CN103611551A - Preparation method of bismuth sulfide/bismuth molybdenum oxide heterojunction photocatalytic composite material - Google Patents
Preparation method of bismuth sulfide/bismuth molybdenum oxide heterojunction photocatalytic composite material Download PDFInfo
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Abstract
The invention relates to a preparation method of a bismuth sulfide/bismuth molybdenum oxide heterojunction photocatalytic composite material. The preparation method is characterized by comprising the steps of dispersing BiOBr micro-sphere particles in de-ionized water in a proportion of 7.7g/L, and uniformly stirring; adding a molybdenum source: sodium molybdate, sodium chloride, sodium thiocyanate and a surfactant to a solution (1) and stirring for 30-60min; regulating pH value of the solution to be acid through hydrochloric acid; pouring the mixed solution into a stainless steel reaction kettle, and reacting for 24-48 hours at 150-200 DEG C; after reaction, naturally cooling, centrifuging and washing a reaction product for times through de-ionized water and ethanol, and drying the product to obtain the Bi2S3/Bi2MoO6 heterojunction composite material. The preparation method is simple and convenient to operate and is low in reaction temperature, and the prepared composite material is excellent in photocatalytic performance.
Description
Technical field
The present invention relates to nano inorganic functional material preparing technical field, relate in particular to a kind of bismuthyl bromide (BiOBr) that utilizes and prepare bismuth sulfide/molybdenum oxide bismuth (Bi as sacrificing template original position
2s
3/ Bi
2moO
6) method of heterojunction photocatalyst.
Technical background
Along with human development and social progress, day by day serious environmental problem has more and more affected and has jeopardized the mankind's productive life.For solving environmental problem, human development multiple physical absorption, biodegradation and chemical breakdown method pollutant is processed, and brought into play certain effect.But these methods all have some limitations, therefore, the environmental protection treatment technology that develops a kind of new and effective practicality becomes the focus of people's research.Photochemical catalyst can be decomposed into CO by organic pollution up hill and dale under illumination condition
2, H
2the inorganic molecules such as O, do not form secondary pollution.Thus, photocatalysis oxidation technique, as a kind of new technique of processing persistent organic pollutants, has been subject to researcher's very big attention.With other method contrast, that the method has is energy-efficient, clean nontoxic, non-secondary pollution and the advantage such as technique is simple, therefore at the aspects such as advanced treating of the organic wastewater of air cleaning, various biological hard degradations, the processing of comprehensive wastewater and domestic water, have boundless application prospect, therefore semiconductor catalyst is also acknowledged as the catalyst of new and effective green.
It is to realize the effective ways that a certain wavelength had to better photocatalysis effect that the semiconducting compound of two kinds of band structure couplings is carried out to the compound heterojunction photocatalyst that builds.Its advantage is: 1, can effectively reduce the compound probability of electron-hole; 2, improve the life-span of carrier; 3, improve interface charge the efficiency that is transferred to adsorbate surface etc. (Catalysis Today, 2005,101:315-321).In general, in the narrower semiconductor of energy gap, due to the close together of light induced electron and photohole, electronics one hole is to easily compound.Therefore, in order to utilize the extinction characteristic of narrow gap semiconductor, and suppress right compound in electronics one hole, narrow gap semiconductor and another kind of semiconductor can be linked together.At present, there is people by Bi
2s
3respectively with TiO
2, SiO
2, ZnO and CdS be joined together to form complex or heterojunction structure.Bi
2S
3-TiO
2(CatalysisToday2007,122:62-65.),Bi
2S
3-SiO
2(ColloidsandSurfaee?sA.2008,328:107-11),Bi
2S
3-ZnO(CrystEngComm,2010,12:3950-3958),Bi
2S
3-Cd?S(.J.Phys.Chem.C.2011,115:13968-13976)。Visible, Bi
2s
3as the narrower semiconductor of a kind of energy gap, it has huge application prospect in the exploitation of complex and heterojunction structure catalysis material.Meanwhile, as a kind of important wide bandgap semiconductor materials, Bi
2moO
6due to its excellent electricity and optical property, be widely used in field (J.Phys.Chem.B, 2006,110 (36): 17790-17797) such as solar cell, gas sensor, particle conductor, catalyst.As these two kinds of semi-conducting materials are carried out to hetero-junctions on micro-nano-scale, close and form Bi2S3/Bi2MoO6 composite, in photocatalysis field, having potential using value.
Summary of the invention
The object of this invention is to provide a kind of Bi
2s
3/ Bi
2moO
6the preparation method of heterojunction photocatalysis composite, adopts the synthetic Bi of hydro-thermal reaction original position
2s
3/ Bi
2moO
6heterojunction composite.
Principle is as follows: first with the standby BiOBr micron ball that goes out pattern homogeneous of hydro-thermal legal system; Then by BiOBr micron ball, adopt hydro-thermal method original position to prepare Bi
2s
3/ Bi
2moO
6heterojunction photocatalysis composite, catalytic performance is good, stability is higher.
Particularly, technical scheme is as follows:
Bi
2s
3/ Bi
2moO
6the preparation method of heterojunction photocatalysis composite, comprises the following steps:
(1) prepare BiOBr micron ball: by Bi (NO3)
35H
2o is dissolved in glycol monoethyl ether, to make concentration be the solution of 0.03-0.04mol/L and stir, in the process stirring, add softex kw (CTAB), guarantee that concentration is 0.2-0.3mol/L, then solution is poured in the reactor of polytetrafluoroethylene (PTFE) and put into baking oven, 150-200 ℃ of reaction 8-12 hour; Question response finishes, and reactor is cooled to room temperature, with deionized water and alcohol cyclic washing.The BiOBr solution having washed is put into baking oven, and temperature 60 C is dried, and obtains dry BiOBr micro particles;
(2) prepare the aqueous solution of BiOBr micron ball: the ratio by BiOBr micron ball particle with 7.7g/L is distributed in deionized water, stirs;
(3) by molybdenum source sodium molybdate, sodium chloride, sodium sulfocyanate and surfactant join in solution (1), and stir 30-60min;
The concentration of sodium molybdate is 5-7g/L; The concentration of sodium chloride is 2-3g/L; The concentration of sodium sulfocyanate is 5-6g/L;
Surfactant is softex kw (CTAB) or TBAB, and concentration is 1.5-2g/L;
(4) use the pH extremely acid (pH value is 2-4) of the hydrochloric acid conditioning solution of 1mol/L;
(5) solution mixing is poured into in teflon-lined stainless steel cauldron, and naturally cooling after 150-200 ℃ of reaction 24-48h;
(6) utilize deionized water, ethanol to carry out repeatedly after centrifuge washing product, by the dry Bi that obtains of product
2s
3/ Bi
2moO
6heterojunction composite.
This method technique simply, rapidly and efficiently, is utilized and is sacrificed template one-step method original position generation Bi
2s
3/ Bi
2moO
6heterojunction structure photocatalyst compound material, crystallinity is good, and appearance and size is controlled, at aspects such as photocatalysis and absorption, has potential using value.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of the BiOBr micron ball of embodiment 1 preparation; Illustrate that BiOBr micron ball is that structure by sheet assembles.
Fig. 2 is the Bi of embodiment 1 preparation
2s
3/ Bi
2moO
6the X ray diffracting spectrum of heterojunction photocatalysis composite; XRD proves from composition and phase structure, successfully prepares Bi
2s
3/ Bi
2moO
6.
Fig. 3 is the Bi of embodiment 2 preparations
2s
3/ Bi
2moO
6the electron scanning micrograph of heterojunction photocatalysis composite; Show that this heterojunction photocatalysis composite is the heterojunction structure that sheet and corynebacterium depend on mutually.
Fig. 4 is Bi prepared by pure BiOBr micron ball and embodiment 1-3
2s
3/ Bi
2moO
6degrade under the visible ray photocatalysis effect figure of RhB of heterojunction photocatalysis composite.Illustrate that composite has better photocatalysis performance than pure BiOBr micron ball, and the heterojunction material in embodiment 2 has best degradation effect, the degradation rate of 90min reaches 91%.
The specific embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1
(1) prepare BiOBr micron ball: by Bi (NO3)
35H
2o is dissolved in glycol monoethyl ether, to make concentration be the solution of 0.03-0.04mol/L and stir, in the process stirring, add softex kw (CTAB), guarantee that concentration is 0.2-0.3mol/L, then solution is poured in the reactor of polytetrafluoroethylene (PTFE) and put into baking oven, reaction temperature 150-200 ℃, the reaction time is 8-12 hour.Question response finishes, and reactor is cooled to room temperature, with deionized water and alcohol cyclic washing.The BiOBr solution having washed is put into baking oven, and temperature 60 C is dried, and obtains dry BiOBr micro particles.
(2) prepare Bi
2s
3/ Bi
2moO
6heterojunction photocatalysis composite: the 0.462g BiOBr micro particles, the 0.3g NaMoO that take
42H
2o, 0.12g NaCl, 0.09g CTAB, 0.3g NaSCN puts into the reactor of 100ml successively, takes 60ml distilled water simultaneously add in reactor and stir 30 minutes with graduated cylinder.The PH to 2 that regulates reaction solution, puts into baking oven by reactor, 160 ℃ of temperature, 24 hours reaction time.Question response finishes, and reactor is down to room temperature, by centrifuge, washs, and wash solution is distilled water and absolute ethyl alcohol, and centrifugal number of times 3~5 times, puts into baking oven by sample, dries, obtains Bi for 60 ℃
2s
3/ Bi
2moO
6heterojunction photocatalysis composite.
The preparation process of the BiOBr micron ball of the present embodiment is identical with embodiment 1.
Different is that step (2) thes contents are as follows: take 0.462g BiOBr, 0.36g NaMoO
42H
2o, 0.15g NaCl, 0.108g CTAB, 0.33g NaSCN put into the reactor of 100ml successively, take 60ml distilled water simultaneously add in reactor and stir 45 minutes with graduated cylinder.The PH to 3 that regulates reaction solution, puts into baking oven by reactor, 180 ℃ of temperature, 36 hours reaction time.Question response finishes, and reactor is down to room temperature, by centrifuge, washs, and wash solution is distilled water and absolute ethyl alcohol, and centrifugal number of times 3~5 times, puts into baking oven by sample, dries for 60 ℃.Can obtain Bi
2s
3/ Bi
2moO
6heterojunction photocatalysis composite.
Embodiment 3
The preparation process of the BiOBr micron ball of the present embodiment is identical with embodiment 1.
Different is theing contents are as follows of step (2):: the 0.462g BiOBr taking is ready to, takes 0.42g NaMoO
42H
2o, 0.18g NaCl, 0.12g TBAB, 0.36g NaSCN puts into the reactor of 100ml successively, takes 60ml distilled water simultaneously add in reactor and stir 60 minutes with graduated cylinder.The PH to 4 that regulates reaction solution, puts into baking oven by reactor, 200 ℃ of temperature, 48 hours reaction time.Question response finishes, and reactor is down to room temperature, by centrifuge, washs, and wash solution is distilled water and absolute ethyl alcohol, and centrifugal number of times 3~5 times, puts into baking oven by sample, dries for 60 ℃.Can obtain Bi
2s
3/ Bi
2moO
6heterojunction photocatalysis composite.
Prepared to Bi in order to check
2s
3/ Bi
2moO
6the degradation property of heterojunction photocatalysis composite, the present invention selects rhodamine B as photocatalytic degradation object.Respectively the sample in embodiment is carried out to Photocatalytic Degradation Property test, the heterojunction photocatalyst of preparing with pure BiOBr and embodiment 1-3 is numbered respectively 1#, 2#, and 3#, the 4# rhodamine B in degradation water (Rh B) molecule under visible ray condition is evaluated.Light source is the xenon lamp of 500W, by 1 * 10 of 100mL
-1the Rh B solution of mol/L is put into beaker, adds the photochemical catalyst of 0.05g, and the ultrasonic mark 10min of lucifuge stirs 20min, makes Rh B reach adsorption equilibrium in photocatalyst surface.Turn on light to irradiate and carry out photocatalytic degradation reaction, after 3 hours, sample respectively 4mL, with centrifuge centrifugation catalyst granules, get supernatant, with UV-vis spectrophotometer, monitor the absorbance of Rh B, and then follow the tracks of the change in concentration of Rh B in solution, obtain the activity figure of photocatalytic degradation RhB.
Claims (6)
1. the preparation method of bismuth sulfide/molybdenum oxide bismuth heterojunction photocatalysis composite, is characterized in that comprising the following steps:
(1) prepare BiOBr micron ball: by Bi (NO3)
35H
2o is dissolved in glycol monoethyl ether, under stirring, adds softex kw; After mixing, solution is poured into 150-200 ℃ of reaction 8-12 hour in reactor; Question response finishes, and is cooled to room temperature, with deionized water and alcohol cyclic washing; Dry BiOBr micro particles;
(2) prepare the aqueous solution of BiOBr micron ball: the ratio by BiOBr micron ball particle with 7.7g/L is distributed in deionized water, stirs;
(3) by molybdenum source sodium molybdate, sodium chloride, sodium sulfocyanate and surfactant join in solution (1), and stir 30-60min;
(4) pH of hydrochloric acid conditioning solution is to acid;
(5) solution mixing is poured into in stainless steel cauldron, and after 150-200 ℃ of reaction 24-48h;
(6) after reaction finishes, naturally cooling, utilize deionized water, ethanol to carry out repeatedly after centrifuge washing product, by the dry Bi that obtains of product
2s
3/ Bi
2moO
6heterojunction composite.
2. the preparation method of bismuth sulfide/molybdenum oxide bismuth heterojunction photocatalysis composite according to claim 1, is characterized in that Bi (NO3) in the solution of step (1)
35H
2the concentration of O is 0.03-0.04mol/L; The concentration of softex kw is 0.2-0.3mol/L.
3. the preparation method of bismuth sulfide/molybdenum oxide bismuth heterojunction photocatalysis composite according to claim 1, is characterized in that the concentration of sodium molybdate in step (2) is 5-7g/L; The concentration of sodium chloride is 2-3g/L; The concentration of sodium sulfocyanate is 5-6g/L; The concentration of surfactant is 1.5-2g/L.
4. the preparation method of bismuth sulfide/molybdenum oxide bismuth heterojunction photocatalysis composite according to claim 1, is characterized in that in step (3), surfactant is softex kw or TBAB.
5. the preparation method of bismuth sulfide/molybdenum oxide bismuth heterojunction photocatalysis composite according to claim 1, is characterized in that in step (4), concentration of hydrochloric acid is 1mol/L, and the pH value of the solution after adjusting is 2-4.
6. the preparation method of bismuth sulfide/molybdenum oxide bismuth heterojunction photocatalysis composite according to claim 1, is characterized in that in step (6), bake out temperature is 60 ℃.
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CN104190450A (en) * | 2014-09-03 | 2014-12-10 | 江南大学 | Bismuth oxyiodide/bismuth molybdate composite photocatalyst and preparation method thereof |
CN104707628A (en) * | 2015-02-27 | 2015-06-17 | 济南大学 | Bi2S3/Bi2MoO6 compound visible-light-induced photocatalyst as well as preparation method and application thereof |
CN105056973A (en) * | 2015-07-16 | 2015-11-18 | 南昌航空大学 | Efficient Bi2S3-BiFeO3 composite visible-light-driven photocatalyst prepared through in-situ growth with chemical corrosion method and application of Bi2S3-BiFeO3 composite visible-light-driven photocatalyst |
CN106890654A (en) * | 2017-01-06 | 2017-06-27 | 华南理工大学 | A kind of bismuthyl bromide/bismuth molybdate heterojunction photocatalyst and preparation and application |
CN108906085A (en) * | 2018-07-17 | 2018-11-30 | 河南师范大学 | A kind of Bi2S3The preparation method and applications of/BiOBr composite photocatalyst material |
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CN113000054A (en) * | 2021-03-30 | 2021-06-22 | 广州大学 | Bi2O2Preparation method of Se material |
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