CN101177302A - Method for preparing nano bismuth oxide - Google Patents
Method for preparing nano bismuth oxide Download PDFInfo
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- CN101177302A CN101177302A CNA2006101182159A CN200610118215A CN101177302A CN 101177302 A CN101177302 A CN 101177302A CN A2006101182159 A CNA2006101182159 A CN A2006101182159A CN 200610118215 A CN200610118215 A CN 200610118215A CN 101177302 A CN101177302 A CN 101177302A
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- bismuth oxide
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- 229910000416 bismuth oxide Inorganic materials 0.000 title claims abstract description 22
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- -1 bismuth salt compound Chemical class 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- QYIGOGBGVKONDY-UHFFFAOYSA-N 1-(2-bromo-5-chlorophenyl)-3-methylpyrazole Chemical compound N1=C(C)C=CN1C1=CC(Cl)=CC=C1Br QYIGOGBGVKONDY-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000002474 experimental method Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 8
- 238000007254 oxidation reaction Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 230000005855 radiation Effects 0.000 abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 229910000831 Steel Inorganic materials 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- 239000010959 steel Substances 0.000 abstract description 2
- 238000004056 waste incineration Methods 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 241001005836 Euchloe ausonia Species 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229940049676 bismuth hydroxide Drugs 0.000 description 1
- TZSXPYWRDWEXHG-UHFFFAOYSA-K bismuth;trihydroxide Chemical compound [OH-].[OH-].[OH-].[Bi+3] TZSXPYWRDWEXHG-UHFFFAOYSA-K 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000007805 chemical reaction reactant Substances 0.000 description 1
- 238000005354 coacervation Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000002013 dioxins Chemical group 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Abstract
The invention provides a preparation method of bismuth oxide. Both bismuth salt compound and alcohol are available and taken as reaction materials. The bismuth oxide product is prepared through microwave radiation. The preparation method provided by the invention has the advantages of environmental friendliness, simple technology, low production cost, narrow distribution of the particle size of the product, strong oxidation, high catalysis activity, non-toxicity and good chemical stability; the invention can be used in the treatment of wastewater, sewage and exhaust gas and the field of energy material; the invention can also be used to reduce the emission of industrial pollutants and can be popularized and applied in the treatment of exhaust gas for waste incineration industry, such as the iron and steel enterprises in China.
Description
Technical field
The present invention relates to the oxide powder preparation field, be specifically related to a kind of preparation technology of bismuth oxide.
Background technology
Bismuth oxide (Bi
2O
3) as a kind of semiconductor catalyst, in the existing application widely of catalytic field, and the research in photocatalysis field is also less relatively.Semi-conductor Bi
2O
3Band-gap energy be 2.8eV (and traditional photocatalyst TiO
2Band-gap energy be 3.2eV), its energy gap and TiO
2Approaching, and because its good stability has good photochemical catalysis development prospect.Nanometer Bi
2O
3Because its specific surface area is big, surfactivity point is many, thereby can show more excellent photocatalysis activity.Have and report the experimental study that contains nitrite waste water and degradating organic dye with the bismuth oxide photochemical catalysis, the result shows, Bi
2O
3Has good photocatalytic activity.People such as Anthony have studied semi-conductor Bi
2O
3Catalyzed degradation organochlorine contamination thing.The fourth roc of Jilin University has been studied Bi
2O
3Photochemical catalytic oxidation character to gaseous-phase organic pollutant has obtained certain achievement.
The nanometer Bi of present report
2O
3The preparation method mainly contain chemical precipitation method, hydrolysis method, sol-gel method, molten atomizing oxidation style, microemulsion method, chemical gas phase coacervation, plasma method etc., the whole bag of tricks all has its characteristics.The precipitator method are simple to operate, the Bi for preparing
2O
3The product purity height, production cost is low.People such as Li Wei (CN 1544337A) disclose a kind of preparation nanometer Bi
2O
3Method, this method adopts pearl white concentrate as raw material, and it is leached, and obtains the nano bismuth oxide product with the sodium hydroxide solution precipitation after the removal of impurities.People such as Patil (Materials letters, 2005,59:2523-2525) obtain bismuth hydroxide by the ammonia precipitation process bismuth nitrate solution, obtain nano bismuth oxide through after the roasting.Hydrolysis method is come the synthesis oxide particle by the control hydrolysis condition, is a kind of method commonly used, very easily generates than coarse particles but use this method.Adopt the raw materials cost of sol-gel method preparation higher, but this method raw material mixes on the molecular level level, mixes highly evenly, the synthesis temperature of material is low, and material is formed easily and controlled, and equipment is simple.(journal of Shandong university (natural science edition) 1997,32 (1): such as Chen Dairong 88~93) with Bi (OR)
3(R:CH
2CH
2OCH
3, Cme
2Et) make presoma, synthesized Bi by the Sol-Gel method
2O
3It is spherical that polycrystal powder, the bismuth oxide micro-powder that obtains at last are approximately, and size range is 60~120nm.Adopt the technical process of molten atomizing oxidation style short, product purity is high, fine size, pollution-free, cost is low, but requires degree higher to equipment and processing parameter.(Wuhan University of Technology's journal, 2006,28 (2): 10~13) adopt bismuth vapor-phase oxidation method to make median size is the bismuth oxide powder of 33.7nm to Hu Hanxiang.The experimental installation of microemulsion method is simple, and energy consumption is low, strong operability, and powder monodispersity, interface property and the good stability of gained are compared with additive method, and particle diameter is easy to control, adapts to wide.But this method production cost is higher, needs to consume a large amount of organic solvent and tensio-active agent.There is report to be equipped with nanometer Bi with the polyhydroxy-alcohol legal system
2O
3, adopt this method effectively to stop particulate to be grown up, the Bi for preparing through this method
2O
3Grain diameter is 70~90nm (Journal of MaterialsScience 36 (2001) 297-299).More than several preparation methods relative merits are respectively arranged, and seek simple to operately, with low cost, monodispersity is good, the nanometer Bi that purity is high
2O
3The preparation method improve the key that it uses the width and the degree of depth.Trade effluent and waste gas are the serious organic pollutants of a kind of environmental pollution, and selecting a kind of catalytic activity height, cheap catalyzer is the key that realizes trade effluent and off gas treatment.
In order to overcome the deficiencies in the prior art, the present inventor utilizes the starting material that are easy to get, and adopts the microwave radiation mode of non-environmental-pollution, obtains the bismuth oxide product, thereby has finished the present invention.
Therefore, the preparation method who the purpose of this invention is to provide a kind of nano bismuth oxide.
Summary of the invention
The preparation method of nano bismuth oxide provided by the invention is called normal pressure liquid phase microwave method, may further comprise the steps:
1) dissolving step: the bismuth salt compound is dissolved in a small amount of organic solvent;
2) microwave irradiation step: carry out in the instrument of microwave transmissive member is housed, the reaction times is 3-60 minute, and reaction power is 180-900 watt;
3) washing step: with step 2) products therefrom water and dehydrated alcohol wash respectively;
4) drying step: drying temperature is 70-100 ℃;
5) calcination steps: maturing temperature is 500-700 ℃, and roasting time is 2-4 hour.
In dissolving step, the bismuth salt compound is selected from five nitric hydrate bismuths, bismuth acetate; Organic solvent is selected from ethylene glycol, propylene glycol; This step also can be used ultrasonic dispersing, and the time is 15-30 minute.
In microwave irradiation step, instrument can adopt household microwave oven, experiment with microwave oven, industrial microwave oven, preferably adopts the household microwave oven of being furnished with the water-cooled reflux after reequiping.Reactive mode can adopt continuous type of heating or be interrupted type of heating, wherein is interrupted type of heating and can adopts every heating in 0-15 minute once, and heating repeatedly repeatedly.
In drying step, its dry atmosphere is air atmosphere.
In calcination steps, preferred 600 ℃ of temperature; Preferred 2 hours of time.
Beneficial effect of the present invention is:
1) prior art for preparing technology relative complex, production cost is higher relatively and time-consuming; The present invention be with the bismuth salt compound that is easy to get and alcohols as the reaction starting material, technology is simple, easy to operate, raw material is easy to get, production cost is low, the synthetic condition is comparatively loose, can produce high value-added product.
2) instrument that microwave transmissive member is housed that the present invention is used can adopt the household microwave oven of being furnished with the water-cooled reflux, and this instrument is easy, be easy to get.The present invention adopts microwave radiation, and non-environmental-pollution is a kind of green synthesis process, is fit to the preparation method of the nano bismuth oxide of Small Scale Industry production.
3) the product particle size distribution of the present invention's preparation is narrower, and oxidation capacity is strong, and the catalytic activity height is nontoxic, and chemical stability is good.The present invention is prepared the experiment (experimental result as shown in Figure 3) that products therefrom carries out photochemical catalytic oxidation nitrite trade effluent, prove that this product is fit to waste gas pollution control and treatment (as the catalytic decomposition of Dioxins etc.), also can be applicable to environmental protection fields such as wastewater treatment, sewage disposal, energy and material.The reduction of discharging that also can be applicable to industrial pollutants is handled, and can be applied to the off gas treatment of domestic iron and steel enterprise, waste incineration industry.
Description of drawings
Fig. 1 is the process flow diagram of preparation bismuth oxide;
Fig. 2 is the XRD figure of presoma and product of roasting;
Fig. 3 is the time-efficiency curve diagram of 0.4g bismuth oxide photochemical catalytic oxidation 10mg/L nitrite trade effluent, and solution system pH value is 2.3.
Embodiment
The present invention is further elaborated with embodiment below, but these embodiment have any restriction to the present invention absolutely not.Any change that those skilled in the art are done in to the invention process under the enlightenment of this specification sheets all will drop in the scope of claims.
Embodiment 1 prepares the method for bismuth oxide
Accurately take by weighing 3.65g five nitric hydrate bismuths, measure the 50ml propylene glycol, both are mixed in beaker, ultra-sonic dispersion 30min dissolves fully to Bismuth trinitrate.Then above-mentioned mixed solution is transferred in the 250ml round-bottomed flask, places in the microwave oven that is connected to reflux and react, microwave power is 360W, microwave radiation 6 minutes (each 2 minutes, midfeather 1 minute, totally 3 times).After reaction finishes, collect product, carry out centrifugation, and respectively wash 3 times with deionized water and dehydrated alcohol.Dry 6h under 80 ℃.Obtain the bismuth oxide product at 600 ℃ of following roasting 2h.
Preparation technology's flow process of this method is seen Fig. 1.
The XRD spectra of products therefrom is seen Fig. 2.As can be seen, microwave product major part is unbodied non-crystalline state from b.As can be seen, sharp-pointed from a through the product X RD peak shape after the roasting, do not have assorted peak and exist, with α-Bi
2O
3Standard x RD spectrogram in full accord.
Embodiment 2
Accurately take by weighing the 1.66g bismuth acetate, measure 50ml ethylene glycol, both are mixed in beaker, ultra-sonic dispersion 20min dissolves fully to bismuth acetate.Then above-mentioned mixed solution is transferred in the 250ml round-bottomed flask, places in the microwave oven that is connected to reflux and react, microwave power is 180W, microwave radiation 20 minutes (each 4 minutes, midfeather 2 minutes, totally 5 times).After reaction finishes, collect product, carry out centrifugation, and respectively wash 3 times with deionized water and dehydrated alcohol.Dry 12h under 60 ℃.Obtain the bismuth oxide product at 550 ℃ of following roasting 2h.
The XRD spectra of products therefrom and Fig. 2 basically identical.
Embodiment 3
Accurately take by weighing the 1.66g bismuth acetate, measure the 50ml propylene glycol, both are mixed in beaker, ultra-sonic dispersion 20min dissolves fully to bismuth acetate.Then above-mentioned mixed solution is transferred in the 250ml round-bottomed flask, places in the microwave oven that is connected to reflux and react, microwave power is 540W, microwave radiation 16 minutes (each 4 minutes, midfeather 2 minutes, totally 4 times).After reaction finishes, collect product, carry out centrifugation, and respectively wash 3 times with deionized water and dehydrated alcohol.Dry 12h under 60 ℃.Obtain the bismuth oxide product at 650 ℃ of following roasting 2h.
The XRD spectra of products therefrom and Fig. 2 basically identical.
Claims (11)
1. the preparation method of a bismuth oxide is characterized in that may further comprise the steps:
1) dissolving step: the bismuth salt compound is dissolved in a small amount of organic solvent;
2) microwave irradiation step: carry out in the instrument of microwave transmissive member is housed, the reaction times is 3-60 minute, and reaction power is 180-900 watt;
3) washing step: with step 2) products therefrom water and dehydrated alcohol wash respectively;
4) drying step: drying temperature is 70-100 ℃;
5) calcination steps: maturing temperature is 500-700 ℃, and roasting time is 2-4 hour.
2. preparation method as claimed in claim 1, wherein said bismuth salt compound is selected from five nitric hydrate bismuths, bismuth acetate.
3. preparation method as claimed in claim 1, wherein said organic solvent is selected from ethylene glycol, propylene glycol.
4. as claim 1 or 2 or 3 described preparation methods, wherein said dissolving step can be used ultrasonic dispersing, and the time is 15-30 minute.
5. preparation method as claimed in claim 1, wherein said instrument is selected from household microwave oven, experiment microwave oven, industrial microwave oven.
6. preparation method as claimed in claim 5, wherein said household microwave oven is furnished with the water-cooled reflux.
7. preparation method as claimed in claim 1, wherein said microwave irradiation step can adopt continuous type of heating or be interrupted type of heating.
8. preparation method as claimed in claim 7, wherein said interruption type of heating can adopt every heating in 0-15 minute once, and heating is repeatedly repeatedly.
9. preparation method as claimed in claim 1, in the wherein said drying step, dry atmosphere is air atmosphere.
10. preparation method as claimed in claim 1, in the wherein said calcination steps, maturing temperature is 600 ℃.
11. preparation method as claimed in claim 1, in the wherein said calcination steps, roasting time is 2 hours.
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Cited By (7)
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CN101824625B (en) * | 2009-03-05 | 2012-05-16 | 南京理工大学 | Method for controllably synthesizing bismuth-based nano-material by directly electrolyzing metal bismuth |
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