CN103933967A - Biomimetic synthesis method of nanometer bismuth molybdate visible-light-induced photocatalyst - Google Patents
Biomimetic synthesis method of nanometer bismuth molybdate visible-light-induced photocatalyst Download PDFInfo
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- CN103933967A CN103933967A CN201410163679.6A CN201410163679A CN103933967A CN 103933967 A CN103933967 A CN 103933967A CN 201410163679 A CN201410163679 A CN 201410163679A CN 103933967 A CN103933967 A CN 103933967A
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Abstract
The invention discloses a biomimetic synthesis method of a nanometer bismuth molybdate visible-light-induced photocatalyst. According to the key points of the technical scheme, the biomimetic synthesis method of the nanometer bismuth molybdate visible-light-induced photocatalyst comprises the following steps of (1) dissolving soluble starch in a 1mol/L nitric acid solution, uniformly stirring, adding bismuth nitrate, and continuing to stir for 2h to obtain a mixing solution, wherein the mole ratio of soluble starch to bismuth nitrate is (1-4) to 1; and (2) adding molybdate to the mixed solution obtained in the step (1), stirring for 0.5h, regulating pH to be equal to 1-7 by using ammonium hydroxide, continuing to stir for 0.5h, performing hydrothermal reaction at 150-210 DEG C for 6-24h in a hydrothermal reaction kettle, performing centrifugal separation, washing, and carrying out 60-DEG C vacuum drying so as to obtain the nanometer bismuth molybdate visible-light-induced photocatalyst, wherein the mole ratio of molybdate to bismuth nitrate is 1 to 2. The bismuth molybdate visible-light-induced photocatalyst prepared by the biomimetic synthesis method provided by the invention is a nanometer material, and has a high visible-light catalytic activity which is higher than that of the bismuth molybdate visible-light-induced photocatalyst prepared by P25 and a common hydrothermal method.
Description
Technical field
The invention belongs to photocatalysis technology field, be specifically related to a kind of biomimetic synthesis method of nano bismuth molybdate visible light catalytic agent.
Background technology
Photocatalytic degradation pollutant, as a high-level oxidation technology, has application prospect for environment remediation, has also obtained increasing concern.And photochemical catalyst is the core of this technology, in numerous semiconductor light-catalysts, TiO
2due to features such as its biologically inert, strong oxidizing property, low-cost high-efficiency, fast light corrosion and chemical corrosivity and stiff stabilitys, be considered to be suitable for most the visible light catalyst of environmental pollution improvement.But TiO
2the shortcoming that still has some self to be difficult to overcome, as low in sunshine utilization rate, only can absorb the ultraviolet light that accounts for sunshine gross energy 4%, in visible-range, almost there is no photoresponse.Therefore, the visible light catalyst of development of new becomes an important research direction of photocatalysis field.
In recent years, some bismuth-system compound oxide photocatalysts had been subject to people's extensive concern, and this is the band gap relative narrower due to this based semiconductor photochemical catalyst, can under visible ray, excite generation photo-generated carrier, and by pollutant catalytic degradation.Occurred in recent years the research about bismuth molybdate, bismuth molybdate shows higher visible light catalysis activity.Crystal phase structure, the appearance and size etc. of photochemical catalyst is the principal element that affects its ultraviolet catalytic activity, and these have inseparable relation with its synthetic method and preparation condition.Nano-photocatalyst material has larger specific area because of it, often shows more excellent photocatalytic activity.And conventionally prepare the method for bismuth molybdate, and as coprecipitation, hydro-thermal method and solid phase method, the more difficult bismuth molybdate of preparing nano particle, therefore finds a kind of simple, easy to operate and eco-friendly method of preparing nano bismuth molybdate visible light catalytic agent highly significant.
Summary of the invention
The biomimetic synthesis method that the object of this invention is to provide a kind of simple and eco-friendly nano bismuth molybdate visible light catalytic agent, the bismuth molybdate visible light catalytic agent that the method makes is the nano material of particle diameter 20-200nm.
Technical scheme of the present invention is: a kind of biomimetic synthesis method of nano bismuth molybdate visible light catalytic agent, it is characterized in that comprising the following steps: (1) is dissolved in soluble starch in the salpeter solution of 1mol/L, after stirring, add bismuth nitrate, continue to stir 2h, obtain mixed solution, wherein the mol ratio of soluble starch and bismuth nitrate is 1-4:1; (2) in the prepared mixed solution of step (1), add molybdate, wherein the mol ratio of molybdate and bismuth nitrate is 1:2, stir 0.5h, regulate pH=1-7 with ammoniacal liquor again, continue to stir 0.5h, proceed to 150-210 DEG C of hydro-thermal reaction 6-24h in hydrothermal reaction kettle, centrifugation, washing, 60 DEG C of vacuum drying, make nano bismuth molybdate visible light catalytic agent.Described molybdate is sodium molybdate or ammonium molybdate.
The present invention compared with prior art has the following advantages: (1) the present invention has avoided synthetic in organic solvent or in the mixed solvent of organic solvent and water, simultaneously also avoided controlling product pattern and size with environmentally harmful organic substrate, because of but a kind of eco-friendly synthetic method; (2) the bismuth molybdate visible light catalytic agent of preparing is nano material, has higher visible light catalysis activity, higher than P25 and the standby bismuth molybdate visible light catalytic agent of common hydro-thermal legal system.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the nano bismuth molybdate visible light catalytic agent that makes of the embodiment of the present invention 1, Fig. 2 is the transmission electron microscope picture of the nano bismuth molybdate visible light catalytic agent that makes of the embodiment of the present invention 1, and Fig. 3 is the correlation curve of the standby bismuth molybdate visible light catalytic agent of the embodiment of the present invention 1 the nano bismuth molybdate visible light catalytic agent, P25 and the common hydro-thermal legal system that make to rhodamine B degradation rate.
Detailed description of the invention
By the following examples foregoing of the present invention is described in further details, but this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment, all technology realizing based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
0.685g soluble starch is dissolved in the salpeter solution of 1mol/L, after stirring, adds 1mmol bismuth nitrate, continue to stir 2h, obtain mixed solution; In this mixed solution, add 0.5mmol sodium molybdate, stir 0.5h, regulate pH=1 with ammoniacal liquor again, continue to stir 0.5h, proceed to 180 DEG C of hydro-thermal reaction 24h in hydrothermal reaction kettle, centrifugation, washing, 60 DEG C of vacuum drying, make nano bismuth molybdate visible light catalytic agent 1, Fig. 1 is the scanning electron microscope (SEM) photograph of the nano bismuth molybdate visible light catalytic agent that makes of the present embodiment, and Fig. 2 is the transmission electron microscope picture of the nano bismuth molybdate visible light catalytic agent that makes of the present embodiment, and the particle diameter of the bismuth molybdate visible light catalytic agent 1 making is as seen from the figure 20-200nm.
Embodiment 2
0.343g soluble starch is dissolved in the salpeter solution of 1mol/L, after stirring, adds 1mmol bismuth nitrate, continue to stir 2h, obtain mixed solution; In this mixed solution, add 0.5mmol ammonium molybdate, stir 0.5h, then regulate pH=3 with ammoniacal liquor, continue to stir 0.5h, proceed to 150 DEG C of hydro-thermal reaction 18h in hydrothermal reaction kettle, centrifugation, washing, 60 DEG C of vacuum drying, make nano bismuth molybdate visible light catalytic agent 2.
Embodiment 3
1.37g soluble starch is dissolved in the salpeter solution of 1mol/L, after stirring, adds 1mmol bismuth nitrate, continue to stir 2h, obtain mixed solution; In this mixed solution, add 0.5mmol sodium molybdate, stir 0.5h, then regulate pH=7 with ammoniacal liquor, continue to stir 0.5h, proceed to 210 DEG C of hydro-thermal reaction 6h in hydrothermal reaction kettle, centrifugation, washing, 60 DEG C of vacuum drying, make nano bismuth molybdate visible light catalytic agent 3.
Embodiment 4
The present embodiment bismuth molybdate visible light catalytic agent used is the prepared visible light catalyst of embodiment 11, in order to contrast, get respectively the visible light catalyst 1 of equivalent (0.1g), the bismuth molybdate visible light catalytic agent that P25 and common hydro-thermal legal system obtain, join in the rhodamine B that 200mL mass concentration is 5mg/L (RhB) solution, after ultrasonic 15min, be transferred in light-catalyzed reaction glass reactor, stir 30min at lucifuge place, to reach adsorption/desorption balance, adopt the xenon lamp of 300W as light source, then pass into air with the speed of 80ml/min, turn on light and continue and stir, sample once at interval of certain hour, centrifugation, get its supernatant and measure the residual concentration of rhodamine B with 722 type ultraviolet-uisible spectrophotometers (λ=554nm).The curve map of these three kinds of visible light catalyst rhodamine B degradations as shown in Figure 3, as can be seen from this figure, in identical degradation time, visible light catalyst 1 to the degradation speed of rhodamine B apparently higher than P25 and the standby bismuth molybdate visible light catalytic agent of common hydro-thermal legal system, therefore the bismuth molybdate visible light catalytic agent that, the photocatalytic activity of visible light catalyst 1 obtains higher than P25 and common hydro-thermal legal system.Equally, show through photocatalytic degradation experiment the bismuth molybdate visible light catalytic agent that nano bismuth molybdate visible light catalytic agent that embodiment 2-3 makes obtains apparently higher than P25 and common hydro-thermal legal system the degradation rate of rhodamine B, the bismuth molybdate visible light catalytic agent that the photocatalytic activity of the nano bismuth molybdate visible light catalytic agent that therefore, prepared by embodiment 2-3 obtains higher than P25 and common hydro-thermal legal system.
Above embodiment has described general principle of the present invention, principal character and advantage; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and description, describes just illustrates principle of the present invention; do not departing under the scope of the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.
Claims (2)
1. the biomimetic synthesis method of a nano bismuth molybdate visible light catalytic agent, it is characterized in that comprising the following steps: (1) is dissolved in soluble starch in the salpeter solution of 1mol/L, after stirring, add bismuth nitrate, continue to stir 2h, obtain mixed solution, wherein the mol ratio of soluble starch and bismuth nitrate is 1-4:1; (2) in the prepared mixed solution of step (1), add molybdate, wherein the mol ratio of molybdate and bismuth nitrate is 1:2, stir 0.5h, regulate pH=1-7 with ammoniacal liquor again, continue to stir 0.5h, proceed to 150-210 DEG C of hydro-thermal reaction 6-24h in hydrothermal reaction kettle, centrifugation, washing, 60 DEG C of vacuum drying, make nano bismuth molybdate visible light catalytic agent.
2. the biomimetic synthesis method of nano bismuth molybdate visible light catalytic agent according to claim 1, is characterized in that: described molybdate is sodium molybdate or ammonium molybdate.
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Cited By (7)
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| CN104984763A (en) * | 2015-07-08 | 2015-10-21 | 上海应用技术学院 | Polythiophene/bismuth molybdate composite photocatalyst and preparation method thereof |
| CN105668627A (en) * | 2016-01-15 | 2016-06-15 | 武汉工程大学 | Nanometer NaBi(MoO4)2 and preparation method thereof |
| CN105731541A (en) * | 2016-01-15 | 2016-07-06 | 武汉工程大学 | Gamma-bismuth molybdate crystal nanosheets and preparation method thereof |
| CN106564950A (en) * | 2016-11-09 | 2017-04-19 | 陕西科技大学 | Magnesium molybdate/graphene nanosheet array and preparation method therefor |
| CN107626301A (en) * | 2016-07-18 | 2018-01-26 | 中国科学院金属研究所 | A kind of bismuth molybdate visible light catalysis material of { 200 }/{ 002 } crystal face preferential growth and its preparation method and application |
| CN109865513A (en) * | 2017-12-05 | 2019-06-11 | 中国科学院金属研究所 | A kind of bismuth molybdate material and its preparation method and application of richness surface Lacking oxygen |
| CN115845879A (en) * | 2022-09-26 | 2023-03-28 | 汉江师范学院 | Simple hydrothermal method for synthesizing MoS 2 /Bi 2 MoO 6 Method for preparing composite material and efficient ciprofloxacin degradation by using same |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104984763A (en) * | 2015-07-08 | 2015-10-21 | 上海应用技术学院 | Polythiophene/bismuth molybdate composite photocatalyst and preparation method thereof |
| CN105668627A (en) * | 2016-01-15 | 2016-06-15 | 武汉工程大学 | Nanometer NaBi(MoO4)2 and preparation method thereof |
| CN105731541A (en) * | 2016-01-15 | 2016-07-06 | 武汉工程大学 | Gamma-bismuth molybdate crystal nanosheets and preparation method thereof |
| CN105731541B (en) * | 2016-01-15 | 2018-03-20 | 武汉工程大学 | A kind of γ bismuth molybdates nanometer chip and preparation method thereof |
| CN107626301A (en) * | 2016-07-18 | 2018-01-26 | 中国科学院金属研究所 | A kind of bismuth molybdate visible light catalysis material of { 200 }/{ 002 } crystal face preferential growth and its preparation method and application |
| CN107626301B (en) * | 2016-07-18 | 2020-05-08 | 中国科学院金属研究所 | Bismuth molybdate visible light photocatalytic material with {200}/{002} crystal face preferentially growing, and preparation method and application thereof |
| CN106564950A (en) * | 2016-11-09 | 2017-04-19 | 陕西科技大学 | Magnesium molybdate/graphene nanosheet array and preparation method therefor |
| CN106564950B (en) * | 2016-11-09 | 2017-12-22 | 陕西科技大学 | A kind of magnesium molybdate/graphene nano chip arrays and preparation method thereof |
| CN109865513A (en) * | 2017-12-05 | 2019-06-11 | 中国科学院金属研究所 | A kind of bismuth molybdate material and its preparation method and application of richness surface Lacking oxygen |
| CN115845879A (en) * | 2022-09-26 | 2023-03-28 | 汉江师范学院 | Simple hydrothermal method for synthesizing MoS 2 /Bi 2 MoO 6 Method for preparing composite material and efficient ciprofloxacin degradation by using same |
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Application publication date: 20140723 |