CN103143362B - Magnetic photocatalyst used for gas waste water treatment and preparation method thereof - Google Patents

Magnetic photocatalyst used for gas waste water treatment and preparation method thereof Download PDF

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CN103143362B
CN103143362B CN201210511134.0A CN201210511134A CN103143362B CN 103143362 B CN103143362 B CN 103143362B CN 201210511134 A CN201210511134 A CN 201210511134A CN 103143362 B CN103143362 B CN 103143362B
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suspension
photochemical catalyst
catalyst
gas waste
magnetic loaded
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CN103143362A (en
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景茂祥
韩翀
沈湘黔
刘瑞江
王舟
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Jiangsu University
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

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Abstract

The invention belongs to the technical field of waste water treatment through photocatalytic oxidation, and particularly relates to a magnetic photocatalyst, a preparation method and a method for advanced treatment of gas waste water. The magnetic composite photocatalyst of a core-shell structure prepared with a continuous homogeneous precipitation-calcination method is good in dispersity, sizes of particles are about 1-9 nanometers, a layer of gamma-aluminium oxide is arranged between a ferrite core and a nanometer titanium dioxide shell layer and serves as a middle layer, the packaging quantity is large and adjustable, the distribution is uniform, the magnetism is strong, the catalytic activity is high, and the magnetic photocatalyst can be excited by sunlight and used for the gas waste water treatment. The treatment speed is fast, the effect is good, the cost is low, the process is simple, and the catalyst in water solution can be recovered fast with a magnet and used repeatedly.

Description

A kind of magnetic loaded type photochemical catalyst for coal gas waste process and preparation method thereof
Technical field
The invention belongs to photocatalysis oxidation treatment waste water technical field, particularly relate to a kind of method of magnetic loaded type photochemical catalyst, preparation method and advanced treating coal gas waste.
Background technology
Coal gas is in washing, cooling, in purification process, the waste water of a large amount of complicated component can be produced, ammonia nitrogen particularly containing high concentration in waste water, COD, the organic matter of phenol and some other difficult for biological degradation, the process of this type of waste water is the difficult problem in water treatment, although with traditional pretreatment---there is a large amount of organic and inorganic pollutions to be removed after Multilevel biochemistry treatment PROCESS FOR TREATMENT, but still containing a certain amount of persistent organic pollutants in water outlet, be difficult to reach discharge standard, and existing treatment process is very complicated, operating cost is expensive, cycle is long, and easily cause secondary environmental pollution, at present, many researchers select the ammonia nitrogen in ammoniomagnesium phosphate crystal method gas treatment waste water, simple, the recyclable ammonia nitrogen of technique, treatment effect are also more satisfactory, reach Resource recovery, the object of protection of the environment, but still have part ammonia nitrogen remaining in the waste water after process, COD, phenol and other organic pollutions still exist in a large number, this method is in fact relatively applicable to the pretreatment of coal gas waste.
Photocatalysis technology is as a kind of emerging organic pollution treatment technology, there is processing speed fast, degrade not selective, equipment is simple, easy to operate, non-secondary pollution, the features such as treatment effect is good, have been applied in antifouling, antibacterial, deodorizing, purification of air, water treatment and environmental pollution improvement etc.; The Peng Xianyu of Hunan University etc. are with TiO 2for catalyst, H 2o 2for oxidant, under UV-irradiation, adopt heterogeneous photocatalysis method to process coking chemical waste water, discussion is studied to the various influence factors of COD clearance, result shows that this method can make coke-oven plant's second pond waste water COD be down to 52. 1mg/ L from 348. 3 mg/ L, and the clearance of COD can reach 85. 0 more than % (University Of Nanhua's journal, 2005,19(1): 64-68), but the shortcoming that this method exists also clearly, catalyst recovery is difficult, and UV-irradiation cost is high; Utilize sunlight photocatalysis process organic wastewater existing large quantity research, especially magnetic loaded type photochemical catalyst TiO at home and abroad 2/ γ-Fe 2o 3, TiO 2/ Fe 3o 4, TiO 2/ CoFe 2o 4, TiO 2/ NiFe 2o 4, TiO 2/ AC/Fe 2o 3, TiO 2/ SiO 2/ Fe 2o 3, TiO 2/ SiO 2/ Fe 3o 4, TiO 2/ SiO 2/ NiFe 2o 4, TiO 2/ SiO 2/ Mn-ZnFe 2o 4, TiO 2/ SiO 2/ BaFe 2o 4, TiO 2/ SiO 2/ CoFe 2o 4, TiO 2/ Al 2o 3/ ZnFe 2o 4deng come out one after another, maintain TiO 2high activity, improves recovery utilization rate, and makes sunlight photocatalysis process organic wastewater become possibility; But these magnetic loaded type photochemical catalysts reported are all sub-micron or nanometer grade powder (being all less than 400 nanometers), reunite serious, magnetic is weak, reclaims ability; Its preparation method is also mostly sol-gal process, self-assembly method, chemical vapour deposition technique etc., be difficult to prepare soilless sticking, purity high, without coming off, uniform load and the high magnetic loaded type photochemical catalyst of magnetic; We report a kind of ferrous acid nickel/titanium dioxide magnetic loaded type photochemical catalyst preparation method in [CN200910087741.7], overcome above-mentioned shortcoming to a great extent, but prepared catalyst must take still ultraviolet light as light source owing to there is not intermediate insulating layer between nickel ferrite based magnetic loaded and titanium dioxide; The present invention improves preparation method, and exploitation has the nucleocapsid structure magnetic loaded type photochemical catalyst in intermediate layer, and can at degradable organic pollutant under sunshine; Not yet there is the report utilizing sunshine and magnetic loaded type photochemical catalyst photocatalysis treatment coal gas waste at present.
Summary of the invention
The object of the invention is the deficiency existed for existing coal gas waste treatment technology and magnetic loaded type photochemical catalyst, a kind of nucleocapsid structure, micron order magnetic loaded type photochemical catalyst and preparation method thereof are provided, and a kind of method utilizing sunshine and this magnetic loaded type photochemical catalyst advanced treating coal gas waste is provided, cost is low, processing speed is fast, catalyst can reclaim in aqueous fast, reuses.
Goal of the invention of the present invention is achieved through the following technical solutions:
A kind of magnetic loaded type photochemical catalyst, it is characterized in that with NiFe 2o 4, CoFe 2o 4, MnFe 2o 4, BaFe 2o 4one in ferrite powder is core, is intermediate layer with gamma-alumina, take nano titanium oxide as shell, and gamma-alumina and ferritic mass ratio are 1 ~ 3:1, and titanium dioxide and ferritic mass ratio are 0.1 ~ 0.5:1, and the particle diameter of photochemical catalyst is 1 ~ 9um.
A kind of magnetic loaded type photochemical catalyst preparation method, is characterized in that preparation process comprises:
(1) be that the ferrite powder of 0.5 ~ 5um is placed in reaction vessel by particle diameter, add water and mechanical agitation forms the suspension of 100 ~ 500g/L;
(2) under mechanical stirring, be that the aluminum ammonium sulfate solution of 0.2 ~ 0.4mol/L and the ammonium bicarbonate soln of 0.8 ~ 1.6mol/L instill in suspension with the speed of 10 ~ 20mL/min respectively simultaneously by concentration, start precipitation reaction, controlling solution ph with carbonic hydroammonium is stabilized between 7 ~ 8, the alum total amount added is scaled aluminium oxide and ferritic mass ratio is 1 ~ 3:1, after reinforced end, obtain the suspension of alumina-coated ferrite presoma;
(3) continue in suspension, to instill the titanium sulfate solution of 0.1 ~ 0.25mol/L and the ammonium bicarbonate soln of 0.4 ~ 1.0mol/L with the speed of 10 ~ 20mL/min simultaneously, mechanical agitation, make titanium ion precipitated crystal on suspended particulate, form integument, controlling solution ph with carbonic hydroammonium is stabilized between 7 ~ 8, the titanium sulfate total amount added is scaled titanium dioxide and ferritic mass ratio is 0.1 ~ 0.5:1, to be fed complete after, at room temperature continue to react half an hour, sediment is filtered, washing, in atmosphere in 60 ~ 80 DEG C of dryings after 10 ~ 12 hours, in 700 ~ 800 DEG C of roastings 1 ~ 3 hour, namely described magnetic loaded type photochemical catalyst is obtained.
A method for advanced treating coal gas waste, is characterized in that its concrete steps comprise:
(1) magnetic loaded type photochemical catalyst is placed in is equipped with in the open glass container of the pretreated coal gas waste of the ammonium magnesium phosphate precipitation method, lucifuge mechanical agitation 30 ~ 60 minutes, form the suspension of catalyst quality concentration 1 ~ 5g/L;
(2) under the glass container filling suspension being placed in sunshine together with mechanical agitator, prolonged exposure also constantly stirs, and irradiation time is 5 ~ 15 hours;
(3), after detection ammonia nitrogen in solution, COD, phenol and other organic component contents reaches sewage drainage standard, stop reaction, and reclaim catalyst with magnet.
Described coal gas waste is through the pretreated coal gas waste of the ammonium magnesium phosphate precipitation method, and ammonia-nitrogen content reduces by 70 ~ 80%, and other component content is constant.
The tool of catalyst provided by the invention, preparation method and application technology has the following advantages:
1, the nucleocapsid structure magnetic loaded type photochemical catalyst adopting the present invention to obtain, good dispersion, particle diameter is at about 1 ~ 9um, one deck gamma-alumina is had as intermediate layer between ferrite core and nano titanium oxide shell, parcel amount is large and adjustable, is evenly distributed, and magnetic is strong, catalytic activity is high, can be excited by sunshine.
2, continuous non-homogeneous phase deposition-roasting method is adopted to prepare nucleocapsid structure magnetic loaded type composite photo-catalyst; compared with existing composite construction powder body material preparation technology; avoid reunion, come off, the shortcoming such as unequal loading, technique, equipment are simply controlled, and cost is low, be easy to large-scale production.
3, adopt coal gas waste processing method provided by the invention, processing speed is fast, and effective, cost is low, and process is simple, and catalyst can reclaim with magnet in aqueous fast, reuses.
Accompanying drawing explanation
Fig. 1 is TiO prepared in the embodiment of the present invention 1 2/ Al 2o 3/ NiFe 2o 4the optical microscope photograph of catalyst;
Fig. 2 is TiO in the embodiment of the present invention 1 2/ Al 2o 3/ NiFe 2o 4the x-ray diffraction pattern (XRD) of composite photo-catalyst and carrier;
Fig. 3 is TiO in the embodiment of the present invention 1 2/ Al 2o 3/ NiFe 2o 4the hysteresis curve (VSM) of composite photo-catalyst;
Fig. 4 is coal gas waste degradation and decolorization change in process photo in the embodiment of the present invention 1;
Table 1 is the embodiment of the present invention 1,2, and Substances variation table before and after coal gas waste degraded in 3.
Detailed description of the invention
A method for magnetic loaded type photochemical catalyst, preparation method and advanced treating coal gas waste, its detailed description of the invention is as follows:
(1) be that the ferrite powder of 0.5 ~ 5um is placed in reaction vessel by particle diameter, add water and mechanical agitation forms the suspension of 100 ~ 500g/L.Under mechanical stirring, be that the aluminum ammonium sulfate solution of 0.2 ~ 0.4mol/L and the ammonium bicarbonate soln of 0.8 ~ 1.6mol/L pass in suspension with the speed of 10 ~ 20mL/min respectively simultaneously by concentration, start precipitation reaction, controlling solution ph with carbonic hydroammonium is stabilized between 7 ~ 8, the alum total amount added is scaled aluminium oxide and ferritic mass ratio is 1 ~ 3:1, after reinforced end, obtain the suspension of alumina-coated ferrite presoma.
(2) continue in suspension, to pass into the titanium sulfate solution of 0.1 ~ 0.25mol/L and the ammonium bicarbonate soln of 0.4 ~ 1.0mol/L with the speed of 10 ~ 20mL/min simultaneously, mechanical agitation, make titanium ion precipitated crystal on suspended particulate, form integument, controlling solution ph with carbonic hydroammonium is stabilized between 7 ~ 8, the titanium sulfate total amount added is scaled titanium dioxide and ferritic mass ratio is 0.1 ~ 0.5:1, to be fed complete after, at room temperature continue to react half an hour, sediment is filtered, washing, in atmosphere in 60 ~ 80 DEG C of dryings after 10 ~ 12 hours, in 700 ~ 800 DEG C of roastings 1 ~ 3 hour, namely the nucleocapsid structure magnetic loaded type photochemical catalyst that particle diameter is 1 ~ 9um is obtained.
(3) nucleocapsid structure magnetic loaded type photochemical catalyst is placed in is equipped with in the open glass container of coal gas waste, lucifuge mechanical agitation 30 ~ 60 minutes, form the suspension of catalyst quality concentration 1 ~ 5g/L;
(4) under the glass container filling suspension being placed in sunshine together with mechanical agitator, prolonged exposure also constantly stirs, and irradiation time overall length is 5 ~ 15 hours;
(5), after detection ammonia nitrogen in solution, COD, phenol and other organic component contents reaches municipal sewage secondary discharge standard, stop reaction, and reclaim catalyst with magnet.
and further illustrated by following examples:
Embodiment 1:
(1) be that the nickel ferrite based magnetic loaded powder of 1 ~ 5um is placed in reaction vessel by particle diameter, add water and the suspension of mechanical agitation formation 200g/L, under mechanical stirring, be that the aluminum ammonium sulfate solution of 0.4mol/L and the ammonium bicarbonate soln of 1.6mol/L pass in suspension with the speed of 10mL/min respectively simultaneously by concentration, start precipitation reaction, controlling solution ph with carbonic hydroammonium is stabilized between 7.5 ~ 8, the alum total amount added is scaled aluminium oxide and nickel ferrite based magnetic loaded mass ratio is 2:1, after reinforced end, obtain the suspension of alumina-coated nickel ferrite based magnetic loaded presoma.
(2) continue in suspension, to pass into the titanium sulfate solution of 0.1mol/L and the ammonium bicarbonate soln of 0.4mol/L with the charging rate of 10mL/min simultaneously, mechanical agitation, make titanium ion precipitated crystal on suspended particulate, form integument, controlling solution ph with carbonic hydroammonium is stabilized between 7 ~ 8, the titanium sulfate total amount added is scaled titanium dioxide and nickel ferrite based magnetic loaded mass ratio is 0.2:1, to be fed complete after, at room temperature continue to react half an hour more than, sediment is filtered, washing, in atmosphere in 80 DEG C of dryings after 10 hours, in 800 DEG C of roastings 1 hour, namely nucleocapsid structure magnetic loaded type photochemical catalyst is obtained.
(3) 2g photochemical catalyst is placed in is equipped with in the open glass container of 1L coal gas waste, lucifuge mechanical agitation 30 minutes, form the suspension of catalyst quality concentration 2g/L.
(3) under the glass container filling suspension being placed in sunshine together with mechanical agitator, prolonged exposure also constantly stirs, and irradiation time overall length is 5 hours.
(4) detect ammonia nitrogen in solution, COD, phenol and other organic component contents, stop reaction, and reclaim catalyst with magnet.
Fig. 1 is TiO 2/ Al 2o 3/ NiFe 2o 4the microphotograph of catalyst, Fig. 2 is the XRD result of photochemical catalyst and carrier, and Fig. 3 is the VSM result of photochemical catalyst, and Fig. 4 is degradation and decolorization change photo, and table 1 is that coal gas waste is degraded front and back Substances variation table.
Found out by the above results: TiO 2/ Al 2o 3/ NiFe 2o 4there is obvious nucleocapsid structure, particle diameter at 3 ~ 7um, good dispersion; XRD result display light catalyst shows obvious anatase TiO 2, γ-Al 2o 3and NiFe 2o 4three-phase; Magnetic property is good, and saturation magnetization has 31emu/g, and soft magnetism is strong; Found out by Fig. 4, the decolorizing effect of coal gas waste is obvious, and the coal gas waste index after table 1 data display light catalytic degradation reaches municipal sewage secondary discharge standard completely.
Embodiment 2:
(1) be that the cobalt ferrite powder of 0.5 ~ 1um is placed in reaction vessel by particle diameter, add water and the suspension of mechanical agitation formation 100g/L, under mechanical stirring, be that the aluminum ammonium sulfate solution of 0.3mol/L and the ammonium bicarbonate soln of 1.2mol/L pass in suspension with the speed of 15mL/min respectively simultaneously by concentration, start precipitation reaction, controlling solution ph with carbonic hydroammonium is stabilized between 7.0 ~ 8, the alum total amount added is scaled aluminium oxide and cobalt ferrite mass ratio is 1:1, after reinforced end, obtain the suspension of alumina-coated cobalt ferrite presoma.
(2) continue in suspension, to pass into the titanium sulfate solution of 0.2mol/L and the ammonium bicarbonate soln of 0.8mol/L with the charging rate of 15mL/min simultaneously, mechanical agitation, make titanium ion precipitated crystal on suspended particulate, form integument, controlling solution ph with carbonic hydroammonium is stabilized between 7 ~ 8, the titanium sulfate total amount added is scaled titanium dioxide and cobalt ferrite mass ratio is 0.1:1, to be fed complete after, at room temperature continue to react half an hour more than, sediment is filtered, washing, in atmosphere in 80 DEG C of dryings after 10 hours, in 700 DEG C of roastings 3 hours, namely nucleocapsid structure magnetic loaded type photochemical catalyst is obtained.
(3) 5g photochemical catalyst is placed in is equipped with in the open glass container of 5L coal gas waste, lucifuge mechanical agitation 60 minutes, form the suspension of catalyst quality concentration 1g/L.
(3) under the glass container filling suspension being placed in sunshine together with mechanical agitator, prolonged exposure also constantly stirs, and irradiation time overall length is 10 hours.
(4) stop reaction, detect ammonia nitrogen in solution, COD, phenol and other organic component contents, and reclaim catalyst with magnet.
TiO 2/ Al 2o 3/ CoFe 2o 4there is obvious nucleocapsid structure, particle diameter at 1 ~ 2um, good dispersion; This powder magnetic can be good, has very strong visible absorption, and the decolorizing effect of coal gas waste is obvious, and effluent index, as table 1, reaches municipal sewage secondary discharge standard completely.
Embodiment 3:
(1) by particle diameter be 1 ~ 5um Manganese Ferrite powder in mass ratio 1:1 be placed in reaction vessel, to add water and mechanical agitation forms the suspension of 500g/L.Under mechanical stirring, be that the aluminum ammonium sulfate solution of 0.2mol/L and the ammonium bicarbonate soln of 0.8mol/L pass in suspension with the speed of 20mL/min respectively simultaneously by concentration, start precipitation reaction, controlling solution ph with carbonic hydroammonium is stabilized between 7.5 ~ 8, the alum total amount added is scaled aluminium oxide and Manganese Ferrite mass ratio is 3:1, after reinforced end, obtain the suspension of alumina-coated Manganese Ferrite presoma.
(2) continue in suspension, to pass into the titanium sulfate solution of 0.25mol/L and the ammonium bicarbonate soln of 1.0mol/L with the charging rate of 20mL/min, mechanical agitation simultaneously, make titanium ion precipitated crystal on suspended particulate, form integument.Control solution ph with carbonic hydroammonium to be stabilized between 7 ~ 8.The titanium sulfate total amount added is scaled titanium dioxide and Manganese Ferrite mass ratio is 0.5:1.To be fed complete after, at room temperature continue reaction half an hour more than, by sediment filter, washing, after 12 hours, in 800 DEG C of roastings 2 hours, namely obtain nucleocapsid structure magnetic loaded type photochemical catalyst in 60 DEG C of dryings in atmosphere.
(3) 10g photochemical catalyst is placed in is equipped with in the open glass container of 2L coal gas waste, lucifuge mechanical agitation 50 minutes, form the suspension of catalyst quality concentration 5g/L.
(3) under the glass container filling suspension being placed in sunshine together with mechanical agitator, prolonged exposure also constantly stirs, and irradiation time overall length is 15 hours.
(4) stop reaction, detect ammonia nitrogen in solution, COD, phenol and other organic component contents, and reclaim catalyst with magnet.
TiO 2/ Al 2o 3/ MnFe 2o 4catalyst has obvious nucleocapsid structure, particle diameter at 4 ~ 9um, good dispersion; This powder magnetic can be good, has very strong visible absorption, and the decolorizing effect of coal gas waste is obvious, and effluent index, as table 1, reaches municipal sewage secondary discharge standard completely.
Table 1

Claims (3)

1. a magnetic loaded type photochemical catalyst, is characterized in that: described photochemical catalyst is with NiFe 2o 4, CoFe 2o 4, MnFe 2o 4, BaFe 2o 4one in ferrite powder is core, is intermediate layer with gamma-alumina, take nano titanium oxide as shell, and gamma-alumina and ferritic mass ratio are 1 ~ 3:1, and titanium dioxide and ferritic mass ratio are 0.1 ~ 0.5:1, and the particle diameter of photochemical catalyst is 1 ~ 9um.
describedmagnetic loaded type photochemical catalyst adopts following preparation method:
Be that the ferrite powder of 0.5 ~ 5um is placed in reaction vessel by particle diameter, add water and mechanical agitation forms the suspension of 100 ~ 500g/L;
Under mechanical stirring, be that the aluminum ammonium sulfate solution of 0.2 ~ 0.4mol/L and the ammonium bicarbonate soln of 0.8 ~ 1.6mol/L instill in suspension with the speed of 10 ~ 20mL/min respectively simultaneously by concentration, start precipitation reaction, controlling solution ph with carbonic hydroammonium is stabilized between 7 ~ 8, the alum total amount added is scaled aluminium oxide and ferritic mass ratio is 1 ~ 3:1, after reinforced end, obtain the suspension of alumina-coated ferrite presoma;
Continue in suspension, to instill the titanium sulfate solution of 0.1 ~ 0.25mol/L and the ammonium bicarbonate soln of 0.4 ~ 1.0mol/L with the speed of 10 ~ 20mL/min simultaneously, mechanical agitation, make titanium ion precipitated crystal on suspended particulate, form integument, controlling solution ph with carbonic hydroammonium is stabilized between 7 ~ 8, the titanium sulfate total amount added is scaled titanium dioxide and ferritic mass ratio is 0.1 ~ 0.5:1, to be fed complete after, at room temperature continue to react half an hour, sediment is filtered, washing, in atmosphere in 60 ~ 80 DEG C of dryings after 10 ~ 12 hours, in 700 ~ 800 DEG C of roastings 1 ~ 3 hour, namely described magnetic loaded type photochemical catalyst is obtained.
2. a kind of magnetic loaded type photochemical catalyst as claimed in claim 1 is in the purposes of gas treatment waste water, it is characterized in that comprising following concrete steps:
Being placed in by magnetic loaded type photochemical catalyst is equipped with in the open glass container of coal gas waste, lucifuge mechanical agitation 30 ~ 60 minutes, forms the suspension of catalyst quality concentration 1 ~ 5g/L;
Under the glass container filling suspension is placed in sunshine together with mechanical agitator, prolonged exposure also constantly stirs, and irradiation time is 5 ~ 15 hours;
After detection ammonia nitrogen in solution, COD, phenol and other organic component contents reach sewage drainage standard, stop reaction, and reclaim catalyst with magnet.
3. a kind of magnetic loaded type photochemical catalyst as claimed in claim 2 is in the purposes of gas treatment waste water, it is characterized in that: described coal gas waste is through the pretreated coal gas waste of the ammonium magnesium phosphate precipitation method, ammonia-nitrogen content reduces by 70 ~ 80%, and other component content is constant.
CN201210511134.0A 2012-12-04 2012-12-04 Magnetic photocatalyst used for gas waste water treatment and preparation method thereof Expired - Fee Related CN103143362B (en)

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