CN102145293A - Soft magnetic composite photocatalyst and preparation method thereof - Google Patents
Soft magnetic composite photocatalyst and preparation method thereof Download PDFInfo
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- CN102145293A CN102145293A CN 201110053927 CN201110053927A CN102145293A CN 102145293 A CN102145293 A CN 102145293A CN 201110053927 CN201110053927 CN 201110053927 CN 201110053927 A CN201110053927 A CN 201110053927A CN 102145293 A CN102145293 A CN 102145293A
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- soft magnetism
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Abstract
The invention discloses a soft magnetic composite photocatalyst and a preparation method thereof, belonging to a sewage treatment technology and aiming to provide the soft magnetic composite photocatalyst easy to separate and recycle and the preparation method thereof. The technical scheme adopted by the invention comprises the following key point that granular active carbon is loaded with soft magnetic Mn0.5Zn0.5Fe2O4 and TiO2. The method for preparing the soft magnetic composite photocatalyst comprises the following steps of: (1) after manganese sulfate, zinc sulfate and green copperas are prepared into a mixed solution by ionized water, adding the granular active carbon into the mixed solution, uniformly stirring and reacting in a hydro-thermal reaction kettle, cooling, filtering, washing and drying a reaction product to obtain soft magnetic active carbon; and (2) preparing tetrabutyl titanate, absolute ethyl alcohol, nitric acid and water into a titanic acid solution, impregnating the soft magnetic active carbon into the titanic acid solution, carrying out stirring, standing, pumping filtration and drying on the impregnated soft magnetic active carbon, then calcining the obtained product in a muffle furnace in an inert atmosphere, and cooling the calcined product to the room temperature to form the soft magnetic composite photocatalyst. The soft magnetic composite photocatalyst is used for organic wastewater treatment.
Description
Technical field:
The present invention relates to a kind of sewage disposal technology, be specially adapted to a kind of soft magnetism composite photo-catalyst that contains the organic pollution wastewater treatment and preparation method thereof.
Background technology:
The conductor photocatalysis oxidation technology is a kind of heterogeneous high-level oxidation technology that develops rapidly in recent years, and it has caused concern widely in the research of handling organic wastewater and application facet.Wherein, nano-TiO
2Have resist chemical and photoetch, stable in properties, nontoxic, photocatalytic activity is high, reaction speed is fast, to organic degraded non-selectivity and easily make it advantages such as permineralization, non-secondary pollution, generally believed it is one of environmental type catalyst of tool application prospect.
The photochemical catalyst that general water treatment system uses all is powder TiO
2, there are the following problems: (1) TiO
2Organic pollutant degradation effect to high concentration is better, and very slow to the organic pollutant degradation speed of low concentration, this has also limited TiO greatly
2Application as photochemical catalyst.(2) TiO
2Powder has the trend of reunion, especially at TiO
2This trend was more obvious when concentration was higher, and the back photochemical catalyst specific area of reuniting declines to a great extent, and the photocatalysis effect also can descend thereupon.(3) because TiO
2Particle diameter is too little, causes its separation recovery and regeneration all very difficult, and this can cause the photochemical catalyst loss seriously, cost rising, TiO
2The advantage of the cheapness that has will not exist.Therefore, prepare nano level TiO
2Catalyst is also sought the appropriate catalyst carrier, is TiO
2The industrialized key of photocatalyst treatment waste water.Active carbon has flourishing pore structure, huge specific area, stable physicochemical properties and powerful absorption property, is a kind of more satisfactory catalyst carrier.It not only can be with TiO
2Thereby be scattered in its huge specific surface uniformly and avoid TiO
2Reunion, and can by to the suction-operated of pollutant to TiO
2Provide the high concentration environment to improve its photocatalytic activity.Yet the active carbon as carrier is micron-sized, though reduced TiO in the removal process to a certain extent
2Loss waste, but catalyst still needs isolated by filtration, this still will consume a large amount of manpower and materials.Simple for simplifying TiO
2The separation process of photochemical catalyst also has research with nano-TiO
2Directly be carried on the magnetic nanoparticle magnetic nanometer photocatalyst that forms nucleocapsid structure, can realize itself and the separating of processed water system easily by externally-applied magnetic field, thus enriching and recovering.But because the pore volume and the specific area of nano magnetic material are little, the load capacity of titanium is low, causes the photocatalytic activity of whole composite photo-catalyst to reduce.
Summary of the invention
The purpose of this invention is to provide a kind of soft magnetism composite photo-catalyst of a kind of photocatalytic activity height, easily separated recovery and preparation method thereof.Technical scheme of the present invention is that a kind of soft magnetism composite photo-catalyst comprises TiO
2, it is characterized in that: load has soft magnetism Mn on the granular activated carbon
0.5Zn
0.5Fe
2O
4And TiO
2It is characterized in that: Mn
2+: Zn
2+: Fe
2+Mol ratio be 1:1:4, granular activated carbon and described soft magnetism Mn
0.5Zn
0.5Fe
2O
4Mass ratio be 5-16:1, load Mn
0.5Zn
0.5Fe
2O
4Soft magnetism active carbon and TiO
2Mass ratio be 1.5-6:1.The method for preparing the soft magnetism composite photo-catalyst is characterized in that following steps are arranged: (1) is with manganese sulfate, zinc sulfate and ferrous sulfate Mn in molar ratio
2+: Zn
2+: Fe
2+=1:1:4 is made into mixed aqueous solution with deionized water, and making the metal ion total concentration is 0.1mol/L, drips NH after the stirring and dissolving
4OH, transferring PH is 9 ~ 11, adds granular activated carbon, moves to behind the stirring and evenly mixing in the hydrothermal reaction kettle, and maintenance is after 4-16 hour down at 160-200 ℃, and cooling is filtered, washing; Through the soft magnetism active carbon that 110 ℃ of dryings obtain having soft magnetism, the addition of described granular activated carbon is Mn
0.5Zn
0.5Fe
2O
4The 5-16 of quality doubly; (2) the above-mentioned soft magnetism active carbon of titanium sol impregnation that is configured to butyl titanate, absolute ethyl alcohol, nitric acid and water; stir; leave standstill; suction filtration; 110 ℃ of dryings are placed in the Muffle furnace; in inert atmosphere protection and 400-600 ℃ calcining 3 hours down, in 250 ℃ and air atmosphere, keep 3 hours, be cooled to room temperature, promptly obtain the soft magnetism composite photo-catalyst.It is characterized in that: described step (2) the above-mentioned soft magnetism active carbon of titanium sol impregnation; stir; leave standstill; suction filtration; 110 ℃ of drying processes repeat 2-3 time and are placed in the Muffle furnace, inert atmosphere protection and 400-600 ℃ of following the calcining 3 hours; in 250 ℃ and air atmosphere, keep 3 hours, be cooled to room temperature, promptly obtain the soft magnetism composite photo-catalyst.The present invention has following remarkable advantage compared with the prior art: 1, the organic pollution to high concentration and low concentration all has very high photocatalytic degradation activity.2, active carbon increases photocatalytic activity component TiO greatly
2Specific area, photocatalytic activity improves.3, external magnetic field separation and concentration photochemical catalyst is simplified separation process, and the reduction photochemical catalyst recycles the operating cost in the process.4, because abundant pore structure of active carbon and powerful absorption property, this soft magnetism composite photo-catalyst also can be used for handling the complicated waste water system that contains organic pollution and inorganic heavy metal ion simultaneously.5, method of the present invention is simple to operate, and is easy to control, and cost is low.
The specific embodiment:
The present invention has following examples:
Embodiment 1
(1) with manganese sulfate, zinc sulfate and ferrous sulfate Mn in molar ratio
2+: Zn
2+: Fe
2+=1:1:4 is made into mixed aqueous solution with deionized water, makes metal ion total concentration M
2+=0.1 mol/L stirs complete molten back and drips NH
4OH transfers PH to 9.Add and be equivalent to Mn in the above-mentioned system
0.5Zn
0.5Fe
2O
4The granular activated carbon that quality is 5 times continues stirring it is fully mixed, and is transferred to then in the hydrothermal reaction kettle, and 160 ℃ keep cooling after 8 hours, filtration, washing, 110 ℃ of dry soft magnetism active carbons that must have soft magnetism; (2) the 15ml butyl titanate dropwise adds in the 75ml absolute ethyl alcohol under magnetic agitation, drips off the back and stirs 5 minutes, and disposable then adding 2ml nitric acid stirred 5 minutes, dropwise added 8ml water, and then, continuation is stirred and obtained titanium colloidal sol half an hour.With this titanium colloidal sol 50ml dipping soft magnetism active carbon 5g, stir half an hour, leave standstill two and one-half-hours then, after suction filtration, washing again, the 110 ℃ of dryings, put into Muffle furnace, in inert atmosphere, be warming up to 600 ℃ and calcining at constant temperature 3 hours, kept 3 hours down in 250 ℃ of air atmospheres again, be cooled to room temperature, promptly get the soft magnetism composite photo-catalyst.Granular activated carbon/Mn wherein
0.5Zn
0.5Fe
2O
4Mass ratio be 5:1, soft magnetism active carbon/TiO
2Mass ratio be 6:1.
Embodiment 2
(1) with manganese sulfate, zinc sulfate and ferrous sulfate Mn in molar ratio
2+: Zn
2+: Fe
2+=1:1:4 is made into mixed aqueous solution with deionized water, makes metal ion total concentration M
2+=0.1 mol/L stirs complete molten back and drips NH
4OH transfers PH to 11.Add and be equivalent to Mn in the above-mentioned system
0.5Zn
0.5Fe
2O
4The granular activated carbon that quality is 16 times continues stirring it is fully mixed, and is transferred to then in the hydrothermal reaction kettle, and 180 ℃ keep cooling after 6 hours, filtration, washing, 110 ℃ of dry soft magnetism active carbons that must have soft magnetism; (2) the 15ml butyl titanate dropwise adds in the 75ml absolute ethyl alcohol under magnetic agitation, drips off the back and stirs 5 minutes, and disposable then adding 2ml nitric acid stirred 5 minutes, dropwise added 8ml water, and then, continuation is stirred and obtained titanium colloidal sol half an hour.With this titanium colloidal sol 50ml dipping soft magnetism active carbon 3g, stir half an hour, leave standstill two and one-half-hours then, after suction filtration, washing again, the 110 ℃ of dryings, again with same operation carry out titanium colloidal sol flood for the second time-stir-leave standstill-suction filtration-washing-drying after, put into Muffle furnace, in inert atmosphere, be warming up to 400 ℃ and calcining at constant temperature 3 hours, kept 3 hours down in 250 ℃ of air atmospheres again, be cooled to room temperature, promptly get the soft magnetism composite photo-catalyst.Granular activated carbon/Mn wherein
0.5Zn
0.5Fe
2O
4Mass ratio be 16:1, soft magnetism active carbon/TiO
2Mass ratio be 2.9:1.
Embodiment 3
(1) with manganese sulfate, zinc sulfate and ferrous sulfate Mn in molar ratio
2+: Zn
2+: Fe
2+=1:1:4 is made into mixed aqueous solution with deionized water, makes metal ion total concentration M
2+=0.1 mol/L stirs complete molten back and drips NH
4OH transfers PH to 10.Add and be equivalent to Mn in the above-mentioned system
0.5Zn
0.5Fe
2O
4The granular activated carbon that quality is 8 times continues stirring it is fully mixed, and is transferred to then in the hydrothermal reaction kettle, and 200 ℃ keep cooling after 4 hours, filtration, washing, 110 ℃ of dry soft magnetism active carbons that must have soft magnetism; (2) the 15ml butyl titanate dropwise adds in the 75ml absolute ethyl alcohol under magnetic agitation, drips off the back and stirs 5 minutes, and disposable then adding 2ml nitric acid stirred 5 minutes, dropwise added 8ml water, and then, continuation is stirred and obtained titanium colloidal sol half an hour.With this titanium colloidal sol 50ml dipping soft magnetism active carbon 3g, stir half an hour, leave standstill two and one-half-hours then, after suction filtration, washing again, the 110 ℃ of dryings, again with same operation carry out titanium colloidal sol for the second time, flood for the third time-stir-leave standstill-suction filtration-washing-drying after, put into Muffle furnace, in inert atmosphere, be warming up to 500 ℃ and calcining at constant temperature 3 hours, kept 3 hours down in 250 ℃ of air atmospheres again, be cooled to room temperature, promptly get the soft magnetism composite photo-catalyst.Granular activated carbon/Mn wherein
0.5Zn
0.5Fe
2O
4Mass ratio be 8:1, soft magnetism active carbon/TiO
2Mass ratio be 1.5:1.
Claims (4)
1. a soft magnetism composite photo-catalyst comprises TiO
2, it is characterized in that: load has soft magnetism Mn on the granular activated carbon
0.5Zn
0.5Fe
2O
4And TiO
2
2. a kind of soft magnetism composite photo-catalyst as claimed in claim 1 is characterized in that: Mn
2+: Zn
2+: Fe
2+Mol ratio be 1:1:4, granular activated carbon and described soft magnetism Mn
0.5Zn
0.5Fe
2O
4Mass ratio be 5-16:1, load Mn
0.5Zn
0.5Fe
2O
4Soft magnetism active carbon and TiO
2Mass ratio be 1.5-6:1.
3. method for preparing the soft magnetism composite photo-catalyst of claim 1 is characterized in that following steps are arranged: (1) is with manganese sulfate, zinc sulfate and ferrous sulfate Mn in molar ratio
2+: Zn
2+: Fe
2+=1:1:4 is made into mixed aqueous solution with deionized water, and making the metal ion total concentration is 0.1mol/L, drips NH after the stirring and dissolving
4OH, transferring PH is 9 ~ 11, adds granular activated carbon, moves to behind the stirring and evenly mixing in the hydrothermal reaction kettle, and maintenance is after 4-16 hour down at 160-200 ℃, and cooling is filtered, washing; Through the soft magnetism active carbon that 110 ℃ of dryings obtain having soft magnetism, the addition of described granular activated carbon is Mn
0.5Zn
0.5Fe
2O
4The 5-16 of quality doubly; (2) the above-mentioned soft magnetism active carbon of titanium sol impregnation that is configured to butyl titanate, absolute ethyl alcohol, nitric acid and water; stir; leave standstill; suction filtration; 110 ℃ of dryings are placed in the Muffle furnace; in inert atmosphere protection and 400-600 ℃ calcining 3 hours down, in 250 ℃ and air atmosphere, keep 3 hours, be cooled to room temperature, promptly obtain the soft magnetism composite photo-catalyst.
4. the method for the soft magnetism composite photo-catalyst of preparation claim 1 as claimed in claim 3; it is characterized in that: described step (2) the above-mentioned soft magnetism active carbon of titanium sol impregnation; stir; leave standstill suction filtration, 110 ℃ of drying processes; repeating 2-3 time is placed in the Muffle furnace; in inert atmosphere protection and 400-600 ℃ calcining 3 hours down, in 250 ℃ and air atmosphere, keep 3 hours, be cooled to room temperature, promptly obtain the soft magnetism composite photo-catalyst.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102773105A (en) * | 2012-08-06 | 2012-11-14 | 河南师范大学 | Supported bismuth tungstate photocatalyst and preparation method thereof |
| CN103111300A (en) * | 2013-01-28 | 2013-05-22 | 中北大学 | Method for preparing TiO2/ni-zn ferrite/carbon (C) magnetic photocatalyst |
| CN104028750A (en) * | 2014-06-05 | 2014-09-10 | 浙江大学 | High-bonding-strength insulated coating treatment method of metal soft magnetic composite material |
| CN104028749A (en) * | 2014-06-05 | 2014-09-10 | 浙江大学 | High-thermal-stability insulated coating treatment method of metal soft magnetic composite material |
| CN104831312A (en) * | 2015-04-07 | 2015-08-12 | 大连理工大学 | Mn0.5Zn0.5Fe2O4 nano particles-composited TiO2 nano nanotube arrays electrodes and preparation method thereof |
| CN105597724A (en) * | 2015-12-15 | 2016-05-25 | 浙江工业大学 | Method for preparing magnetic-biochar-supported photocatalyst |
| CN107140775A (en) * | 2017-07-17 | 2017-09-08 | 福建工程学院 | A kind for the treatment of method of printing and dying wastewater and device |
| CN109261176A (en) * | 2018-09-17 | 2019-01-25 | 重庆大学 | A method of it preparing iodine seven and aoxidizes five bismuths/manganese-zinc ferrite composite magnetic catalysis material |
| CN109331836A (en) * | 2018-10-10 | 2019-02-15 | 重庆大学 | It is a kind of to prepare β-Bi2O3/MnxZn1-xFe2O4The new method of composite magnetic catalysis material |
| CN114917922A (en) * | 2022-06-21 | 2022-08-19 | 杭州星宇炭素环保科技有限公司 | Magnetically separable photocatalytic regenerated active carbon and preparation method thereof |
| CN115925027A (en) * | 2023-03-10 | 2023-04-07 | 湖南国重环境科技有限责任公司 | Pretreatment of water system is failed in antibiotic production of fermentation class |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102773105A (en) * | 2012-08-06 | 2012-11-14 | 河南师范大学 | Supported bismuth tungstate photocatalyst and preparation method thereof |
| CN102773105B (en) * | 2012-08-06 | 2013-12-11 | 河南师范大学 | Supported bismuth tungstate photocatalyst and preparation method thereof |
| CN103111300A (en) * | 2013-01-28 | 2013-05-22 | 中北大学 | Method for preparing TiO2/ni-zn ferrite/carbon (C) magnetic photocatalyst |
| CN104028750A (en) * | 2014-06-05 | 2014-09-10 | 浙江大学 | High-bonding-strength insulated coating treatment method of metal soft magnetic composite material |
| CN104028749A (en) * | 2014-06-05 | 2014-09-10 | 浙江大学 | High-thermal-stability insulated coating treatment method of metal soft magnetic composite material |
| CN104831312A (en) * | 2015-04-07 | 2015-08-12 | 大连理工大学 | Mn0.5Zn0.5Fe2O4 nano particles-composited TiO2 nano nanotube arrays electrodes and preparation method thereof |
| CN105597724A (en) * | 2015-12-15 | 2016-05-25 | 浙江工业大学 | Method for preparing magnetic-biochar-supported photocatalyst |
| CN107140775A (en) * | 2017-07-17 | 2017-09-08 | 福建工程学院 | A kind for the treatment of method of printing and dying wastewater and device |
| CN109261176A (en) * | 2018-09-17 | 2019-01-25 | 重庆大学 | A method of it preparing iodine seven and aoxidizes five bismuths/manganese-zinc ferrite composite magnetic catalysis material |
| CN109331836A (en) * | 2018-10-10 | 2019-02-15 | 重庆大学 | It is a kind of to prepare β-Bi2O3/MnxZn1-xFe2O4The new method of composite magnetic catalysis material |
| CN114917922A (en) * | 2022-06-21 | 2022-08-19 | 杭州星宇炭素环保科技有限公司 | Magnetically separable photocatalytic regenerated active carbon and preparation method thereof |
| CN115925027A (en) * | 2023-03-10 | 2023-04-07 | 湖南国重环境科技有限责任公司 | Pretreatment of water system is failed in antibiotic production of fermentation class |
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Application publication date: 20110810 |