CN112138675A - Composite magnetic photocatalyst for treating printing and dyeing discharge liquid and preparation method thereof - Google Patents
Composite magnetic photocatalyst for treating printing and dyeing discharge liquid and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 41
- 238000004043 dyeing Methods 0.000 title claims abstract description 28
- 239000007788 liquid Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 54
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 38
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000001035 drying Methods 0.000 claims abstract description 36
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000004005 microsphere Substances 0.000 claims abstract description 22
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 20
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000007790 solid phase Substances 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 20
- HVENHVMWDAPFTH-UHFFFAOYSA-N iron(3+) trinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HVENHVMWDAPFTH-UHFFFAOYSA-N 0.000 claims abstract description 18
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- 238000003837 high-temperature calcination Methods 0.000 claims description 17
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 14
- 239000002077 nanosphere Substances 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 24
- 239000010865 sewage Substances 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 9
- 239000003344 environmental pollutant Substances 0.000 abstract description 8
- 231100000719 pollutant Toxicity 0.000 abstract description 8
- 229910052797 bismuth Inorganic materials 0.000 abstract description 7
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 7
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000696 magnetic material Substances 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 238000001354 calcination Methods 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 11
- 238000006731 degradation reaction Methods 0.000 description 11
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 9
- 229940043267 rhodamine b Drugs 0.000 description 9
- 230000001699 photocatalysis Effects 0.000 description 8
- 229910000416 bismuth oxide Inorganic materials 0.000 description 5
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 5
- 229920001661 Chitosan Polymers 0.000 description 4
- 239000002202 Polyethylene glycol Substances 0.000 description 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910002900 Bi2MoO6 Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000000017 hydrogel Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000006249 magnetic particle Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
-
- 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
- B01J35/33—Electric or magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
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- Hydrology & Water Resources (AREA)
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Abstract
The invention relates to the field of sewage treatment, and discloses a composite magnetic photocatalyst for treating printing and dyeing discharge liquid and a preparation method thereof. The preparation method comprises the following preparation processes: (1) mixing ferric nitrate hexahydrate, nickel nitrate hexahydrate, citric acid, glycerol and isopropanol, carrying out hydrothermal reaction, and calcining a solid phase at high temperature to obtain porous nickel ferrite nano microspheres; (2) and adding the nano-microspheres into a sodium tungstate and bismuth nitrate aqueous solution, performing hydrothermal reaction, centrifuging, washing and drying to obtain the composite magnetic photocatalyst for treating printing and dyeing effluent. According to the composite material prepared by the invention, the bismuth tungstate nanometer material grows on the porous nickel ferrite nanometer microsphere, so that the obtained composite magnetic catalyst is uniform in appearance, large in specific surface area and excellent in adsorption performance, and meanwhile, the catalyst is firmly combined with the magnetic material, has a good photocatalytic degradation effect on pollutants in sewage, is convenient to recycle, is simple in preparation process, can be produced in a large scale, and has a wide application prospect.
Description
Technical Field
The invention relates to the field of sewage treatment, and discloses a composite magnetic photocatalyst for treating printing and dyeing discharge liquid and a preparation method thereof.
Background
Industrial wastewater contains a large amount of pollutants such as heavy metal ions, organic dyes and the like, and the treatment mode thereof is a research hotspot in recent years. Compared with the traditional treatment modes such as electrodeposition, filtration and the like, the physical adsorption has the advantages of low cost, simplicity in operation, no secondary pollution and the like. However, the traditional adsorbing materials including activated carbon, wood chips, coal slag, volcanic ash and the like generally have the defects of low adsorption efficiency, poor selective adsorption, difficult recovery and the like.
In recent years, researches show that the porous structure inside the hydrogel endows the hydrogel with a huge specific surface area, and can provide a large number of attachment sites for pollutant adsorption. Therefore, the recognition of a good contaminant adsorbent material is being relied upon by numerous researchers. The ideal adsorbent for removing heavy metal ions, organic pollutants, dyes and the like in the polluted water body, which has the advantages of high adsorption efficiency, high adsorption speed, large adsorption capacity, low price and easy recovery, becomes very important.
The current important research direction is that the preparation process of the novel sewage adsorption material is simple and effective, the particle has excellent characteristics of micron/nanometer, porosity, large specific surface area and the like, and particularly the adsorption material and the precious metal ions can be quickly separated under the action of an external magnetic field, so that the adsorption material and the precious metal ions can be recovered and recycled. Under the visible light response, bismuth tungstate can effectively degrade organic dye wastewater, so that bismuth tungstate has very important practical value in the fields of degradation of organic pollutants and sewage treatment.
The Chinese invention patent application No. 201611037394.3 discloses a magnetic photocatalytic nanocomposite material adopting bismuth oxide and nickel ferrite and a preparation method thereof, the magnetic photocatalytic nanocomposite material adopting bismuth oxide and nickel ferrite mainly comprises bismuth oxide, nickel ferrite and ferroferric oxide, the bismuth oxide is in the form of nano powder, the nickel ferrite is in the form of nano powder, and the ferroferric oxide is in the form of nano powder; due to the existence of silver, the photocatalytic composite material realizes the catalytic degradation of organic pollutants under the excitation of visible light, the application range of the photocatalytic composite material is expanded, meanwhile, bismuth oxide and nickel ferrite are combined to form a heterojunction, the light energy utilization region is expanded to a visible light region, and the matched energy band structure is favorable for the separation of photoproduction electrons and holes, so that the photocatalytic degradation efficiency is improved.
The Chinese patent application No. 201711237202.8 discloses a magnetic sewage treatment agent, which comprises the following components in parts by weight: 30-50 parts of ferroferric oxide nano magnetic particles, 30-50 parts of polyethylene glycol chitosan graft and Bi2MoO61-5 parts of a catalyst and 10-25 parts of a dispersing agent; wherein polyethylene glycol chitosan graft is coated on the surface of ferroferric oxide nano magnetic particles, and Bi2MoO6The catalyst is loaded on the polyethylene glycol chitosan grafting material, and the grafting molar ratio of the polyethylene glycol to the chitosan is 1: 1. The sewage treatment agent can degrade pollutants in a water body only by sunlight, has high solar energy utilization rate and strong activity, can effectively reduce the content of the pollutants in the water body, has magnetism, is easy to recover after being used, has good water solubility, strong adsorption capacity and simple process, can be repeatedly utilized to reduce the cost, and is suitable for practical production and application.
According to the above, the composite magnetic material for sewage treatment in the existing scheme often has the problems of low specific surface area, poor pollutant treatment effect and the like, and restricts the further application of the composite magnetic material in the field of sewage treatment.
Disclosure of Invention
The prior composite photocatalytic magnetic material which is widely applied and used for sewage treatment generally has the problems of low specific surface area, weak adsorption capacity, poor pollutant treatment effect and the like.
In order to solve the problems, the invention adopts the following technical scheme:
a preparation method of a composite magnetic photocatalyst for treating printing and dyeing discharge liquid comprises the following specific steps:
(1) uniformly mixing ferric nitrate hexahydrate, nickel nitrate hexahydrate, glycerol and isopropanol under an ultrasonic condition, adding citric acid, carrying out hydrothermal reaction, centrifugally washing after the reaction is finished, drying a solid phase, and then carrying out high-temperature calcination under an air atmosphere to prepare the porous nickel ferrite nanospheres;
(2) dispersing sodium tungstate and bismuth nitrate in deionized water under an ultrasonic condition, then adding the porous nickel ferrite nano microspheres prepared in the step (1), performing hydrothermal reaction after uniform dispersion, centrifugally washing after the reaction is finished, and drying a solid phase to prepare the composite magnetic photocatalyst for treating printing and dyeing discharge liquid.
Preferably, the raw materials in the step (1) comprise the following components in parts by weight: 15-20 parts of ferric nitrate hexahydrate, 15-20 parts of nickel nitrate hexahydrate, 20-30 parts of glycerol, 20-45 parts of isopropanol and 5-10 parts of citric acid.
Preferably, the ultrasonic frequency of the ultrasonic dispersion in the step (1) is 50-100 kHz, and the treatment time is 15-30 min.
Preferably, the temperature of the hydrothermal reaction in the step (1) is 180-200 ℃ and the time is 3-5 h.
Preferably, the high-temperature calcination in the step (1) is carried out at 500-600 ℃ for 1-2 h.
Preferably, the weight parts of the raw materials in the step (2) are as follows: 18-22 parts of sodium tungstate, 18-22 parts of bismuth nitrate, 46-59 parts of deionized water and 5-10 parts of porous nickel ferrite nano microspheres.
Preferably, the ultrasonic frequency of the ultrasonic dispersion in the step (2) is 30-60 kHz, and the power is 100-200W.
Preferably, the temperature of the hydrothermal reaction in the step (2) is 140-160 ℃, and the time is 6-8 h.
Preferably, the drying temperature in the step (2) is 60-80 ℃, and the time is 12-18 h.
The composite magnetic photocatalyst for treating printing and dyeing effluent prepared by the method is prepared by mixing ferric nitrate hexahydrate, nickel nitrate hexahydrate, glycerol and isopropanol under an ultrasonic condition, adding citric acid, carrying out hydrothermal reaction, centrifugally washing after the reaction is finished, drying a solid phase, and then carrying out high-temperature calcination under the protection of air atmosphere to obtain porous nickel ferrite nanospheres; and dispersing sodium tungstate and bismuth nitrate in deionized water under an ultrasonic condition, adding porous nickel ferrite nano microspheres, performing hydrothermal reaction after uniform dispersion, centrifugally washing after the reaction is finished, taking a solid phase, and drying.
Compared with the prior art, the invention provides the composite magnetic photocatalyst for treating the printing and dyeing discharge liquid and the preparation method thereof, and the outstanding characteristics and excellent effects are as follows:
1. provides a method for preparing a composite magnetic photocatalyst for treating printing and dyeing discharge liquid by growing bismuth tungstate on porous nickel ferrite nano microspheres.
2. By growing the bismuth tungstate nano material on the porous nickel ferrite nano microsphere, the prepared composite magnetic material has the advantages of uniform appearance, large specific surface area and excellent adsorption performance.
3. In the composite magnetic photocatalyst prepared by the invention, the catalyst is firmly combined with a magnetic material, the good photocatalytic activity of bismuth tungstate can be effectively exerted, the composite magnetic photocatalyst has good degradation effect on pollutants in sewage, and meanwhile, the composite magnetic photocatalyst is convenient to recycle.
4. The method has simple preparation process, can be used for mass production, and has wide application prospect.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
(1) Uniformly mixing ferric nitrate hexahydrate, nickel nitrate hexahydrate, glycerol and isopropanol under an ultrasonic condition, adding citric acid, carrying out hydrothermal reaction, centrifugally washing after the reaction is finished, drying a solid phase, and then carrying out high-temperature calcination under an air atmosphere to prepare the porous nickel ferrite nanospheres; the ultrasonic frequency of ultrasonic dispersion is 60kHz, and the processing time is 26 min; the temperature of the hydrothermal reaction is 185 ℃, and the time is 4.5 h; the high-temperature calcination is carried out at the temperature of 550 ℃ for 1 h;
wherein: 16 parts of ferric nitrate hexahydrate, 16 parts of nickel nitrate hexahydrate, 22 parts of glycerol, 40 parts of isopropanol and 6 parts of citric acid;
(2) dispersing sodium tungstate and bismuth nitrate in deionized water under an ultrasonic condition, then adding the porous nickel ferrite nano microspheres prepared in the step (1), performing hydrothermal reaction after uniform dispersion, centrifugally washing after the reaction is finished, and drying a solid phase to prepare a composite magnetic photocatalyst for treating printing and dyeing discharge liquid; the ultrasonic frequency of ultrasonic dispersion is 40kHz, and the power is 120W; the temperature of the hydrothermal reaction is 145 ℃, and the time is 7.5 h; the drying temperature is 65 ℃ and the drying time is 17 h;
wherein: 19 parts of sodium tungstate, 19 parts of bismuth nitrate, 55 parts of deionized water and 7 parts of porous nickel ferrite nano microspheres.
The specific surface area, rhodamine B adsorption amount, and degradation rate of the composite magnetic photocatalyst prepared in example 1 are shown in table 1.
Example 2
(1) Uniformly mixing ferric nitrate hexahydrate, nickel nitrate hexahydrate, glycerol and isopropanol under an ultrasonic condition, adding citric acid, carrying out hydrothermal reaction, centrifugally washing after the reaction is finished, drying a solid phase, and then carrying out high-temperature calcination under an air atmosphere to prepare the porous nickel ferrite nanospheres; the ultrasonic frequency of ultrasonic dispersion is 90kHz, and the processing time is 18 min; the temperature of the hydrothermal reaction is 195 ℃ and the time is 3.5 h; the high-temperature calcination temperature is 550 ℃, and the time is 1.5 h;
wherein: 19 parts of ferric nitrate hexahydrate, 19 parts of nickel nitrate hexahydrate, 27 parts of glycerol, 26 parts of isopropanol and 9 parts of citric acid;
(2) dispersing sodium tungstate and bismuth nitrate in deionized water under an ultrasonic condition, then adding the porous nickel ferrite nano microspheres prepared in the step (1), performing hydrothermal reaction after uniform dispersion, centrifugally washing after the reaction is finished, and drying a solid phase to prepare a composite magnetic photocatalyst for treating printing and dyeing discharge liquid; the ultrasonic frequency of ultrasonic dispersion is 50kHz, and the power is 180W; the temperature of the hydrothermal reaction is 155 ℃, and the time is 6.5 h; the drying temperature is 75 ℃, and the drying time is 14 h;
wherein: 21 parts of sodium tungstate, 21 parts of bismuth nitrate, 50 parts of deionized water and 8 parts of porous nickel ferrite nano microspheres.
The specific surface area, rhodamine B adsorption amount, and degradation rate of the composite magnetic photocatalyst prepared in example 2 are shown in table 1.
Example 3
(1) Uniformly mixing ferric nitrate hexahydrate, nickel nitrate hexahydrate, glycerol and isopropanol under an ultrasonic condition, adding citric acid, carrying out hydrothermal reaction, centrifugally washing after the reaction is finished, drying a solid phase, and then carrying out high-temperature calcination under an air atmosphere to prepare the porous nickel ferrite nanospheres; the ultrasonic frequency of ultrasonic dispersion is 70kHz, and the processing time is 17 min; the temperature of the hydrothermal reaction is 188 ℃, and the time is 4 h; the high-temperature calcination temperature is 580 ℃, and the time is 1 h;
wherein: 17 parts of ferric nitrate hexahydrate, 17 parts of nickel nitrate hexahydrate, 24 parts of glycerol, 33 parts of isopropanol and 7 parts of citric acid;
(2) dispersing sodium tungstate and bismuth nitrate in deionized water under an ultrasonic condition, then adding the porous nickel ferrite nano microspheres prepared in the step (1), performing hydrothermal reaction after uniform dispersion, centrifugally washing after the reaction is finished, and drying a solid phase to prepare a composite magnetic photocatalyst for treating printing and dyeing discharge liquid; the ultrasonic frequency of ultrasonic dispersion is 50kHz, and the power is 160W; the temperature of the hydrothermal reaction is 148 ℃ and the time is 7 h; the drying temperature is 68 ℃ and the drying time is 14 h;
wherein: 19 parts of sodium tungstate, 20 parts of bismuth nitrate, 54 parts of deionized water and 7 parts of porous nickel ferrite nano microspheres.
The specific surface area, the rhodamine B adsorption amount, and the degradation rate of the composite magnetic photocatalyst prepared in example 3 are shown in table 1.
Example 4
(1) Uniformly mixing ferric nitrate hexahydrate, nickel nitrate hexahydrate, glycerol and isopropanol under an ultrasonic condition, adding citric acid, carrying out hydrothermal reaction, centrifugally washing after the reaction is finished, drying a solid phase, and then carrying out high-temperature calcination under an air atmosphere to prepare the porous nickel ferrite nanospheres; the ultrasonic frequency of ultrasonic dispersion is 50kHz, and the processing time is 30 min; the temperature of the hydrothermal reaction is 180 ℃ and the time is 5 h; the high-temperature calcination temperature is 500 ℃, and the time is 2 hours;
wherein: 15 parts of ferric nitrate hexahydrate, 15 parts of nickel nitrate hexahydrate, 20 parts of glycerol, 45 parts of isopropanol and 5 parts of citric acid;
(2) dispersing sodium tungstate and bismuth nitrate in deionized water under an ultrasonic condition, then adding the porous nickel ferrite nano microspheres prepared in the step (1), performing hydrothermal reaction after uniform dispersion, centrifugally washing after the reaction is finished, and drying a solid phase to prepare a composite magnetic photocatalyst for treating printing and dyeing discharge liquid; the ultrasonic frequency of ultrasonic dispersion is 30kHz, and the power is 100W; the temperature of the hydrothermal reaction is 140 ℃ and the time is 8 h; the drying temperature is 60 ℃, and the drying time is 18 h;
wherein: 18 parts of sodium tungstate, 18 parts of bismuth nitrate, 59 parts of deionized water and 5 parts of porous nickel ferrite nano microspheres.
The specific surface area, the rhodamine B adsorption amount, and the degradation rate of the composite magnetic photocatalyst prepared in example 4 are shown in table 1.
Example 5
(1) Uniformly mixing ferric nitrate hexahydrate, nickel nitrate hexahydrate, glycerol and isopropanol under an ultrasonic condition, adding citric acid, carrying out hydrothermal reaction, centrifugally washing after the reaction is finished, drying a solid phase, and then carrying out high-temperature calcination under an air atmosphere to prepare the porous nickel ferrite nanospheres; the ultrasonic frequency of ultrasonic dispersion is 50kHz, and the processing time is 30 min; the temperature of the hydrothermal reaction is 200 ℃ and the time is 3 h; the high-temperature calcination temperature is 500 ℃, and the time is 1.5 h;
wherein: 20 parts of ferric nitrate hexahydrate, 20 parts of nickel nitrate hexahydrate, 30 parts of glycerol, 20 parts of isopropanol and 10 parts of citric acid;
(2) dispersing sodium tungstate and bismuth nitrate in deionized water under an ultrasonic condition, then adding the porous nickel ferrite nano microspheres prepared in the step (1), performing hydrothermal reaction after uniform dispersion, centrifugally washing after the reaction is finished, and drying a solid phase to prepare a composite magnetic photocatalyst for treating printing and dyeing discharge liquid; the ultrasonic frequency of ultrasonic dispersion is 60kHz, and the power is 200W; the temperature of the hydrothermal reaction is 160 ℃, and the time is 6 h; the drying temperature is 80 ℃, and the drying time is 12 hours;
wherein: 22 parts of sodium tungstate, 22 parts of bismuth nitrate, 46 parts of deionized water and 10 parts of porous nickel ferrite nano microspheres.
The specific surface area, the rhodamine B adsorption amount, and the degradation rate of the composite magnetic photocatalyst prepared in example 5 are shown in table 1.
Example 6
(1) Uniformly mixing ferric nitrate hexahydrate, nickel nitrate hexahydrate, glycerol and isopropanol under an ultrasonic condition, adding citric acid, carrying out hydrothermal reaction, centrifugally washing after the reaction is finished, drying a solid phase, and then carrying out high-temperature calcination under an air atmosphere to prepare the porous nickel ferrite nanospheres; the ultrasonic frequency of ultrasonic dispersion is 80kHz, and the processing time is 22 min; the temperature of the hydrothermal reaction is 200 ℃ and the time is 4 h; the high-temperature calcination is carried out at the temperature of 600 ℃ for 1 h;
wherein: 18 parts of ferric nitrate hexahydrate, 12 parts of nickel nitrate hexahydrate, 25 parts of glycerol, 32 parts of isopropanol and 8 parts of citric acid;
(2) dispersing sodium tungstate and bismuth nitrate in deionized water under an ultrasonic condition, then adding the porous nickel ferrite nano microspheres prepared in the step (1), performing hydrothermal reaction after uniform dispersion, centrifugally washing after the reaction is finished, and drying a solid phase to prepare a composite magnetic photocatalyst for treating printing and dyeing discharge liquid; the ultrasonic frequency of ultrasonic dispersion is 45kHz, and the power is 150W; the temperature of the hydrothermal reaction is 150 ℃ and the time is 7 h; the drying temperature is 70 ℃, and the drying time is 15 h;
wherein: 20 parts of sodium tungstate, 20 parts of bismuth nitrate, 52 parts of deionized water and 8 parts of porous nickel ferrite nano microspheres.
The specific surface area, the rhodamine B adsorption amount, and the degradation rate of the composite magnetic photocatalyst prepared in example 6 are shown in table 1.
Comparative example 1
Dispersing sodium tungstate and bismuth nitrate in deionized water under an ultrasonic condition, carrying out hydrothermal reaction, centrifugally washing after the reaction is finished, and drying a solid phase to obtain a photocatalyst for treating printing and dyeing wastewater; the ultrasonic frequency of ultrasonic dispersion is 40kHz, and the power is 120W; the temperature of the hydrothermal reaction is 145 ℃, and the time is 7.5 h; the drying temperature is 65 ℃ and the drying time is 17 h;
wherein: 19 parts of sodium tungstate, 19 parts of bismuth nitrate and 55 parts of deionized water.
Comparative example 1 no porous nickel ferrite nanosphere was added to prepare a single bismuth tungstate photocatalyst, and the specific surface area, rhodamine B adsorption amount and degradation rate of the prepared photocatalyst are shown in table 1.
The performance index testing method comprises the following steps:
specific surface area: the photocatalysts prepared in examples 1-6 and comparative example 1 were tested for specific surface area according to GB/T19587-.
The adsorption rate and the degradation rate of rhodamine B are as follows: the photocatalytic experiments were carried out in a home-made double-layer photocatalytic reactor made of quartz glass. Flowing water through the interlayer to cool the reactor, and keeping the temperature of the reactor at room temperature; mixing 100mL of 20mg/L rhodamine B solution and 0.5g of photocatalyst, then pouring the mixture into a reactor, placing the suspension in a dark place, strongly stirring for 30min, testing the adsorption rate by adopting a spectrophotometry after adsorption balance, irradiating the suspension for a certain time by using a 1000W xenon lamp, measuring the absorbance of the suspension at the maximum absorption wavelength by using a spectrophotometer, and calculating the removal rate according to the change of the absorbance before and after the illumination: r = (A)0-A）/A0X 100%, the test time is respectively 30min, 60min and 120min and 180 min.
Table 1:
Claims (10)
1. a preparation method of a composite magnetic photocatalyst for treating printing and dyeing discharge liquid is characterized by comprising the following specific steps:
(1) uniformly mixing ferric nitrate hexahydrate, nickel nitrate hexahydrate, glycerol and isopropanol under an ultrasonic condition, adding citric acid, carrying out hydrothermal reaction, centrifugally washing after the reaction is finished, drying a solid phase, and then carrying out high-temperature calcination under an air atmosphere to prepare the porous nickel ferrite nanospheres;
(2) dispersing sodium tungstate and bismuth nitrate in deionized water under an ultrasonic condition, then adding the porous nickel ferrite nano microspheres prepared in the step (1), performing hydrothermal reaction after uniform dispersion, centrifugally washing after the reaction is finished, and drying a solid phase to prepare the composite magnetic photocatalyst for treating printing and dyeing discharge liquid.
2. The method for preparing the composite magnetic photocatalyst for treating printing and dyeing discharged liquid according to claim 1, characterized in that: the weight parts of the raw materials in the step (1) are as follows: 15-20 parts of ferric nitrate hexahydrate, 15-20 parts of nickel nitrate hexahydrate, 20-30 parts of glycerol, 20-45 parts of isopropanol and 5-10 parts of citric acid.
3. The method for preparing the composite magnetic photocatalyst for treating printing and dyeing discharged liquid according to claim 1, characterized in that: the ultrasonic frequency of the ultrasonic dispersion in the step (1) is 50-100 kHz, and the processing time is 15-30 min.
4. The method for preparing the composite magnetic photocatalyst for treating printing and dyeing discharged liquid according to claim 1, characterized in that: the temperature of the hydrothermal reaction in the step (1) is 180-200 ℃, and the time is 3-5 h.
5. The method for preparing the composite magnetic photocatalyst for treating printing and dyeing discharged liquid according to claim 1, characterized in that: the high-temperature calcination in the step (1) is carried out at the temperature of 500-600 ℃ for 1-2 h.
6. The method for preparing the composite magnetic photocatalyst for treating printing and dyeing discharged liquid according to claim 1, characterized in that: the weight parts of the raw materials in the step (2) are as follows: 18-22 parts of sodium tungstate, 18-22 parts of bismuth nitrate, 46-59 parts of deionized water and 5-10 parts of porous nickel ferrite nano microspheres.
7. The method for preparing the composite magnetic photocatalyst for treating printing and dyeing discharged liquid according to claim 1, characterized in that: and (3) the ultrasonic frequency of the ultrasonic dispersion in the step (2) is 30-60 kHz, and the power is 100-200W.
8. The method for preparing the composite magnetic photocatalyst for treating printing and dyeing discharged liquid according to claim 1, characterized in that: the temperature of the hydrothermal reaction in the step (2) is 140-160 ℃, and the time is 6-8 h.
9. The method for preparing the composite magnetic photocatalyst for treating printing and dyeing discharged liquid according to claim 1, characterized in that: and (3) drying at the temperature of 60-80 ℃ for 12-18 h.
10. A composite magnetic photocatalyst for treating a printing and dyeing effluent, prepared by the method of any one of claims 1 to 9.
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