CN105236480B - HCOOBiO nanocrystalline with unique morphology and preparation method therefor - Google Patents
HCOOBiO nanocrystalline with unique morphology and preparation method therefor Download PDFInfo
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- CN105236480B CN105236480B CN201410315980.4A CN201410315980A CN105236480B CN 105236480 B CN105236480 B CN 105236480B CN 201410315980 A CN201410315980 A CN 201410315980A CN 105236480 B CN105236480 B CN 105236480B
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Abstract
The present invention discloses a preparation method for Bismuth formic acid (HCOOBiO) nanocrystalline. By a hydrothermal process, ultra long nano wire HCOOBiO nanocrystalline is prepared. The preparation method for the HCOOBiO nanocrystalline comprises the following steps: dissolving Bi(NO3)3.5H2O in DMF; placing the solution into a reaction kettle for reaction; and after the reaction, washing the reaction products to obtain the ultra long nano wire HCOOBiO nanocrystalline. The HCOOBiO nanocrystalline obtained in the reaction is unique in morphology and large in specific surface area, so that the performance of the material is effectively improved. The HCOOBiO nanocrystalline prepared by the method in the present invention is excellent in adsorption of heavy metals and colorants in adsorption test, thus the HCOOBiO nanocrystalline has a good application prospect in removing pollutants, such as colorants and heavy metals, in industrial waste water.
Description
Technical field
The present invention relates to HCOOBiO is nanocrystalline and preparation method thereof, particularly nanometer wire HCOOBiO is nanocrystalline and its system
Preparation Method, belongs to field of inorganic nano-material preparation.
Background technology
In recent years, one-dimentional structure nano material such as nanometer rods, nanotube, especially overlong nanowire have been obtained widely
Using.For example, nano wire is due to making which be widely used in lithium-ion electric with high-specific surface area and excellent ionic conducting property
The aspects such as pond, gas sensor and photocatalysis.
With industrial expansion, dyestuff and heavy metal have become main environmental contaminants.Absorption method is simple due to which
It is easy, small investment, high efficiency and restorability have become a kind of effective decontamination method.Formic acid oxidation bismuth is as which is by more
Green element (C, H and O) replace poisonous halogen in BiXO (X=Cl, Br, I), be likely to become new photocatalysis material
Material and adsorbent.
There is formic acid oxygen bismuth good photocatalysis performance, Fang Duan et al. to adopt with bismuth nitrate as raw material, DMF conducts
Reactant, used as solvent, at 120 DEG C, hydro-thermal is obtained flower-shaped HCOOBiO to water；Jinyan Xiong et al. are with sodium formate and nitric acid
Bismuth is raw material, and with Mannitol, EG, DEG, TEG as solvent, the hydro-thermal at 150 DEG C is obtained HCOOBiO, obtained HCOOBiO respectively
It is nanometer sheet and assembles the flower-like structure to be formed.Two prepared HCOOBiO of report of the above are flower-shaped or spherical structure, separately
Outward, document only reports photocatalysis performance, does not have the absorption property for studying its heavy metal ion and dyestuff.
The content of the invention
It is an object of the invention to provide nanometer wire HCOOBiO is nanocrystalline and preparation method thereof.
The technical solution for realizing the object of the invention is：A kind of HCOOBiO of unique morphology is nanocrystalline, described
HCOOBiO is nanocrystalline for nanometer wire.
The nanocrystalline methods of the above-mentioned HCOOBiO with unique morphology are prepared using soft chemical method, is comprised the following steps：
Step one：By Bi (NO3)3·5H2O is dissolved in DMF；
Step 2：Step one solution is placed in into reaction kettle for reaction；
Step 3：Reaction terminate after washing to obtain final product nanometer wire HCOOBiO nanocrystalline.
Bi (NO in resulting solution in step one3)3·5H2O molar concentrations are 0.033mol/L.
Reaction temperature described in step 2 is 120 DEG C, and the response time is 6-24h.
The present invention has following remarkable advantage：
1st, method is simple, need not add any catalyst and template, only be obtained using two kinds of raw materials of DMF and bismuth nitrate
HCOOBiO is nanocrystalline；
2nd, obtained HCOOBiO is nanocrystalline for overlength wire, and its winding can form network structure, with larger ratio table
Area and pore structure, are conducive to the raising of its performance；
4th, the dyestuff such as the nanocrystalline heavy metal ion Cr (VI) and methyl orange shows excellent absorption property, than flower-shaped
The absorption property of structure is high 3 times, is expected to have good application in industrial wastewater treatment field.
Description of the drawings
Fig. 1 is that hydro-thermal method of the present invention prepares the schematic flow sheet for having the HCOOBiO of unique morphology nanocrystalline.
TEM figure ((a) embodiments 1 of Fig. 2 for nanometer wire HCOOBiO obtained in embodiment 1-3；(b) embodiment 2；(c)
(d) embodiment is 3).
Fig. 3 obtains nanometer wire 20mg HCOOBiO to variable concentrations K for the present invention2Cr2O7The absorption of solution and methyl orange
Amount changes over figure ((a) K2Cr2O7；(b) methyl orange).
Fig. 4 is that ((a) comparative example 1, (b) comparative example is 2) for the TEM figures of comparative example 1 and flower-shaped HCOOBiO obtained in comparative example 2.
Fig. 5 is obtained sample to K for comparative example 22Cr2O7The adsorbance of solution and methyl orange changes over figure, and ((c) be
K2Cr2O7Solution, is (d) methyl orange).
Specific embodiment
With reference to the accompanying drawings and detailed description the present invention is described in further detail.
With reference to Fig. 1, the present invention is that the HCOOBiO that solvent and reactant are prepared with unique morphology is nanocrystalline using DMF
Method, its feature are comprised the following steps：
Step one：By Bi (NO3)3·5H2O is dissolved in DMF, wherein Bi (NO3)3·5H2O molar concentrations are 0.033mol/
L；
Step 2：Step one solution is placed in into reaction kettle for reaction 6-24h, wherein reaction temperature is 120 DEG C；
Step 3：Reaction terminate after washing to obtain final product nanometer wire HCOOBiO nanocrystalline.
Embodiment 1：
Step one：By 1mmol Bi (NO3)3·5H2O is dissolved in 30ml DMF；
Step 2：The isothermal reaction in closed reactor by the solution obtained by step one, 120 DEG C of reaction temperature, during reaction
Between be 6h；
Step 3：It is nanocrystalline by nanometer wire HCOOBiO is obtained final product after the product washing obtained by step 2.
Shown in transmission electron microscope picture 2 (a) of products therefrom, product defines a nanometer linear structure.But nano wire is shorter,
Only 2-5 μm or so.
Embodiment 2：
Step one：By 1mmol Bi (NO3)3·5H2O is dissolved in 30ml DMF；
Step 2：The isothermal reaction in closed reactor by the solution obtained by step one, 120 DEG C of reaction temperature, during reaction
Between be 12h；
Step 3：It is nanocrystalline by nanometer wire HCOOBiO is obtained final product after the product washing obtained by step 2.
Shown in transmission electron microscope picture 2 (b) of products therefrom, product is still nanometer linear structure, but length increases.
Embodiment 3：
Step one：By 1mmol Bi (NO3)3·5H2O is dissolved in 30ml DMF；
Step 2：The isothermal reaction in closed reactor by the solution obtained by step one, 120 DEG C of reaction temperature, during reaction
Between be 24h；
Step 3：It is nanocrystalline by nanometer wire HCOOBiO is obtained final product after the product washing obtained by step 2.
Shown in transmission electron microscope picture 2 (c) and (d) of products therefrom, product is still nanometer linear structure, and length is longer.
Pass through its K to variable concentrations in Fig. 3 (a)2Cr2O7The adsorption experiment of solution and methyl orange finds：With K2Cr2O7The increasing of concentration
Plus, the adsorbance of sample gradually increases, and maximal absorptive capacity is up to 174mg/g；To the adsorbance of methyl orange also up to 93mg/g,
And its rate of adsorption is very fast, has reached in a basic balance during 30s.
Using 120 DEG C of ＞ reaction temperature when, form flaky nanometer structure.
Comparative example 1：
Step one：By 1mmol Bi (NO3)3·5H2O is dissolved in 5ml DMF, is added 25ml ethanol, is stirred；
Step 2：The isothermal reaction in closed reactor by the solution obtained by step one, 120 DEG C of reaction temperature, during reaction
Between be 24h；
Step 3：It is nanocrystalline by flower-shaped HCOOBiO is obtained final product after the product washing obtained by step 2.
Shown in transmission electron microscope picture 4 (a) of products therefrom, product is the flower-like structure of nanometer sheet composition, with document report
Structure is essentially identical.
Comparative example 2：
Step one：By 2mmol Bi (NO3)3·5H2O is dissolved in 30ml DMF；
Step 2：The isothermal reaction in closed reactor by the solution obtained by step one, 120 DEG C of reaction temperature, during reaction
Between be 48h；
Step 3：It is nanocrystalline by flower-shaped HCOOBiO is obtained final product after the product washing obtained by step 2.
Shown in transmission electron microscope picture 4 (b) of products therefrom, product is the flower-like structure of nanometer sheet composition, with document report
Structure is essentially identical.By to K in Fig. 5 (c) and (d)2Cr2O7The adsorption experiment of solution and methyl orange finds：Which is to K2Cr2O7's
Adsorbance is only 43mg/g, only the 1/4 of the nanometer linear structure adsorbance of comparable sodium；Its adsorbance to methyl orange is only
The 1/2 of the nanometer linear structure adsorbance of 37mg/g, only comparable sodium.
Claims (2)
1. a kind of HCOOBiO of unique morphology is nanocrystalline, it is characterised in that described HCOOBiO is nanocrystalline micro- with nanometer wire
Structure is seen, prepared by the nanocrystalline employing following steps：
Step one：By Bi (NO3)3·5H2O is dissolved in DMF, Bi (NO in resulting solution3)3·5H2The molar concentration of O is
0.033mol/L；
Step 2：Step one solution is placed in into reaction kettle for reaction, described reaction temperature is 120 DEG C, and the response time is 6-
24h；
Step 3：Reaction terminate after washing to obtain final product nanometer wire HCOOBiO nanocrystalline.
2. a kind of HCOOBiO of unique morphology nanocrystalline preparation method, it is characterised in that adopt soft chemical method, its concrete preparation
Step is：
Step 1：By Bi (NO3)3·5H2O is dissolved in DMF, Bi (NO in resulting solution3)3·5H2O molar concentrations are 0.033mol/
L；
Step 2：Step 1 solution is placed in into reaction kettle for reaction, described reaction temperature is 120 DEG C, and the response time is 6-24h；
Step 3：Reaction terminate after washing to obtain final product nanometer wire HCOOBiO nanocrystalline.
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| CN110586181A (en) * | 2018-06-13 | 2019-12-20 | 南京理工大学 | HCOOBiO photocatalyst prepared by room-temperature solid-phase grinding method and method thereof |
| CN108786895B (en) * | 2018-07-06 | 2020-12-22 | 兰州大学 | BiOCOOH/g-C3N4Composite photocatalyst and preparation method and application thereof |
| CN110508320A (en) * | 2019-08-22 | 2019-11-29 | 南京理工大学 | BiO(HCOO)xIyBr1-x-yThe solid-phase grinding preparation method of mischcrystal photocatalyst |
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| PT104751A (en) * | 2009-09-18 | 2011-03-18 | Univ Aveiro | METHOD FOR THE PREPARATION OF LOW TEMPERATURES OF FERROELECTRIC FINE FILMS, THE FERROELECTRIC FINE FILMS SO OBTAINED AND THEIR APPLICATIONS |
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| F. Duan et al.."Synthesis and photocatalytic behaviour of 3D fl * |
| owerlike bismuth oxide formate architectures".《Materials Letters》.2010,第64卷实验部分第2小节及图2. * |
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