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 7
- 230000003197 catalytic effect Effects 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- -1 operates repeatedly Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 11
- 238000001914 filtration Methods 0.000 claims 2
- 239000002689 soil Substances 0.000 claims 2
- 230000008961 swelling Effects 0.000 claims 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- 239000006227 byproduct Substances 0.000 claims 1
- 150000004985 diamines Chemical class 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 18
- 239000000463 material Substances 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 6
- 230000002378 acidificating effect Effects 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 3
- 230000006641 stabilisation Effects 0.000 abstract description 3
- 238000011105 stabilization Methods 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 2
- 230000004043 responsiveness Effects 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 description 18
- 238000012545 processing Methods 0.000 description 9
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 9
- 238000004065 wastewater treatment Methods 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000007689 inspection Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 230000010355 oscillation Effects 0.000 description 3
- 238000012946 outsourcing Methods 0.000 description 3
- 238000006385 ozonation reaction Methods 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 239000012028 Fenton's reagent Substances 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 229910001453 nickel ion Inorganic materials 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 1
- 241000052343 Dares Species 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 208000036119 Frailty Diseases 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 159000000013 aluminium salts Chemical class 0.000 description 1
- 206010003549 asthenia Diseases 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- DJFBJKSMACBYBD-UHFFFAOYSA-N phosphane;hydrate Chemical compound O.P DJFBJKSMACBYBD-UHFFFAOYSA-N 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical class O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Analytical Chemistry (AREA)
- Water Treatment By Sorption (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of N-TiO2/ calcium system bentonite composite adsorption catalyst and application, the calcium system bentonite of purifying is first made, then titanium dioxide acidic sol is distributed in ethylenediamine solution, forms white suspension, the calcium system bentonite of purifying is added in above-mentioned suspension again and is reacted, N-TiO is obtained after post-processing2/ calcium system bentonite composite adsorption catalyst.The present invention can improve the characteristic of material visible-light responsiveness and the catalysis of visible light synergy ozone using nitrogen-doped titanium dioxide;On the one hand the calcium system bentonite of Simultaneous purification can give N-TiO2Attachment site is provided, another aspect material itself has good adsorption precipitation effect to pollutant, meanwhile, alkaline earth material bentonite itself has buffer function to the variation of pH value in waste water, guarantees the stabilization of wastewater pH;Preparation method simple possible of the present invention, it is easily operated, it is suitble to industrialized production.
Description
Technical field
The invention belongs to technical field of waste water processing, concretely relate to a kind of N-TiO2The compound suction of/calcium system bentonite
Attached catalyst and application.
Background technique
In electroplating wastewater processing, phosphorus is one of current most scabrous index, because of some electroplate factories, Electronics Factory, line
Road Ban Chang involves nickel chemical plating technology, which provides electronics to nickel ion, so that nickel ion is reduced to nickel
Metal, in most of chemical plating fluid, mostly using sodium hypophosphite is reducing agent, this results in containing phosphorus in cleaning waste water, and
And the epidemic situation comparison of phosphorus is special, different from general total phosphorus, the phosphorus in waste water is mainly that hypophosphites and its product being oxidized are sub-
Phosphate.
Traditional dephosphorization process mostly uses dephosphorization agent dephosphorization made by lime or other aluminium salts, and this dephosphorization agent can be with
Positive phosphorus, which combines, forms precipitating, so that phosphorus ligands are relatively applicable in some phosphorus-containing wastewaters;However in chemical nickel waste water
Phosphorus can not generate stable sediment, therefore traditional handicraft can not dephosphorization since its state is time phosphorous with lime.Have at present
Enterprise uses Fenton oxidation technology, time phosphorous is first aoxidized the phosphorus that is positive, then add dephosphorization agent and handled, but since Fenton tries
Agent oxidation efficiency is limited, if largely addition Fenton reagent is first is that cost Tai Gao enterprise holds and dares not accept and excessive hydrogen peroxide and sulphur
Sour ferrous iron will lead to COD raising, second is that it is that acidity is unfavorable for subsequent heavy metal that the Best of Fenton reagent, which requires waste water,
Precipitating, need to adjust back pH carry out heavy metal removal, therefore this method do not obtain it is generally applicable.
Simultaneously as the processing and monitoring of electroplating industry waste water all only lay particular emphasis on the removal of heavy metal ion in the past, even if
The electroplating sewerage processing system for being currently in operation and constructing is also without the treatment process or processing list for its organic pollutant
Member.State Ministry of Environmental Protection in 2008 has promulgated " discharge standard for electroplating pollutants " (GB21900-2008), wherein looking forward to newly-built plating
The COD of industry discharge is made that strict regulations, it is desirable that general area COD is less than 80mg/L, and environmental carrying capacity is small, ecological environment frailty
Regional COD is less than 50mg/L.
Secondary phosphorous both effectively can be aoxidized the phosphorus that is positive for electroplating wastewater processing and be conducive to subsequent processing by ozone system,
The oxidation removal of organic matter can be carried out on the basis of not newly-increased processing unit again, meanwhile, ozone system will not change substantially
Wastewater pH, but cause the system cost performance low since ozone utilization efficiency is low, to limit being widely used for the system.This
Outside, ultraviolet catalytic oxidation has good effect in terms of the removal of pollutant, and has good cooperate between ozone oxidation
Effect.But ultraviolet light it is shared in sunlight ratio it is very small, and penetration power is very weak, is easy to be absorbed by atmosphere.Manually
The energy consumption of ultraviolet source in the actual production process is very big, it is difficult to large-scale application.
Summary of the invention
In order to overcome the shortcomings of the prior art, the present invention provides be used to change under a kind of visible light synergy ozone system
Learn the novel N-TiO of nickel-plating waste water processing2/ calcium system bentonite composite adsorption catalyst and application can be improved visible light and smelly
Oxygen transfer efficiency effectively removes total phosphorus and organic matter in electroplating wastewater.
A kind of N-TiO2/ calcium system bentonite composite adsorption catalyst, is prepared by following step:
(1) calcium-base bentonite is added in hydrochloric acid solution and is made into calcium-base bentonite suspension, carried out after ultrasonic reaction permanent
Temperature reaction, calcium chloride is then added, and the reaction was continued moves back oscillating reactions in constant-temperature table, the post-treated calcium system purified
Bentonite;
(2) titanium tetrachloride is added in hydrochloric acid solution, stirs to get TiO 2 sol, TiO 2 sol is added to
It in ethylenediamine solution, is stirred after ultrasonic disperse, obtains white suspension;
(3) the calcium system bentonite purified is added in above-mentioned white suspension simultaneously isothermal reaction, cools down after reaction, will
After product is post-processed, N-TiO is obtained2/ calcium system bentonite composite adsorption catalyst.
The present invention uses nitrogen-doped titanium dioxide (N-TiO2), the visible light photocatalytic degradation effect of titanium dioxide can be improved
Rate, calcium-base bentonite can both give N-TiO as a kind of cheap alkaline earth porous adsorbing material2Attachment site is provided, and can be right
Part Phos and heavy metal in waste water carry out absorption degradation, meanwhile, alkaline earth material bentonite itself is to pH value in waste water
Variation has buffer function, guarantees the stabilization of wastewater pH.
Preferably, titanium tetrachloride, ethylenediamine, the bentonitic liquor capacity ratio of calcium system are 0.05~0.12:5~12:1.
Preferably, the mass fraction of the hydrochloric acid solution is 7~11%, calcium-base bentonite suspension in step (1)
Mass fraction is 8~15%, and the dosage of calcium chloride is the 15~25% of calcium-base bentonite quality, and isothermal reaction temperature is 60~80
DEG C, calcium chloride the reaction was continued 10~40min is added, post-processing step is centrifugation, it washs, dries, sieving.
Preferably, titanium tetrachloride, concentration of hydrochloric acid solution 0.8 is added in hydrochloric acid solution at room temperature in step (2)
~1.2mol/L.
Preferably, the mass fraction of the calcium system bentonite solution of purifying is 0.5~1.5%, and constant temperature is anti-in step (3)
Answering temperature is 110~150 DEG C, and post-processing step is that product is transferred in beaker, is stood, and centrifugation, product, which is adjusted to pH, is
Neutrality collects centrifugation product, after drying, the calcination at 400~500 DEG C.
Preferably, the N-TiO2/ calcium system bentonite composite adsorption catalyst, is prepared by following step:
(1) calcium-base bentonite is added in the hydrochloric acid solution that mass fraction is 9%, is made into the calcium that mass fraction is 12%
Base bentonite suspension moves into magnetic agitation under 70 DEG C of constant temperature water baths after ultrasonic reaction 30min and reacts 1.5h, calcium base is then added
The reaction was continued 20min the moves back oscillating reactions into 28 DEG C, the constant-temperature table of 140r/min of the calcium chloride of bentonite quality 20%
For 24 hours, it is centrifuged after reaction, is washed with distilled water solid deposits to no Cl-In the presence of solid sample obtained is at 105 DEG C
Drying, sieves with 100 mesh sieve, the calcium system bentonite purified;
(2) at room temperature, titanium tetrachloride is added in the hydrochloric acid solution of 1mol/L, stirs 1h, obtains the two of pale yellow transparent
Titanium oxide acidic sol;TiO 2 sol is added in ethylenediamine solution, ultrasonic disperse 30min is placed on mixing platform and stirs
30min is mixed, white suspension is obtained;
(3) the calcium system bentonite solution of the purifying of configuration 1% is added in above-mentioned suspension simultaneously 130 DEG C of oil bath heated at constant temperature
12h is reacted, room temperature is down under agitation after reaction, is down to room temperature to product, product is transferred in beaker, is stood
For 24 hours, centrifuge separation removal supernatant, operates repeatedly, and product is adjusted to pH as neutrality, collects centrifugation product, 80 DEG C of bakings
After dry, it is placed in capping ceramic crucible the calcination 3h at 450 DEG C of muffle furnace, obtains N-TiO2/ calcium system bentonite composite adsorption is urged
Agent;
Wherein, titanium tetrachloride, ethylenediamine, calcium system bentonite solution volume ratio are 0.08:8:1.
The present invention also provides the N-TiO2/ calcium system bentonite composite adsorption catalyst is catalyzed in visible light synergy ozone
The application of degradation electroplating wastewater, i.e. visible light cooperate with lower N-TiO2/ calcium system bentonite Catalytic Ozonation electroplating wastewater.
Preferably, the N-TiO2The application of/calcium system bentonite composite adsorption catalyst, includes the following steps:
(1) waste water is taken to adjust pH value to 2~4;
(2) the N-TiO2/ calcium system bentonite composite adsorption catalyst of 0.1~0.3g/L is added, is irradiated under xenon lamp, uses
Optical filter cuts off wavelength 400nm light below;Under visible light illumination condition, it is passed through the ozone that concentration is 3~7mg/L, not
With time sampling and detect total phosphorus and COD concentration.
Preferably, the N-TiO2The application of/calcium system bentonite composite adsorption catalyst, includes the following steps:
(1) 150mL waste water is taken to adjust pH value to 3;
(2) N-TiO of 0.2g/L is added2/ calcium system bentonite composite adsorption catalyst, irradiates under the xenon lamp of 300W,
Wavelength 400nm light below is cut off with optical filter;Under visible light illumination condition, it is passed through the ozone that concentration is 5mg/L, in the time
Total phosphorus and COD concentration are sampled and detected for 5~80min.
Titanium dioxide (the N-TiO of nonmetallic N doping2) due to stronger visible light catalysis activity it is known as second
For photochemical catalyst, there is vast potential for future development.Calcium system bentonite can effectively adsorption precipitation be catalyzed through visible light synergy ozone
The Phos of oxidation, to load N-TiO2Calcium system bentonite be catalyst, in visible light synergy ozone catalysis oxidation time simultaneously
There is not been reported for phosphorous and degradation Organic substance in water.
The present invention can improve material visible-light responsiveness using nitrogen-doped titanium dioxide and visible light synergy ozone is catalyzed
Characteristic;On the one hand the calcium system bentonite of Simultaneous purification can give N-TiO2Attachment site is provided, another aspect material itself is to dirt
Dye object has good adsorption precipitation effect, meanwhile, alkaline earth material bentonite itself there is buffering to make the variation of pH value in waste water
With guaranteeing the stabilization of wastewater pH;Preparation method simple possible of the present invention, it is easily operated, it is suitble to industrialized production.
Detailed description of the invention
Fig. 1 is the total phosphorus degradation effect figure during the present invention is implemented under different condition;
Fig. 2 is the COD degradation effect picture during the present invention is implemented under different condition.
Specific embodiment
The present invention is further explained in the light of specific embodiments, but invention which is intended to be protected is not limited to
This.
Embodiment 1
Visible light cooperates with lower N-TiO2/ calcium system bentonite Catalytic Ozonation electroplating wastewater
A kind of N-TiO2/ calcium system bentonite composite adsorption catalyst, is prepared by following step:
(1) outsourcing calcium-base bentonite is added in the hydrochloric acid solution that mass fraction is 9%, being made into mass fraction is 12%
Calcium-base bentonite suspension, magnetic agitation under 70 DEG C of constant temperature water baths is moved into after ultrasonic reaction 30min and reacts 1.5h, is then added
The reaction was continued that 20min moves back into 28 DEG C, the constant-temperature table of 140r/min that oscillation is anti-for the calcium chloride of calcium-base bentonite quality 20%
It should be centrifuged after reaction for 24 hours, be washed with distilled water solid deposits to no Cl-In the presence of (using AgNO3, solution inspection), it is made
Solid sample dried at 105 DEG C, sieve with 100 mesh sieve, the calcium system bentonite purified;
(2) at room temperature, titanium tetrachloride is added in the hydrochloric acid solution of 1mol/L, stirs 1h, obtains the two of pale yellow transparent
Titanium oxide acidic sol;TiO 2 sol is added in ethylenediamine solution, ultrasonic disperse 30min is sufficiently mixed the two
It is even, it is subsequently placed on mixing platform and stirs 30min, obtain white suspension;
(3) the calcium system bentonite solution of the purifying of configuration 1% is added in above-mentioned suspension simultaneously 130 DEG C of oil bath heated at constant temperature
12h is reacted, room temperature is down under agitation after reaction, is down to room temperature to product, product is transferred in beaker, is stood
For 24 hours, centrifuge separation removal supernatant, operates repeatedly, and product is adjusted to pH as neutrality, collects centrifugation product, 80 DEG C of bakings
After dry, it is placed in capping ceramic crucible the calcination 3h at 450 DEG C of muffle furnace, obtains N-TiO2/ calcium system bentonite composite adsorption is urged
Agent;
In reaction system, titanium tetrachloride, ethylenediamine, calcium system bentonite solution volume ratio are 0.08:8:1.
For electroplating wastewater derives from Xinchang Hardwear Pty Ltd. wastewater treatment, the factory waste water total phosphorus 48.6mg/L, COD
477mg/L。
It takes 150mL waste water to adjust pH value to 3, the N-TiO of 0.2g/L is then added2/ calcium system bentonite adsorption catalyst,
It is irradiated under the xenon lamp of 300W, cuts off wavelength 400nm light below with optical filter;Under visible light (λ > 400nm) illumination condition,
It is passed through the ozone that concentration is 5mg/L, is respectively 5min, 10min, 20min, 30min, 40min, 60min and 80min in the time
Sample and detect total phosphorus and COD concentration.
Total phosphorus degradation effect figure under above-mentioned condition is as shown in Figure 1, COD degradation effect picture such as Fig. 2 institute under above-mentioned condition
Show.As shown in Figure 1, total phosphorus is in 80min removal rate up to 96.2% under this experiment condition;As shown in Fig. 2, COD under this experiment condition
In 80min removal rate up to 76.3%.
Embodiment 2
A kind of N-TiO2/ calcium system bentonite composite adsorption catalyst, is prepared by following step:
(1) outsourcing calcium-base bentonite is added in the hydrochloric acid solution that mass fraction is 9%, being made into mass fraction is 12%
Calcium-base bentonite suspension, magnetic agitation under 70 DEG C of constant temperature water baths is moved into after ultrasonic reaction 30min and reacts 1.5h, is then added
The reaction was continued that 20min moves back into 28 DEG C, the constant-temperature table of 140r/min that oscillation is anti-for the calcium chloride of calcium-base bentonite quality 20%
It should be centrifuged after reaction for 24 hours, be washed with distilled water solid deposits to no Cl-In the presence of (using AgNO3, solution inspection), it is made
Solid sample dried at 105 DEG C, sieve with 100 mesh sieve, the calcium system bentonite purified;
(2) at room temperature, titanium tetrachloride is added in the hydrochloric acid solution of 1mol/L, stirs 1h, obtains the two of pale yellow transparent
Titanium oxide acidic sol;TiO 2 sol is added in ethylenediamine solution, ultrasonic disperse 30min is sufficiently mixed the two
It is even, it is subsequently placed on mixing platform and stirs 30min, obtain white suspension;
(3) the calcium system bentonite solution of the purifying of configuration 1% is added in above-mentioned suspension simultaneously 130 DEG C of oil bath heated at constant temperature
12h is reacted, room temperature is down under agitation after reaction, is down to room temperature to product, product is transferred in beaker, is stood
For 24 hours, centrifuge separation removal supernatant, operates repeatedly, and product is adjusted to pH as neutrality, collects centrifugation product, 80 DEG C of bakings
After dry, it is placed in capping ceramic crucible the calcination 3h at 450 DEG C of muffle furnace, obtains N-TiO2/ calcium system bentonite composite adsorption is urged
Agent;
In reaction system, titanium tetrachloride, ethylenediamine, calcium system bentonite solution volume ratio are 0.06:10:1.
For electroplating wastewater derives from Xinchang Hardwear Pty Ltd. wastewater treatment, the factory waste water total phosphorus 48.6mg/L, COD
477mg/L。
It takes 150mL waste water to adjust pH value to 3, the N-TiO of 0.2g/L is then added2/ calcium system bentonite adsorption catalyst,
It is irradiated under the xenon lamp of 300W, cuts off wavelength 400nm light below with optical filter;Under visible light (λ > 400nm) illumination condition,
It is passed through the ozone that concentration is 5mg/L.
Total phosphorus is in 80min removal rate up to 92.1% under this experiment condition, and COD is reached in 80min removal rate under this experiment condition
71.5%.
Embodiment 3
A kind of N-TiO2/ calcium system bentonite composite adsorption catalyst, is prepared by following step:
(1) outsourcing calcium-base bentonite is added in the hydrochloric acid solution that mass fraction is 9%, being made into mass fraction is 12%
Calcium-base bentonite suspension, magnetic agitation under 70 DEG C of constant temperature water baths is moved into after ultrasonic reaction 30min and reacts 1.5h, is then added
The reaction was continued that 20min moves back into 28 DEG C, the constant-temperature table of 140r/min that oscillation is anti-for the calcium chloride of calcium-base bentonite quality 20%
It should be centrifuged after reaction for 24 hours, be washed with distilled water solid deposits to no Cl-In the presence of (using AgNO3, solution inspection), it is made
Solid sample dried at 105 DEG C, sieve with 100 mesh sieve, the calcium system bentonite purified;
(2) at room temperature, titanium tetrachloride is added in the hydrochloric acid solution of 1mol/L, stirs 1h, obtains the two of pale yellow transparent
Titanium oxide acidic sol;TiO 2 sol is added in ethylenediamine solution, ultrasonic disperse 30min is sufficiently mixed the two
It is even, it is subsequently placed on mixing platform and stirs 30min, obtain white suspension;
(3) the calcium system bentonite solution of the purifying of configuration 1% is added in above-mentioned suspension simultaneously 130 DEG C of oil bath heated at constant temperature
12h is reacted, room temperature is down under agitation after reaction, is down to room temperature to product, product is transferred in beaker, is stood
For 24 hours, centrifuge separation removal supernatant, operates repeatedly, and product is adjusted to pH as neutrality, collects centrifugation product, 80 DEG C of bakings
After dry, it is placed in capping ceramic crucible the calcination 3h at 450 DEG C of muffle furnace, obtains N-TiO2/ calcium system bentonite composite adsorption is urged
Agent;
In reaction system, titanium tetrachloride, ethylenediamine, calcium system bentonite solution volume ratio are 0.01:7:1.
For electroplating wastewater derives from Xinchang Hardwear Pty Ltd. wastewater treatment, the factory waste water total phosphorus 48.6mg/L, COD
477mg/L。
It takes 150mL waste water to adjust pH value to 3, the N-TiO of 0.2g/L is then added2/ calcium system bentonite adsorption catalyst,
It is irradiated under the xenon lamp of 300W, cuts off wavelength 400nm light below with optical filter;Under visible light (λ > 400nm) illumination condition,
It is passed through the ozone that concentration is 5mg/L.
Total phosphorus is in 80min removal rate up to 90.4% under this experiment condition, and COD is reached in 80min removal rate under this experiment condition
70.1%.
Embodiment 4
Catalyst preparation is referring to embodiment 1.
For electroplating wastewater derives from Xinchang Hardwear Pty Ltd. wastewater treatment, the factory waste water total phosphorus 48.6mg/L, COD
477mg/L。
It takes 150mL waste water to adjust pH value to 3, the N-TiO of 0.1g/L is then added2/ calcium system bentonite adsorption catalyst,
It is irradiated under the xenon lamp of 300W, cuts off wavelength 400nm light below with optical filter;Under visible light (λ > 400nm) illumination condition,
It is passed through the ozone that concentration is 5mg/L.
Total phosphorus is in 80min removal rate up to 89.3% under this experiment condition, and COD is reached in 80min removal rate under this experiment condition
66.1%.
Embodiment 5
Catalyst preparation is referring to embodiment 1.
For electroplating wastewater derives from Xinchang Hardwear Pty Ltd. wastewater treatment, the factory waste water total phosphorus 48.6mg/L, COD
477mg/L。
It takes 150mL waste water to adjust pH value to 3, the N-TiO of 0.3g/L is then added2/ calcium system bentonite adsorption catalyst,
It is irradiated under the xenon lamp of 300W, cuts off wavelength 400nm light below with optical filter;Under visible light (λ > 400nm) illumination condition,
It is passed through the ozone that concentration is 5mg/L.
Total phosphorus is in 80min removal rate up to 91.9% under this experiment condition, and COD is reached in 80min removal rate under this experiment condition
73.1%.
Embodiment 6
N-TiO2/ calcium system bentonite Catalytic Ozonation electroplating wastewater
Catalyst preparation is referring to embodiment 1.
For electroplating wastewater derives from Xinchang Hardwear Pty Ltd. wastewater treatment, the factory waste water total phosphorus 48.6mg/L, COD
477mg/L。
It takes 150mL waste water to adjust pH value to 3, the N-TiO of 0.2g/L is then added2/ calcium system bentonite adsorption catalyst,
Be passed through under the conditions of being protected from light concentration be 5mg/L ozone, respectively be passed through the time be 5min, 10min, 20min, 30min, 40min,
60min and 80min samples and detects total phosphorus and COD concentration.
Total phosphorus degradation effect figure under above-mentioned condition is as shown in Figure 1, COD degradation effect picture such as Fig. 2 institute under above-mentioned condition
Show.As shown in Figure 1, total phosphorus is in 80min removal rate 83.1% under this experiment condition;As shown in Fig. 2, COD exists under this experiment condition
80min removal rate 63%.
Embodiment 7
N-TiO2/ calcium system bentonite catalytic degradation electroplating wastewater
Catalyst preparation is referring to embodiment 1.
For electroplating wastewater derives from Xinchang Hardwear Pty Ltd. wastewater treatment, the factory waste water total phosphorus 48.6mg/L, COD
477mg/L.It takes 150mL waste water to adjust pH value to 3, the N-TiO of 0.2g/L is then added2/ calcium system bentonite adsorption catalyst,
It is respectively that 5min, 10min, 20min, 30min, 40min, 60min and 80min are sampled simultaneously the time is added under the conditions of being protected from light
Detect total phosphorus and COD concentration.
Total phosphorus degradation effect figure under above-mentioned condition is as shown in Figure 1, COD degradation effect picture such as Fig. 2 institute under above-mentioned condition
Show.As shown in Figure 1, total phosphorus is in 80min removal rate 49.9% under this experiment condition;As shown in Fig. 2, COD exists under this experiment condition
80min removal rate 9.7%.
Embodiment 8
Ozone oxidation degradation electroplating wastewater
For electroplating wastewater derives from Xinchang Hardwear Pty Ltd. wastewater treatment, the factory waste water total phosphorus 48.6mg/L, COD
477mg/L。
It takes 150mL waste water to adjust pH value to 3, then under the conditions of being protected from light, is passed through the ozone that concentration is 5mg/L, exists respectively
Being passed through the time is that 5min, 10min, 20min, 30min, 40min, 60min and 80min sample and detect total phosphorus and COD concentration.
Total phosphorus degradation effect figure under above-mentioned condition is as shown in Figure 1, COD degradation effect picture such as Fig. 2 institute under above-mentioned condition
Show.As shown in Figure 1, total phosphorus is in 80min removal rate 19.5% under this experiment condition;As shown in Fig. 2, COD exists under this experiment condition
80min removal rate 40%.
Embodiment 9
Visible light (λ > 400nm) illumination degrading electroplating wastewater
For electroplating wastewater derives from Xinchang Hardwear Pty Ltd. wastewater treatment, the factory waste water total phosphorus 48.6mg/L, COD
477mg/L。
150mL waste water is taken to adjust pH value to 3, then under visible light (λ > 400nm) illumination condition, respectively in light application time
Total phosphorus and COD concentration are sampled and detected for 5min, 10min, 20min, 30min, 40min, 60min and 80min.
Total phosphorus degradation effect figure under above-mentioned condition is as shown in Figure 1, COD degradation effect picture such as Fig. 2 institute under above-mentioned condition
Show.As shown in Figure 1, total phosphorus is in 80min removal rate 10% under this experiment condition;As shown in Fig. 2, COD exists under this experiment condition
80min removal rate 9.1%.
Claims (9)
1. a kind of N-TiO2/ calcium system bentonite composite adsorption catalyst, it is characterised in that be prepared by following step:
(1) calcium-base bentonite is added in hydrochloric acid solution and is made into calcium-base bentonite suspension, it is anti-that constant temperature is carried out after ultrasonic reaction
It answers, calcium chloride is then added, and the reaction was continued moves back oscillating reactions in constant-temperature table, the post-treated calcium system swelling purified
Soil;
(2) titanium tetrachloride is added in hydrochloric acid solution, stirs to get TiO 2 sol, TiO 2 sol is added to second two
It in amine aqueous solution, is stirred after ultrasonic disperse, obtains white suspension;
(3) the calcium system bentonite purified is added in above-mentioned white suspension simultaneously isothermal reaction, cools down after reaction, by product
After being post-processed, N-TiO is obtained2/ calcium system bentonite composite adsorption catalyst.
2. N-TiO according to claim 12/ calcium system bentonite composite adsorption catalyst, it is characterised in that: titanium tetrachloride, second
Diamines, the bentonitic liquor capacity ratio of calcium system are 0.05~0.12:5~12:1.
3. N-TiO according to claim 12/ calcium system bentonite composite adsorption catalyst, it is characterised in that: in step (1), institute
The mass fraction for stating hydrochloric acid solution is 7~11%, and the mass fraction of calcium-base bentonite suspension is 8~15%, the use of calcium chloride
Amount is the 15~25% of calcium-base bentonite quality, and isothermal reaction temperature is 60~80 DEG C, calcium chloride is added the reaction was continued 10~
40min, post-processing step are centrifugation, wash, dry, sieving.
4. N-TiO according to claim 12/ calcium system bentonite composite adsorption catalyst, it is characterised in that: in step (2), room
Titanium tetrachloride is added under temperature in hydrochloric acid solution, concentration of hydrochloric acid solution is 0.8~1.2mol/L.
5. N-TiO according to claim 12/ calcium system bentonite composite adsorption catalyst, it is characterised in that: pure in step (3)
The mass fraction of the calcium system bentonite solution of change is 0.5~1.5%, and isothermal reaction temperature is 110~150 DEG C, post-processing step
For product to be transferred in beaker, stands, centrifugation, product is adjusted to pH as neutrality, centrifugation product is collected, after drying, in 400
Calcination at~500 DEG C.
6. N-TiO according to claim 12/ calcium system bentonite composite adsorption catalyst, it is characterised in that pass through following step
It is prepared:
(1) calcium-base bentonite is added in the hydrochloric acid solution that mass fraction is 9%, it is swollen is made into the calcium base that mass fraction is 12%
Moisten native suspension, magnetic agitation under 70 DEG C of constant temperature water baths is moved into after ultrasonic reaction 30min and reacts 1.5h, the swelling of calcium base is then added
The reaction was continued 20min moves back into 28 DEG C, the constant-temperature table of the 140r/min oscillating reactions of the calcium chloride of soil property amount 20% for 24 hours, instead
It is centrifuged after answering, is washed with distilled water solid deposits to no Cl-In the presence of solid sample obtained is dried at 105 DEG C, mistake
100 meshes, the calcium system bentonite purified;
(2) at room temperature, titanium tetrachloride is added in the hydrochloric acid solution of 1mol/L, stirs 1h, obtains the titanium dioxide of pale yellow transparent
Titanium colloidal sol;TiO 2 sol is added in ethylenediamine solution, ultrasonic disperse 30min, which is placed on mixing platform, stirs 30min,
Obtain white suspension;
(3) the calcium system bentonite solution of the purifying of configuration 1% is added in above-mentioned white suspension simultaneously 130 DEG C of oil bath heated at constant temperature
12h is reacted, room temperature is down under agitation after reaction, is down to room temperature to product, product is transferred in beaker, is stood
For 24 hours, centrifuge separation removal supernatant, operates repeatedly, and product is adjusted to pH as neutrality, collects centrifugation product, 80 DEG C of bakings
After dry, it is placed in capping ceramic crucible the calcination 3h at 450 DEG C of muffle furnace, obtains N-TiO2/ calcium system bentonite composite adsorption is urged
Agent;
Wherein, titanium tetrachloride, ethylenediamine, calcium system bentonite solution volume ratio are 0.08:8:1.
7. N-TiO described in a kind of claim 12/ calcium system bentonite composite adsorption catalyst is in visible light synergy ozone catalytic degradation
The application of electroplating wastewater.
8. N-TiO according to claim 72The application of/calcium system bentonite composite adsorption catalyst, it is characterised in that including under
State step:
(1) waste water is taken to adjust pH value to 2~4;
(2) N-TiO of 0.1~0.3g/L is added2/ calcium system bentonite composite adsorption catalyst, irradiates under xenon lamp, with optical filtering
Piece cuts off wavelength 400nm light below;Under visible light illumination condition, it is passed through the ozone that concentration is 3~7mg/L, when different
Between sample and detect total phosphorus and COD concentration.
9. N-TiO according to claim 82The application of/calcium system bentonite composite adsorption catalyst, it is characterised in that including under
State step:
(1) 150mL waste water is taken to adjust pH value to 3;
(2) N-TiO of 0.2g/L is added2/ calcium system bentonite composite adsorption catalyst, irradiates under the xenon lamp of 300W, with optical filtering
Piece cuts off wavelength 400nm light below;Under visible light illumination condition, be passed through concentration be 5mg/L ozone, the time be 5~
80min samples and detects total phosphorus and COD concentration.
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