CN104941675A - Preparation method of bismuth phosphate photocatalyst with controllable shape - Google Patents
Preparation method of bismuth phosphate photocatalyst with controllable shape Download PDFInfo
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- CN104941675A CN104941675A CN201510260564.3A CN201510260564A CN104941675A CN 104941675 A CN104941675 A CN 104941675A CN 201510260564 A CN201510260564 A CN 201510260564A CN 104941675 A CN104941675 A CN 104941675A
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- phosphate
- bismuth
- photocatalyst
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Abstract
The invention discloses a preparation method of a bismuth phosphate photocatalyst with controllable shape, comprising the following steps: (1) putting glycol and glycerol into a reaction container and stirring uniformly, then adding tartaric acid, and continuing to stir uniformly to obtain a mixed solution; (2) adding bismuth nitrate pentahydrate to the mixed solution obtained in step (1) and stirring uniformly, then adding soluble phosphate with mole number equal to that of bismuth nitrate pentahydrate, uniformly stirring and then transferring into a hydrothermal reaction kettle to perform thermal reaction with a solvent for 24h at the temperature of 160 DEG C, carrying out centrifugal separation, washing, and carrying out vacuum drying for 12h at the temperature of 60 DEG C, thus preparing the bismuth phosphate photocatalyst with different microstructures. According to the method, change of the microstructure of a product can be realized by changing the molar ratio of tartaric acid and bismuth nitrate pentahydrate, and therefore, the method is simple and easily-available, and prepared BiPO4 is novel in shape and relatively high in photocatalytic activity.
Description
Technical field
The invention belongs to the synthesis technical field of bismuth phosphate photocatalyst, be specifically related to a kind of preparation method of bismuth phosphate photocatalyst of morphology controllable.
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 chemical corrosivity, the features such as stiff stability are considered to be suitable for the control of environmental pollution 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.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.And common BiPO
4the method of preparation has coprecipitation, hydro-thermal method and solid phase method etc., because of BiPO
4be easy to formation block and bar-shaped, these conventional methods are for change BiPO
4pattern and size more difficult.Solvent-thermal method is that conventional organic matter revulsion can prepare the photochemical catalyst with certain pattern, and some researchers investigated a little BiPO by the method in recent years
4new pattern, but its photocatalytic activity has much room for improvement.Therefore, a kind of morphology controllable is found and the high novel B iPO of photocatalytic activity
4synthetic method is significant.
Summary of the invention
The technical problem that the present invention solves there is provided a kind of preparation method of bismuth phosphate photocatalyst of morphology controllable, and this preparation method is simple, and the product of gained has higher photocatalytic activity.
The present invention adopts following technical scheme for solving the problems of the technologies described above, the preparation method of the bismuth phosphate photocatalyst of morphology controllable, it is characterized in that comprising the steps: that ethylene glycol and glycerine are placed in reaction vessel and are uniformly mixed by (1), then add tartaric acid and continue to be uniformly mixed and obtain mixed solution; (2) add five nitric hydrate bismuths in the mixed solution obtained to step (1) and be uniformly mixed, then add and the equimolar soluble phosphate of five nitric hydrate bismuths, proceed to after being uniformly mixed in hydrothermal reaction kettle in 160 DEG C of solvent thermal reaction 24h, centrifugation, washing, 60 DEG C of vacuum drying 12h, the bismuth phosphate photocatalyst of obtained diverse microcosmic appearance; The average diameter that the irregular particle that it is 25nm that the mol ratio of its mesotartaric acid and five nitric hydrate bismuths obtains by average diameter when being 3:1 is assembled into is the porous pumpkin of 1250nm; The average diameter that the nanometer sheet that it is 12nm that the mol ratio of tartaric acid and five nitric hydrate bismuths obtains by average thickness when being 1.5:1 is assembled into is the porous hexagonal prism of 880nm; The average diameter that the nanometer sheet that it is 17nm that the mol ratio of tartaric acid and five nitric hydrate bismuths obtains by average thickness when being 0.75:1 is assembled into is the porous cylindrical body of 900nm.
Further restriction, the volume ratio of the ethylene glycol described in step (1) and glycerine is 1:1.
Further restriction, the soluble phosphate described in step (2) is sodium dihydrogen phosphate, ammonium dihydrogen phosphate (ADP), sodium hydrogen phosphate, diammonium hydrogen phosphate, sodium phosphate or ammonium phosphate.
The present invention and the BiPO adopting other method to prepare
4photochemical catalyst is compared and is had the following advantages: (1) this method is common solvent-thermal method, and operation is simple; (2) this method can realize to product microscopic appearance by means of only the mol ratio changing tartaric acid and five nitric hydrate bismuths modulation, simple; (3) BiPO for preparing of this method
4novel in shape and there is higher photocatalytic activity.
Accompanying drawing explanation
Fig. 1-3 is microscopic appearance figure of the bismuth phosphate photocatalyst obtained under different pulp furnish of the embodiment of the present invention 1, and Fig. 4 is the degradation rate curve of bismuth phosphate photocatalyst 1 pair of rhodamine B prepared by the embodiment of the present invention 1.
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
Add 25mL glycerine in ethylene glycol respectively to 3 parts of 25mL, stir 20min and make it mix, add 9mmol, 4.5mmol and 2.25mmol tartaric acid respectively, continue to stir 1h, obtain 3 parts of mixed solutions; Then respectively to adding 3mmol five nitric hydrate bismuth in mixed solution, continue to stir 2h, add 3mmol soluble phosphate (being respectively sodium dihydrogen phosphate, ammonium dihydrogen phosphate (ADP) and sodium hydrogen phosphate) more respectively, continue to stir 2h, proceed in 160 DEG C of solvent thermal reaction 24h in the hydrothermal reaction kettle of 80mL, centrifugation, washing, 60 DEG C of vacuum drying 12h, namely obtain the bismuth phosphate photocatalyst 1,2 and 3 of diverse microcosmic appearance.The pattern of bismuth phosphate photocatalyst 1 as shown in Figure 1, the porous pumpkin of to be average diameter that the irregular particle being 25nm by average diameter is assembled into be 1250nm; The pattern of bismuth phosphate photocatalyst 2 as shown in Figure 2, the porous hexagonal prism of to be average diameter that the nanometer sheet being 12nm by average thickness is assembled into be 880nm; The pattern of bismuth phosphate photocatalyst 3 as shown in Figure 3, be the average diameter that the nanometer sheet being 17nm by average thickness is assembled into is the porous cylindrical body of 900nm.
Embodiment 2
The BiPO that the present embodiment is used
4bismuth phosphate photocatalyst 1 prepared by embodiment 1.In order to test its performance, getting 0.05g bismuth phosphate photocatalyst 1 joins 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, wherein do blank experiment not add catalyst.Adopt the high-pressure sodium lamp of 125W as light source, then pass into air with 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).As shown in Figure 4, as can be seen from this figure, the degraded of bismuth phosphate photocatalyst 1 pair of rhodamine B shows good photocatalytic activity to the degradation rate curve of bismuth phosphate photocatalyst 1 rhodamine B degradation.Equally, show through photocatalytic degradation experiment the photocatalytic activity that the degraded of the bismuth phosphate photocatalyst 2 that embodiment 1 is obtained and 3 pairs of rhodamine Bs all shows.Therefore, the photocatalytic activity of the bismuth phosphate photocatalyst of the embodiment of the present invention 1 preparation is better.
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 (3)
1. the preparation method of the bismuth phosphate photocatalyst of morphology controllable, is characterized in that comprising the steps: that ethylene glycol and glycerine are placed in reaction vessel and are uniformly mixed by (1), then adds tartaric acid and continues to be uniformly mixed and obtain mixed solution; (2) add five nitric hydrate bismuths in the mixed solution obtained to step (1) and be uniformly mixed, then add and the equimolar soluble phosphate of five nitric hydrate bismuths, proceed to after being uniformly mixed in hydrothermal reaction kettle in 160 DEG C of solvent thermal reaction 24h, centrifugation, washing, 60 DEG C of vacuum drying 12h, the bismuth phosphate photocatalyst of obtained diverse microcosmic appearance; The average diameter that the irregular particle that it is 25nm that the mol ratio of its mesotartaric acid and five nitric hydrate bismuths obtains by average diameter when being 3:1 is assembled into is the porous pumpkin of 1250nm; The average diameter that the nanometer sheet that it is 12nm that the mol ratio of tartaric acid and five nitric hydrate bismuths obtains by average thickness when being 1.5:1 is assembled into is the porous hexagonal prism of 880nm; The average diameter that the nanometer sheet that it is 17nm that the mol ratio of tartaric acid and five nitric hydrate bismuths obtains by average thickness when being 0.75:1 is assembled into is the porous cylindrical body of 900nm.
2. the preparation method of the bismuth phosphate photocatalyst of morphology controllable according to claim 1, is characterized in that: the volume ratio of the ethylene glycol described in step (1) and glycerine is 1:1.
3. the preparation method of the bismuth phosphate photocatalyst of morphology controllable according to claim 1, is characterized in that: the soluble phosphate described in step (2) is sodium dihydrogen phosphate, ammonium dihydrogen phosphate (ADP), sodium hydrogen phosphate, diammonium hydrogen phosphate, sodium phosphate or ammonium phosphate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111111717A (en) * | 2020-01-18 | 2020-05-08 | 云南大学 | Novel photocatalyst bismuth hydroxyphosphate Bi3O(PO4)2Atmospheric preparation method of (OH) |
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| WO2009133413A1 (en) * | 2008-04-28 | 2009-11-05 | Novatech D.O.O. | Formulation based on micronized clinoptilolite as a therapeutic agent for removal of toxins, bacteria and viruses from organism |
| CN103073049A (en) * | 2011-10-26 | 2013-05-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Complexing-agent-assisted preparation method of cadmium sulfide multi-level-structured nano-grade material |
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2015
- 2015-05-21 CN CN201510260564.3A patent/CN104941675A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2009133413A1 (en) * | 2008-04-28 | 2009-11-05 | Novatech D.O.O. | Formulation based on micronized clinoptilolite as a therapeutic agent for removal of toxins, bacteria and viruses from organism |
| CN103073049A (en) * | 2011-10-26 | 2013-05-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Complexing-agent-assisted preparation method of cadmium sulfide multi-level-structured nano-grade material |
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| 刘芳芳 等: "酒石酸对直接沉淀法制备纳米Bi2O3晶体结构的影响", 《中国粉体技术》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111111717A (en) * | 2020-01-18 | 2020-05-08 | 云南大学 | Novel photocatalyst bismuth hydroxyphosphate Bi3O(PO4)2Atmospheric preparation method of (OH) |
| 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) |
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Application publication date: 20150930 |