CN104014352A - Multivariate controllable synthesis method of BiOCl photocatalyst - Google Patents
Multivariate controllable synthesis method of BiOCl photocatalyst Download PDFInfo
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- CN104014352A CN104014352A CN201410201908.9A CN201410201908A CN104014352A CN 104014352 A CN104014352 A CN 104014352A CN 201410201908 A CN201410201908 A CN 201410201908A CN 104014352 A CN104014352 A CN 104014352A
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Abstract
The invention discloses a multivariate controllable synthesis method of a BiOCl photocatalyst, and belongs to the technical field of photocatalytic water treatment of environmental chemical engineering. The multivariate controllable synthesis method is characterized by comprising the following steps: adding BiCl3 with proper concentration to diethylene glycol or a mixed solvent of diethylene glycol and water; adding a urea precipitation agent, directly transferring sol or transferring sol subjected to ultrasonic pretreatment into a Teflon high-pressure reaction kettle to carry out solvothermal reaction at certain temperature to generate sediments after evenly mixing; and baking the sediments at 80 DEG C after washing with water and ethanol, so as to obtain BiOCl photocatalyst powder with different morphologies. The synthesis method disclosed by the invention has the characteristics that the preparation cycle of BiOCl is short, use of a surfactant is avoided, grains with controllable crystal faces (110 and 102) and controllable morphologies (two-dimensional flakes, three-dimensional flowers or spheres) can be conveniently achieved by controlling and ultrasonic pretreatment on the solvent. The catalyst is applied to photocatalytic degradation of carbamazepine medicine wastewater, displays the photocatalytic activity superior to that of TiO2(P25) under ultraviolet light and simulated sunlight, and has a practical application prospect.
Description
Technical field
The polynary controllable synthesis method of a kind of BiOCl photochemical catalyst of the present invention, belong to environmental chemical engineering photocatalysis water-treatment technology field, be specifically related to a kind of solvent and template effect that utilizes polyalcohol, by controlling response parameter, prepare crystal face and pattern polynary controlled and typical medicaments in water is there is to the BiOCl photochemical catalyst of efficient degradation ability.
Background technology
In a very long time in the past, the research emphasis of World Water process field concentrates on some preferential pollutant of controlling, as persistence organic pollutant, agricultural chemicals, industrial chemical and heavy metal etc.But along with the continuous progress of technological means, output and the consumption of medicine and personal-care supplies (pharmaceuticals and personal care products, PPCPs) day by day increase.Because PPCPs is difficult to be completely removed in sewage treatment process, cause the PPCPs in environment water to be remarkable characteristics of SSTA persistence.PPCPs is residual not only produces harmful effect to environment and the ecosystem, can also pass through food chain enrichment, and the mankind's health is caused to persistent harm, and this is own through having caused domestic and international scientist and the public's extensive concern.
Photocatalysis technology is to utilize semiconductor catalysis material to absorb electron-hole pair induced oxidation and reduction reaction that light produces, thus degraded and mineralising water body and airborne each pollutant.The core of photocatalysis technology is photochemical catalyst, and the activity of photochemical catalyst and the exposure of its crystal face and shape characteristic are closely related.Light-catalyzed reaction occurs in the surface of semi-conducting material, so the crystal face exposing has determined that can light-catalyzed reaction occur and efficiency.BiOCl is as novel photocatalyst, and the research that its crystal face exposes also makes some progress: in document, reported the BiOCl activity higher (J.Alloy.Compd., 2013,549, pp70 – 76) that (110) crystal face exposes.In addition, the pattern of photochemical catalyst directly affects its photocatalytic activity.At present the control of BiOCl pattern is often needed to introduce surfactant (Cryst.Eng.Comm., 2009,11, pp1857 – 1862), generated time is grown (Cryst.Growth Des., 2010,10, pp2522-2527), its application also mainly concentrates on dyestuff and effluent containing heavy metal ions aspect.Regulate and control by the crystal face exposure to BiOCl and pattern growth, more excellent photocatalysis performance will likely be obtained, but up to now, also do not control BiOCl crystal face and pattern, and be applied to the report of typical medicaments aspect in photocatalytic degradation water simultaneously.
Summary of the invention
The polynary controllable synthesis method of a kind of BiOCl photochemical catalyst of the present invention.According to the present invention, adopt polyhydroxy-alcohol diethylene glycol simultaneously as solvent and template, by can conveniently realize particle crystal face and the controlled preparation of pattern to the control of response parameter, the method is easy and simple to handle, manufacturing cycle is short, avoided the use of surfactant, effectively typical medicaments in degradation water, solves the problem of environmental pollution.
The polynary controllable synthesis method of a kind of BiOCl photochemical catalyst of the present invention, it is characterized in that the preparation method of the simultaneously controlled BiOCl photochemical catalyst powder of a kind of crystal face and pattern, and its concrete preparation process is:
1) with BiCl
3for bismuth source, adopt one or both mixed solvents of diethylene glycol and water as solvent, by BiCl
3join in solvent, stirring or ultrasonic dissolution assisting and before hydro-thermal reaction, carry out ultrasonic processing, dissolve after 0.5～3h, and formation concentration is 0.025～0.25molL
-1clarification bismuth precursor;
2) to step 1) form bismuth precursor in, add urea, urea and BiCl
3mol ratio is 2:1～40:1, continues to stir, and obtains vitreosol;
3) by step 2) form colloidal sol proceed in Teflon autoclave, solvent thermal reaction 0.5～72h at 100～200 DEG C of temperature, is precipitated;
4) will precipitate water and ethanol washing, 75～80 DEG C of oven dry, obtain 110 or 102 different crystal face exposures and two-dimensional sheet, three-dimensional flower-shaped or spherical pattern, for the BiOCl photochemical catalyst powder of the micro-difficult degradation drug contamination of degradation water thing carbamazepine.
The polynary controllable synthesis method of above-mentioned a kind of BiOCl photochemical catalyst, is characterized in that the described reaction condition for the micro-difficult degradation drug contamination of degradation water thing carbamazepine is: water Chinese traditional medicine treating capacity is 2.5mgL
-1, under the irradiation of uviol lamp or simulated solar irradiation xenon lamp, catalyst amount is 0.5gL
-1, blast air from reactor bottom.
The advantage of the polynary controllable synthesis method of a kind of BiOCl photochemical catalyst of the present invention is:
(1) before hydro-thermal reaction, introduce first ultrasonic processing, compared with currently available technology, manufacturing cycle short (hydro-thermal 30min);
(2) BiOCl preparation technology provided by the invention easily controls, and has avoided the use of surfactant, environmentally friendly, does not produce poisonous and harmful accessory substance;
(3) the invention provides the synthetic method of the BiOCl photochemical catalyst of typical medicaments in a kind of efficient degradation water, the BiOCl photochemical catalyst that ultrasonic pre-treatment hydro-thermal reaction is prepared is under UV-irradiation, 70min reaches 98.54% to the degradation rate of carbamazepine, TiO under equal conditions
2(P25) cannot degrade;
(4) the BiOCl photochemical catalyst that ultrasonic pre-treatment hydro-thermal reaction is prepared is under simulated solar irradiation, and 150min reaches 96.73% to the degradation rate of carbamazepine, is obviously better than TiO
2(P25,33.30%);
(5) can utilize typical medicaments in solar radiation photocatalytic degradation water, method is simple to operate, and reaction condition gentleness can realize the original position reparation to contaminant water, and operating cost is low, has also increased the economic feasibility of this method.
Brief description of the drawings
Fig. 1 a, b, c is embodiment 1,2, the XRD figure of the BiOCl photochemical catalyst of 3 preparations;
Fig. 2 a, b, c is embodiment 1,2, the low power SEM figure of the BiOCl photochemical catalyst of 3 preparations, Fig. 2 d, e, f is embodiment 1,2, the high power SEM figure of the BiOCl photochemical catalyst of 3 preparations;
Fig. 3 a, b, c is embodiment 1,2, the ultraviolet catalytic degradation rate figure (ultraviolet source that test adopt be 250W uviol lamp, dominant wavelength be 365nm) of the BiOCl photochemical catalyst of 3 preparations to carbamazepine solution;
Fig. 4 a, b, c is embodiment 1,2, the simulated solar photocatalytic activity figure (simulated solar radiant be 500W xenon lamp, optical source wavelength scope be 200～800nm) of the BiOCl photochemical catalyst of 3 preparations to carbamazepine solution.
Detailed description of the invention
In order to make technical scheme of the present invention clearer, will specifically describe in detail with embodiment below, but content of the present invention is not confined to the scope of cited embodiment.
Embodiment 1
By BiCl
3join in diethylene glycol, stirring at room temperature 1.5h, formation concentration is 0.06molL
-1bismuth precursor, add urea and water, wherein urea and BiCl
3mol ratio is 10:1, and the ratio of diethylene glycol and water is 1:1, continues to stir 1.5h, obtains milky turbid solution; The turbid solution of formation is proceeded in Teflon autoclave to solvent thermal reaction 0.5h at 120 DEG C of temperature; By distilled water and ethanol washing for the precipitation obtaining, dry, obtain BiOCl photochemical catalyst powder.
Gained photochemical catalyst is for the oxidation processes carbamazepine aqueous solution.Its reaction condition is: water Chinese traditional medicine treating capacity is 2.5mgL
-1, under the irradiation of uviol lamp or simulated solar irradiation xenon lamp, catalyst amount is 0.5gL
-1, blast air from reactor bottom.At interval of 5～30min time sampling, and measure the absorbance of carbamazepine solution and calculate its conversion ratio with UV-VIS spectrophotometry, the results are shown in Figure 3.
Embodiment 2
By BiCl
3join in diethylene glycol solvent, stirring at room temperature 1.5h, formation concentration is 0.06molL
-1bismuth precursor; Add urea, wherein urea and BiCl
3mol ratio is 10:1, continues to stir to obtain vitreosol; The colloidal sol of formation is proceeded in Teflon autoclave to solvent thermal reaction 0.5h at 120 DEG C of temperature; By distilled water and ethanol washing for the precipitation obtaining, dry, obtain BiOCl photochemical catalyst powder.
Gained photochemical catalyst is for the oxidation processes carbamazepine aqueous solution.Its reaction condition is: water Chinese traditional medicine treating capacity is 2.5mgL
-1, under the irradiation of uviol lamp or simulated solar irradiation xenon lamp, catalyst amount is 0.5gL
-1, blast air from reactor bottom.At interval of 5～30min time sampling, and measure the absorbance of carbamazepine solution and calculate its conversion ratio with UV-VIS spectrophotometry, the results are shown in Figure 3.
Embodiment 3
By BiCl
3join in diethylene glycol solvent ultrasonic (40kHz, 90W/cm
2) hydrotropy, formation concentration is 0.06molL
-1bismuth precursor; Add urea, wherein urea and BiCl
3mol ratio is 10:1, the ultrasonic vitreosol that obtains; Continue ultrasonic 5min, intermittently 2min, carries out 6 circulations; The colloidal sol of formation is proceeded in Teflon autoclave to solvent thermal reaction 0.5h at 120 DEG C of temperature; By distilled water and ethanol washing for the precipitation obtaining, dry, obtain BiOCl photochemical catalyst powder.
Gained photochemical catalyst is for the oxidation processes carbamazepine aqueous solution.Its reaction condition is: water Chinese traditional medicine treating capacity is 2.5mgL
-1, under the irradiation of uviol lamp or simulated solar irradiation xenon lamp, catalyst amount is 0.5gL
-1, blast air from reactor bottom.At interval of 5～30min time sampling, and measure the absorbance of carbamazepine solution and calculate its conversion ratio with UV-VIS spectrophotometry, the results are shown in Figure 3.
It is pure that in above embodiment, medicine and reagent used is analysis.
Claims (2)
1. a polynary controllable synthesis method for BiOCl photochemical catalyst, it is characterized in that the preparation method of the simultaneously controlled BiOCl photochemical catalyst powder of a kind of crystal face and pattern, and its concrete preparation process is:
1) with BiCl
3for bismuth source, adopt one or both mixed solvents of diethylene glycol and water as solvent, by BiCl
3join in solvent, stirring or ultrasonic dissolution assisting and before hydro-thermal reaction, carry out ultrasonic processing, dissolve after 0.5 ~ 3 h, and forming concentration is 0.025 ~ 0.25 molL
-1clarification bismuth precursor;
2), in the bismuth precursor forming to step 1), add urea, urea and BiCl
3mol ratio is 2:1 ~ 40:1, continues to stir, and obtains vitreosol;
3) by step 2) form colloidal sol proceed in Teflon autoclave, at 100 ~ 200 DEG C of temperature, solvent thermal reaction 0.5 ~ 72 h, is precipitated;
4) water and ethanol washing be will precipitate, 75 ~ 80 DEG C of oven dry, 110 or 102 different crystal face exposures and two-dimensional sheet, three-dimensional flower-shaped or spherical pattern obtained, for the BiOCl photochemical catalyst powder of the micro-difficult degradation drug contamination of degradation water thing carbamazepine.
2. according to the polynary controllable synthesis method of a kind of BiOCl photochemical catalyst described in claim 1, it is characterized in that the described reaction condition for the micro-difficult degradation drug contamination of degradation water thing carbamazepine is: water Chinese traditional medicine treating capacity is 2.5 mgL
-1, under the irradiation of uviol lamp or simulated solar irradiation xenon lamp, catalyst amount is 0.5 g L
-1, blast air from reactor bottom.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104368362A (en) * | 2014-09-18 | 2015-02-25 | 太原理工大学 | Microemulsion-like photocatalyst, preparation method and applications thereof |
| CN104511293A (en) * | 2014-10-31 | 2015-04-15 | 北京理工大学 | Bismuth oxychloride-iron bismuth titanate composite photocatalyst and preparation method thereof |
| CN104689838A (en) * | 2015-02-13 | 2015-06-10 | 湘潭大学 | Preparation method for BiOCl photocatalyst with controllable morphology and crystal face |
| CN104841461A (en) * | 2015-05-25 | 2015-08-19 | 中南民族大学 | Preparation method and application of novel hexagonal-prism BiOCl nanometer photocatalytic materials |
| CN105195183A (en) * | 2015-10-19 | 2015-12-30 | 太原理工大学 | Preparation method of Co3O4@ACSs/BiOCl spherical adsorption and photocatalysis compound catalyst |
| CN106732684A (en) * | 2016-12-07 | 2017-05-31 | 西南大学 | Double salt Hydrolyze method prepares high activity BiOX catalysis material |
| CN107399762A (en) * | 2017-09-08 | 2017-11-28 | 济南大学 | A kind of method that bismoclite superthin section is prepared based on electrolyte coagulation magnanimity |
| CN107497491A (en) * | 2017-08-29 | 2017-12-22 | 电子科技大学 | A kind of preparation method of composite Nano catalysis material |
| CN108178192A (en) * | 2018-01-17 | 2018-06-19 | 南京信息工程大学 | BiOF electrode materials of a kind of nanometer of chip architecture and preparation method thereof and electrochemical energy storage application |
| CN109550511A (en) * | 2018-12-14 | 2019-04-02 | 西安理工大学 | A kind of preparation method at carbon doping perite nanometer pollen end |
| CN110201685A (en) * | 2019-06-05 | 2019-09-06 | 江南大学 | A kind of preparation method and application with the bismuth oxychloride for adjusting position of energy band function |
| CN110560099A (en) * | 2019-09-30 | 2019-12-13 | 中国科学院青岛生物能源与过程研究所 | Preparation method and application of BiOI nanoflower with three-dimensional layered structure |
| CN111889063A (en) * | 2020-09-01 | 2020-11-06 | 福州大学 | BiOCl adsorbent, preparation method and application thereof in room temperature desulfurization |
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| CN104511293A (en) * | 2014-10-31 | 2015-04-15 | 北京理工大学 | Bismuth oxychloride-iron bismuth titanate composite photocatalyst and preparation method thereof |
| CN104511293B (en) * | 2014-10-31 | 2019-03-26 | 北京理工大学 | A kind of bismuth oxychloride-iron titanate bismuth composite photo-catalyst and preparation method thereof |
| CN104689838A (en) * | 2015-02-13 | 2015-06-10 | 湘潭大学 | Preparation method for BiOCl photocatalyst with controllable morphology and crystal face |
| CN104841461A (en) * | 2015-05-25 | 2015-08-19 | 中南民族大学 | Preparation method and application of novel hexagonal-prism BiOCl nanometer photocatalytic materials |
| CN105195183A (en) * | 2015-10-19 | 2015-12-30 | 太原理工大学 | Preparation method of Co3O4@ACSs/BiOCl spherical adsorption and photocatalysis compound catalyst |
| CN105195183B (en) * | 2015-10-19 | 2017-07-21 | 太原理工大学 | A kind of Co3O4The preparation method of the spherical adsorption photochemical catalysis composite catalysts of@ACSs/BiOCl |
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| CN106732684B (en) * | 2016-12-07 | 2018-04-20 | 西南大学 | Double salt Hydrolyze method prepares high activity BiOX catalysis material |
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| CN112569969A (en) * | 2020-12-14 | 2021-03-30 | 太原理工大学 | Synthesis and application method of BiOBr photocatalyst containing optically controlled oxygen vacancies |
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