CN103934011B - A kind of biomimetic synthesis method of high-activity nano bismuth phosphate photocatalyst - Google Patents
A kind of biomimetic synthesis method of high-activity nano bismuth phosphate photocatalyst Download PDFInfo
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- CN103934011B CN103934011B CN201410163637.2A CN201410163637A CN103934011B CN 103934011 B CN103934011 B CN 103934011B CN 201410163637 A CN201410163637 A CN 201410163637A CN 103934011 B CN103934011 B CN 103934011B
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Abstract
The invention discloses a kind of biomimetic synthesis method of high-activity nano bismuth phosphate photocatalyst.Drip irrigation device of the present invention is: a kind of biomimetic synthesis method of high-activity nano bismuth phosphate photocatalyst, comprise the following steps: soluble starch is dissolved in the salpeter solution of 1mol/L by (1), 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 mixed solution obtained by step (1), the equimolar phosphate with bismuth nitrate is added, stir 0.5h, pH=1-7 is regulated with ammoniacal liquor, 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 4h, then in 400-500 DEG C of temperature calcination 2h, i.e. obtained high-activity nano bismuth phosphate photocatalyst.High-activity nano bismuth phosphate photocatalyst prepared by the present invention is nano material, has higher photocatalytic activity, higher than P25 and the standby bismuth phosphate photocatalyst of common hydro-thermal legal system.
Description
Technical field
The invention belongs to photocatalysis technology field, be specifically related to a kind of biomimetic synthesis method of high-activity nano bismuth phosphate photocatalyst.
Background technology
Photocatalytic pollutant degradation, as a high-level oxidation technology, has application prospect for environment remediation, have also been obtained increasing concern.And photochemical catalyst is the core of this technology, in numerous semiconductor light-catalysts, TiO
2due to its biologically inert, strong oxidizing property, low-cost high-efficiency, resistance to photoetch and the feature such as chemical corrosivity and stiff stability, be considered to the photochemical catalyst being suitable for environmental pollution improvement most.But TiO
2still have some self to be difficult to the shortcoming overcome, as low in sunshine utilization rate, the recombination rate of photohole-electronics is high, difficult separation and recycling etc.Therefore, the photochemical catalyst of development of new becomes an important research direction of photocatalysis field.
In recent years to BiPO
4the research of photocatalytic activity increases gradually, BiPO
4show very high ultraviolet catalytic active.The crystal phase structure, appearance and size etc. of photochemical catalyst are the principal elements affecting 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 common BiPO
4the method of preparation, as coprecipitation, hydro-thermal method and solid phase method, the more difficult BiPO preparing nano particle
4, therefore find a kind of simple, easy to operate and eco-friendlyly prepare high-activity nano BiPO
4the method of photochemical catalyst highly significant.
Summary of the invention
The object of this invention is to provide a kind of simple and biomimetic synthesis method of eco-friendly high-activity nano bismuth phosphate photocatalyst, the bismuth phosphate photocatalyst that the method obtains is the nano material of particle diameter 10-50nm.
Technical scheme of the present invention is: a kind of biomimetic synthesis method of high-activity nano bismuth phosphate photocatalyst, it is characterized in that comprising the following steps: soluble starch is dissolved in the salpeter solution of 1mol/L by (1), 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 mixed solution obtained by step (1), the equimolar phosphate with bismuth nitrate is added, stir 0.5h, pH=1-7 is regulated with ammoniacal liquor, 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 4h, then in 400-500 DEG C of temperature calcination 2h, i.e. obtained high-activity nano bismuth phosphate photocatalyst.Described phosphate is sodium dihydrogen phosphate, ammonium dihydrogen phosphate (ADP), sodium hydrogen phosphate, diammonium hydrogen phosphate, sodium phosphate or ammonium phosphate.
The present invention compared with prior art has the following advantages: (1) present invention, avoiding in organic solvent or synthesizes in the mixed solvent of organic solvent and water, it also avoid simultaneously use environmentally harmful organic substrate to control pattern and size, because of but a kind of eco-friendly synthetic method; (2) BiPO prepared
4for nano material, there is very high photocatalytic activity, higher than P25 and the standby BiPO of common hydro-thermal legal system
4photochemical catalyst.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the high-activity nano bismuth phosphate photocatalyst that the embodiment of the present invention 1 obtains, Fig. 2 is the transmission electron microscope picture of the obtained high-activity nano bismuth phosphate photocatalyst of the embodiment of the present invention 1, and Fig. 3 is that the standby bismuth phosphate photocatalyst of obtained high-activity nano bismuth phosphate photocatalyst 1, P25 and the common hydro-thermal legal system of the embodiment of the present invention 1 is to the correlation curve of rhodamine B degradation rate.
Detailed description of the invention
Be described in further details foregoing of the present invention by the following examples, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized 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, 1mmol sodium dihydrogen phosphate is added in this mixed solution, stir 0.5h, pH=1 is regulated with ammoniacal liquor, 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 4h, again in 450 DEG C of temperature calcination 2h, i.e. obtained high-activity nano bismuth phosphate photocatalyst 1, Fig. 1 is the scanning electron microscope (SEM) photograph of the high-activity nano bismuth phosphate photocatalyst that the present embodiment obtains, Fig. 2 is the transmission electron microscope picture of the high-activity nano bismuth phosphate photocatalyst that the present embodiment obtains, the particle diameter of bismuth phosphate photocatalyst 1 obtained is as seen from the figure 10-50nm.
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; 1mmol ammonium dihydrogen phosphate (ADP) is added in this mixed solution, stir 0.5h, pH=4 is regulated with ammoniacal liquor, 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 4h, then in 400 DEG C of temperature calcination 2h, i.e. obtained high-activity nano bismuth phosphate photocatalyst 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; 1mmol sodium hydrogen phosphate is added in this mixed solution, stir 0.5h, pH=7 is regulated 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 4h, then in 500 DEG C of temperature calcination 2h, i.e. obtained high-activity nano bismuth phosphate photocatalyst 3.
Embodiment 4
0.6g soluble starch is dissolved in the salpeter solution of 1mol/L, after stirring, adds 1mmol bismuth nitrate, continue to stir 2h, obtain mixed solution; 1mmol diammonium hydrogen phosphate is added in this mixed solution, stir 0.5h, pH=2 is regulated with ammoniacal liquor, continue to stir 0.5h, proceed to 210 DEG C of hydro-thermal reaction 8h in hydrothermal reaction kettle, centrifugation, washing, 60 DEG C of vacuum drying 4h, then in 480 DEG C of temperature calcination 2h, i.e. obtained high-activity nano bismuth phosphate photocatalyst 4.
Embodiment 5
0.5g soluble starch is dissolved in the salpeter solution of 1mol/L, after stirring, adds 1mmol bismuth nitrate, continue to stir 2h, obtain mixed solution; 1mmol sodium phosphate is added in this mixed solution, stir 0.5h, pH=4 is regulated with ammoniacal liquor, continue to stir 0.5h, proceed to 150 DEG C of hydro-thermal reaction 24h in hydrothermal reaction kettle, centrifugation, washing, 60 DEG C of vacuum drying 4h, then in 430 DEG C of temperature calcination 2h, i.e. obtained high-activity nano bismuth phosphate photocatalyst 5.
Embodiment 6
0.9g soluble starch is dissolved in 1mol/L salpeter solution, after stirring, adds 1mmol bismuth nitrate, continue to stir 2h, obtain mixed solution; 1mmol ammonium phosphate is added in this mixed solution, stir 0.5h, pH=3 is regulated with ammoniacal liquor, continue to stir 0.5h, proceed to 170 DEG C of hydro-thermal reaction 18h in hydrothermal reaction kettle, centrifugation, washing, 60 DEG C of vacuum drying 4h, then in 500 DEG C of temperature calcination 2h, i.e. obtained high-activity nano bismuth phosphate photocatalyst 6.
Embodiment 7
The BiPO that the present embodiment is used
4the photochemical catalyst 1 of photochemical catalyst prepared by embodiment 1, in order to contrast, gets the BiPO that the photochemical catalyst 1, P25 of equivalent (0.1g) and common hydro-thermal legal system obtain respectively
4photochemical catalyst, join in rhodamine B (RhB) solution that 200mL mass concentration is 5mg/L, be transferred in light-catalyzed reaction glass reactor after ultrasonic 15min, 30min is stirred at lucifuge place, to reach adsorption/desorption balance, adopt the high-pressure sodium lamp of 125W as light source, then air is passed into the speed of 80ml/min, turn on light and Keep agitation, at interval of certain hour sampling once, centrifugation, gets its supernatant measures rhodamine B residual concentration with 722 type ultraviolet-uisible spectrophotometers (λ=554nm).The curve map of these three kinds of photocatalyst for degrading rhodamine Bs as shown in Figure 3, as can be seen from this figure, in identical degradation time, the BiPO that the degradation speed of photochemical catalyst 1 pair of rhodamine B is prepared apparently higher than P25 and hydro-thermal method
4photochemical catalyst, therefore, the BiPO that the photocatalytic activity of photochemical catalyst 1 is prepared higher than P25 and hydro-thermal method
4photochemical catalyst.Equally, show through photocatalytic degradation experiment the BiPO that the high-activity nano bismuth phosphate photocatalyst that embodiment 2-6 obtains obtains apparently higher than P25 and common hydro-thermal legal system the degradation rate of rhodamine B
4photochemical catalyst, therefore, the BiPO that the photocatalytic activity of high-activity nano bismuth phosphate photocatalyst prepared by embodiment 2-6 obtains higher than P25 and common hydro-thermal legal system
4photochemical catalyst.
Embodiment above describes 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; what describe in above-described embodiment and description just illustrates principle of the present invention; under the scope not departing from 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 (1)
1. the biomimetic synthesis method of a high-activity nano bismuth phosphate photocatalyst, it is characterized in that comprising the following steps: soluble starch is dissolved in the salpeter solution of 1mol/L by (1), 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 mixed solution obtained by step (1), the equimolar phosphate with bismuth nitrate is added, stir 0.5h, pH=1-7 is regulated with ammoniacal liquor, 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 4h, again in 400-500 DEG C of temperature calcination 2h, i.e. obtained high-activity nano bismuth phosphate photocatalyst, described phosphate is sodium dihydrogen phosphate, ammonium dihydrogen phosphate (ADP), sodium hydrogen phosphate, diammonium hydrogen phosphate, sodium phosphate or ammonium phosphate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104525229A (en) * | 2014-12-26 | 2015-04-22 | 清华大学 | BiPO4 nanoparticle as well as preparation method and application of BiPO4 nanoparticle |
| CN104907086A (en) * | 2015-05-21 | 2015-09-16 | 河南师范大学 | Bionic synthesis method of flower-shaped bismuth phosphate photocatalyst with microscopic hierarchical structure |
| CN104888820A (en) * | 2015-05-21 | 2015-09-09 | 河南师范大学 | Preparation method of flower-shaped bismuth phosphate photocatalyst with microscopic graded structure |
| CN107029763A (en) * | 2017-05-26 | 2017-08-11 | 桂林理工大学 | A kind of preparation method of bismuth phosphate/carbon composite photocatalyst |
| CN111804318A (en) * | 2019-04-10 | 2020-10-23 | 天津大学 | Adsorption photocatalyst and preparation method and application thereof |
| CN110075884A (en) * | 2019-05-30 | 2019-08-02 | 江汉大学 | A kind of BiPO4The preparation method of nano-photocatalyst |
| CN111675202B (en) * | 2019-06-11 | 2023-01-03 | 宁波大学 | Bismuth phosphate nano powder and synthesis method thereof |
| CN111111717B (en) * | 2020-01-18 | 2022-07-29 | 云南大学 | Photocatalyst bismuth oxyphosphate Bi 3 O(PO 4 ) 2 Atmospheric preparation method of (OH) |
| CN113479858B (en) * | 2021-07-01 | 2023-08-11 | 中国石油大学(华东) | Composite material for high-performance alkali metal ion battery cathode |
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| CN103111315A (en) * | 2013-03-15 | 2013-05-22 | 南开大学 | Preparation method of bismuth phosphate (BiPO4) photocatalysts differing in structure |
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