CN105032452B - Preparation method for high-visible-light-activity K-doped BiOCl photocatalyst - Google Patents
Preparation method for high-visible-light-activity K-doped BiOCl photocatalyst Download PDFInfo
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- CN105032452B CN105032452B CN201510407997.7A CN201510407997A CN105032452B CN 105032452 B CN105032452 B CN 105032452B CN 201510407997 A CN201510407997 A CN 201510407997A CN 105032452 B CN105032452 B CN 105032452B
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Abstract
The invention relates to a preparation method for a high-visible-light-activity K-doped BiOCl photocatalyst. The preparation method comprises the following steps: (1) dissolving a proper amount of a bismuth nitrate solution in deionized water and stirring the solution to obtain a clarified solution; (2) weighing potassium nitrate, ammonium chloride and citric acid and adding the mixture into the solution; and (3) heating the obtained solution to 250-400 DEG C, and continuously evaporating a solvent till no gas emerge so as to obtain the K-doped BiOCl photocatalyst. The preparation method is low in temperature, simple in process and easy to operate and can be used for continuous production; the photocatalyst prepared by the method has an excellent photo-catalytic performance.
Description
Technical field
The invention belongs to catalysis material water treatment field, especially relate to a kind of k doping biocl of high visible-light activity
The preparation method of catalyst.
Background technology
With the progressively deterioration of environment, the exhaustion of the energy, water pollution problems highlights, how highly efficient, greenly solve
Water pollution problems receives much concern.Wherein based on the photocatalysis technology of quasiconductor be considered as solve water pollution problems maximally efficient,
One of the most promising method.At present, the waste water control method having adopted, such as filters, absorption and biotechnology etc. be although work
Skill is ripe, it is easy to accomplish, but so that pollutant is destroyed and realize innoxious.Photocatalysis technology is then by absorbing too
Sunlight, drives redox reaction, destroys the harmful organic pollution in water body, will not produce secondary pollution.Wherein tio2
Based photocatalyst is widely used with cheap, nontoxic and very high stability, but tio2There is higher taboo
Bandwidth, can only be excited ultraviolet region (accounting for sunlight 2-3%), be limited its utilization rate to sunlight, therefore extensively
Big researcher is devoted to finding visible light-responded catalyst.
Bismuth oxychloride (biocl) is the quasiconductor that energy gap is 3.46 ev.Research finds, biocl is as bi base recently
Photocatalyst, under ultraviolet excitation, shows and compares tio2Higher photocatalytic degradation capability.But can only be using in sunlight
Ultraviolet light.The visible light catalytic performance of the biocl in order to improve, researcher proposes a lot of methods, such as metal-modified,
Doping and other materials be combined etc..Wherein, doping is a very effective method, and such as li wen ting et al. passes through hydro-thermal
Method, spent glycol auxiliary dissolving is prepared for zn2+Doping biocl photocatalyst, research finds doping zn2+Cause the injustice of electric charge
Weighing apparatus, forms hole trap, improves photoinduced electron hole separation efficiency, increase specific surface area simultaneously, improve visible ray and urge
Change active [journal of alloys and compounds, 2015,638,148-154]；Xie fangxia et al. uses
Oxidation-reduction method is prepared for sn doping biocl, and sn doping leads to biocl energy gap to reduce, and then improves radiation of visible light
Under photocatalytic activity [materials science in semiconductor processing, 2014,27,380-
389]；Milka nussbaum et al. has synthesized a series of codope biocl photocatalysts, have studied them and drops under visible light
The catalysis activity of solution rhodamine b, result shows, fe and nb is co-doped with the high absorbability of comparison, shows preferably simultaneously
Photocatalytic degradation capability [journal of photochemistry and photobiology a:chemistry, 2014,
290, 11-21].
Although above doping obtains visible light-responded biocl catalysis material, photocatalysis efficiency increases,
Preparation process is loaded down with trivial details, and the time is long, wherein rare earth doped relatively costly, is unfavorable for industrialized production and practical application.
For this problem, the present invention prepares a kind of k doping biocl photocatalyst of high visible-light activity.This catalyst
Preparation method is only to be quickly generated using the high temperature that the violent redox reaction between citric acid and nitrate produces
Biocl, and by k doping biocl, change the pattern of catalyst and increase specific surface area of catalyst, can be significantly
Improve its absorbability to organic pollution, and then be greatly enhanced photocatalytic activity；In addition, the method also has cost
Low, process is simple, easily operated and the feature that can be continuously produced.
Content of the invention
The present invention has prepared a kind of k doping biocl photocatalyst of responding to visible light, and gained photocatalyst has high
Visible light photocatalysis active, can extensively apply in fields such as sewage disposals；This method for preparing catalyst has low cost, process letter
Single, easily operated, the advantages of can be continuously produced.
A kind of preparation method of the k doping biocl photocatalyst of high visible-light activity, its step is as follows:
(1) appropriate bismuth nitrate is dissolved in deionized water, stirring obtains settled solution；
(2) weigh potassium nitrate, ammonium chloride and citric acid to add in above-mentioned solution；
(3) resulting solution is heated to 250-400 DEG C, constantly evaporates solvent, till not having gas to emerge, obtain final product
To k doping biocl visible light catalyst.
Described preparation method is it is preferred that the amount of step (2) potassium nitrate material is the amount of material of bismuth nitrate
0.06-0.25 times (preferably, the amount of potassium nitrate material is 0.20 times of the amount of material of bismuth nitrate).
Described preparation method is it is preferred that the amount of step (2) ammonium chloride material is bismuth nitrate and potassium nitrate total material
2-4 times (preferably, the amount of ammonium chloride material is 3 times of the amount of bismuth nitrate and potassium nitrate total material) of amount.
Described preparation method is it is preferred that the amount of step (2) Fructus Citri Limoniae acid substance is bismuth nitrate and potassium nitrate total material
0.5-1.2 times (preferred, the amount of Fructus Citri Limoniae acid substance is 0.8 times of the amount of bismuth nitrate and potassium nitrate total material) of amount.
This preparation method temperature is low, and process simply it is easy to operation, can be continuously produced；The method is obtained photocatalyst tool
There is excellent visible light catalytic performance.
The preparation method of biocl photocatalyst the present invention relates to a kind of k of high visible-light activity adulterates, belongs to photocatalysis material
Material field.The present invention adopts a step combustion method, with bismuth nitrate, potassium nitrate, ammonium chloride and citric acid as raw material, by nitrate and
Redox reaction between citric acid, prepares k doping biocl photocatalyst.K doping biocl photocatalyst can absorb visible
Light degradation organic pollution.The present invention changes biocl catalyst pattern by the k element that adulterates and increases specific surface area, significantly
Improve the absorbability of photocatalyst, and then improve the speed of photocatalytic degradation.The present invention's with low cost, preparation method
Process is simple is it is easy to operation, it is not necessary to complex device, can be continuously produced.
The invention has the following beneficial effects:
(1) the k doping biocl photocatalyst that the method is obtained, has high visible light catalysis activity, in environmental conservation
Field extensive application prospect；
(2) preparation method low cost of the present invention, process simple it is easy to operation is it is not necessary to complex device, can continuous metaplasia
Produce.
Brief description
Fig. 1 is the x-ray diffraction collection of illustrative plates of the k doping biocl photocatalyst of embodiment 1 preparation；
Fig. 2 is the k doping degradation effect curve to rhodamine b for the biocl photocatalyst of embodiment 1 preparation.
Specific embodiment
In order to show substantive distinguishing features and the marked improvement of the present invention, further illustrate reality with following nonlimiting examples
Apply mode and effect.
Embodiment 1
A kind of preparation method of the k doping biocl photocatalyst of high visible-light activity, comprises the steps:
(1) weigh 0.012 mol bismuth nitrate successively and be dissolved in 50 ml deionized waters, stirring obtains settled solution.
(2) weigh 0.003 mol potassium nitrate, 0.045 mol ammonium chloride and 0.012 mol citric acid to add in (1)
To solution in.
(3) obtained mixed liquor is heated to 300 DEG C, with evaporation of water, solution gradually becomes gluey, occurs a large amount of
Flue gas.When not having flue gas to produce, stop heating, be cooled to room temperature, that is, obtain k doping biocl photocatalyst.
Fig. 1 be the x-ray diffraction collection of illustrative plates of gained sample it can be seen that Tetragonal biocl, do not find bi2o3Or kcl etc. is miscellaneous
Phase.Fig. 2 be sample to rhodamine visible light catalytic effect curve；As can be seen that under visible light illumination, k doping biocl
To the degradation rate of rhodamine more than 95%, illustrate that k doping biocl has excellent visible light catalytic ability.
Embodiment 2
A kind of preparation method of the k doping biocl photocatalyst of high visible-light activity, comprises the steps:
(1) weigh 0.01425 mol bismuth nitrate successively and be dissolved in 50 ml deionized waters, stirring obtains settled solution.
(2) weigh 0.00075 mol potassium nitrate, 0.045 mol ammonium chloride and 0.012 mol citric acid to add in (1)
In the solution obtaining.
(3) obtained mixed liquor is heated to 300 DEG C, with evaporation of water, solution gradually becomes gluey, occurs a large amount of
Flue gas.When not having flue gas to produce, stop heating, be cooled to room temperature, that is, obtain k doping biocl photocatalyst.
Embodiment 3
A kind of preparation method of the k doping biocl photocatalyst of high visible-light activity, comprises the steps:
(1) weigh 0.0135 mol bismuth nitrate successively and be dissolved in 50 ml deionized waters, stirring obtains settled solution.
(2) weigh 0.0015 mol potassium nitrate, 0.045 mol ammonium chloride and 0.012 mol citric acid to add in (1)
To solution in.
(3) obtained mixed liquor is heated to 300 DEG C, with evaporation of water, solution gradually becomes gluey, occurs a large amount of
Flue gas.When not having flue gas to produce, stop heating, be cooled to room temperature, that is, obtain k doping biocl photocatalyst.
Embodiment 4
A kind of preparation method of k doping biocl photocatalyst, comprises the steps:
(1) weigh 0.01275 mol bismuth nitrate successively and be dissolved in 50 ml deionized waters, stirring obtains settled solution.
(2) weigh 0.00225 mol potassium nitrate, 0.045 mol ammonium chloride and 0.012 mol citric acid to add in (1)
In the solution obtaining.
(3) obtained mixed liquor is heated to 400 DEG C, with evaporation of water, solution gradually becomes gluey, occurs a large amount of
Flue gas.When not having flue gas to produce, stop heating, be cooled to room temperature, that is, obtain k doping biocl photocatalyst.
Certainly, the above embodiment of the present invention only example to illustrate the invention, and it is not the tool to the present invention
The restriction of body embodiment.For those of ordinary skill in the field, can also be done it on the basis of the example above
The change of his multi-form or variation.Here all of embodiment cannot be illustrated in detail.Every belong to the present invention's
Obvious change that technical scheme is amplified out or change the row still in protection scope of the present invention.
The research and development of this patent are subject to institution of higher education of Shandong Province plan of science and technology (j15la10), Liaocheng University's science fund
(318011319) and Liaocheng University's SRF (sf2014001) subsidy.
Claims (4)
1. the preparation method of the k doping biocl photocatalyst of a kind of high visible-light activity, is characterized in that, step is as follows:
(1) appropriate bismuth nitrate is dissolved in deionized water, stirring obtains settled solution；
(2) weigh potassium nitrate, ammonium chloride and citric acid to add in above-mentioned solution；The amount of potassium nitrate material is the material of bismuth nitrate
0.06-0.25 times of amount；The amount of ammonium chloride material is 2-4 times of the amount of bismuth nitrate and potassium nitrate total material；Fructus Citri Limoniae acid substance
Measure the amount for bismuth nitrate and potassium nitrate total material 0.5-1.2 times；
(3) resulting solution is heated to 250-400 DEG C, constantly evaporates solvent, till not having gas to emerge, that is, obtain k
Doping biocl visible light catalyst.
2. preparation method according to claim 1, is characterized in that, the amount of step (2) potassium nitrate material is the thing of bismuth nitrate
0.20 times of the amount of matter.
3. preparation method according to claim 1, is characterized in that, the amount of step (2) ammonium chloride material is bismuth nitrate and nitre
3 times of the amount of sour potassium total material.
4. preparation method according to claim 1, is characterized in that, the amount of step (2) Fructus Citri Limoniae acid substance is bismuth nitrate and nitre
0.8 times of the amount of sour potassium total material.
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| CN105688949B (en) * | 2016-02-25 | 2018-02-09 | 聊城大学 | Bi1‑x‑yErxYbyUpper converting photocatalysis materials of OBr/BiOCl and preparation method thereof |
| CN107876069A (en) * | 2017-11-29 | 2018-04-06 | 安徽师范大学 | BiOCl photochemical catalysts and its synthetic method with highlight catalytic active |
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