CN101811733A - Visible light-responded basic bismuth bromide nanostructured microsphere material and preparation method thereof - Google Patents
Visible light-responded basic bismuth bromide nanostructured microsphere material and preparation method thereof Download PDFInfo
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- CN101811733A CN101811733A CN200910273074A CN200910273074A CN101811733A CN 101811733 A CN101811733 A CN 101811733A CN 200910273074 A CN200910273074 A CN 200910273074A CN 200910273074 A CN200910273074 A CN 200910273074A CN 101811733 A CN101811733 A CN 101811733A
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Abstract
The invention relates to a visible light-responded basic bismuth bromide nanostructured microsphere material and a preparation method thereof, and belongs to the field of chemical preparation of metal materials by a wet method. The preparation method is characterized in that: bismuthous salt and bromide are taken as raw materials, and are dissolved in a non-aqueous solvent to form precursor solution; hydro-thermal reaction is carried out in a reaction kettle so as to obtain a product; and the product is filtered, washed, and dried in the air atmosphere at certain temperature to form the basic bismuth bromide microsphere photocatalytic material with a nanosheet microstructure. The basic bismuth bromide nanostructured microsphere synthesized by the method has the diameter ranged from 2 to 8 mu m, and the nanosheet forming the basic bismuth bromide nanostructured microsphere has the thickness below 100nm. The visible light-responded basic bismuth bromide nanostructured microsphere material has high purity, good dispersibility and high visible light photocatalytic activity; under the radiation of visible light with the wavelength more than 420nm, the removal rate for nitric oxide gas with the initial concentration of 400ppb in 30 minutes reaches 30 percent. The synthetic route is simple; the whole technological process is easily controlled; and the preparation method is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of visible light-responded basic bismuth bromide nanostructured microsphere, belong to wet chemistry and make field of nanometer material technology.
Background technology
In recent years, nano structural material, because its particular structure characteristics, have simultaneously that specific surface area is big, surfactivity is high, Surface Permeability is strong and characteristics such as surperficial easily functionalization, can satisfy multiple new application requiring, thereby more and more receive publicity in fields such as environment, the energy, material, life sciences, and use to some extent in fields such as solar photocell, biological medicine, chemical storage, high selection catalysis.Research based on the photocatalysis technology of nano semiconductor material is also very noticeable.Nano titanium oxide (TiO
2) because better comprehensive performance is arranged, be most popular simplification mixture catalyst in research and the application.But, TiO
2Photocatalytic activity can only be excited by the near ultraviolet part that wavelength is equal to or less than 387nm, thereby has limited its effective utilization to sun power.Existing increasing work concentrates on the visible light-responded novel photocatalysis agent of research, and some impressive progresses have been obtained, as oxynitride, sulfide, titanate, niobate, tantalate, vanadate and chromic salt etc., in the various photocatalysts of having researched and developed at present, bismuth (Bi) based semiconductor photocatalyst is to have visible light-responded photocatalyst, has good photocatalysis performance under visible light.
Have not yet to see patent report about the preparation of preparation basic bismuth bromide nanostructured microsphere material, domestic is that the patent of nano structural material only limits to the nano-powder particle about bismuth, as adopting the visible light-responded bismuthic acid barium sodium light catalyzer of Hydrothermal Preparation (Chinese patent application number: 200610024280.5); Adopt the synthetic a kind of visible light-responded bismuthic acid barium photocatalyst of low-temperature burning method (Chinese patent application number: 200810036882); Prepare sheet BiOX (Chinese patent application number: 200710178744) by hydrolysis Bismuth trinitrate in halide anion type ionic liquid at room temperature; Adopt electrophoretic deposition to prepare a kind of strontium bismuth tantalite nanometer line (Chinese patent application number: 200810064756); Perhaps prepare pucherite nano-powder (Chinese patent application number: 200810048418) by hydro-thermal reaction.
The present invention utilizes the Hydrothermal Preparation basic bismuth bromide nanostructured microsphere material, and technology is simple, mild condition, cost is low, and the bismuthyl bromide microsphere particle that makes is more even, and surface-area is bigger, have the visible light-responded good and high characteristics of photocatalytic activity, be convenient to further extension and produce.
Summary of the invention
The object of the present invention is to provide a kind of visible light-responded basic bismuth bromide nanostructured microsphere material and preparation method.This basic bismuth bromide nanostructured microsphere material has visible light-responded photocatalysis performance, and under the visible light irradiation of wavelength greater than 420nm, starting point concentration is that the interior clearance of the nitric oxide gas 30min of 400ppb reaches 30%.
Realize a kind of visible light-responded basic bismuth bromide nanostructured microsphere material of above-mentioned purpose, it is characterized in that: this micro-sphere material is made up of the bismuthyl bromide nanometer sheet, nanometer sheet thickness is below 100nm, diameter of micro ball is in 2～8 mu m ranges, this basic bismuth bromide nanostructured microsphere material has visible light-responded photocatalysis performance, under the visible light irradiation of wavelength greater than 420nm, starting point concentration is that the interior clearance of the nitric oxide gas 30min of 400ppb reaches 30%.
Visible light-responded basic bismuth bromide nanostructured microsphere material of the present invention adopts hydrothermal method synthetic, with bismuthous salt and bromide is starting material, it is dissolved in obtains precursor solution in the non-aqueous solvent, in reactor, carry out hydro-thermal reaction and obtain product, product is drying to obtain the bismuthyl bromide microballoon photocatalyst material with nanometer sheet microtexture with washing back certain temperature in air atmosphere after filtration, and concrete preparation process is as follows:
Step 1, the bismuthous salt of employing are starting material, wiring solution-forming in non-aqueous solvent, and wherein the content of bismuth is 0.1-1mmol/L;
Step 2, in another container, the employing bromide is starting material, wiring solution-forming in non-aqueous solvent, the content of bromine is 0.1-1mmol/L in the solution;
Step 3, be under the stirring condition at the solution of step 1 gained, the solution of step 2 gained poured in the solution of step 1 gained, the content of bromine and bismuthous content equate in the solution;
Step 4, the solution of step 3 gained is poured in the hydrothermal reaction kettle, 180～200 ℃ of reactions 6～24 hours down;
Step 5, after the reaction process of step 4 finishes, solid product is filtered, and with distilled water or ethanol drip washing product more than 3 times;
Step 6, with the product of step 5 50～80 ℃ of air atmosphere dry 2～10 hours down, promptly obtain gray basic bismuth bromide nanostructured microsphere material;
Wherein said non-aqueous solvent is ethylene glycol or phenylcarbinol.
Described trivalent bismuth salt is Bismuth trinitrate, bismuth citrate or Trichlorobismuthine.
Described bromide is cetyl trimethylammonium bromide, Potassium Bromide or Sodium Bromide.
Advantage of the present invention:
1, synthetic route is simple, and whole technological process is controlled easily, is suitable for suitability for industrialized production.
2, synthetic basic bismuth bromide nanostructured microsphere material purity height, good dispersity;
3, the diameter of micron ball is in 2～8 mu m ranges, and the nanometer sheet thickness of forming microballoon is below 100nm, and specific surface area is big, visible light-responded good and photocatalytic activity height.
Description of drawings
Fig. 1 is the scanning electron microscope diagram of 3,000 times of amplifications of the basic bismuth bromide nanostructured microsphere for preparing of the present invention;
Fig. 2 is the scanning electron microscope diagram of 20,000 times of amplifications of the basic bismuth bromide nanostructured microsphere for preparing of the present invention;
Fig. 3 is the XRD figure of the basic bismuth bromide nanostructured microsphere for preparing of the present invention.
From Fig. 1 as seen, the gained sample is observed down through 3,000 times of amplifications of scanning electron microscope diagram (JSM-5600)), diameter of micro ball is at 2～8 μ m; From Fig. 2 as seen, the observations explanation ball under 20,000 times of amplifications of scanning electronic microscope is assembled by nanometer sheet, and nanometer sheet thickness is below 100nm.From Fig. 3 as seen, the gained sample is tested through XRD, and the peak value of characteristic peak in the diffracting spectrum and standard diffracting spectrum (BiOBr PDF 73-2061) coincide.
Embodiment
The present invention is further described below by embodiment.
Embodiment 1
The preparation basic bismuth bromide nanostructured microsphere, preparation process is:
Step 1, employing Bismuth trinitrate are starting material, are made into 0.1mmol/L solution in ethylene glycol;
Step 2, in another container, the employing Potassium Bromide is starting material, is made into the 0.1mmol/L ethylene glycol solution;
Step 3, be under the stirring condition, the solution of step 2 gained poured in the solution of step 1 gained at the solution of step 1 gained;
Step 4, pour in the hydrothermal reaction kettle, 180 ℃ of reactions 6 hours down at the solution of step 3 gained;
Step 5, after the reaction process of step 4 finishes, solid product is filtered, and with distilled water or ethanol drip washing product repeatedly;
Step 6, with the product of step 5 50 ℃ of air atmosphere dry 4 hours down, promptly obtain gray basic bismuth bromide nanostructured microsphere material.This micro-sphere material is made up of the bismuthyl bromide nanometer sheet, and nanometer sheet thickness is below 100nm, and diameter of micro ball is in 2～8 mu m ranges.
Embodiment 2
The preparation basic bismuth bromide nanostructured microsphere, preparation process is:
Step 1, employing Bismuth trinitrate are starting material, are made into 0.2mmol/L solution in ethylene glycol;
Step 2, in another container, the employing Sodium Bromide is starting material, is made into the 0.2mmol/L ethylene glycol solution;
Step 3, be under the stirring condition, the solution of step 2 gained poured in the solution of step 1 gained at the solution of step 1 gained;
Step 4, pour in the hydrothermal reaction kettle, 200 ℃ of reactions 12 hours down at the solution of step 3 gained;
Step 5, after the reaction process of step 4 finishes, solid product is filtered, and with distilled water or ethanol drip washing product repeatedly;
Step 6, with the product of step 5 80 ℃ of air atmosphere dry 2 hours down, promptly obtain gray basic bismuth bromide nanostructured microsphere material.This micro-sphere material is made up of the bismuthyl bromide nanometer sheet, and nanometer sheet thickness is below 100nm, and diameter of micro ball is in 2～8 mu m ranges.
Embodiment 3
The preparation basic bismuth bromide nanostructured microsphere, preparation process is:
Step 1, employing bismuth citrate are starting material, are made into 0.5mmol/L solution in ethylene glycol;
Step 2, in another container, the employing cetyl trimethylammonium bromide is starting material, is made into the 1mmol/L ethylene glycol solution;
Step 3, be under the stirring condition, the solution of step 2 gained poured in the solution of step 1 gained at the solution of step 1 gained;
Step 4, pour in the hydrothermal reaction kettle, 180 ℃ of reactions 24 hours down at the solution of step 3 gained;
Step 5, after the reaction process of step 4 finishes, solid product is filtered, and with distilled water or ethanol drip washing product repeatedly;
Step 6, with the product of step 5 50 ℃ of air atmosphere dry 10 hours down, can obtain gray basic bismuth bromide nanostructured microsphere material.This micro-sphere material is made up of the bismuthyl bromide nanometer sheet, and nanometer sheet thickness is below 100nm, and diameter of micro ball is in 2～8 mu m ranges.
Embodiment 4
The preparation basic bismuth bromide nanostructured microsphere, preparation process is:
Step 1, employing bismuth citrate are starting material, are made into 1mmol/L solution in phenylcarbinol;
Step 2, in another container, the employing cetyl trimethylammonium bromide is starting material, is made into the 1mmol/L benzyl alcohol solution;
Step 3, be under the stirring condition, the solution of step 2 gained poured in the solution of step 1 gained at the solution of step 1 gained;
Step 4, pour in the hydrothermal reaction kettle, 180 ℃ of reactions 6 hours down at the solution of step 3 gained;
Step 5, after the reaction process of step 4 finishes, solid product is filtered, and with distilled water or ethanol drip washing product repeatedly;
Step 6, with the product of step 5 50 ℃ of air atmosphere dry 10 hours down, can obtain gray basic bismuth bromide nanostructured microsphere material.This micro-sphere material is made up of the bismuthyl bromide nanometer sheet, and nanometer sheet thickness is below 100nm, and diameter of micro ball is in 2～8 mu m ranges.
Embodiment 5
The preparation basic bismuth bromide nanostructured microsphere, preparation process is:
Step 1, employing Trichlorobismuthine are starting material, are made into 0.5mmol/L solution in phenylcarbinol;
Step 2, in another container, the employing Sodium Bromide is starting material, is made into the 0.5mmol/L benzyl alcohol solution;
Step 3, be under the stirring condition, the solution of step 2 gained poured in the solution of step 1 gained at the solution of step 1 gained;
Step 4, pour in the hydrothermal reaction kettle, 200 ℃ of reactions 6 hours down at the solution of step 3 gained;
Step 5, after the reaction process of step 4 finishes, solid product is filtered, and with distilled water or ethanol drip washing product repeatedly;
Step 6, with the product of step 5 80 ℃ of air atmosphere dry 2 hours down, promptly obtain gray basic bismuth bromide nanostructured microsphere material.This micro-sphere material is made up of the bismuthyl bromide nanometer sheet, and nanometer sheet thickness is below 100nm, and diameter of micro ball is in 2～8 mu m ranges.
Embodiment 6
The preparation basic bismuth bromide nanostructured microsphere, preparation process is:
Step 1, employing Trichlorobismuthine salt are starting material, are made into 0.1mmol/L solution in phenylcarbinol;
Step 2, in another container, the employing Sodium Bromide is starting material, is made into the 0.1mmol/L benzyl alcohol solution;
Step 3, be under the stirring condition, the solution of step 2 gained poured in the solution of step 1 gained at the solution of step 1 gained;
Step 4, pour in the hydrothermal reaction kettle, 190 ℃ of reactions 12 hours down at the solution of step 3 gained;
Step 5, after the reaction process of step 4 finishes, solid product is filtered, and with distilled water or ethanol drip washing product repeatedly;
Step 6, with the product of step 5 60 ℃ of air atmosphere dry 6 hours down, promptly obtain gray basic bismuth bromide nanostructured microsphere material.This micro-sphere material is made up of the bismuthyl bromide nanometer sheet, and nanometer sheet thickness is below 100nm, and diameter of micro ball is in 2～8 mu m ranges.
Embodiment 7
With the basic bismuth bromide nanostructured microsphere material of embodiment 1-6 preparation, under the visible light irradiation of wavelength greater than 420nm, starting point concentration is that the interior clearance result of the nitric oxide gas 30min of 400ppb is as follows:
| Time (min) | Clearance (%) |
| ??1 | ??0 |
| ??2 | ??0 |
| Time (min) | Clearance (%) |
| ??3 | ??0.64 |
| ??4 | ??12.154 |
| ??5 | ??21.748 |
| ??6 | ??24.52 |
| ??7 | ??26.652 |
| ??8 | ??27.505 |
| ??9 | ??29.638 |
| ??10 | ??30.277 |
| ??11 | ??29.638 |
| ??12 | ??30.277 |
| ??13 | ??30.704 |
| ??14 | ??30.917 |
| ??15 | ??30.917 |
| ??16 | ??31.13 |
| ??17 | ??31.13 |
| ??18 | ??31.77 |
| ??19 | ??31.557 |
| ??20 | ??31.557 |
| ??21 | ??32.196 |
| ??22 | ??31.557 |
| ??23 | ??31.983 |
| ??24 | ??31.557 |
| Time (min) | Clearance (%) |
| ??25 | ??31.77 |
| ??26 | ??31.77 |
| ??27 | ??31.557 |
| ??28 | ??32.409 |
| ??29 | ??31.983 |
| ??30 | ??31.13 |
Claims (4)
1. visible light-responded basic bismuth bromide nanostructured microsphere, it is characterized in that: this microballoon is made up of the bismuthyl bromide nanometer sheet, nanometer sheet thickness is below 100nm, diameter of micro ball is in 2～8 mu m ranges, this basic bismuth bromide nanostructured microsphere material has visible light-responded photocatalysis performance, under the visible light irradiation of wavelength greater than 420nm, starting point concentration is that the interior clearance of the nitric oxide gas 30min of 400ppb reaches 30%.
2. the preparation method of the described visible light-responded basic bismuth bromide nanostructured microsphere of claim 1 is characterized in that preparation process is:
Step 1, the bismuthous salt of employing are starting material, wiring solution-forming in non-aqueous solvent, and wherein the content of bismuth is 0.1-1mmol/L;
Step 2, in another container, the employing bromide is starting material, wiring solution-forming in non-aqueous solvent, the content of bromine is 0.1-1mmol/L in the solution;
Step 3, be under the stirring condition at the solution of step 1 gained, the solution of step 2 gained poured in the solution of step 1 gained, the content of bromine and bismuthous content equate in the solution;
Step 4, the solution of step 3 gained is poured in the hydrothermal reaction kettle, 180～200 ℃ of reactions 6～24 hours down;
Step 5, after the reaction process of step 4 finishes, solid product is filtered, and with distilled water or ethanol drip washing product more than 3 times;
Step 6, with the product of step 5 50～80 ℃ of air atmosphere dry 2～10 hours down, promptly obtain gray basic bismuth bromide nanostructured microsphere material;
Wherein said non-aqueous solvent is ethylene glycol or phenylcarbinol.
3. the preparation method of 2 described visible light-responded basic bismuth bromide nanostructured microspheres as requested, it is characterized in that: described trivalent bismuth salt is Bismuth trinitrate, bismuth citrate or Trichlorobismuthine.
4. the preparation method of 2 described visible light-responded basic bismuth bromide nanostructured microspheres as requested, it is characterized in that: described bromide is cetyl trimethylammonium bromide, Potassium Bromide or Sodium Bromide.
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