CN104907086A - Bionic synthesis method of flower-shaped bismuth phosphate photocatalyst with microscopic hierarchical structure - Google Patents
Bionic synthesis method of flower-shaped bismuth phosphate photocatalyst with microscopic hierarchical structure Download PDFInfo
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- CN104907086A CN104907086A CN201510260241.4A CN201510260241A CN104907086A CN 104907086 A CN104907086 A CN 104907086A CN 201510260241 A CN201510260241 A CN 201510260241A CN 104907086 A CN104907086 A CN 104907086A
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Abstract
The invention discloses a bionic synthesis method of a flower-shaped bismuth phosphate photocatalyst with a microscopic hierarchical structure. The method comprises the specific steps that: L-cysteine hydrochloride is dissolved in a nitric acid solution with a molar concentration of 1mol/L; the materials are stirred until well mixed; bismuth nitrate pentahydrate is added, and stirring is continued for 2h, such that a mixed solution is obtained; soluble phosphate with a same molar amount with bismuth nitrate pentahydrate is added to the mixed solution, and the mixture is well mixed by stirring; the pH value of the reaction system is regulated to 1-7 with ammonia water; stirring is continued for 0.5h; the mixture is allowed to stand for 12-120h under room temperature; centrifugal separation and washing are carried out; vacuum drying is carried out for 12h under a temperature of 60 DEG C; and calcination is carried out for 4h under a temperature of 550 DEG C, such that the flower-shaped bismuth phosphate photocatalyst composed of nanowires with an average diameter of 20nm is obtained. The photocatalyst has an average particle size of 1400nm, and has a microscopic hierarchical structure. The method provided by the invention is simple and feasible, and has the advantages of mild reaction conditions, high operability, and low cost. The prepared bismuth phosphate photocatalyst has relatively high photocatalytic activity.
Description
Technical field
The invention belongs to the synthesis technical field of bismuth phosphate photocatalyst, be specifically related to a kind of biomimetic synthesis method with the flower-shaped bismuth phosphate photocatalyst of microcosmic hierarchy.
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
2because its biologically inert, strong oxidizing property, low-cost high-efficiency, resistance to photoetch and the feature such as chemical corrosivity and stiff stability are considered to the photochemical catalyst being suitable for environmental pollution improvement most.But TiO
2some are still had self to be difficult to the shortcoming overcome, high and difficult separation and recycling of recombination rate that is as low in sunshine utilization rate, photohole-electronics 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 of photochemical catalyst and appearance and size are the principal elements affecting its ultraviolet catalytic activity, and the crystal phase structure of catalyst and appearance and size have inseparable relation with its synthetic method and preparation condition.Usual synthesis BiPO
4method have 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 or conventional organic matter revulsion can prepare the photochemical catalyst with certain pattern, but due to process with an organic solvent or poisonous and hazardous organic reagent, increase preparation cost, also can bring pressure to environment, therefore find a kind of simple, easy to operate and eco-friendly method synthesis pattern is special and activity is higher bismuth phosphate photocatalyst is significant.
Summary of the invention
The technical problem that the present invention solves there is provided a kind of biomimetic synthesis method with the flower-shaped bismuth phosphate photocatalyst of microcosmic hierarchy, and the simple and environmental friendliness of the method, the bismuth phosphate photocatalyst of gained has higher photocatalytic activity.
The present invention adopts following technical scheme for solving the problems of the technologies described above, there is the biomimetic synthesis method of the flower-shaped bismuth phosphate photocatalyst of microcosmic hierarchy, it is characterized in that concrete steps are: it is in the salpeter solution of 1mol/L that L-cysteine hydrochloride is dissolved in molar concentration by (1), five nitric hydrate bismuths are added after being uniformly mixed, continue to stir 2h and obtain mixed solution, wherein the mol ratio of L-cysteine hydrochloride and five nitric hydrate bismuths is 1-2:1; (2) add and the equimolar soluble phosphate of five nitric hydrate bismuths in the mixed solution obtained to step (1), be uniformly mixed, then regulate the pH of reaction system to be 1-7 with ammoniacal liquor, continue to stir 0.5h; (3) left at room temperature 12-20h, centrifugation, washing, 60 DEG C of vacuum drying 12h, the average grain diameter then obtaining being made up of the nano wire of average diameter 20nm in 550 DEG C of calcining 4h is 1400nm and has the flower-shaped bismuth phosphate photocatalyst of microcosmic hierarchy.
Further restriction, described soluble phosphate is sodium dihydrogen phosphate, ammonium dihydrogen phosphate (ADP), sodium hydrogen phosphate, diammonium hydrogen phosphate, sodium phosphate or ammonium phosphate.
The present invention has the following advantages compared with the bismuth phosphate photocatalyst adopting other method to prepare:
(1) the flower-shaped bismuth phosphate of microcosmic hierarchy is utilized biological reagent L-cysteine hydrochloride to synthesize to have in aqueous, avoid the use of organic solvent, it also avoid simultaneously and add poisonous and hazardous organic substrate and carry out the pattern of modulation product, because of but a kind of eco-friendly biomimetic synthesis method; (2) this synthetic method mild condition, simple, workable and with low cost; (3) bismuth phosphate photocatalyst prepared has higher photocatalytic activity, higher than bismuth phosphate photocatalyst prepared by ordinary precipitation process.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the bismuth phosphate photocatalyst that the embodiment of the present invention 1 obtains, the bismuth phosphate photocatalyst that the obtained bismuth phosphate photocatalyst 1 of Fig. 2 to be the field emission scanning electron microscope figure of the obtained bismuth phosphate photocatalyst of the embodiment of the present invention 1, Fig. 3 be embodiment of the present invention 1 and ordinary precipitation process synthesize 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
Getting L-cysteine hydrochloride 3mmol is dissolved in the salpeter solution (1mol/L) of 50ml, after being uniformly mixed, adds 3mmol five nitric hydrate bismuth, continues to stir 2h and obtains mixed solution; Add 3mmol sodium dihydrogen phosphate again, stir 0.5h, then regulate pH to be 1 with ammoniacal liquor, continue to stir 0.5h; Be placed on experimental bench and leave standstill 120h in room temperature, centrifugation, washing, 60 DEG C of vacuum drying 12h, then bismuth phosphate photocatalyst 1 is obtained in 550 DEG C of calcining 4h, respectively as depicted in figs. 1 and 2, the average grain diameter be made up of the nano wire of average diameter 20nm the known obtained bismuth phosphate photocatalyst 1 of Fig. 1 and Fig. 2 is 1400nm and has the flower-shaped bismuth phosphate photocatalyst of microcosmic hierarchy for its scanning electron microscope (SEM) photograph and field emission scanning electron microscope figure.
Embodiment 2
Getting L-cysteine hydrochloride 6mmol is dissolved in the salpeter solution (1mol/L) of 50ml, after being uniformly mixed, adds 3mmol five nitric hydrate bismuth, continues to stir 2h and obtains mixed solution; Add 3mmol ammonium dihydrogen phosphate (ADP) again, stir 0.5h, then regulate pH to be 7 with ammoniacal liquor, continue to stir 0.5h; Be placed on experimental bench and leave standstill 96h in room temperature, centrifugation, washing, 60 DEG C of vacuum drying 12h, then obtain the flower-shaped bismuth phosphate photocatalyst 2 with microcosmic hierarchy in 550 DEG C of calcining 4h.
Embodiment 3
Getting L-cysteine hydrochloride 3mmol is dissolved in the salpeter solution (1mol/L) of 50ml, after being uniformly mixed, adds 3mmol five nitric hydrate bismuth, continues to stir 2h and obtains mixed solution; Add 3mmol sodium hydrogen phosphate again, stir 0.5h, then regulate pH to be 4 with ammoniacal liquor, continue to stir 0.5h; Be placed on experimental bench and leave standstill 12h in room temperature, centrifugation, washing, 60 DEG C of vacuum drying 12h, then obtain the flower-shaped bismuth phosphate photocatalyst 3 with microcosmic hierarchy in 550 DEG C of calcining 4h.
Embodiment 4
Getting L-cysteine hydrochloride 6mmol is dissolved in the salpeter solution (1mol/L) of 50ml, after being uniformly mixed, adds 3mmol five nitric hydrate bismuth, continues to stir 2h and obtains mixed solution; Add 3mmol diammonium hydrogen phosphate again, stir 0.5h, then regulate pH to be 2 with ammoniacal liquor, continue to stir 0.5h; Be placed on experimental bench and leave standstill 48h in room temperature, centrifugation, washing, 60 DEG C of vacuum drying 12h, then obtain the flower-shaped bismuth phosphate photocatalyst 4 with microcosmic hierarchy in 550 DEG C of calcining 4h.
Embodiment 5
Getting L-cysteine hydrochloride 3mmol is dissolved in the salpeter solution (1mol/L) of 50ml, after being uniformly mixed, adds 3mmol five nitric hydrate bismuth, continues to stir 2h and obtains mixed solution; Add 3mmol sodium phosphate again, stir 0.5h, then regulate pH to be 1 with ammoniacal liquor, continue to stir 0.5h; Be placed in left at room temperature 72h on experimental bench, centrifugation, washing, 60 DEG C of vacuum drying 12h, then obtain the flower-shaped bismuth phosphate photocatalyst 5 with microcosmic hierarchy in 550 DEG C of calcining 4h.
Embodiment 6
Getting L-cysteine hydrochloride 6mmol is dissolved in the salpeter solution (1mol/L) of 50ml, after being uniformly mixed, adds 3mmol five nitric hydrate bismuth, continues to stir 2h and obtains mixed solution; Add 3mmol ammonium phosphate again, stir 0.5h, then regulate pH to be 3 with ammoniacal liquor, continue to stir 0.5h; Be placed in left at room temperature 96h on experimental bench, centrifugation, washing, 60 DEG C of vacuum drying 12h, then obtain the flower-shaped bismuth phosphate photocatalyst 6 with microcosmic hierarchy in 550 DEG C of calcining 4h.
Embodiment 7
The BiPO that the present embodiment is used
4for the bismuth phosphate photocatalyst 1 that embodiment 1 is obtained.In order to contrast, get the bismuth phosphate photocatalyst 1 of equivalent (0.05g) and the obtained BiPO of ordinary precipitation process respectively
4, join in rhodamine B (RhB) solution that 200mL mass concentration is 5mg/L, be transferred in light-catalyzed reaction glass reactor after ultrasonic 15min, stir 30min at lucifuge place, to reach adsorption/desorption balance.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).The curve of these two 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 bismuth phosphate photocatalyst 1 pair of rhodamine B is prepared apparently higher than ordinary precipitation process
4.Equally, show through photocatalytic degradation experiment the BiPO that the bismuth phosphate photocatalyst that embodiment 2-6 obtains obtains apparently higher than ordinary precipitation process the degradation rate of rhodamine B
4, therefore, the photocatalytic activity of the bismuth phosphate photocatalyst that embodiment 2-6 obtains is higher than the obtained BiPO of ordinary precipitation process
4.
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 (2)
1. there is the biomimetic synthesis method of the flower-shaped bismuth phosphate photocatalyst of microcosmic hierarchy, it is characterized in that concrete steps are: it is in the salpeter solution of 1mol/L that L-cysteine hydrochloride is dissolved in molar concentration by (1), five nitric hydrate bismuths are added after being uniformly mixed, continue to stir 2h and obtain mixed solution, wherein the mol ratio of L-cysteine hydrochloride and five nitric hydrate bismuths is 1-2:1; (2) add and the equimolar soluble phosphate of five nitric hydrate bismuths in the mixed solution obtained to step (1), be uniformly mixed, then regulate the pH of reaction system to be 1-7 with ammoniacal liquor, continue to stir 0.5h; (3) left at room temperature 12-20h, centrifugation, washing, 60 DEG C of vacuum drying 12h, the average grain diameter then obtaining being made up of the nano wire of average diameter 20nm in 550 DEG C of calcining 4h is 1400nm and has the flower-shaped bismuth phosphate photocatalyst of microcosmic hierarchy.
2. the biomimetic synthesis method with the flower-shaped bismuth phosphate photocatalyst of microcosmic hierarchy according to claim 1, is characterized in that: described soluble phosphate 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 |
|---|---|---|---|---|
| CN113479858A (en) * | 2021-07-01 | 2021-10-08 | 中国石油大学(华东) | Composite material for high-performance alkali metal ion battery cathode |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006182791A (en) * | 2003-02-10 | 2006-07-13 | Kansai Paint Co Ltd | Coating material for forming photocatalyst film |
| CN103896236A (en) * | 2014-03-24 | 2014-07-02 | 上海大学 | Preparation method of bismuth phosphate nanoparticle photocatalytic material |
| CN103934011A (en) * | 2014-04-23 | 2014-07-23 | 河南师范大学 | Biomimetic synthesis method of high-activity nanometer bismuth phosphate photocatalyst |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006182791A (en) * | 2003-02-10 | 2006-07-13 | Kansai Paint Co Ltd | Coating material for forming photocatalyst film |
| CN103896236A (en) * | 2014-03-24 | 2014-07-02 | 上海大学 | Preparation method of bismuth phosphate nanoparticle photocatalytic material |
| CN103934011A (en) * | 2014-04-23 | 2014-07-23 | 河南师范大学 | Biomimetic synthesis method of high-activity nanometer bismuth phosphate photocatalyst |
Non-Patent Citations (1)
| Title |
|---|
| 周娟: "含铟硫化物及其复合材料的制备与可见光催化性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113479858A (en) * | 2021-07-01 | 2021-10-08 | 中国石油大学(华东) | Composite material for high-performance alkali metal ion battery cathode |
| 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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Application publication date: 20150916 |