CN102671674A - Magnetically supported silver bromide photochemical catalysis material and preparation method thereof - Google Patents

Magnetically supported silver bromide photochemical catalysis material and preparation method thereof Download PDF

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CN102671674A
CN102671674A CN201210166515XA CN201210166515A CN102671674A CN 102671674 A CN102671674 A CN 102671674A CN 201210166515X A CN201210166515X A CN 201210166515XA CN 201210166515 A CN201210166515 A CN 201210166515A CN 102671674 A CN102671674 A CN 102671674A
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silver bromide
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catalysis material
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silver
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田宝柱
王婷婷
李艺茹
张金龙
董荣芳
李套云
熊天庆
陈星�
杨钒
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East China University of Science and Technology
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Abstract

The invention relates to a magnetically supported silver bromide photochemical catalysis material and a preparation method thereof. The photochemical catalysis material is composed of a ferroferric oxide/silicon dioxide nuclear shell structure and a silver bromide supported by an outer layer of the ferroferric oxide/silicon dioxide nuclear shell structure. The preparation method comprises the steps: (1) using perchloride iron as a precursor, using polyethylene glycol as a dispersing agent, using a ethylene glycol as a high-boiling-point solvent and utilizing a hydrothermal method to prepare monodisperse magnetic ferroferric oxide nanometer particles; (2) cladding silicon dioxide to form the ferroferric oxide/silicon dioxide nuclear shell structure; and (3) using silver nitrate as a silver source, using potassium bromide or other bromides as a bromine source, supporting silver bromide on the ferroferric oxide/silicon dioxide surface, and using ultraviolet light to perform photo-reduction to silver bromide microcrystal to enable the surface to form silver nanometer particles in a in-situ mode. Compared with existing methods, the magnetically supported silver bromide photochemical catalysis material and the preparation method have the advantages that a catalyst is controllable in morphology and can be recycled in a magnetic control mode and the like. The catalyst prepared by means of the method can efficiently degrade organic pollutants including dyestuffs and the like.

Description

A kind of magnetic carries silver bromide catalysis material and preparation method thereof
Technical field
The present invention relates to a kind of catalysis material that can be applicable to water pollutant degraded and photolysis water hydrogen and preparation method thereof, belong to the photocatalysis technology field.
Background technology
Because the development of industry and human social economy, the mankind make more people be devoted to the research to solar energy utilization rate to the attention rate of energy and environment is increasingly high.The artificial photosynthesis system receives an acclaim because of abundant solar energy resources and less carbon footprint, like photolysis water hydrogen, and photocatalysis, photovoltaic cell.
After titanium dioxide in 1969 demonstrated the conversion capability between Optical Electro-Chemistry and solar energy, this semi-conducting material caused the extensive concern of academia immediately.Nano titanium oxide can utilize sunshine that most organic pollutions in the environment thoroughly are degraded to nontoxic, harmless water and carbon dioxide; Do not produce secondary pollution; And cheap and easy to get, at solar energy photodissociation water, there is important application prospects aspects such as sewage disposal.
Yet really being moved towards the industrialization, titanium dioxide must solve two technical barriers: the about 3.2eV of energy gap of (1) titanium dioxide; Can only under ultraviolet excitation, produce electron-hole pair; And ultraviolet light only accounts for about 3~5% of sunshine, and this has just caused titanium dioxide extremely low to the utilization ratio of sunshine; (2) reduce owing to there are the serious compound photochemically reactive carrier quantity of effective participation that makes in titanium dioxide photoproduction electronics and hole, thereby cause the whole quantum conversion low (≤4%) of catalysis material.Therefore, the visible light-responded photochemical catalyst of preparation has become the important research direction in this field.Big quantity research shows through mixing can effectively improve the photocatalytic activity of titanium dioxide, widens its photoresponse scope.
In order to improve the utilization ratio of titanium dioxide to sunshine, modified measures such as researcher's applied metal doping on the one hand, nonmetal doping, dye sensitization are expanded the response range of titanium dioxide to visible light; On the other hand, also there are some research work to launch around the narrow band gap catalysis material of non-titanium dioxide; In recent years, silver halide receives researcher's extensive concern in the application of photocatalysis field.Silver bromide can effectively utilize visible light, is a kind of photochemical catalyst with broad prospect of application.Yet, bromizate silver-colored photochemical catalyst and really move towards practicability, must solve it and be difficult to the difficult problem that repeats to recycle.In recent years, people are to being that the photochemical catalyst of carrier has launched extensive studies with magnetic materials such as tri-iron tetroxides.Can solve this difficult problem preferably and silver bromide loaded on the magnetic carrier material.
Summary of the invention
The present invention is through the Hydrothermal Preparation nano ferriferrous oxide; With improved
Figure BSA00000723636900021
method it being carried out skin coats; At its area load silver bromide, prepared magnetic and carried the silver bromide catalysis material then.Prepared catalysis material can utilize the Nano silver grain responding to visible light that original position forms in the photo-reduction process, realizes the efficient degradation of organic pollution under the sunshine.
The preparation method that magnetic of the present invention carries the silver bromide catalysis material may further comprise the steps:
(1) ferric sesquichloride is dissolved in the ethylene glycol, adds anhydrous sodium acetate and polyethylene glycol, vigorous stirring 30 minutes is carried out hydro-thermal reaction then.After reaction finishes, wash each with absolute ethyl alcohol, secondary water washing and be dispersed in the absolute ethyl alcohol for three times.
(2) get above-mentioned ethanolic solution, add absolute ethyl alcohol, secondary water, ultrasonic dispersion slowly drips ethyl orthosilicate, and dropping ammonia keeps ultrasonic under the room temperature fast.Reaction is washed repeatedly with absolute ethyl alcohol, secondary water washing after finishing, and magnetic separates, and is dispersed in the water.
(3) under the ultrasonic mechanical stirring condition, get the said goods, silver nitrate, ammoniacal liquor are added fast, slowly splash into kbr aqueous solution, reacted 4 hours.Then, wash successively, magnetic separation, oven dry, calcination processing.At last, with the 300W high-pressure sodium lamp silver bromide crystallite is carried out photo-reduction and handled 3 hours, make its surface in situ form Nano silver grain.
In the step (1), the concentration of polyethylene glycol is 12~36g/L, is preferably 24g/L.
In the step (2), the mol ratio of ethyl orthosilicate and tri-iron tetroxide is 0.6: 1~1.4: 1, is preferably 1: 1.
In the step (3), optional softex kw in bromine source or KBr are preferably KBr; The mol ratio of KBr and tri-iron tetroxide is 0.6: 1~1.5: 1, is preferably 1: 1; Calcining heat is 450 ℃~600 ℃, is preferably 550 ℃.Can adopt high-pressure sodium lamp, black light lamp or other can produce ultraviolet light source, preferred high-pressure sodium lamp (100~1000W).
This paper adopts hydrothermal synthesis method to prepare ferriferrous oxide nano-particle; Form tri-iron tetroxide/silicon dixoide nucleocapsid structure with method coated silica, and at its outer load silver bromide.It is high that its degraded AO7 has very high active and recyclable utilization rate.
Photocatalytic Activity for Degradation AO7 reaction:
Under 20 ℃, be visible light source, in the 100mL quartz reactor, add 100mLAO7 solution (10mg/L) and 0.05g catalyst with the purple tungsten lamp of 500W; The distance of light source and crystal reaction tube is 10cm, and dark reaction absorption 30 minutes makes dyestuff after catalyst surface reaches the adsorption-desorption balance; Begin to carry out light-catalyzed reaction, took a sample once in per 5 minutes, after the centrifugation; Survey its absorbance with ultraviolet-visible spectrophotometer, and calculate the concentration of residual AO7.
Description of drawings
Fig. 1 is the scanning electron microscope diagram that embodiment 1 obtains product.
Fig. 2 is the x-ray diffraction pattern that embodiment 1 obtains product.
Fig. 3 is the photocatalytic activity figure that embodiment 1 obtains product photocatalytic degradation AO7.
The specific embodiment
Below in conjunction with instance the present invention is further detailed.
Embodiment 1
Ferric sesquichloride is dissolved in the ethylene glycol, adds the polyethylene glycol of anhydrous sodium acetate and 24g/L, mixture vigorous stirring 30 minutes is carried out hydro-thermal reaction then.Reaction is respectively washed three times with absolute ethyl alcohol, secondary water after finishing, and is dispersed in the absolute ethyl alcohol; Get above-mentioned ethanolic solution, add absolute ethyl alcohol, secondary water, ultrasonic dispersion slowly drips ethyl orthosilicate (mol ratio of ethyl orthosilicate and tri-iron tetroxide 1: 1), and dropping ammonia keeps ultrasonic reaction under the room temperature fast.After the end, wash repeatedly with absolute ethyl alcohol, secondary water washing, magnetic separates, and is dispersed in the water; Under ultrasonic, the mechanical agitation condition, get the said goods, silver nitrate, ammoniacal liquor are added fast, slowly drip KBr (mol ratio of KBr and tri-iron tetroxide is 1: the 1) aqueous solution, continue reaction 4 hours.Wash successively then, magnetic separates, oven dry, 550 ℃ of calcinings 3 hours; With the 300W high-pressure sodium lamp silver bromide crystallite is carried out photo-reduction and handled 3 hours, make its surface in situ form Nano silver grain.Obtain magnetic and carry the silver bromide catalyst and be nucleocapsid structure, it is active to have high efficiency photocatalysis degraded AO7 under the visible light.
The sem photograph of embodiment 1 products obtained therefrom is as shown in Figure 1, and as can be seen from the figure, products obtained therefrom is the sphere of homogeneous.The X-ray crystallogram of embodiment 1 products obtained therefrom is as shown in Figure 2, and as can be seen from the figure, the standard diffracting spectrum (JCPDS:06-0438) of the diffraction maximum of products obtained therefrom and silver bromide is in full accord.Fig. 3 is embodiment 1 sample and nitrogen-doped titanium dioxide (N-TiO 2) to the visible light degradation curve of AO7.The photocatalysis experimental result shows that the magnetic of embodiment 1 preparation carries silver bromide photocatalytic degradation AO7 activity far above nitrogen-doped titanium dioxide (N-TiO 2).
Embodiment 2
Ferric sesquichloride is dissolved in the ethylene glycol, adds the polyethylene glycol of anhydrous sodium acetate and 12g/L, mixture vigorous stirring 30 minutes is carried out hydro-thermal reaction then.Reaction is respectively washed three times with absolute ethyl alcohol, secondary water after finishing, and is dispersed in the absolute ethyl alcohol; Get above-mentioned ethanolic solution, add absolute ethyl alcohol, secondary water, ultrasonic dispersion slowly drips ethyl orthosilicate (mol ratio of ethyl orthosilicate and tri-iron tetroxide 1: 1), and dropping ammonia keeps ultrasonic reaction under the room temperature fast.After the end, wash repeatedly with absolute ethyl alcohol, secondary water washing, magnetic separates, and is dispersed in the water; Under ultrasonic, the mechanical agitation condition, get the said goods, silver nitrate, ammoniacal liquor are added fast, slowly drip KBr (mol ratio of KBr and tri-iron tetroxide is 1: the 1) aqueous solution, continue reaction 4 hours.Wash successively then, magnetic separates, oven dry, 550 ℃ of calcinings 3 hours; With the 300W high-pressure sodium lamp silver bromide crystallite is carried out photo-reduction and handled 3 hours, make its surface in situ form Nano silver grain.Obtain magnetic and carry the silver bromide catalyst and be nucleocapsid structure, it is active to have high efficiency photocatalysis degraded AO7 under the visible light.
Embodiment 3
Ferric sesquichloride is dissolved in the ethylene glycol, adds the polyethylene glycol of anhydrous sodium acetate and 24g/L, mixture vigorous stirring 30 minutes is carried out hydro-thermal reaction then.Reaction is respectively washed three times with absolute ethyl alcohol, secondary water after finishing, and is dispersed in the absolute ethyl alcohol; Get above-mentioned ethanolic solution, add absolute ethyl alcohol, secondary water, ultrasonic dispersion slowly drips ethyl orthosilicate (mol ratio of ethyl orthosilicate and tri-iron tetroxide 1.2: 1), and dropping ammonia keeps ultrasonic reaction under the room temperature fast.After the end, wash repeatedly with absolute ethyl alcohol, secondary water washing, magnetic separates, and is dispersed in the water; Under ultrasonic, the mechanical agitation condition, get the said goods, silver nitrate, ammoniacal liquor are added fast, slowly drip KBr (mol ratio of KBr and tri-iron tetroxide is 1: the 1) aqueous solution, continue reaction 4 hours.Wash successively then, magnetic separates, oven dry, 550 ℃ of calcinings 3 hours; With the 300W high-pressure sodium lamp silver bromide crystallite is carried out photo-reduction and handled 3 hours, make its surface in situ form Nano silver grain.Obtain magnetic and carry the silver bromide catalyst and be nucleocapsid structure, it is active to have high efficiency photocatalysis degraded AO7 under the visible light.
Embodiment 4
Ferric sesquichloride is dissolved in the ethylene glycol, adds the polyethylene glycol of anhydrous sodium acetate and 24g/L, mixture vigorous stirring 30 minutes is carried out hydro-thermal reaction then.Reaction is respectively washed three times with absolute ethyl alcohol, secondary water after finishing, and is dispersed in the absolute ethyl alcohol; Get above-mentioned ethanolic solution, add absolute ethyl alcohol, secondary water, ultrasonic dispersion slowly drips ethyl orthosilicate (mol ratio of ethyl orthosilicate and tri-iron tetroxide 1: 1), and dropping ammonia keeps ultrasonic reaction under the room temperature fast.After the end, wash repeatedly with absolute ethyl alcohol, secondary water washing, magnetic separates, and is dispersed in the water; Under ultrasonic, the mechanical agitation condition, get the said goods, silver nitrate, ammoniacal liquor are added fast, slowly drip the softex kw aqueous solution, continue reaction 4 hours.Wash successively then, magnetic separates, oven dry, 550 ℃ of calcinings 3 hours; With the 300W high-pressure sodium lamp silver bromide crystallite is carried out photo-reduction and handled 3 hours, make its surface in situ form Nano silver grain.Obtain magnetic and carry the silver bromide catalyst and be nucleocapsid structure, it is active to have high efficiency photocatalysis degraded AO7 under the visible light.
Embodiment 5
Ferric sesquichloride is dissolved in the ethylene glycol, adds the polyethylene glycol of anhydrous sodium acetate and 24g/L, mixture vigorous stirring 30 minutes is carried out hydro-thermal reaction then.Reaction is respectively washed three times with absolute ethyl alcohol, secondary water after finishing, and is dispersed in the absolute ethyl alcohol; Get above-mentioned ethanolic solution, add absolute ethyl alcohol, secondary water, ultrasonic dispersion slowly drips ethyl orthosilicate (mol ratio of ethyl orthosilicate and tri-iron tetroxide 1: 1), and dropping ammonia keeps ultrasonic reaction under the room temperature fast.After the end, wash repeatedly with absolute ethyl alcohol, secondary water washing, magnetic separates, and is dispersed in the water; Under ultrasonic, the mechanical agitation condition, get the said goods, KBr (mol ratio of KBr and tri-iron tetroxide is 1: the 1) aqueous solution is added fast, slowly drip the solution that contains silver nitrate, ammoniacal liquor, continue reaction 4 hours.Wash successively then, magnetic separates, oven dry, 550 ℃ of calcinings 3 hours; With the 300W high-pressure sodium lamp silver bromide crystallite is carried out photo-reduction and handled 3 hours, make its surface in situ form Nano silver grain.Obtain magnetic and carry the silver bromide catalyst and be nucleocapsid structure, it is active to have high efficiency photocatalysis degraded AO7 under the visible light.
Embodiment 6
Ferric sesquichloride is dissolved in the ethylene glycol, adds the polyethylene glycol of anhydrous sodium acetate and 24g/L, mixture vigorous stirring 30 minutes is carried out hydro-thermal reaction then.Reaction is respectively washed three times with absolute ethyl alcohol, secondary water after finishing, and is dispersed in the absolute ethyl alcohol; Get above-mentioned ethanolic solution, add absolute ethyl alcohol, secondary water, ultrasonic dispersion slowly drips ethyl orthosilicate (mol ratio of ethyl orthosilicate and tri-iron tetroxide 1: 1), and dropping ammonia keeps ultrasonic reaction under the room temperature fast.After the end, wash repeatedly with absolute ethyl alcohol, secondary water washing, magnetic separates, and is dispersed in the water; Under ultrasonic, the mechanical agitation condition, get the said goods, silver nitrate, ammoniacal liquor are added fast, slowly drip KBr (mol ratio of KBr and tri-iron tetroxide is 1.5: the 1) aqueous solution, continue reaction 4 hours.Wash successively then, magnetic separates, oven dry, 550 ℃ of calcinings 3 hours; With the 300W high-pressure sodium lamp silver bromide crystallite is carried out photo-reduction and handled 3 hours, make its surface in situ form Nano silver grain.Obtain magnetic and carry the silver bromide catalyst and be nucleocapsid structure, it is active to have high efficiency photocatalysis degraded AO7 under the visible light.
Embodiment 7
Ferric sesquichloride is dissolved in the ethylene glycol, adds the polyethylene glycol of anhydrous sodium acetate and 24g/L, mixture vigorous stirring 30 minutes is carried out hydro-thermal reaction then.Reaction is respectively washed three times with absolute ethyl alcohol, secondary water after finishing, and is dispersed in the absolute ethyl alcohol; Get above-mentioned ethanolic solution, add absolute ethyl alcohol, secondary water, ultrasonic dispersion slowly drips ethyl orthosilicate (mol ratio of ethyl orthosilicate and tri-iron tetroxide 1: 1), and dropping ammonia keeps ultrasonic reaction under the room temperature fast.After the end, wash repeatedly with absolute ethyl alcohol, secondary water washing, magnetic separates, and is dispersed in the water; Under ultrasonic, the mechanical agitation condition, get the said goods, silver nitrate, ammoniacal liquor are added fast, slowly drip KBr (mol ratio of KBr and tri-iron tetroxide is 1: the 1) aqueous solution, continue reaction 2 hours.Wash successively then, magnetic separates, oven dry, 550 ℃ of calcinings 3 hours; With the 300W high-pressure sodium lamp silver bromide crystallite is carried out photo-reduction and handled 3 hours, make its surface in situ form Nano silver grain.Obtain magnetic and carry the silver bromide catalyst and be nucleocapsid structure, it is active to have high efficiency photocatalysis degraded AO7 under the visible light.
Embodiment 8
Ferric sesquichloride is dissolved in the ethylene glycol, adds the polyethylene glycol of anhydrous sodium acetate and 24g/L, mixture vigorous stirring 30 minutes is carried out hydro-thermal reaction then.Reaction is respectively washed three times with absolute ethyl alcohol, secondary water after finishing, and is dispersed in the absolute ethyl alcohol; Get above-mentioned ethanolic solution, add absolute ethyl alcohol, secondary water, ultrasonic dispersion slowly drips ethyl orthosilicate (mol ratio of ethyl orthosilicate and tri-iron tetroxide 1: 1), and dropping ammonia keeps ultrasonic reaction under the room temperature fast.After the end, wash repeatedly with absolute ethyl alcohol, secondary water washing, magnetic separates, and is dispersed in the water; Under ultrasonic, the mechanical agitation condition, get the said goods, silver nitrate, ammoniacal liquor are added fast, slowly drip KBr (mol ratio of KBr and tri-iron tetroxide is 1: the 1) aqueous solution, continue reaction 6 hours.Wash successively then, magnetic separates, oven dry, 550 ℃ of calcinings 3 hours; With the 300W high-pressure sodium lamp silver bromide crystallite is carried out photo-reduction and handled 3 hours, make its surface in situ form Nano silver grain.Obtain magnetic and carry the silver bromide catalyst and be nucleocapsid structure, it is active to have high efficiency photocatalysis degraded AO7 under the visible light.
Embodiment 9
Ferric sesquichloride is dissolved in the ethylene glycol, adds the polyethylene glycol of anhydrous sodium acetate and 24g/L, mixture vigorous stirring 30 minutes is carried out hydro-thermal reaction then.Reaction is respectively washed three times with absolute ethyl alcohol, secondary water after finishing, and is dispersed in the absolute ethyl alcohol; Get above-mentioned ethanolic solution, add absolute ethyl alcohol, secondary water, ultrasonic dispersion slowly drips ethyl orthosilicate (mol ratio of ethyl orthosilicate and tri-iron tetroxide 1: 1), and dropping ammonia keeps ultrasonic reaction under the room temperature fast.After the end, wash repeatedly with absolute ethyl alcohol, secondary water washing, magnetic separates, and is dispersed in the water; Under ultrasonic, the mechanical agitation condition, get the said goods, silver nitrate, ammoniacal liquor are added fast, slowly drip KBr (mol ratio of KBr and tri-iron tetroxide is 1: the 1) aqueous solution, continue reaction 8 hours.Wash successively then, magnetic separates, oven dry, 550 ℃ of calcinings 3 hours; With the 300W high-pressure sodium lamp silver bromide crystallite is carried out photo-reduction and handled 3 hours, make its surface in situ form Nano silver grain.Obtain magnetic and carry the silver bromide catalyst and be nucleocapsid structure, it is active to have high efficiency photocatalysis degraded AO7 under the visible light.
Embodiment 10
Ferric sesquichloride is dissolved in the ethylene glycol, adds the polyethylene glycol of anhydrous sodium acetate and 24g/L, mixture vigorous stirring 30 minutes is carried out hydro-thermal reaction then.Reaction is respectively washed three times with absolute ethyl alcohol, secondary water after finishing, and is dispersed in the absolute ethyl alcohol; Get above-mentioned ethanolic solution, add absolute ethyl alcohol, secondary water, ultrasonic dispersion slowly drips ethyl orthosilicate (mol ratio of ethyl orthosilicate and tri-iron tetroxide 1: 1), and dropping ammonia keeps ultrasonic reaction under the room temperature fast.After the end, wash repeatedly with absolute ethyl alcohol, secondary water washing, magnetic separates, and is dispersed in the water; Under ultrasonic, the mechanical agitation condition, get the said goods, silver nitrate, ammoniacal liquor are added fast, slowly drip KBr (mol ratio of KBr and tri-iron tetroxide is 1: the 1) aqueous solution, stop ultrasonicly, continued stirring reaction 4 hours.Wash successively then, magnetic separates, oven dry, 550 ℃ of calcinings 3 hours; With the 300W high-pressure sodium lamp silver bromide crystallite is carried out photo-reduction and handled 3 hours, make its surface in situ form Nano silver grain.Obtain magnetic and carry the silver bromide catalyst and be nucleocapsid structure, it is active to have high efficiency photocatalysis degraded AO7 under the visible light.
Embodiment 11
Ferric sesquichloride is dissolved in the ethylene glycol, adds the polyethylene glycol of anhydrous sodium acetate and 24g/L, mixture vigorous stirring 30 minutes is carried out hydro-thermal reaction then.Reaction is respectively washed three times with absolute ethyl alcohol, secondary water after finishing, and is dispersed in the absolute ethyl alcohol; Get above-mentioned ethanolic solution, add absolute ethyl alcohol, secondary water, ultrasonic dispersion slowly drips ethyl orthosilicate (mol ratio of ethyl orthosilicate and tri-iron tetroxide 1: 1), and dropping ammonia keeps ultrasonic reaction under the room temperature fast.After the end, wash repeatedly with absolute ethyl alcohol, secondary water washing, magnetic separates, and is dispersed in the water; Under ultrasonic, the mechanical agitation condition, get the said goods, silver nitrate, ammoniacal liquor are added fast, slowly drip KBr (mol ratio of KBr and tri-iron tetroxide is 1: the 1) aqueous solution, continue reaction 4 hours.Wash successively then, magnetic separates, oven dry, 500 ℃ of calcinings 3 hours; With the 300W high-pressure sodium lamp silver bromide crystallite is carried out photo-reduction and handled 3 hours, make its surface in situ form Nano silver grain.Obtain magnetic and carry the silver bromide catalyst and be nucleocapsid structure, it is active to have high efficiency photocatalysis degraded AO7 under the visible light.

Claims (9)

1. a magnetic carries the silver bromide catalysis material, it is characterized in that, said catalyst is made up of tri-iron tetroxide, silica, silver bromide.
2. magnetic according to claim 1 carries the silver bromide catalysis material, it is characterized in that, but prepared catalyst magnetic control separates.
3. the described magnetic of claim 1 carries the preparation method of silver bromide catalysis material, it is characterized in that this preparation method may further comprise the steps:
(1) adopts Hydrothermal Preparation tri-iron tetroxide particle.The employing ferric sesquichloride is a presoma, and polyethylene glycol is a dispersant, and ethylene glycol is high boiling solvent, the control reaction temperature, and polyethylene glycol consumptions etc. can make the spherical tri-iron tetroxide particle of homogeneous.
(2) adopt
Figure FSA00000723636800011
method coated silica to form tri-iron tetroxide/silicon dixoide nucleocapsid structure.
(3) be the bromine source with KBr or other bromide; At tri-iron tetroxide/silica surface load silver bromide, remove impurity through secondary water, washing with alcohol, high-temperature calcination; With ultraviolet light the silver bromide crystallite is carried out photo-reduction and handle, make its surface in situ form Nano silver grain.
4. carry the preparation method of silver bromide catalysis material according to the described magnetic of claim 3 (1), it is characterized in that the concentration of polyethylene glycol is 12~36g/L, is preferably 24g/L.
5. carry the preparation method of silver bromide catalysis material according to the described magnetic of claim 3 (2), it is characterized in that the mol ratio of ethyl orthosilicate and tri-iron tetroxide is 0.6: 1~1.4: 1, is preferably 1: 1.
6. carry the preparation method of silver bromide catalysis material according to the described magnetic of claim 3 (3), it is characterized in that the optional softex kw in employed bromine source, sodium bromide or KBr are preferably KBr.
7. carry the preparation method of silver bromide catalysis material according to the described magnetic of claim 3 (3), it is characterized in that the mol ratio of KBr and tri-iron tetroxide is 0.6: 1~1.5: 1, is preferably 1: 1.
8. carry the preparation method of silver bromide catalysis material according to the described magnetic of claim 3 (3), it is characterized in that calcining heat is 450 ℃~600 ℃, be preferably 550 ℃.
9. carry the preparation method of silver bromide catalysis material according to the described magnetic of claim 3 (3), it is characterized in that, can adopt high-pressure sodium lamp, black light lamp and other can produce ultraviolet light source, preferred high-pressure sodium lamp.
CN201210166515XA 2012-05-25 2012-05-25 Magnetically supported silver bromide photochemical catalysis material and preparation method thereof Pending CN102671674A (en)

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CN103223322B (en) * 2013-05-13 2015-02-04 洛阳师范学院 Preparation method of nanosilver and sulfydryl jointly modified magnetic microspheres
CN103801257A (en) * 2014-02-14 2014-05-21 中国科学院合肥物质科学研究院 Synthetic method of sliver/ferroferric oxide/silicon dioxide/titanium dioxide four-layer nuclear shell structure and application thereof
CN103801257B (en) * 2014-02-14 2015-12-02 中国科学院合肥物质科学研究院 The synthetic method of silver/tri-iron tetroxide/earth silicon/titanic oxide four layers of nucleocapsid structure and purposes
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CN104353495A (en) * 2014-10-09 2015-02-18 济南大学 Preparation method and application of multiple magnetic mesoporous catalysts
CN105363479A (en) * 2015-11-20 2016-03-02 太原理工大学 Magnetic nano photocatalytic material Ag/AgCl@Fe3O4, preparation method and application thereof
CN106513023A (en) * 2016-04-01 2017-03-22 郑州大学 Fe3O4/ BiOI/AgBr magnetic composite visible-light-driven photocatalyst and preparation thereof
CN111068722A (en) * 2019-12-28 2020-04-28 合肥学院 Silver bromide/silicon dioxide composite powder and preparation method thereof

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Application publication date: 20120919