CN114210353A - Preparation method of bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material - Google Patents
Preparation method of bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material Download PDFInfo
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- GMZOPRQQINFLPQ-UHFFFAOYSA-H dibismuth;tricarbonate Chemical compound [Bi+3].[Bi+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GMZOPRQQINFLPQ-UHFFFAOYSA-H 0.000 abstract 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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Abstract
The invention discloses a preparation method of a bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material, which comprises the following steps: (1) adding urea into deionized water, stirring to dissolve, and adding Bi (NO)3)3·5H2Continuously stirring the mixture O, and adding sodium sulfide to obtain a mixed solution; (2) and stirring the mixed solution, then carrying out closed reaction, naturally cooling to room temperature after the reaction is finished, centrifuging, washing with water, washing with alcohol, and drying at room temperature to obtain the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material. The invention can effectively solve the problem of carbonic acidThe bismuth oxide serving as a photocatalytic material has insufficient response to ultraviolet light, and compared with other bismuth carbonate oxide-bismuth sulfide heterojunctions, the bismuth oxide-bismuth sulfide heterojunction has the advantages of simple preparation method, low cost and easiness in large-scale production.
Description
Technical Field
The invention relates to the technical field of photocatalyst synthesis, in particular to a preparation method of a bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material.
Background
In the research of the photocatalytic technology, semiconductor photocatalysts are always concerned, and the degradation of organic matters is effectively carried out by utilizing visible light which accounts for the maximum ratio in the solar spectrum, which is one of the extremely promising technologies for solving the energy problem.
The nanometer titanium dioxide has higher photocatalytic activity and stability, has the characteristics of low price, no toxicity and the like, but can only receive the excitation of short-wave ultraviolet light due to larger band gap energy of the titanium dioxide, can not effectively utilize most visible light, and electrons and holes generated after the titanium dioxide is subjected to photocatalysis are easy to recombine, so that the efficiency of generating carriers by light is greatly reduced, and the application value of the titanium dioxide material in actual life is limited to a certain extent. Therefore, it is very urgent to find a semiconductor photocatalyst which can respond to a wide-range solar spectrum and has high stability and high catalytic activity.
In recent two years, Bi-based semiconductor photocatalytic materials have attracted attention, and among them, bismuth oxyhalide catalysts also exhibit good photocatalytic activity, and in order to further improve the photocatalytic activity, various attempts have been made, such as doping, morphology adjustment, and shortening of the transfer distance of carriers. However, bismuth oxycarbonate as a photocatalytic material has a problem of insufficient response to ultraviolet light, and Bi was found in the course of the trial2O2CO3/Bi2S3The heterojunction is able to utilize more visible light and is able to efficiently induce electron-hole recombination,greatly improves the catalytic effect of the photocatalyst, but Bi is in various researches at present2O2CO3/Bi2S3The preparation method is almost prepared by two steps by using bismuth oxycarbonate as a precursor. In order to overcome the problem of insufficient response of bismuth subcarbonate to ultraviolet light, simultaneously further improve the catalytic effect of the heterojunction containing bismuth subcarbonate, simplify the preparation method of the heterojunction containing bismuth subcarbonate and enable the heterojunction to be widely applied.
Disclosure of Invention
Aiming at the prior art, the invention aims to provide a preparation method of a bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material. The invention can effectively solve the problem that bismuth subcarbonate as a photocatalytic material has insufficient response to ultraviolet light. Compared with other preparation methods of bismuth oxycarbonate-bismuth sulfide heterojunction, the method adopts a one-step synthesis method, is simpler and lower in cost compared with the existing two-step preparation method, and is easy for large-scale production.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, a preparation method of a bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material is provided, which comprises the following steps:
(1) adding urea into deionized water, stirring to dissolve, and adding Bi (NO)3)3·5H2Continuously stirring the mixture O, and adding sodium sulfide to obtain a mixed solution;
(2) and stirring the mixed solution, then carrying out closed reaction, naturally cooling to room temperature after the reaction is finished, centrifuging, washing with water, washing with alcohol, and drying at room temperature to obtain the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material.
Preferably, in step (1), the urea is reacted with Bi (NO)3)3·5H2The molar ratio of O is (6-10) to (1-3).
Preferably, in step (1), Bi (NO) is used3)3·5H2O and Na2S3The molar ratio of (1-3) to (1-4).
Preferably, in the step (2), the stirring is magnetic stirring, and the stirring time is 15-60 min.
Preferably, in the step (2), the temperature of the closed reaction is 150-240 ℃, and the reaction time is 12-48 h.
Preferably, in the step (2), the temperature of the centrifugation is 4-25 ℃, the rotation speed of the centrifugation is 4000-12000rpm, and the time of the centrifugation is 5-15 min.
In a second aspect of the invention, the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material prepared by the preparation method is provided.
Preferably, in the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material, the bismuth oxycarbonate is blocky, and the bismuth sulfide is rod-shaped.
In a third aspect of the invention, the application of the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material in photocatalytic degradation of plasticizers is provided.
The invention has the beneficial effects that:
(1) the invention adopts Bi (NO)3)3·5H2Bismuth oxycarbonate-bismuth sulfide (Bi) produced with O as raw material and water as solvent2O2CO3/Bi2S3) The heterostructure photocatalytic material is a composite material of rod-shaped bismuth sulfide and blocky bismuth oxycarbonate. Bi in various studies at present2O2CO3/Bi2S3The preparation method almost adopts the bismuthyl carbonate as a precursor for two-step preparation, and the binary composite material is synthesized by adopting a one-step method, so that the method has the characteristics of simpler process flow, low cost and easiness in large-scale production.
(2) Bi prepared by the invention2O2CO3/Bi2S3The heterojunction is tested and found to have the following advantages: the optical property of the prepared sample is verified through UV-Vis diffuse reflection spectrum, after bismuth sulfide is added, the light absorption capacity of bismuth oxycarbonate is greatly enhanced, the absorption band is widened to the visible light range, and the photocatalytic performance of the product is obviously improved. The bismuth sulfide heterojunction can accelerate the separation of electron-hole, prolong the service life of photo-generated electron or hole, and thus effectively improve the photocatalytic activity of the photocatalyst. Thus, bismuth oxycarbonate and sulfurBismuth oxide can play a synergistic role, further improve the photocatalytic capacity of the material and effectively degrade pollutants such as plasticizers.
Drawings
FIG. 1 shows Bi prepared in example 22O2CO3/Bi2S3XRD patterns of the heterostructure photocatalytic materials.
FIG. 2 shows preparation of Bi prepared in example 22O2CO3/Bi2S3SEM photographs of the heterostructure photocatalytic material.
FIG. 3 is a graph comparing the change in DBP content with time after xenon lamp irradiation of the product prepared in example 2 with the degradation of bismuth sulfide alone and bismuth oxycarbonate alone.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
In order to make the technical solutions of the present application more clearly understood by those skilled in the art, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The test materials used in the examples of the present invention are all conventional in the art and commercially available.
Example 1:
adding 0.5g of urea into deionized water, stirring to dissolve, adding 2.75mmol of Bi (NO) into the solution3)3·5H2And O, mechanically stirring. After the stirring, 3mmol of sodium sulfide was added to obtain a mixed solution. The mixed solution was placed on a magnetic stirrer and mechanically stirred for 30 min. Transferring the mixed solution into a lining made of polytetrafluoroethylene, and placing the lining in a reaction kettle for reaction at 200 ℃ for 24 hours; and after the reaction is finished, naturally cooling to room temperature, centrifuging, washing with water, washing with alcohol, and drying at room temperature to obtain the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material.
The XRD pattern of the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material is shown in FIG. 1, and it can be seen from FIG. 1 that this example indeed produces a bismuth oxycarbonate-bismuth sulfide heterojunction. An SEM image of the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material is shown in figure 2, and as can be seen from figure 2, in the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material, bismuth oxycarbonate is blocky, and bismuth sulfide is rod-shaped. And the particle size of the bismuth oxycarbonate-bismuth sulfide heterojunction is found to be between 200 and 800nm through SEM, TEM and other tests.
Example 2
Adding 0.5g of urea into deionized water, stirring to dissolve, adding 2.75mmol of Bi (NO) into the solution3)3·5H2And O, mechanically stirring. After the stirring was completed, 4mmol of sodium sulfide was added to obtain a mixed solution. The mixed solution was placed on a magnetic stirrer and mechanically stirred for 30 min. Transferring the mixed solution into a lining made of polytetrafluoroethylene, and placing the lining in a reaction kettle for reaction at 200 ℃ for 24 hours; and after the reaction is finished, naturally cooling to room temperature, centrifuging, washing with water, washing with alcohol, and drying at room temperature to obtain the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material.
Example 3
Adding 0.5g of urea into deionized water, stirring to dissolve, adding 2.75mmol of Bi (NO) into the solution3)3·5H2And O, mechanically stirring. After the stirring was completed, 4mmol of sodium sulfide was added to obtain a mixed solution. The mixed solution was placed on a magnetic stirrer and mechanically stirred for 30 min. Transferring the mixed solution into a lining made of polytetrafluoroethylene, and placing the lining in a reaction kettle for reaction at 180 ℃ for 24 hours; and after the reaction is finished, naturally cooling to room temperature, centrifuging, washing with water, washing with alcohol, and drying at room temperature to obtain the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material.
Comparative example 1: preparation of bismuth oxycarbonate photocatalyst
Adding 0.5g of urea into deionized water, stirring to dissolve, adding 2.75mmol of Bi (NO) into the solution3)3·5H2And O, mechanically stirring. After completion of stirring, a mixed solution was obtained. Placing the mixed solution in a magnetic forceMechanically stirring for 30 min. Transferring the mixed solution into a lining made of polytetrafluoroethylene, and placing the lining in a reaction kettle for reaction at 200 ℃ for 24 hours; and after the reaction is finished, naturally cooling to room temperature, centrifuging, washing with water and alcohol, and drying at room temperature to obtain the bismuthyl carbonate photocatalytic material.
Comparative example 2: preparation of bismuth sulfide photocatalyst
0.73g of Bi (NO)3)3Adding into 5mL of ethylene glycol, stirring with a stirrer for 5min to dissolve completely to obtain clear solution A, adding 1.5g Na2S·9H2Dissolving O in 10mL of deionized water to obtain a solution B, slowly and dropwise adding the solution B into the solution A, and continuously and rapidly stirring to form a black precursor; finally, 0.76g of CO (NH) was added to the precursor2)2Preparing 30mL of solution (the volume ratio of the deionized water to the organic solution is 5: 1), pouring the solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, the capacity of which is 50mL, placing the reaction kettle in a constant temperature oven at 120 ℃ to heat at constant temperature for 12h, washing the product with the deionized water for several times after the reaction is finished, and drying the product at 80 ℃ for 6h (Liuyun, Nao Guo Qiang, Zhu Qiang, S and Bi ratio for hydrothermal synthesis of Bi2S3Influence of powder morphology [ J]Journal of Shanxi university of science and technology (Nature science edition), 2010,28(02):40-44.)
Application example: application of composite photocatalyst in degrading organic pollutant DBP under visible light
50mg of the catalysts prepared in the example 2 and the comparative examples 1-2 are respectively placed in a 100mL beaker, 25mL of ultrapure water is added, the mixture is subjected to ultrasonic treatment for 20min to be uniformly dispersed, 25mL of 20mg/L DBP solution is added to the uniform solution after ultrasonic treatment, and a photocatalytic system of 10mg/L DBP solution and 0.5g/L of catalyst are obtained. Stirring with a magnetic stirrer. And (3) placing the beaker on a magnetic stirrer, and carrying out dark reaction under the stirring condition to uniformly disperse the catalyst in the system and achieve adsorption balance.
After the dark reaction (sampling 2mL), the beaker is surrounded by a self-made ice bag, and a xenon lamp light source is turned on to carry out a visible light catalytic degradation experiment. In the process of photocatalytic reaction, 2mL samples are taken every 20min, and the reaction time is 3h in total.
Centrifuging in a centrifuge tube at 10000 rpm for 5min, separating solid and liquid, recovering catalyst, filtering the liquid with 0.45 μm filter head (organic system), placing into a chromatographic bottle, and storing at 4 deg.C.
And (3) measuring the pollutant concentration of the prepared sample by using high performance liquid chromatography to judge the degradation efficiency of the composite material. As can be seen from FIG. 3, the catalyst prepared in example 2 can effectively degrade DBP, and the retention rate of DBP after degradation is only about 30%; after the DBP is degraded by the bismuthyl carbonate of the comparative example 1, the retention rate of the DBP is about 80 percent; the retention of DBP after degradation of DBP by bismuth sulfide of comparative example 2 was around 60%. Therefore, the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material prepared by the method can realize effective degradation of plasticizers such as DBP and the like.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (9)
1. A preparation method of a bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material is characterized by comprising the following steps:
(1) adding urea into deionized water, stirring to dissolve, and adding Bi (NO)3)3·5H2Continuously stirring the mixture O, and adding sodium sulfide to obtain a mixed solution;
(2) and stirring the mixed solution, then carrying out closed reaction, naturally cooling to room temperature after the reaction is finished, centrifuging, washing with water, washing with alcohol, and drying at room temperature to obtain the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material.
2. The method according to claim 1, wherein in the step (1), the urea is mixed with Bi (NO)3)3·5H2The molar ratio of O is (6-10) to (1-3).
3. The method according to claim 2, wherein in the step (1), said Bi (NO) is3)3·5H2O and Na2The molar ratio of S is (1-3) to (1-4).
4. The method according to claim 1, wherein in the step (2), the stirring is magnetic stirring, and the stirring time is 15-60 min.
5. The method as claimed in claim 1, wherein in the step (2), the temperature of the sealing reaction is 150 ℃ to 240 ℃, and the reaction time is 12-48 h.
6. The method as claimed in claim 1, wherein in the step (2), the temperature of the centrifugation is 4-25 ℃, the rotation speed of the centrifugation is 4000-12000rpm, and the time of the centrifugation is 5-15 min.
7. The bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material prepared by the preparation method of any one of claims 1 to 6.
8. The bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material of claim 7, wherein the bismuth oxycarbonate is bulk and the bismuth sulfide is rod-shaped.
9. Use of the bismuth oxycarbonate-bismuth sulfide heterostructure photocatalytic material of claim 7 or 8 in the photocatalytic degradation of plasticizers.
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