CN105664982A - Novel magneto-optical dual-functional catalyst with Fe3O4/BiOI core/shell structure - Google Patents

Novel magneto-optical dual-functional catalyst with Fe3O4/BiOI core/shell structure Download PDF

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Publication number
CN105664982A
CN105664982A CN201610121758.XA CN201610121758A CN105664982A CN 105664982 A CN105664982 A CN 105664982A CN 201610121758 A CN201610121758 A CN 201610121758A CN 105664982 A CN105664982 A CN 105664982A
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China
Prior art keywords
core
magnetic
bioi
shell structure
fe3o4
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Pending
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CN201610121758.XA
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Chinese (zh)
Inventor
郑立允
王书岭
赵立新
刘晓艳
梁顺星
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Hebei University of Engineering
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Hebei University of Engineering
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Priority to CN201610121758.XA priority Critical patent/CN105664982A/en
Publication of CN105664982A publication Critical patent/CN105664982A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/06Halogens; Compounds thereof
    • B01J27/128Halogens; Compounds thereof with iron group metals or platinum group metals
    • B01J35/33
    • B01J35/39
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
    • B01J37/343Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

Abstract

The invention belongs to the field of preparation of a magnetic nano photocatalyst, and in particular relates to magnetic nano photocatalytic particles with a core/shell structure and a preparation method thereof. The nano particles are Fe3O4/BiOI prepared by performing microwave chemical synthesis on nano Fe3O4 and BiI3 which serve as raw materials and ethylene glycol serving as a solvent and a surfactant. The Fe3O4/BiOI nano particles with the core/shell structure are higher in photocatalysis performance. The magnetic nano photocatalyst can be used for catalytically degrading azo-group dyes, has paramagnetism and catalysis stability, and can be recycled for multiple times.

Description

Novel Fe3O4/ BiOI core/shell structure magneto-optic double-function catalyzer
Technical field
The invention belongs to magnetic nanometer photocatalyst field, in particular to magnetic nano photochemical catalyst particle and its preparation method of a kind of core/shell structure.
Background technology
Conductor photocatalysis technology can carry out at normal temperatures and pressures, to pollution degraded almost without any selectivity, can be nontoxic inorganic molecules by contaminant degradation, however recovery utilization rate low be a principal element of its industrialization of restriction. Fe3O4Being that one has good paramagnetism, stable in properties, the activity of photochemical catalysis part can not be produced bigger disadvantageous effect, nontoxic, harmless, pollution-free, raw material is easy to get, the simple magnetic carrier of preparation technology. BiOI is laminate structure, and crystals has built in field, it is possible to effectively improve light induced electron hole to separation efficiency. By the Fe after both compounds3O4/ BiOI not only has unique crystalline structure, energy band structure, stable performance and has paramagnetism so that photocatalyst can reclaim separation efficiently. This nano-magnetic photocatalyst is the focus studying catalyzer at present.
In sum, the research stable novel magnetic/light dual-function catalyst of preparation can solve the problem that current nanocatalyst is difficult to reclaim, and the development of environmentally friendly type photocatalysis technology has important meaning.
Summary of the invention
For the problems referred to above, the present invention provides magnetic nano photochemical catalyst particle and its preparation method of a kind of core/shell structure. Make to realize semiconductor light-catalyst recycling and become possibility.
The principle of the present invention is: adopt nanometer Fe3O4And BiI3As raw material, ethylene glycol, as solvent and tensio-active agent, prepares Fe by microwave chemical synthetic method3O4/BiOI。
For achieving the above object, in conjunction with the principle of the invention, the present invention provides following technical scheme: the magnetic nano photochemical catalyst particle Fe of a kind of core/shell structure3O4/ BiOI, is prepared by microwave chemical synthetic method. It is characterized in that: this magnetic nanoparticle is by nanometer Fe3O4With micron BiI3As raw material, ethylene glycol, as solvent and tensio-active agent, prepares nanometer Fe by microwave chemical synthetic method3O4/ BiOI catalyzer.
The magnetic nano photochemical catalyst particle Fe of this core/shell structure3O4/ BiOI is prepared by following step:
1) appropriate BiI is got3It is dissolved in 100ml ethylene glycol, by the Fe of 1mmol3O4Nano particle adds BiI3Ethylene glycol solution in, carry out ultrasonic disperse 20min and make it Homogeneous phase mixing.
2) above-mentioned mixing solutions is put into microwave chemosynthesis instrument and carry out microwave chemical synthesis, simultaneously magnetic agitation, generated time 5-10min.
3) naturally cooling to room temperature, magnetic resolution is respectively with deionized water, absolute ethanol washing three times, and 60 DEG C of oven dry in air dry oven, obtain the Fe of core/shell structure3O4/ BiOI magnetic nanoparticle.
Compared with prior art, the useful effect of the present invention is:
The magnetic nano photochemical catalyst particle Fe of core/shell structure of the present invention3O4/ BiOI has unique crystalline structure and energy band structure, has higher photocatalysis performance, and this magnetic nano photochemical catalyst has paramagnetism, it is possible to repeatedly recycles and has good catalytic stability.
Below in conjunction with embodiment, the specific embodiment of the present invention is described in further detail.
The magnetic nano photochemical catalyst particle Fe of the core/shell structure of the present invention3O4/ BiOI, is prepared by microwave chemical synthetic method.
The concrete preparation method of this catalyzer is as follows:
Adopting BiI3 as presoma, the ethylene glycol solution of preparation BiI3, adds nanometer Fe_3O_4, and ultrasonic disperse is even, puts into microwave chemosynthesis instrument and carries out microwave chemical building-up reactions, cleaning, centrifugation, drying.
Magnetism testing tests magnetic hysteresis loop on VersaLab vibrating sample magnetometer, and maximum magnetic field is 30kOe.
Catalytic performance testing method: photocatalysis performance is characterized by methyl orange aqueous solution degraded fade curves under visible light, visible light source is the xenon lamp of 300W, methyl orange aqueous solution concentration is 0.5mol/l, getting 2g catalyzer adds in 50ml methyl orange solution, before illumination, in the dark by solution continuously stirring 1h so that it is fully absorption/de-attached reaches balance, degraded product UV-2450 ultraviolet-visible pectrophotometer test analysis, calculates methyl orange degradation rate.
Embodiment 1:
The microwave chemical synthetic method of the present invention is adopted to prepare the magnetic nano photochemical catalyst particle Fe of core/shell structure3O4/ BiOI, first, by 589mg(1mmol) BiI3Join in 100ml ethylene glycol, magnetic stirring apparatus fully stirs and obtains settled solution, by the 232mgFe of above-mentioned preparation3O4Powder is dispersed in above-mentioned settled solution, and ultrasonic 20min puts into Microwave synthesize instrument, magnetic agitation, carries out microwave chemical building-up reactions 5min, product magnetic resolution and by deionized water, washing with alcohol three times, 60 DEG C of oven dry in air dry oven, obtain the Fe of nucleocapsid structure3O4/ BiOI magnetic nanoparticle.
Under above-mentioned preparation process condition, the Fe of prepared core/shell structure3O4The saturation magnetization of/BiOI nano particle is 61.5emu/g. The methyl orange degradation rate of this catalyzer reaches 95.6%.
Embodiment 2:
The microwave chemical synthetic method of the present invention is adopted to prepare the magnetic nano photochemical catalyst particle Fe of core/shell structure3O4/ BiOI, first, by 589mg(1mmol) BiI3Join in 100ml ethylene glycol, magnetic stirring apparatus fully stirs and obtains settled solution, by the 232mgFe of above-mentioned preparation3O4Powder is dispersed in above-mentioned settled solution, and ultrasonic 20min puts into Microwave synthesize instrument, magnetic agitation, carries out microwave chemical building-up reactions 10min, product magnetic resolution and by deionized water, washing with alcohol three times, 60 DEG C of oven dry in air dry oven, obtain the Fe of nucleocapsid structure3O4/ BiOI magnetic nanoparticle.
Under above-mentioned preparation process condition, the saturation magnetization of prepared nano particle is 62emu/g. The methyl orange degradation rate of this catalyzer reaches 95.7%.

Claims (3)

1. the magnetic nano photochemical catalyst particle Fe of a core/shell structure3O4/ BiOI, is made up of microwave chemical synthetic method, it is characterised in that: this magnetic nanoparticle is by nanometer Fe3O4And BiI3As raw material, ethylene glycol, as solvent and tensio-active agent, prepares Fe by microwave chemical synthetic method3O4/BiOI。
2. the magnetic nano photochemical catalyst particle of core/shell structure as claimed in claim 1, it is characterised in that: this magnetic nanoparticle is prepared by following step:
Get appropriate BiI3The solution being dissolved in ethylene glycol being made into 0.01M, by the Fe of 1mmol3O4Nano particle adds the BiI of 100ml3In solution, carry out ultrasonic disperse 20min and make it Homogeneous phase mixing, put into microwave chemosynthesis instrument and carry out microwave chemical synthesis, magnetic agitation simultaneously, generated time 5-10min, naturally cools to room temperature, magnetic resolution, respectively with deionized water, absolute ethanol washing three times, 60 DEG C of oven dry, obtain the Fe of core/shell structure3O4/ BiOI magnetic nanoparticle.
3. the magnetic nanoparticle of a core/shell structure as described in one of claim 1 and 2, it is characterised in that:
Catalyzed degradation azo-based dye, has paramagnetism simultaneously and catalytic stability can repeatedly be recycled.
CN201610121758.XA 2016-03-04 2016-03-04 Novel magneto-optical dual-functional catalyst with Fe3O4/BiOI core/shell structure Pending CN105664982A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109836515A (en) * 2019-02-22 2019-06-04 湖南理工学院 A kind of Fe3O4/BiOI/Cu2O is the method for the atom transfer radical polymerization of photoinitiator
CN110075877A (en) * 2019-03-26 2019-08-02 东北大学 A kind of preparation method of ZnO-BiOI composite photo-catalyst

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103285892A (en) * 2013-06-07 2013-09-11 南昌航空大学 Method for preparing Lewis acidic molecular imprinting type BiOI photo-catalyst with visible-light response and high selectivity by hydrothermal method
CN103373750A (en) * 2012-04-20 2013-10-30 苏州晶能科技有限公司 Light source device for removing organic matters and heavy metal ions by visible light and preparation method thereof
CN103623803A (en) * 2012-08-30 2014-03-12 上海纳晶科技有限公司 Visible light photocatalyst and preparation method therefor

Patent Citations (3)

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CN103373750A (en) * 2012-04-20 2013-10-30 苏州晶能科技有限公司 Light source device for removing organic matters and heavy metal ions by visible light and preparation method thereof
CN103623803A (en) * 2012-08-30 2014-03-12 上海纳晶科技有限公司 Visible light photocatalyst and preparation method therefor
CN103285892A (en) * 2013-06-07 2013-09-11 南昌航空大学 Method for preparing Lewis acidic molecular imprinting type BiOI photo-catalyst with visible-light response and high selectivity by hydrothermal method

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109836515A (en) * 2019-02-22 2019-06-04 湖南理工学院 A kind of Fe3O4/BiOI/Cu2O is the method for the atom transfer radical polymerization of photoinitiator
CN110075877A (en) * 2019-03-26 2019-08-02 东北大学 A kind of preparation method of ZnO-BiOI composite photo-catalyst

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Application publication date: 20160615