CN109772373A - A kind of preparation method with visible light-responded rGO/ black bismuth oxychloride-bismuth-bismuth oxide heterojunction photocatalyst - Google Patents
A kind of preparation method with visible light-responded rGO/ black bismuth oxychloride-bismuth-bismuth oxide heterojunction photocatalyst Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods with visible light-responded rGO/ black bismuth oxychloride-bismuth-bismuth oxide heterojunction photocatalyst, method includes 1) sufficiently dissolving in chlorine source in GO solution, form precursor solution, bismuth source is dissolved in this precursor solution again afterwards, PH is adjusted with ammonium hydroxide, product as off-white solid is obtained, this product is washed with deionized as neutrality, it is dry at 60 DEG C, obtain BiOCl/GO compound；2) BiOCl/GO compound 3.0g is taken to be dissolved in 150ml deionized water, excessive reduced iron powder is added after mixing, 20ml hydrochloric acid is added after a period of time, 8h is persistently stirred at room temperature, first residual F e powder is removed after fully reacting, products therefrom is washed with deionized as neutrality again, it is dry at 80 DEG C, obtain rGO/ black bismuth oxychloride-bismuth-bismuth oxide heterojunction photocatalyst.Photochemical catalyst chemical property prepared by the present invention is stable, forbidden bandwidth is narrow, has compared with strong light absorption, preferable photocatalysis degradation organic contaminant ability, and higher power of regeneration.
Description
Technical field
The present invention relates to method for preparing catalyst technical fields, and in particular to a kind of with visible light-responded rGO/ black
Bismuth oxychloride-bismuth-bismuth oxide heterojunction photocatalyst preparation method.
Background technique
Now, social economy's high speed development, the following environmental problem can not be ignored, and water pollution is as environment dirt
One of main aspect of dye, the concern vast by all circles, and the main reason for the discharge of industrial wastewater is then water pollution.For a long time
Larger potential risk, or even meeting carcinogenic, teratogenesis and mutagenesis can be constituted to human health by drinking contaminated water, therefore, urgently
It needs environmentalist to develop some efficient technologies to handle actual industrial waste water, reaches the discharge mark of national defined
It is quasi-.
Conductor photocatalysis is as a kind of very promising high-level oxidation technology, the mild, preparation process with reaction condition
Easy, the advantages that low energy consumption, reaction speed is fast, can efficient degradation Some Organic Pollutants, or even can also be translated into CO2、
H2The inorganic molecules substance such as O.Therefore, flat to mitigating circumstances problem, maintenance ecology using photocatalysis technology processing industrial wastewater
Weighing apparatus realizes that sustainable development is of great significance.
Traditional photochemical catalyst such as TiO2With ZnO have broad-band gap, only it is active in the ultraviolet region (UV), light induced electron and
The recombination rate in hole is fast, and quantum efficiency is low, limits their practical applications in the treatment of waste water；The BiOCl then researched and developed
Photochemical catalyst is because of its unique electrical and optical properties, non-toxic, highly corrosion resistant, and compares TiO2In degradation of organic substances more
High ultraviolet light photocatalysis is active and is greatly paid close attention to.But and TiO2Similar, BiOCl has the broad-band gap of 3.4eV, only
With UV activation, cause visible light photocatalysis active poor.
Based on BiOCl nanoparticle band-gap energy it is larger only to ultraviolet light response the shortcomings that, we using surface defect improve
Method, while introduce with the matched Bi of its bandgap structure2O3And reduced graphene goes to improve its photocatalysis performance.Resulting production
Object has good light sensitivity, stability and an inoxidizability, and it is visible light-responded it is strong, reusing is good, in photocatalytic degradation
Organic substance, photocatalytic water, photoelectric conversion in actual industrial waste water etc. have significant effect.
Currently, researcher has gone out black BiOCl by Fe powder reduction synthesis, also graphene oxide is restored using Fe powder
Reduced graphene is made, but still there is the problems such as to visible light-responded difference.The present invention relates to one kind with visible light-responded
Graphene/blackBiOCl-Bi-Bi2O3The preparation method of heterojunction photocatalyst, the photochemical catalyst have high stability, height
The advantages that adsorptivity, high reusing, has preferable photocatalysis performance under visible light.
Summary of the invention
Problem to be solved by this invention is: providing a kind of with visible light-responded rGO/ black bismuth oxychloride-bismuth-three
The preparation of two bismuth heterojunction photocatalysts is aoxidized, the chemical property of the photochemical catalyst prepared is stable, forbidden bandwidth is narrow, has
The ability of stronger light absorption, preferable photocatalysis degradation organic contaminant, and there is higher power of regeneration.
The present invention in order to solve the above problem provided by technical solution are as follows: it is a kind of with visible light-responded rGO/ black chlorine
The preparation of bismuth oxide-bismuth-bismuth oxide heterojunction photocatalyst, the preparation method comprises the following steps,
1) chlorine source is sufficiently dissolved in GO solution, forms precursor solution, is then again dissolved completely in bismuth source before this
It drives in liquid solution, adjusts PH with ammonia spirit, be continuously stirred at room temperature a period of time, finally obtain product as off-white solid,
Product as off-white solid is washed with deionized as neutrality, it is then dry at 60 DEG C, obtain BiOCl/GO compound；
2) above-mentioned BiOCl/GO compound 3.0g is taken to be dissolved in 150ml deionized water, uniformly rear be added to be mixed is excessively gone back
Former iron powder is added 20ml hydrochloric acid, is continuously stirred at room temperature 8h, first removes remaining Fe powder after fully reacting after a period of time
It goes, then products therefrom is washed with deionized as neutrality, it is then dry at 80 DEG C, finally obtain rGO/ black oxychloride
Bismuth-bismuth-bismuth oxide (rGO/black BiOCl-Bi-Bi2O3) heterojunction photocatalyst.
Preferably, the chlorine source in the step 1) is any in potassium chloride or sodium chloride.
Preferably, the bismuth source in the step 1) is five nitric hydrate bismuths.
Preferably, the chlorine source in the step 1) and bismuth source molar ratio are 1:1.
Preferably, the quality of the GO can be any one in 0.02g, 0.04g, 0.08g, 0.15g, 0.30g, 0.45g
Kind.
Compared with prior art, the invention has the advantages that
(1) preparation method of photochemical catalyst of the present invention is that coprecipitation, reaction condition easily reach at room temperature, and operation is simple,
Low energy consumption, and applicability is wide；
(2) present invention can regulate and control rGO/ black bismuth oxychloride-bismuth-bismuth oxide by the dosage (g) of regulation GO
(rGO/black BiOCl-Bi-Bi2O3) heterojunction photocatalyst spectral absorption range；
(3) chemical property of photochemical catalyst prepared by the present invention is stablized, and has stronger light absorption and light to urge under visible light
Change degradation capability, and there is higher stability and regenerability.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present invention, constitutes a part of the invention, this hair
Bright illustrative embodiments and their description are used to explain the present invention, and are not constituted improper limitations of the present invention.
Fig. 1 is black bismuth oxychloride-bismuth-three of different GO contents (g) prepared in the embodiment of the present invention 1 and example 6
Aoxidize two bismuth black BiOCl-Bi-Bi2O3Heterojunction photocatalyst: a:black BiOCl-Bi-Bi2O3(GO content is 0g),
b:black BiOCl-Bi-Bi2O3/rGO0.3(GO content is 0.30g).The XRD spectrum of contrast sample is as seen from the figure, appropriate to increase
Less change occurs for the X-ray diffraction peak of the amount of more GO, sample, and peak is more sharp, illustrates the crystallinity of material after reduction
It improves, is conducive to photocatalysis.
Fig. 2 is the diffusing reflection figure and band-gap energy map of prepared photochemical catalyst in the embodiment of the present invention 1 and example 6.By scheming
It is found that response of the catalyst to visible light has been widened in the increase of GO amount, its forbidden bandwidth is made to become smaller.
Fig. 3 is that nitrogen adsorption-desorption of prepared photochemical catalyst and pore-size distribution are bent in the embodiment of the present invention 1 and example 6
Line, as seen from the figure, when GO is 0g, specific surface area 8.91m2/g；When GO is 0.30g, specific surface area 18.95m2/g.With
Increasing for GO amount, specific surface area increases with it, and illustrates that the Surface and internal structure of material changes, this also demonstrates iron
A possibility that powder restores.
Fig. 4 is degradation o-nitrophenol under the visible light of photochemical catalyst prepared in the embodiment of the present invention 1 and example 6
Curve, as seen from the figure, the appropriate amount for increasing GO, hence it is evident that be conducive to improve photocatalytic activity.
Specific embodiment
Carry out the embodiment that the present invention will be described in detail below in conjunction with accompanying drawings and embodiments, how the present invention is applied whereby
Technological means solves technical problem and reaches the realization process of technical effect to fully understand and implement.
Embodiment 1
(1) KCl of 0.02mol is added in 150ml deionized water, ultrasonic dissolution, forms clear solution.
(2) by the Bi (NO of 0.02mol3)3·5H2O is added in the above solution, magnetic agitation, it is to be mixed uniformly after use ammonia
Solution PH is adjusted to 10 by water, persistently stirs 12h at room temperature, obtains product as off-white solid.
(3) product as off-white solid is washed with deionized as neutrality, it is then dry at 60 DEG C, it is multiple to obtain BiOCl/GO
Close object.
(4) above-mentioned BiOCl/GO compound 3.0g is taken to be added in the three-necked flask for filling 150ml deionized water, stirring one
Section time, uniformly rear addition 2.4g reduced iron powder to be mixed are added 20ml hydrochloric acid, are continuously stirred at room temperature after a period of time
8h removes remaining reduction Fe powder after fully reacting.
(5) products therefrom is washed with deionized until neutral, the then drying at 80 DEG C.Up to rGO/ black oxychloride
Bismuth-bismuth-bismuth oxide (rGO/black BiOCl-Bi-Bi2O3) heterojunction photocatalyst
Embodiment 2
(1) KCl of 0.02mol is added in the GO solution containing 0.02g, ultrasonic dissolution, forms clear solution.
(2) by the Bi (NO of 0.02mol3)3·5H2O is added in the above solution, magnetic agitation, it is to be mixed uniformly after use ammonia
Solution PH is adjusted to 10 by water, persistently stirs 12h at room temperature, obtains product as off-white solid.
(3) product as off-white solid is washed with deionized as neutrality, it is then dry at 60 DEG C, it is multiple to obtain BiOCl/GO
Close object.
(4) above-mentioned BiOCl/GO compound 3.0g is taken to be added in the three-necked flask for filling 150ml deionized water, stirring one
Section time, the uniformly rear excessive reduced iron powder of addition to be mixed are added 20ml hydrochloric acid, are continuously stirred at room temperature 8 after a period of time
H removes remaining reduction Fe powder after fully reacting.
(5) products therefrom is washed with deionized until neutral, the then drying at 80 DEG C.Up to rGO/ black oxychloride
Bismuth-bismuth-bismuth oxide (rGO/black BiOCl-Bi-Bi2O3) heterojunction photocatalyst.
Embodiment 3
(1) KCl of 0.02mol is added in the GO solution containing 0.04g, ultrasonic dissolution, forms clear solution.
(2) by the Bi (NO of 0.02mol3)3·5H2O is added in the above solution, magnetic agitation, it is to be mixed uniformly after use ammonia
Solution PH is adjusted to 10 by water, persistently stirs 12h at room temperature, obtains product as off-white solid.
(3) product as off-white solid is washed with deionized as neutrality, it is then dry at 60 DEG C, it is multiple to obtain BiOCl/GO
Close object.
(4) above-mentioned BiOCl/GO compound 3.0g is taken to be added in the three-necked flask for filling 150ml deionized water, stirring one
Section time, uniformly rear addition 2.4g reduced iron powder to be mixed are added 20ml hydrochloric acid, are continuously stirred at room temperature after a period of time
8h removes remaining reduction Fe powder after fully reacting.
(5) products therefrom is washed with deionized until neutral, the then drying at 80 DEG C.Up to rGO/ black oxychloride
Bismuth-bismuth-bismuth oxide (rGO/black BiOCl-Bi-Bi2O3) heterojunction photocatalyst
Embodiment 4
(1) KCl of 0.02mol is added in the GO solution containing 0.08g, ultrasonic dissolution, forms clear solution.
(2) by the Bi (NO of 0.02mol3)3·5H2O is added in the above solution, magnetic agitation, it is to be mixed uniformly after use ammonia
Solution PH is adjusted to 10 by water, persistently stirs 12h at room temperature, obtains product as off-white solid.
(3) product as off-white solid is washed with deionized as neutrality, it is then dry at 60 DEG C, it is multiple to obtain BiOCl/GO
Close object.
(4) above-mentioned BiOCl/GO compound 3.0g is taken to be added in the three-necked flask for filling 150ml deionized water, stirring one
Section time, the uniformly rear excessive reduced iron powder of addition to be mixed are added 20ml hydrochloric acid, are continuously stirred at room temperature 8 after a period of time
H removes remaining reduction Fe powder after fully reacting.
(5) products therefrom is washed with deionized until neutral, the then drying at 80 DEG C.Up to rGO/ black oxychloride
Bismuth-bismuth-bismuth oxide (rGO/black BiOCl-Bi-Bi2O3) heterojunction photocatalyst
Embodiment 5
(1) KCl of 0.02mol is added in the GO solution containing 0.15g, ultrasonic dissolution, forms clear solution.
(2) by the Bi (NO of 0.02mol3)3·5H2O is added in the above solution, magnetic agitation, it is to be mixed uniformly after use ammonia
Solution PH is adjusted to 10 by water, persistently stirs 12h at room temperature, obtains product as off-white solid.
(3) product as off-white solid is washed with deionized as neutrality, it is then dry at 60 DEG C, it is multiple to obtain BiOCl/GO
Close object.
(4) above-mentioned BiOCl/GO compound 3.0g is taken to be added in the three-necked flask for filling 150ml deionized water, stirring one
Section time, the uniformly rear excessive reduced iron powder of addition to be mixed are added 20ml hydrochloric acid, are continuously stirred at room temperature 8 after a period of time
H removes remaining reduction Fe powder after fully reacting.
(5) products therefrom is washed with deionized until neutral, the then drying at 80 DEG C.Up to rGO/ black oxychloride
Bismuth-bismuth-bismuth oxide (rGO/black BiOCl-Bi-Bi2O3) heterojunction photocatalyst.
Embodiment 6
(1) KCl of 0.02mol is added in the GO solution containing 0.30g, ultrasonic dissolution, forms clear solution.
(2) by the Bi (NO of 0.02mol3)3·5H2O is added in the above solution, magnetic agitation, it is to be mixed uniformly after use ammonia
Solution PH is adjusted to 10 by water, persistently stirs 12h at room temperature, obtains product as off-white solid.
(3) product as off-white solid is washed with deionized as neutrality, it is then dry at 60 DEG C, it is multiple to obtain BiOCl/GO
Close object.
(4) above-mentioned BiOCl/GO compound 3.0g is taken to be added in the three-necked flask for filling 150ml deionized water, stirring one
Section time, the uniformly rear excessive reduced iron powder of addition to be mixed are added 20ml hydrochloric acid, are continuously stirred at room temperature 8 after a period of time
H removes remaining reduction Fe powder after fully reacting.
(5) products therefrom is washed with deionized until neutral, the then drying at 80 DEG C.Up to rGO/ black oxychloride
Bismuth-bismuth-bismuth oxide (rGO/black BiOCl-Bi-Bi2O3) heterojunction photocatalyst.
Embodiment 7
(1) KCl of 0.02mol is added in the GO solution containing 0.45g, ultrasonic dissolution, forms clear solution.
(2) by the Bi (NO of 0.02mol3)3·5H2O is added in the above solution, magnetic agitation, it is to be mixed uniformly after use ammonia
Solution PH is adjusted to 10 by water, persistently stirs 12h at room temperature, obtains product as off-white solid.
(3) product as off-white solid is washed with deionized as neutrality, it is then dry at 60 DEG C, it is multiple to obtain BiOCl/GO
Close object.
(4) above-mentioned BiOCl/GO compound 3.0g is taken to be added in the three-necked flask for filling 150ml deionized water, stirring one
Section time, the uniformly rear excessive reduced iron powder of addition to be mixed are added 20ml hydrochloric acid, are continuously stirred at room temperature 8 after a period of time
H removes remaining reduction Fe powder after fully reacting.
(5) products therefrom is washed with deionized until neutral, the then drying at 80 DEG C.Up to rGO/ black oxychloride
Bismuth-bismuth-bismuth oxide (rGO/black BiOCl-Bi-Bi2O3) heterojunction photocatalyst.
The beneficial effects of the present invention are:
(1) preparation method of photochemical catalyst of the present invention is that coprecipitation, reaction condition easily reach at room temperature, and operation is simple,
Low energy consumption, and applicability is wide；
(2) present invention can regulate and control rGO/ black bismuth oxychloride-bismuth-bismuth oxide by the dosage (g) of regulation GO
(rGO/black BiOCl-Bi-Bi2O3) heterojunction photocatalyst spectral absorption range；
(3) chemical property of photochemical catalyst prepared by the present invention is stablized, and has stronger light absorption and light to urge under visible light
Change degradation capability, and there is higher stability and regenerability.
Only highly preferred embodiment of the present invention is described above, but is not to be construed as limiting the scope of the invention.This
Invention is not only limited to above embodiments, and specific structure is allowed to vary.All protection models in independent claims of the present invention
Interior made various change is enclosed to all fall in the scope of protection of the present invention.
Claims (5)
1. a kind of preparation with visible light-responded rGO/ black bismuth oxychloride-bismuth-bismuth oxide heterojunction photocatalyst
Method, it is characterised in that: the preparation method comprises the following steps,
1) chlorine source is sufficiently dissolved in GO solution, precursor solution is formed, bismuth source is then dissolved completely in this presoma again
In solution, PH is adjusted with ammonia spirit, a period of time is continuously stirred at room temperature, finally obtains product as off-white solid, it will be grey
White solid product is washed with deionized as neutrality, then dry at 60 DEG C, obtains BiOCl/GO compound；
2) above-mentioned BiOCl/GO compound 3.0g, is taken to be dissolved in 150ml deionized water, the uniformly rear excessive reduced iron of addition to be mixed
Powder is added 20ml hydrochloric acid, is continuously stirred at room temperature 8h after a period of time, first remove remaining Fe powder after fully reacting, then
Products therefrom is washed with deionized as neutrality, it is then dry at 80 DEG C, finally rGO/ black bismuth oxychloride-bismuth-three
Aoxidize two bismuth (rGO/blackBiOCl-Bi-Bi2O3) heterojunction photocatalyst.
2. according to claim 1 a kind of different with visible light-responded rGO/ black bismuth oxychloride-bismuth-bismuth oxide
The preparation method of matter knot photochemical catalyst, it is characterised in that: the chlorine source in the step 1) is any in potassium chloride or sodium chloride
It is a kind of.
3. according to claim 1 a kind of different with visible light-responded rGO/ black bismuth oxychloride-bismuth-bismuth oxide
The preparation method of matter knot photochemical catalyst, it is characterised in that: the bismuth source in the step 1) is five nitric hydrate bismuths.
4. according to claim 1 a kind of different with visible light-responded rGO/ black bismuth oxychloride-bismuth-bismuth oxide
The preparation method of matter knot photochemical catalyst, it is characterised in that: chlorine source and bismuth source molar ratio in the step 1) are 1:1.
5. according to claim 1 a kind of different with visible light-responded rGO/ black bismuth oxychloride-bismuth-bismuth oxide
The preparation method of matter knot photochemical catalyst, it is characterised in that: the quality of the GO can for 0.02g, 0.04g, 0.08g, 0.15g,
It is any in 0.30g, 0.45g.
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