CN106807411A - A kind of preparation method of ferrous acid La doped silver bromide compound photocatalyst - Google Patents

A kind of preparation method of ferrous acid La doped silver bromide compound photocatalyst Download PDF

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CN106807411A
CN106807411A CN201710144608.5A CN201710144608A CN106807411A CN 106807411 A CN106807411 A CN 106807411A CN 201710144608 A CN201710144608 A CN 201710144608A CN 106807411 A CN106807411 A CN 106807411A
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preparation
silver bromide
bromide compound
compound photocatalyst
ferrous acid
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CN106807411B (en
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李忠玉
宋彦任
金杰
徐松
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Changzhou University
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Changzhou University
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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
    • B01J35/39
    • 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

Abstract

It is the present invention relates to a kind of preparation method of ferrous acid La doped silver bromide compound photocatalyst, including content:The preparation of cadmium ferrite and the preparation of ferrous acid La doped silver bromide compound photocatalyst.The beneficial effects of the invention are as follows:The preparation method is relatively simple, and preparation condition is easily controlled, and prepared ferrous acid La doped silver bromide compound photocatalyst is environmental protection high performance catalyst, pollution-free, high catalytic efficiency, with certain application value.

Description

A kind of preparation method of ferrous acid La doped silver bromide compound photocatalyst
Technical field
Urge material to prepare and applied technical field the invention belongs to light, be related to a kind of ferrous acid La doped silver bromide complex light to urge The preparation method of agent.
Background technology
Photocatalysis technology receives the widely studied of scientist in recent years as a kind of emerging technology of problem of environmental pollution And concern.Research shows that photocatalysis technology has therefore it has dual value in theoretical research and practical application.And it is traditional Photochemical catalyst have specific surface small, photocatalysis efficiency is low, the shortcomings of quantum yield and separation rate not high.Therefore find new Visible light catalyst be photocatalysis technology development the most important thing.Research finds:Perovskite (ABO3) type composite oxides tool Have the advantages that it is excellent electromagnetically, high catalytic property, stable chemical nature, so being considered as the light of 21 century most development potentiality One of catalysis material.Cadmium ferrite as a kind of perovskite rare earth catalyst while with above-mentioned advantage, also with band-gap energy Smaller, nontoxic the advantages of, but research finds that its utilization rate to solar energy is low, and photocatalysis efficiency is poor, and quantum efficiency is relatively low. Therefore, it is very significant to improve the photocatalysis efficiency of cadmium ferrite.
, used as a kind of narrow gap semiconductor, the absorption good to visible ray can be as in photocatalytic system for silver bromide Light-absorption layer.But because of its light sensitivity and less stable, greatly limit its application and research in photocatalysis field.In recent years one Can after a little bromination silver-based composite photocatalyst materials are widely studied, and research finds silver bromide and the doping of other semi-conducting materials To lift the stability and photocatalysis performance of composite catalyst.So cadmium ferrite is combined with silver bromide can not only promote light The transfer of raw carrier, improves photocatalysis efficiency, can also efficiently separate the light induced electron on silver bromide and avoid reducing silver ion, Ensure that stability of the silver bromide in catalyst system and catalyzing.Therefore, the research and development of the composite catalyst is very significant.
The content of the invention
The technical problem to be solved in the present invention is:Based on above mentioned problem, the present invention provides a kind of ferrous acid La doped silver bromide The preparation method of composite photo-catalyst.
The present invention solves a technical scheme being used of its technical problem:A kind of ferrous acid La doped silver bromide complex light The preparation method of catalyst, comprises the following steps:
(1) preparation of cadmium ferrite:In reaction vessel, lanthanum nitrate, ferric nitrate and citric acid are dissolved in solvent I, heated To 60~80 DEG C and stir 30~60min, regulation pH value forms gel to 6~8, be heated to 60~80 DEG C and stirring 30~ 60min, regulation pH value to 6~8 forms gel, and 60~80 DEG C of 6~12h of drying are put into Muffle furnace, 500~600 DEG C of sintering 2 ~3h, grinding, obtains cadmium ferrite;
(2) preparation of ferrous acid La doped silver bromide compound photocatalyst:The cadmium ferrite that will be prepared in step (1) adds solvent In II, 30~60min of ultrasonic disperse;Silver nitrate is added, 30~60min is stirred;Bromine source is added, 30~60min is stirred, is centrifuged, Washing, 60~80 DEG C of 4~6h of drying.
Further, solvent I is water or ethanol in step (1).
Further, the quality of lanthanum nitrate is the 35~75% of ferric nitrate in step (1), and the quality of citric acid is ferric nitrate 50~100%.
Further, the adjusting method of pH value is adjusted using ammoniacal liquor or sodium hydroxide solution in step (2).
Further, bromine source is sodium bromide or KBr in step (2).
Further, solvent II is water, methyl alcohol or ethanol in step (2), the quality of cadmium ferrite for silver nitrate 10~ 40%, the quality in bromine source is the 60~70% of silver nitrate.
The beneficial effects of the invention are as follows:The preparation method is relatively simple, and preparation condition is easily controlled, prepared cadmium ferrite Doping silver bromide compound photocatalyst is environmental protection high performance catalyst, pollution-free, high catalytic efficiency.
Brief description of the drawings
The present invention is further described below in conjunction with the accompanying drawings.
Fig. 1 is the X-ray diffractogram of cadmium ferrite/silver bromide compound photocatalyst prepared by embodiment 1;
Fig. 2 is the scanning electron microscope (SEM) photograph of cadmium ferrite/silver bromide compound photocatalyst prepared by embodiment 1;
Fig. 3 is the transmission electron microscope picture of cadmium ferrite/silver bromide compound photocatalyst prepared by embodiment 1;
Fig. 4 is the degradation property figure of the cadmium ferrite/silver bromide compound photocatalyst to rhodamine B of the preparation of embodiment 1.
Specific embodiment
Presently in connection with specific embodiment, the invention will be further described, and following examples are intended to illustrate rather than Limitation of the invention further.
Embodiment 1
(1) in beaker, 1.2g lanthanum nitrates, 1.6g ferric nitrates and 1.6g citric acids are dissolved in 100ml water, are heated to 60 DEG C and 30min is stirred, pH value to 6 is adjusted with ammoniacal liquor, form gel, 60 DEG C dry 6h, are put into Muffle furnace, 500 DEG C of sintering 2h, obtains cadmium ferrite after grinding.
(2) the 0.018g cadmium ferrites in step (1) are dispersed in 20ml absolute ethyl alcohols, ultrasonic 30min, add 0.18g Silver nitrate, stirs 30min, adds 0.108g KBrs, stirs 30min, and centrifugation is washed, and 60 DEG C dry 4h.
Embodiment 2
(1) in beaker, 0.56g lanthanum nitrates, 1.6g ferric nitrates and 0.8g citric acids are dissolved in 50ml ethanol, are heated To 80 DEG C and 60min is stirred, pH value to 8 is adjusted with ammoniacal liquor, form gel, 80 DEG C dry 12h, are put into Muffle furnace, 600 DEG C of burnings Knot 3h, obtains cadmium ferrite after grinding.
(2) the 0.072g cadmium ferrites in step (1) are dispersed in the deionized water of 30ml, ultrasonic 60min, are added 0.18g silver nitrates, stir 60min, add 0.126g sodium bromides, stir 60min, and centrifugation is washed, and 80 DEG C dry 6h.
1st, the performance measurement of cadmium ferrite/silver bromide compound photocatalyst
The crystal phase structure of the cadmium ferrite/silver bromide compound photocatalyst prepared by embodiment 1 is by Rigaku D/ Max2500PC rotations x-ray diffractometer is analyzed, wherein, X-ray is Cu target K αVoltage 40kV, electric current 100mA, step-length is 0.02 °, 5 °~80 ° of sweep limits.X ray diffracting spectrum as shown in figure 1, as seen from the figure, the ferrous acid of preparation See in lanthanum/silver bromide compound photocatalyst XRD diffraction patterns 26.66 °, 30.95 °, 44.30 °, 55.00 °, 64.36 °, Occur silver bromide diffraction maximum at 73.18 ° six, 22.52 °, 32.14 °, 39.76 °, 46.18 °, 52.43 °, 57.27 °, 67.29 °, 76.65 ° is cadmium ferrite characteristic diffraction peak, therefore, it can prove that silver bromide is combined with each other with cadmium ferrite.
Cadmium ferrite/silver bromide the complex light prepared using Japanese JSM-6360A types SEM observation embodiment 1 The pattern of catalyst, scanning electron microscope (SEM) photograph are as shown in Fig. 2 as can be seen from Fig., cadmium ferrite/silver bromide prepared by present embodiment is multiple The pattern of closing light catalyst is the cadmium ferrite that granular silver bromide area load has Perovskite Phase.
Cadmium ferrite/silver bromide the complex light prepared using Japanese JEM-2100 types transmission electron microscope observation embodiment 1 The pattern of catalyst, transmission electron microscope picture are as shown in figure 3, as can be seen from Fig., average grain diameter is that the silver bromide of 100~50nm is (black The bulky grain of color) be loaded with the less cadmium ferrite of particle (little particle of grey) nano particle on particle, and cadmium ferrite distribution It is more uniform, it is consistent with ESEM result.
Therefore, it can prove that cadmium ferrite/silver bromide compound photocatalyst is successfully prepared.
2nd, the photocatalysis performance of cadmium ferrite/silver bromide compound photocatalyst and potential application Journal of Sex Research
The cadmium ferrite that will be prepared in embodiment 1/silver bromide compound photocatalyst rhodamine B degradation solution, wherein rhodamine B Solution concentration 10mg/L, takes cadmium ferrite/silver bromide compound photocatalyst 25mg, first dark reaction 30min and reaches adsorption-desorption balance, Visible light catalytic reaction is carried out again, using 1000w xenon lamps as light source, extracts 1.5ml reaction solutions with dropper at regular intervals, It is put into supercentrifuge and is centrifuged 8 minutes, the light degradation situation of rhodamine B is detected using ultraviolet-uisible spectrophotometer.
Cadmium ferrite/silver bromide compound photocatalyst prepared by embodiment 1 is as shown in Figure 4 to the degradation property of rhodamine B. From fig. 4, it can be seen that rhodamine B degradation rate is 92% or so in 30 minutes, it is seen that have with cadmium ferrite/silver bromide compound photocatalyst There is photocatalytic activity higher.
With above-mentioned according to desirable embodiment of the invention as enlightenment, by above-mentioned description, relevant staff is complete Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention Property scope is not limited to the content on specification, it is necessary to its technical scope is determined according to right.

Claims (6)

1. a kind of preparation method of ferrous acid La doped silver bromide compound photocatalyst, it is characterized in that:Comprise the following steps:
(1) preparation of cadmium ferrite:In reaction vessel, lanthanum nitrate, ferric nitrate and citric acid are dissolved in solvent I, are heated to 60 ~80 DEG C and 30~60min of stirring, regulation pH value to 6~8, form gel, and 60~80 DEG C of 6~12h of drying are put into Muffle furnace In, 500~600 DEG C of 2~3h of sintering, grinding obtains cadmium ferrite;
(2) preparation of ferrous acid La doped silver bromide compound photocatalyst:The cadmium ferrite that will be prepared in step (1) adds solvent II In, 30~60min of ultrasonic disperse;Silver nitrate is added, 30~60min is stirred;Bromine source is added, 30~60min is stirred, centrifugation is washed Wash, 60~80 DEG C of 4~6h of drying.
2. the preparation method of a kind of ferrous acid La doped silver bromide compound photocatalyst according to claim 1, it is characterized in that: Solvent I is water or ethanol in described step (1).
3. the preparation method of a kind of ferrous acid La doped silver bromide compound photocatalyst according to claim 1, it is characterized in that: The quality of lanthanum nitrate is the 35~75% of ferric nitrate in described step (1), the quality of citric acid for ferric nitrate 50~ 100%.
4. the preparation method of a kind of ferrous acid La doped silver bromide compound photocatalyst according to claim 1, it is characterized in that: The adjusting method of pH value is adjusted using ammoniacal liquor or sodium hydroxide solution in described step (2).
5. the preparation method of a kind of ferrous acid La doped silver bromide compound photocatalyst according to claim 1, it is characterized in that: Bromine source is sodium bromide or KBr in described step (2).
6. the preparation method of a kind of ferrous acid La doped silver bromide compound photocatalyst according to claim 1, it is characterized in that: Solvent II is water, methyl alcohol or ethanol in described step (2), and the quality of cadmium ferrite is the 10~40% of silver nitrate, the matter in bromine source Measure is the 60~70% of silver nitrate.
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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN107081161A (en) * 2017-06-16 2017-08-22 天津工业大学 In AgBr catalysis materials and its synthetic method
CN107469846A (en) * 2017-09-22 2017-12-15 常州大学 A kind of preparation method of phosphorus doping ferrous acid Mn catalyst
CN108745378A (en) * 2018-06-12 2018-11-06 常州大学 A kind of LaFeO3/ZnIn2S4The preparation method of composite photo-catalyst
CN110860302A (en) * 2019-11-15 2020-03-06 辽宁师范大学 AgI/LaFeO3/g-C3N4Preparation method of composite photocatalyst
CN111389425A (en) * 2020-05-15 2020-07-10 福州大学 Perovskite photocatalytic material for removing algae in water body and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107081161A (en) * 2017-06-16 2017-08-22 天津工业大学 In AgBr catalysis materials and its synthetic method
CN107469846A (en) * 2017-09-22 2017-12-15 常州大学 A kind of preparation method of phosphorus doping ferrous acid Mn catalyst
CN108745378A (en) * 2018-06-12 2018-11-06 常州大学 A kind of LaFeO3/ZnIn2S4The preparation method of composite photo-catalyst
CN110860302A (en) * 2019-11-15 2020-03-06 辽宁师范大学 AgI/LaFeO3/g-C3N4Preparation method of composite photocatalyst
CN111389425A (en) * 2020-05-15 2020-07-10 福州大学 Perovskite photocatalytic material for removing algae in water body and preparation method thereof
CN111389425B (en) * 2020-05-15 2022-08-12 福州大学 Perovskite photocatalytic material for removing algae in water body and preparation method thereof

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