CN108043429A - A kind of preparation method of composite nano Tb/BiOCl materials - Google Patents

A kind of preparation method of composite nano Tb/BiOCl materials Download PDF

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CN108043429A
CN108043429A CN201810035900.8A CN201810035900A CN108043429A CN 108043429 A CN108043429 A CN 108043429A CN 201810035900 A CN201810035900 A CN 201810035900A CN 108043429 A CN108043429 A CN 108043429A
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solution
biocl
composite nano
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黄凤萍
辛萌
崔梦丽
刘博学
周鑫敏
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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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
    • B01J27/08Halides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/002Catalysts characterised by their physical properties
    • B01J35/004Photocatalysts
    • 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
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

Abstract

The invention discloses a kind of preparation methods of composite nano Tb/BiOCl materials, first add in potassium chloride in ethylene glycol, form solution A;Five nitric hydrate bismuths are added in ethylene glycol, solution B is formed, solution B then is added dropwise in solution A, and makes n (Bi):N (Cl)=1:1, continue to stir after being added dropwise to complete, then add in six nitric hydrate terbiums, and carry out ultrasonic vibration and obtain mixed solution;Then mixed solution is transferred in reaction kettle and sealed, be then placed in baking oven and reacted;After reaction, by reaction kettle cooled to room temperature, solid precipitation is collected, composite nano Tb/BiOCl materials are drying to obtain after washing.Nanometer Tb/BiOCl catalyst prepared by the present invention has higher catalytic degradation ability to methyl orange under visible light.

Description

A kind of preparation method of composite nano Tb/BiOCl materials
Technical field
The present invention relates to field of photocatalytic material, and in particular to a kind of preparation side of composite nano Tb/BiOCl materials Method.
Background technology
With the industrialized development of society, environmental pollution gradually aggravates.It produces and is sharply increased with the discharge capacity of sanitary sewage, Global water pollution is on the rise, and threatens social economy or even the sustainable development of mankind itself.Therefore, new dirt is developed It is extremely urgent to contaminate object treatment technology.Photocatalitic Technique of Semiconductor due to its application low energy consumption, scope it is wide and to environment without secondary The advantages that pollution, has got most of the attention since 20th century were found, and more and more researchers throw oneself into the research in this field.
Document " Chinese patent CN105214694A " discloses a kind of method that soft template method prepares BiOCl hollow shells, belongs to In nano-photocatalyst material preparation field.The invention synthesizes catalysis material by simple synthetic method and innocuous agents, full The environmentally protective requirement of foot, ionic liquid is not only used as bromine source and solvent, while is also served as oil phase and formed micro emulsion drop, right The formation important role of BiOCl hollow shells, prepared BiOCl hollow shells are prepared and selected in pollution control, new energy There is higher application value in the fields such as property catalysis oxidation.
Document " Chinese patent CN106391062A " discloses a kind of BiVO4/BiOCl heterojunction photocatalysts, the catalysis Agent is using BiOCl as core, and BiVO4 nanometer sheets are wrapped in the microballoon outside BiOCl cores, and microsphere diameter is 1~5 μm.The invention is closed Into BiVO4/ BiOCl photochemical catalysts have higher crystallinity, and are generated without other impurity;With wider photoresponse model It encloses, and there is higher Photocatalytic activity to organic dyestuff.
Document " Chinese patent CN105032452A " discloses a kind of K doping BiOCl photochemical catalysts of high visible-light activity Preparation method, the preparation method temperature is low, and process is simple, easily operated, can be continuously produced;Photochemical catalyst is made in this method With excellent visible light catalytic performance.
Document " Chinese patent CN103433022A " discloses a kind of visible-light response type Tb/BiVO4Catalyst and its system Preparation Method and application, main component BiVO4, for cubic zircon phase structure, and BiVO4Lattice in contain Tb3+.The invention Firing rate is fast, and homogeneous heating shortens the reaction time, improves work efficiency, the visible-light response type Tb/BiVO of synthesis4 Catalyst has higher photocatalytic activity, can be applied to environmental contaminants processing.
Document " Chinese patent CN104475133A " discloses a kind of preparation method of Bi/BiOCl photochemical catalysts, belongs to light Catalysis material field.The present invention is using a step combustion method, using bismuth nitrate, ammonium chloride and citric acid as raw material, by nitrate and Redox reaction between citric acid prepares Bi/BiOCl composite photo-catalysts.Unique Interaction enhanced of Bi and BiOCl Catalyst is to the absorbent properties of visible ray and accelerates the transport process of photo-generated carrier, reduces the compound of electron-hole pair Probability improves the quantum efficiency of visible light catalytic.There is the composite catalyzing material high degradation to have engine dyeing under visible light The performance of material.The preparation method of the present invention is simple for process, and preparation time is short, mild condition, of low cost, easily operated, is not required to Complex device is wanted, can be continuously produced.
In recent years, bismuth oxychloride (BiOCl) is paid close attention to be subject to more and more researchers, due to its unique two-dimensional layer The strong internal electric field effect of structure and its Internal architecture so that light induced electron is with hole under the action of its strong internal electric field It can reach and efficiently separate, thus BiOCl possesses and compares TiO2Higher photocatalysis efficiency.But on the one hand since BiOCl light is inhaled Side is received close to ultraviolet region, oneself is too weak in visible region absorption, causes too low to the utilization ratio of light;On the other hand its forbidden band Width is excessive (3.2-3.6eV), and light induced electron and hole excitation are difficult, its application is caused to be very restricted.
Rare earth element is applied to Photocatalyst field very early, and achieves success, such as La doping TiO2, Pr mixes Miscellaneous TiO2, Er doping ZnO, La, Nd, Sm doping ZnO, Y doping C3N4.Rare earth element introducing not only can effectively promote photocatalysis The response range to light of agent, and can narrow photochemical catalyst band gap.There is multinomial result of study to confirm rare earth doped Success, such as Gd doping β-Bi are also achieved in the modification field of bismuth series photocatalyst2O3, Er doping Bi24O31Br10, La doping Bi2MoO6, Nd doping BiFeO3, Eu doping Bi2S3.But the research being modified at present using rare earth element to BiOCl is less.
The content of the invention
It is above-mentioned existing to overcome it is an object of the invention to provide a kind of preparation method of composite nano Tb/BiOCl materials The defects of with the presence of technology, nanometer Tb/BiOCl catalyst prepared by the present invention have higher urge to methyl orange under visible light Change degradation capability.
In order to achieve the above objectives, the present invention adopts the following technical scheme that:
A kind of preparation method of composite nano Tb/BiOCl materials, comprises the following steps:
Step 1:KCl is added in into (CH2OH)2In, form solution A;By Bi (NO3)3·5H2O adds in (CH2OH)2In, shape Into solution B, wherein per 17mL (CH2OH)2The middle KCl for adding in 0.2g~0.3g, per 17mL (CH2OH)2It is middle to add in 0.9g~1g's Bi(NO3)3·5H2O;
Step 2:Solution B is added dropwise in solution A, and makes n (Bi):N (Cl)=1:1, continue to stir after being added dropwise to complete, Then Tb (NO are added in3)3·6H2O, and Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 0.1% of the mole of O~ 5%, and carry out ultrasonic vibration and obtain mixed solution;
Step 3:Mixed solution is transferred in reaction kettle and is sealed, baking oven is then placed in and is reacted;
Step 4:After reaction, by reaction kettle cooled to room temperature, solid precipitation is collected, is drying to obtain after washing Composite nano Tb/BiOCl materials.
Further, continue to stir 30min after being added dropwise to complete in step 2.
Further, the power of ultrasonic vibration is 40kHz, time 15min in step 2.
Further, reaction temperature is 140~200 DEG C in step 3, and the reaction time is 3~12h.
Further, washed respectively 3 times using deionized water and ethyl alcohol in step 4.
Further, drying temperature is 80 DEG C in step 4, time 12h.
Compared with prior art, the present invention has technique effect beneficial below:
The present invention is doped modification with rare earth element terbium to BiOCl.Since BiOCl optical absorption edges lean on black light Area, it is too weak from being absorbed in visible region, cause too low to the utilization ratio of light;On the other hand excessive (the 3.2- of its energy gap 3.6eV), light induced electron and hole excitation are difficult, its application is caused to be very restricted.With reference to the characteristics of rare earth element, fortune Compound Tb/BiOCl is prepared with solvent-thermal method, the doping of rare earth terbium can effectively reduce BiOCl energy gaps, the band gap of sample Width reduces so that sample is more easy to be excited, while the distance shortening of electron hole mobility prevents light induced electron and hole moving Occur compound during moving, also, Tb can effectively capture the electronics being excited, so as to reduce light induced electron and hole Compound probability.In addition the preparation method of the composite material is simple, easy to operate, is conducive to mass produce.It is dropped in photocatalysis Application in solution, experiments have shown that Tb/BiOCl prepared by the present invention has reached the photocatalytic degradation effect of methyl orange in 120min To 75%, therefore the nanometer Tb/BiOCl catalyst prepared has higher catalytic degradation energy to methyl orange under visible light Power.
Description of the drawings
Fig. 1 is the XRD spectra for the bismuth oxychloride photocatalyst that terbium doped amount is 1%;
Fig. 2 is that the SEM of pure bismuth oxychloride schemes;
Fig. 3 is the energy spectrum diagram of pure bismuth oxychloride;
Fig. 4 is the SEM figures for the compound bismuth oxychloride that terbium volume is 1%;
Fig. 5 is the energy spectrum diagram for the compound bismuth oxychloride that terbium volume is 1%;
Fig. 6 is degradation comparison diagram of the pure bismuth oxychloride with the bismuth oxychloride that terbium volume is 1% to methyl orange.
Specific embodiment
Embodiments of the present invention are described in further detail below:
The present invention prepares the composite nano Tb/ under visible light with excellent photocatalysis performance using solvent-thermal method The method of BiOCl materials, with (CH2OH)2、KCl、Bi(NO3)3·5H2O is raw material, n (Bi):N (Cl)=1:1, temperature 140 ~200 DEG C, Tb (NO3)3·6H2O (Tb molar fractions are 0.1%~5%), blank sample is added without Tb (NO3)3·6H2O, Anti- 3~12h in 40mL stainless steel Teflon liner reaction kettles, prepares composite nano Tb/BiOCl, is as follows:
1) 17mL (CH at room temperature, are taken2OH)2In beaker, the KCl of 0.2~0.3g is added in, until it is molten to form clear Liquid A;Take 17mL (CH2OH)2In three-necked flask, the Bi (NO of 0.9~1g are added in3)3·5H2O, mechanical agitation are clarified until being formed Clear solution B;
2) solution B is added dropwise in solution A, and ensures n (Bi):N (Cl)=1:1, continue to be vigorously stirred after being added dropwise to complete 30min adds in Tb (NO3)3·6H2O, and Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 0.1% of the mole of O~ 5%, it is put into 40kHz in ultrasonic cleaner and shakes 15min;
3) stop ultrasonic vibration, acquired solution is transferred in 40mL stainless steel Teflon liner reaction kettles, is put into after sealing 3~12h is reacted in baking oven at a temperature of 140~200 DEG C;
4) reaction kettle cooled to room temperature outwells liquid in reaction kettle, collects solid precipitation, deionized water, ethyl alcohol are each It washes 3 times, dry 12h, obtains sample at 80 DEG C.
The present invention is described in further detail with reference to embodiment:
Embodiment 1
1) 17mL (CH at room temperature, are taken2OH)2In beaker, the KCl of 0.2g is added in, until forming clear transparent solutions A;It takes 17mL(CH2OH)2In three-necked flask, the Bi (NO of 0.9g are added in3)3·5H2O, mechanical agitation is until form clear transparent solutions B;
2) solution B is added dropwise in solution A, continues to be vigorously stirred 30min after being added dropwise to complete, add in Tb (NO3)3·6H2O, And Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 1% of the mole of O is put into 40kHz in ultrasonic cleaner and shakes 15min;
3) stop ultrasonic vibration, acquired solution is transferred in 40mL stainless steel Teflon liner reaction kettles, is put into after sealing 180 DEG C of reaction 9h in baking oven;
4) reaction kettle cooled to room temperature outwells liquid in reaction kettle, collects solid precipitation, deionized water, ethyl alcohol are each It washes 3 times, dry 12h, obtains sample at 80 DEG C.
Embodiment 2
1) 17mL (CH at room temperature, are taken2OH)2In beaker, the KCl of 0.28g is added in, until forming clear transparent solutions A; Take 17mL (CH2OH)2In three-necked flask, the Bi (NO of 0.97g are added in3)3·5H2O, mechanical agitation is until formation clear is molten Liquid B;
2) solution B is added dropwise in solution A, continues to be vigorously stirred 30min after being added dropwise to complete, add in Tb (NO3)3·6H2O, And Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 1% of the mole of O is put into 40kHz in ultrasonic cleaner and shakes 15min;
3) stop ultrasonic vibration, acquired solution is transferred in 40mL stainless steel Teflon liner reaction kettles, is put into after sealing 180 DEG C of reaction 9h in baking oven;
4) reaction kettle cooled to room temperature outwells liquid in reaction kettle, collects solid precipitation, deionized water, ethyl alcohol are each It washes 3 times, dry 12h, obtains sample at 80 DEG C.
Embodiment 3
1) 17mL (CH at room temperature, are taken2OH)2In beaker, the KCl of 0.3g is added in, until forming clear transparent solutions A;It takes 17mL(CH2OH)2In three-necked flask, the Bi (NO of 1g are added in3)3·5H2O, mechanical agitation is until form clear transparent solutions B;
2) solution B is added dropwise in solution A, continues to be vigorously stirred 30min after being added dropwise to complete, add in Tb (NO3)3·6H2O, And Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 1% of the mole of O is put into 40kHz in ultrasonic cleaner and shakes 15min;
3) stop ultrasonic vibration, acquired solution is transferred in 40mL stainless steel Teflon liner reaction kettles, is put into after sealing 180 DEG C of reaction 9h in baking oven;
4) reaction kettle cooled to room temperature outwells liquid in reaction kettle, collects solid precipitation, deionized water, ethyl alcohol are each It washes 3 times, dry 12h, obtains sample at 80 DEG C.
Embodiment 4
1) 17mL (CH at room temperature, are taken2OH)2In beaker, the KCl of 0.28g is added in, until forming clear transparent solutions A; Take 17mL (CH2OH)2In three-necked flask, the Bi (NO of 0.97g are added in3)3·5H2O, mechanical agitation is until formation clear is molten Liquid B;
2) solution B is added dropwise in solution A, continues to be vigorously stirred 30min after being added dropwise to complete, add in Tb (NO3)3·6H2O, And Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 0.1% of the mole of O is put into 40kHz in ultrasonic cleaner and shakes Swing 15min;
3) stop ultrasonic vibration, 3) acquired solution is transferred in 40mL stainless steel Teflon liner reaction kettles, is put after sealing Enter 180 DEG C of reaction 9h in baking oven;
4) reaction kettle cooled to room temperature outwells liquid in reaction kettle, collects solid precipitation, deionized water, ethyl alcohol are each It washes 3 times, dry 12h, obtains sample at 80 DEG C.
Embodiment 5
1) 17mL (CH at room temperature, are taken2OH)2In beaker, the KCl of 0.28g is added in, until forming clear transparent solutions A; Take 17mL (CH2OH)2In three-necked flask, the Bi (NO of 0.97g are added in3)3·5H2O, mechanical agitation is until formation clear is molten Liquid B;
2) solution B is added dropwise in solution A, continues to be vigorously stirred 30min after being added dropwise to complete, add in Tb (NO3)3·6H2O, And Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 5% of the mole of O is put into 40kHz in ultrasonic cleaner and shakes 15min;
3) stop ultrasonic vibration, acquired solution is transferred in 40mL stainless steel Teflon liner reaction kettles, is put into after sealing 180 DEG C of reaction 9h in baking oven;
4) reaction kettle cooled to room temperature outwells liquid in reaction kettle, collects solid precipitation, deionized water, ethyl alcohol are each It washes 3 times, dry 12h, obtains sample at 80 DEG C.Alcohol is respectively washed 3 times, and dry 12h, obtains sample at 80 DEG C.
Embodiment 6
1) 17mL (CH at room temperature, are taken2OH)2In beaker, the KCl of 0.28g is added in, until forming clear transparent solutions A; Take 17mL (CH2OH)2In three-necked flask, the Bi (NO of 0.97g are added in3)3·5H2O, mechanical agitation is until formation clear is molten Liquid B;
2) solution B is added dropwise in solution A, continues to be vigorously stirred 30min after being added dropwise to complete, add in Tb (NO3)3·6H2O, And Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 1% of the mole of O is put into 40kHz in ultrasonic cleaner and shakes 15min;
3) stop ultrasonic vibration, acquired solution is transferred in 40mL stainless steel Teflon liner reaction kettles, is put into after sealing 160 DEG C of reaction 9h in baking oven;
4) reaction kettle cooled to room temperature outwells liquid in reaction kettle, collects solid precipitation, deionized water, ethyl alcohol are each It washes 3 times, dry 12h, obtains sample at 80 DEG C.
Embodiment 7
1) 17mL (CH at room temperature, are taken2OH)2In beaker, the KCl of 0.28g is added in, until forming clear transparent solutions A; Take 17mL (CH2OH)2In three-necked flask, the Bi (NO of 0.97g are added in3)3·5H2O, mechanical agitation is until formation clear is molten Liquid B;
2) solution B is added dropwise in solution A, continues to be vigorously stirred 30min after being added dropwise to complete, add in Tb (NO3)3·6H2O, And Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 1% of the mole of O is put into 40kHz in ultrasonic cleaner and shakes 15min;
3) stop ultrasonic vibration, acquired solution is transferred in 40mL stainless steel Teflon liner reaction kettles, is put into after sealing 140 DEG C of reaction 9h in baking oven;
4) reaction kettle cooled to room temperature outwells liquid in reaction kettle, collects solid precipitation, deionized water, ethyl alcohol are each It washes 3 times, dry 12h, obtains sample at 80 DEG C.
Embodiment 8
1) 17mL (CH at room temperature, are taken2OH)2In beaker, the KCl of 0.28g is added in, until forming clear transparent solutions A; Take 17mL (CH2OH)2In three-necked flask, the Bi (NO of 0.97g are added in3)3·5H2O, mechanical agitation is until formation clear is molten Liquid B;
2) solution B is added dropwise in solution A, continues to be vigorously stirred 30min after being added dropwise to complete, add in Tb (NO3)3·6H2O, And Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 1% of the mole of O is put into 40kHz in ultrasonic cleaner and shakes 15min;
3) stop ultrasonic vibration, acquired solution is transferred in 40mL stainless steel Teflon liner reaction kettles, is put into after sealing 200 DEG C of reaction 9h in baking oven;
4) reaction kettle cooled to room temperature outwells liquid in reaction kettle, collects solid precipitation, deionized water, ethyl alcohol are each It washes 3 times, dry 12h, obtains sample at 80 DEG C.
Embodiment 9
1) 17mL (CH at room temperature, are taken2OH)2In beaker, the KCl of 0.28g is added in, until forming clear transparent solutions A; Take 17mL (CH2OH)2In three-necked flask, the Bi (NO of 0.97g are added in3)3·5H2O, mechanical agitation is until formation clear is molten Liquid B;
2) solution B is added dropwise in solution A, continues to be vigorously stirred 30min after being added dropwise to complete, add in Tb (NO3)3·6H2O, And Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 1% of the mole of O is put into 40kHz in ultrasonic cleaner and shakes 15min;
3) stop ultrasonic vibration, acquired solution is transferred in 40mL stainless steel Teflon liner reaction kettles, is put into after sealing 180 DEG C of reaction 3h in baking oven;
4) reaction kettle cooled to room temperature outwells liquid in reaction kettle, collects solid precipitation, deionized water, ethyl alcohol are each It washes 3 times, dry 12h, obtains sample at 80 DEG C.
Embodiment 10
1) 17mL (CH at room temperature, are taken2OH)2In beaker, the KCl of 0.28g is added in, until forming clear transparent solutions A; Take 17mL (CH2OH)2In three-necked flask, the Bi (NO of 0.97g are added in3)3·5H2O, mechanical agitation is until formation clear is molten Liquid B;
2) solution B is added dropwise in solution A, continues to be vigorously stirred 30min after being added dropwise to complete, add in Tb (NO3)3·6H2O, And Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 1% of the mole of O is put into 40kHz in ultrasonic cleaner and shakes 15min;
3) stop ultrasonic vibration, acquired solution is transferred in 40mL stainless steel Teflon liner reaction kettles, is put into after sealing 160 DEG C of reaction 6h in baking oven;
4) reaction kettle cooled to room temperature outwells liquid in reaction kettle, collects solid precipitation, deionized water, ethyl alcohol are each It washes 3 times, dry 12h, obtains sample at 80 DEG C.
Embodiment 11
1) 17mL (CH at room temperature, are taken2OH)2In beaker, the KCl of 0.28g is added in, until forming clear transparent solutions A; Take 17mL (CH2OH)2In three-necked flask, the Bi (NO of 0.97g are added in3)3·5H2O, mechanical agitation is until formation clear is molten Liquid B;
2) solution B is added dropwise in solution A, continues to be vigorously stirred 30min after being added dropwise to complete, add in Tb (NO3)3·6H2O, And Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 1% of the mole of O is put into 40kHz in ultrasonic cleaner and shakes 15min;
3) stop ultrasonic vibration, acquired solution is transferred in 40mL stainless steel Teflon liner reaction kettles, is put into after sealing 160 DEG C of reaction 12h in baking oven;
4) reaction kettle cooled to room temperature outwells liquid in reaction kettle, collects solid precipitation, deionized water, ethyl alcohol are each It washes 3 times, dry 12h, obtains sample at 80 DEG C.
The present invention takes the photocatalysis performance of compound nanometer Tb/BiOCl materials the method for degradation methyl orange to carry out Test, nanometer Tb/BiOCl and pure BiOCl microballoons are put into the methyl orange solution of 50ml concentration 10mg/L, it is seen that light source irradiates Its absorbance is surveyed in separation after 2h, and the degradation rate for calculating methyl orange is understood, in the compound nanometer Tb/BiOCl of embodiment 1 to methyl orange Degradation reach 75%, pure BiOCl microballoons are only 54% to the degradation rate of methyl orange, it is seen that the light of BiOCl is urged in the doping of terbium Changing activity has a larger impact, and the doping of rare earth Tb effectively reduces the energy gap of BiOCl, the band gap width of sample become smaller so that Sample is more easy to be excited by light, while the distance shortening of electron hole mobility prevents light induced electron and hole in transition process Compound, raising photocatalytic activity occurs.

Claims (6)

1. a kind of preparation method of composite nano Tb/BiOCl materials, which is characterized in that comprise the following steps:
Step 1:KCl is added in into (CH2OH)2In, form solution A;By Bi (NO3)3·5H2O adds in (CH2OH)2In, form solution B, wherein per 17mL (CH2OH)2The middle KCl for adding in 0.2g~0.3g, per 17mL (CH2OH)2The middle Bi for adding in 0.9g~1g (NO3)3·5H2O;
Step 2:Solution B is added dropwise in solution A, and makes n (Bi):N (Cl)=1:1, continue to stir after being added dropwise to complete, then Add in Tb (NO3)3·6H2O, and Tb (NO3)3·6H2O additions are Bi (NO3)3·5H2The 0.1%~5% of the mole of O, and It carries out ultrasonic vibration and obtains mixed solution;
Step 3:Mixed solution is transferred in reaction kettle and is sealed, baking oven is then placed in and is reacted;
Step 4:After reaction, by reaction kettle cooled to room temperature, solid precipitation is collected, is drying to obtain after washing compound Type nanometer Tb/BiOCl materials.
A kind of 2. preparation method of composite nano Tb/BiOCl materials according to claim 1, which is characterized in that step Continue to stir 30min after being added dropwise to complete in two.
A kind of 3. preparation method of composite nano Tb/BiOCl materials according to claim 1, which is characterized in that step The power of ultrasonic vibration is 40kHz, time 15min in two.
A kind of 4. preparation method of composite nano Tb/BiOCl materials according to claim 1, which is characterized in that step Reaction temperature is 140~200 DEG C in three, and the reaction time is 3~12h.
A kind of 5. preparation method of composite nano Tb/BiOCl materials according to claim 1, which is characterized in that step It is washed respectively 3 times using deionized water and ethyl alcohol in four.
A kind of 6. preparation method of composite nano Tb/BiOCl materials according to claim 1, which is characterized in that step Drying temperature is 80 DEG C in four, time 12h.
CN201810035900.8A 2018-01-15 2018-01-15 A kind of preparation method of composite nano Tb/BiOCl materials Pending CN108043429A (en)

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CN110270365A (en) * 2019-07-23 2019-09-24 福州大学 A kind of preparation and application of carbonitride/Lanthanum monochloride monoxide composite material
CN111250142A (en) * 2020-03-31 2020-06-09 上海电力大学 Preparation method, product and application of graphite-phase carbon nitride/high-iodine bismuth oxyiodide heterojunction with up-conversion characteristic
CN111569913A (en) * 2020-05-13 2020-08-25 南昌航空大学 Gd (Gd)3+Preparation method of doped BiOBr photocatalytic material
CN112619674A (en) * 2020-12-29 2021-04-09 桐乡市启诚科技合伙企业(有限合伙) Tb-doped spherical BiOCl loaded ZnO photocatalytic degradation material and preparation method thereof
CN112844361A (en) * 2021-01-25 2021-05-28 江南大学 Tb3+ -B codoped modified TiO2Photocatalytic film and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN110270365A (en) * 2019-07-23 2019-09-24 福州大学 A kind of preparation and application of carbonitride/Lanthanum monochloride monoxide composite material
CN110270365B (en) * 2019-07-23 2021-04-27 福州大学 Preparation and application of carbon nitride/lanthanum oxychloride composite material
CN111250142A (en) * 2020-03-31 2020-06-09 上海电力大学 Preparation method, product and application of graphite-phase carbon nitride/high-iodine bismuth oxyiodide heterojunction with up-conversion characteristic
CN111569913A (en) * 2020-05-13 2020-08-25 南昌航空大学 Gd (Gd)3+Preparation method of doped BiOBr photocatalytic material
CN112619674A (en) * 2020-12-29 2021-04-09 桐乡市启诚科技合伙企业(有限合伙) Tb-doped spherical BiOCl loaded ZnO photocatalytic degradation material and preparation method thereof
CN112844361A (en) * 2021-01-25 2021-05-28 江南大学 Tb3+ -B codoped modified TiO2Photocatalytic film and preparation method thereof

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