CN109701563B - Preparation method of bismuth sulfide-bismuth oxybromide magnetic ternary composite visible-light-driven photocatalyst - Google Patents
Preparation method of bismuth sulfide-bismuth oxybromide magnetic ternary composite visible-light-driven photocatalyst Download PDFInfo
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Abstract
The invention relates to a preparation method of a bismuth sulfide-bismuth oxybromide magnetic ternary composite visible-light-induced photocatalyst, belonging to the technical field of inorganic photocatalytic materials. The method is mainly characterized in that the magnetic composite Bi is prepared by adopting a one-step hydrothermal method2S3/BiOBr visible light catalyst, wherein the p-n heterojunction formed between the catalysts effectively inhibits the recombination of photo-generated electrons and holes, SrFe12O19And Bi2S3The addition of the catalyst is beneficial to widening the photoresponse range of the catalyst, and the catalyst has strong stability and can be recycled; the preparation condition of the catalyst is mild, other organic matters are not involved, the preparation time of the catalyst is short, and the magnetic composite material is convenient to recover. SrFe12O19/Bi2S3The BiOBr is irradiated for 20min under visible light, so that the degradation rate of the simulated organic pollutant rhodamine B reaches 91.6 percent, and Bi without magnetism is added2S3the/BiOBr has the degradation efficiency of only 73.8 percent, can be separated and recovered through a simple external magnetic field, has the average recovery rate of 82.3 percent, and has good photocatalytic activity after being recovered.
Description
Technical Field
The invention relates to a preparation method of a bismuth sulfide-bismuth oxybromide magnetic ternary composite visible-light-induced photocatalyst, belonging to the technical field of inorganic photocatalytic materials.
Background
As is well known, the photocatalytic technology has the advantages of low energy consumption, simple operation and mild reaction conditions, can be carried out at normal temperature and normal pressure, and becomes a research hotspot in the aspect of processing environmental problems. Bismuth-based photocatalysts have been widely paid attention as a novel visible-light photocatalyst having a layered structure and a reasonable band gap width, and currently, bismuth-based compounds include bismuth oxyhalide, bismuth sulfide, bismuth oxide, bismuth molybdate, bismuth vanadate, and the like. Bismuth oxyhalide (BiOX, X ═ Cl, Br, I) has attracted attention as a p-type semiconductor due to its characteristics such as simple preparation method, good photocatalytic effect, and no toxicity. Wherein, bismuth oxybromide (BiOBr) has response in a visible light region and moderate forbidden band width, is an indirect semiconductor, and has great application prospect in visible light catalytic materials due to the advantages. However, the application of the BiOBr in the fields of environment, energy and the like is limited due to the defects of low visible light utilization rate, easy recombination of holes and electrons, too regular conduction band position and the like. Therefore, it is the basic starting point of the invention to modify the BiOBr to increase the visible light utilization rate, hinder the recombination of holes and electrons and improve the reduction capability of photo-generated electrons.
Bismuth sulfide (Bi)2S3) Is an important layered semiconductor material and has potential application value in thermoelectric, electronic and optoelectronic devices and infrared spectroscopy. In addition, it has a band gap energy of 1.2eV-1.7eV, and is a potential photocatalyst responding to visible light. However, the single bismuth sulfide has low photocatalytic efficiency because the valence band and conduction band are relatively close to each other and the rate of recombination of photogenerated electrons and holes is high. Adding Bi2S3The BiOBr is used for modifying the BiOBr to form a compound, and the response capability of the BiOBr to visible light can be enhanced.
The problem of difficult catalyst recovery usually exists in the process of photocatalytic degradation of organic wastewater. In order to prevent the secondary pollution caused by incomplete recovery of the photocatalyst and reduce the use cost, the photocatalyst is magnetized, and the separation, recovery and reuse are convenient. SrFe12O19As a typical hard magnetic material, the material has higher saturation magnetization and produces a synergistic effect on photocatalysis; loading magnetic strontium ferrite to Bi2S3The BiOBr compound can improve the photocatalytic activity and is beneficial to the recovery of the catalyst.
No magnetic Bi has been found2S3The research of the/BiOBr composite catalyst is reported. Existing Bi2S3The preparation method of the/BiOBr composite photocatalyst comprises the following steps: "Photocosmetic activities of Bi" in Applied Surface Science "vol 2014 290, page 233-2S3[ BIOBr nanocomposites synthesized by a simple hydrothermatic Process ] (COMPARATIVE DOCUMENT 1)The preparation method is characterized in that bismuth nitrate, thiourea, ethylene glycol and potassium bromide are used as raw materials and react in a hydrothermal kettle for 24 hours to obtain the bismuth nitrate/thiourea composite material, and the method has the following defects: (1) the sample is prepared by adopting the mixed reaction of an inorganic reagent and an organic reagent, the appearance is uneven (the appearance diagram of the product is not given), and the reaction time is too long; (2) in the sample preparation process, various organic matters (thiourea, ethylene glycol and ethanol) are used, peculiar smell and odor can be generated, high-concentration nitrogen-containing organic wastewater is generated, and the environment-friendly requirement is not met; (3) the degradation rate of methyl orange under visible light is low, and 40mL of 0.05g of composite catalyst is degraded to 3.05X 10-5mol·L-1The degradation rate of the (10mg/L) methyl orange solution in 2h is only 60 percent. (4) No method for recovering the catalyst and no recovery rate are given.
As another example is the literature: "RSC Advances" volume 5 of 2015 16239 and 16249 of "One-pot synthesis of heterologous Bi2S3BiOBr microspheres with high sensitivity light photocatalytic performance (reference 2), the preparation method is to prepare Bi by using bismuth nitrate, thiourea and potassium bromide as raw materials and adopting a solvothermal method2S3and/BiOBr. The method has the following defects: (1) the whole synthesis process is carried out in 2-methoxy ethanol (solvent), the cost for preparing the catalyst by the solvothermal method is high, the preparation period is long, and the synthesis and drying need 12 hours respectively; (2) the activity of the composite catalyst is limited, and when 100mg of the catalyst degrades 100ml of rhodamine B with the concentration of 50mg/L under the irradiation of visible light, the degradation rate of 80min is 98.6%; (3) thioacetamide is used as a sulfur source, 2-methoxy ethanol is used as a solvent, so that odor substances are generated in the reaction process, and the solvent generated by filtering after the reaction is finished is dangerous waste and does not meet the requirement of clean production.
Further, as In "Materials Science and Engineering B" In 2017, volume 224, pages 69 to 77, "In situ synthesis of a nanoplate-like Bi-based heterojunction for photocatalytic degradation of ciprofloxacin" (reference 3), the preparation method thereof: firstly preparing single BiOBr by a water bath heating method, then adding thioacetamide into the prepared BiOBr, and then preparing the BiOBr by the water bath heating method through an ion exchange reactionBi2S3and/BiOBr. The method has the following defects: (1) the preparation method adopts a two-step method, each step needs heating reaction and long-time drying, and the experimental process is complicated and time-consuming. (2) The prepared composite catalyst has low degradation to the ciprofloxacin, and the degradation rate of 50mg of the composite to 100mL of 10mg/L ciprofloxacin aqueous solution in 3h under visible light is less than 80%. (3) Various organic matters (thioacetamide, glycol and ethanol) are used in the preparation process of the sample, odor can be generated, high-concentration nitrogen-containing organic wastewater is generated, and the preparation method does not meet the environment-friendly requirement. Thus, the hydrothermal method is used to prepare SrFe12O19And optimizing Bi2S3Method for preparing BiOBr, and SrFe12O19And Bi2S3Bi improved by/BiOBr compounding2S3The catalytic effect, recovery rate and magnetic stability of/BiOBr are necessary.
Disclosure of Invention
The invention belongs to the field of semiconductor visible light catalytic materials, and relates to a method for preparing magnetic composite Bi by adopting a one-step hydrothermal method2S3The p-n heterojunction formed in the/BiOBr visible light catalyst effectively inhibits the recombination of photo-generated electrons and holes, so that the photoresponse range of the catalyst is widened, the catalyst is high in stability, can be recycled, the preparation condition is mild, the time consumption is less, and the magnetic composite material is convenient to recycle.
Bi of the present invention2S3/BiOBr/SrFe12O19The preparation method of the composite visible-light-driven photocatalyst comprises the following steps:
weighing 2mmol of Bi (NO)3)3Dissolving 0.1g of PVP into 10mL of nitric acid solution with the concentration of 2mol/L to obtain solution A, weighing 2mmol of NaBr to dissolve into 10mL of sodium hydroxide solution with the concentration of 2mol/L to obtain solution B, weighing 0.3mmol of sodium sulfide to dissolve into 10mL of water to obtain solution C; adding the solution A into the solution B, adjusting the pH value to 5-9 by using 2mol/L sodium hydroxide solution, fully stirring for 30min, adding the solution C, ultrasonically stirring for 1h, and then adding 0.03-0.12 g of SrFe12O19Fully stirring to obtain suspension D; putting the suspension D into a 100mL reaction kettle, reacting for 4h at 140-180 ℃, and naturally coolingCooling to room temperature, filtering, washing with deionized water for several times, and drying in a 60 ℃ oven for 8h to obtain Bi2S3/BiOBr/SrFe12O19And compounding the visible light catalyst.
By adopting the technical scheme, the invention mainly has the following effects:
(1) the magnetic composite Bi prepared by the method of the invention2S3/BiOBr/SrFe12O19The visible light catalyst is prepared by one-step hydrothermal synthesis, has the advantages of simple steps, mild reaction conditions, short reaction time and no need of organic solvents compared with the comparison documents 1, 2 and 3.
(2) The magnetic composite Bi prepared by the method of the invention2S3/BiOBr/SrFe12O19The visible light photocatalyst has uniform granularity and good stability, can be separated and recovered by a simple external magnetic field, has an average recovery rate of 82.3 percent, and can be repeatedly used.
(3) The magnetic composite Bi prepared by the method of the invention2S3/BiOBr/SrFe12O19Catalytic performance of visible light catalyst relative to single Bi2S3And BiOBr, the catalytic effect is remarkably improved, the degradation rate of rhodamine B reaches 91.6% after the rhodamine B is irradiated for 20min under visible light, and the result is obviously superior to that of the comparison document 1 and the comparison document 2.
Drawings
FIG. 1 shows Bi prepared in example 22S3/BiOBr、Bi2S3/BiOBr/SrFe12O19X-ray diffraction pattern (XRD) of the composite visible-light catalyst.
FIG. 2 shows Bi prepared in example 22S3/BiOBr/SrFe12O19An infrared spectrum (FTIR) of the composite visible light catalyst.
FIG. 3 shows Bi prepared in example 22S3/BiOBr、Bi2S3/BiOBr/SrFe12O19A test curve of the photocatalytic degradation performance of the composite visible-light-induced photocatalyst on rhodamine B is provided.
FIG. 4 shows Bi prepared in example 22S3/BiOBr/SrFe12O19VSM spectrum of composite visible photocatalyst.
FIG. 5 shows Bi prepared in example 22S3/BiOBr/SrFe12O19A comparative graph of the recycling degradation effect of the composite visible-light-driven photocatalyst.
Detailed Description
The present invention will be further described with reference to the following specific embodiments.
Example 1
The preparation method of the bismuth sulfide-bismuth oxybromide magnetic ternary composite visible-light-driven photocatalyst comprises the following specific steps:
weighing 2mmol of Bi (NO)3)3Dissolving 0.1g of PVP into 10mL of nitric acid solution with the concentration of 2mol/L to obtain solution A, weighing 2mmol of NaBr to dissolve into 10mL of sodium hydroxide solution with the concentration of 2mol/L to obtain solution B, weighing 0.3mmol of sodium sulfide to dissolve into 10mL of water to obtain solution C; adding the solution A into the solution B, adjusting the pH value to 5 by using 2mol/L sodium hydroxide solution, fully stirring for 30min, adding the solution C, ultrasonically stirring for 1h, and then adding 0.03g of SrFe12O19Fully stirring to obtain suspension D; putting the suspension D into a 100mL reaction kettle, reacting for 4h at 140 ℃, naturally cooling to room temperature, filtering, washing with deionized water for several times, and drying in a 60 ℃ oven for 8h to obtain Bi2S3/BiOBr/SrFe12O19And compounding the visible light catalyst.
Example 2
The preparation method of the bismuth sulfide-bismuth oxybromide magnetic ternary composite visible-light-driven photocatalyst comprises the following specific steps:
weighing 2mmol of Bi (NO)3)3Dissolving 0.1g of PVP into 10mL of nitric acid solution with the concentration of 2mol/L to obtain solution A, weighing 2mmol of NaBr to dissolve into 10mL of sodium hydroxide solution with the concentration of 2mol/L to obtain solution B, weighing 0.3mmol of sodium sulfide to dissolve into 10mL of water to obtain solution C; adding the solution A into the solution B, adjusting the pH value to 7 by using 2mol/L sodium hydroxide solution, fully stirring for 30min, adding the solution C, ultrasonically stirring for 1h, and then adding 0.06g of SrFe12O19Stirring thoroughlyObtaining a suspension D; putting the suspension D into a 100mL reaction kettle, reacting for 4h at 160 ℃, naturally cooling to room temperature, filtering, washing with deionized water for several times, and putting into a 60 ℃ oven for drying for 8h to obtain Bi2S3/BiOBr/SrFe12O19And compounding the visible light catalyst.
Example 3
The preparation method of the bismuth sulfide-bismuth oxybromide magnetic ternary composite visible-light-driven photocatalyst comprises the following specific steps:
weighing 2mmol of Bi (NO)3)3Dissolving 0.1g of PVP into 10mL of nitric acid solution with the concentration of 2mol/L to obtain solution A, weighing 2mmol of NaBr to dissolve into 10mL of sodium hydroxide solution with the concentration of 2mol/L to obtain solution B, weighing 0.3mmol of sodium sulfide to dissolve into 10mL of water to obtain solution C; adding the solution A into the solution B, adjusting the pH to 9 with 2mol/L sodium hydroxide solution, stirring for 30min, adding the solution C, stirring for 1h with ultrasonic wave, and adding 0.12g SrFe12O19Fully stirring to obtain suspension D; putting the suspension D into a 100mL reaction kettle, reacting for 4h at 180 ℃, naturally cooling to room temperature, filtering, washing with deionized water for several times, and drying in a 60 ℃ oven for 8h to obtain Bi2S3/BiOBr/SrFe12O19And compounding the visible light catalyst.
Results of the experiment
Bi prepared in example 22S3/BiOBr/SrFe12O19The catalytic degradation activity is optimal. For convenience of comparison, Bi was prepared2S3the/BiOBr sample. Bi2S3The preparation method of the/BiOBr is that in example 2, SrFe is not added12O19。
Bi prepared in example 22S3/BiOBr、Bi2S3/BiOBr/SrFe12O19The XRD spectrum of (A) is shown in FIG. 1. It can be seen that the complex Bi2S3The diffraction peak of BiOBr in BiOBr almost matches with the diffraction peak of standard card (73-2061), and is tetragonal BiOBr. Having a major exposed crystal face of [001 ]]、[011]、[012]、[110]、[020]、[014]、[114]And [212 ]]Corresponding to 2 theta10.946 degrees, 25.260 degrees, 31.810 degrees, 32.311 degrees, 39.432 degrees, 50.841 degrees, 56.355 degrees and 57.309 degrees, and the positions of diffraction peaks are not found to be shifted, which indicates that the composite Bi is2S3The crystal structure of the BiOBr is not changed later. However, Bi could not be found2S3Is probably due to Bi2S3May also be present in amorphous form due to too low a reaction temperature, failing to expose diffraction peaks; the remainder did not show any hetero-peaks. Bi2S3/BiOBr/SrFe12O19With simultaneous exposure of BiOBr [001 ] in the complex]、[011]、[012]、[110]、[020]、[014]、[114]And [212 ]]Standard diffraction peaks corresponding to crystal planes, and two peaks at 30.325 DEG and 34.182 DEG corresponding to SrFe12O19Characteristic peak crystal plane [114 ]]And [110 ]]Indicates the presence of SrFe12O19And no other miscellaneous peaks.
Bi prepared in example 22S3/BiOBr/SrFe12O19The FTIR spectrum of (A) is shown in FIG. 2, wherein 554.0cm-1And 604.0cm-1The left and right are SrFe12O19Characteristic absorption peak of 490cm-1Is a characteristic absorption peak of Bi-O, 1390cm-1Is CO in the air2Typical symmetrical telescopic vibration of 1400cm-1Near is the expansion vibration peak of Bi-S, 1600cm-1Nearby is the bending vibration peak of H-O-H of physically adsorbed water, 3440cm-1The vicinity is a stretching vibration peak of-OH on the catalyst surface. From the FT-IR plot again it is evident that SrFe is present in addition to BiOBr12O19And also demonstrates Bi that is not detectable in XRD2S3Is present.
Bi prepared in example 22S3/BiOBr、Bi2S3/BiOBr/SrFe12O19The result of the visible light photocatalyst on the photodegradability test of 100mL rhodamine B (RhB) with the concentration of 20mg/L is shown in FIG. 3. When Bi is present2S3After the BiOBr is illuminated for 20min, the photocatalytic degradation efficiency is only 73.8 percent, and 10 percent of SrFe is compounded12O19Of Bi2S3/BiOBr/SrFe12O19The degradation efficiency reaches 91.6 percent, which indicates that when a proper amount of SrFe is compounded12O19The photocatalytic performance of the photocatalyst can be enhanced, on the one hand, due to SrFe12O19The forbidden band width is low, and the excitation can be realized under visible light, so that the response intensity to light is improved; can generate photoproduction electrons and holes under the illumination condition, and SrFe12O19Energy band position and composite Bi2S3The BiOBr is different, and energy band difference can be generated between the BiOBr and the BiOBr, so that separation of photogenerated electron holes is facilitated; on the other hand, the magnetic substance can generate a relatively stable magnetic field, and when the composite magnetic photocatalyst is excited by light to generate electron transition, the magnetic field can promote the shunting of photo-generated electrons, so that the separation efficiency of the photo-generated electrons and holes is effectively improved.
FIG. 4 shows Bi prepared in example 22S3/BiOBr/SrFe12O19According to the VSM spectrum of the visible light photocatalyst, the saturation magnetization (Ms) and the residual magnetization (Mr) of the catalyst are 4.247emu/G and 1.521emu/G respectively, the coercive force (Hc) is 971.62G, and the strong coercive force of the catalyst is due to good demagnetization resistance, so that the catalyst is a hard magnetic material. Under the action of an external magnetic field, the recovery of the catalyst is facilitated, and the average recovery rate of the catalyst is 82.3%.
FIG. 5 shows Bi prepared in example 22S3/BiOBr/SrFe12O19The degradation efficiency of the catalyst after the visible light photocatalyst is recycled can be seen from the graph, the degradation efficiency is not obviously reduced after the catalyst is recycled, and the catalyst has better stability and can be reused.
Claims (4)
1. A preparation method of a bismuth sulfide-bismuth oxybromide magnetic ternary composite visible-light-driven photocatalyst is characterized by comprising the following steps:
weighing 2mmol of Bi (NO)3)3Dissolving 0.1g PVP in 10mL of 2mol/L nitric acid solution to obtain solution A, weighing 2mmol NaBr in 10mL of 2mol/L sodium hydroxide solution to obtain solution B, weighing 0.3mmol sodium sulfide in 10mL of water to obtain solution BSolution C; adding the solution A into the solution B, adjusting the pH value to 5-9 by using 2mol/L sodium hydroxide solution, fully stirring for 30min, adding the solution C, ultrasonically stirring for 1h, and then adding 0.03-0.12 g of SrFe12O19Fully stirring to obtain suspension D; putting the suspension D into a 100mL reaction kettle, reacting for 4h at 140-180 ℃, naturally cooling to room temperature, carrying out suction filtration, washing with deionized water for several times, and putting into a 60 ℃ oven for drying for 8h to obtain Bi2S3/BiOBr/SrFe12O19And compounding the visible light catalyst.
2. The preparation method of the bismuth sulfide-bismuth oxybromide magnetic ternary composite visible-light-driven photocatalyst according to claim 1, characterized by simple steps, mild reaction conditions, short reaction time and no need of organic solvents.
3. The preparation method of the bismuth sulfide-bismuth oxybromide magnetic ternary composite visible-light-driven photocatalyst according to claim 1, wherein the catalyst has uniform particle size and good stability, can be separated and recovered by a simple external magnetic field, has an average recovery rate of 82.3%, and can be reused.
4. The preparation method of the bismuth sulfide-bismuth oxybromide magnetic ternary composite visible-light-driven photocatalyst according to claim 1, characterized in that the catalyst is irradiated for 20min under visible light, so that the degradation rate of rhodamine B can reach 91.6%, and the photocatalyst has high catalytic activity.
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