CN105236480A - HCOOBiO nanocrystalline with unique morphology and preparation method therefor - Google Patents

HCOOBiO nanocrystalline with unique morphology and preparation method therefor Download PDF

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CN105236480A
CN105236480A CN201410315980.4A CN201410315980A CN105236480A CN 105236480 A CN105236480 A CN 105236480A CN 201410315980 A CN201410315980 A CN 201410315980A CN 105236480 A CN105236480 A CN 105236480A
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hcoobio
nanocrystalline
reaction
preparation
unique morphology
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CN105236480B (en
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韩巧凤
汪信
杨丽丽
赵靳
朱俊武
武晓东
卑凤利
刘孝恒
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Nanjing University of Science and Technology
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Nanjing University of Science and Technology
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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

A kind of HCOOBiO of unique morphology is nanocrystalline and preparation method thereof
Technical field
The present invention relates to HCOOBiO nanocrystalline and preparation method thereof, particularly nanometer wire HCOOBiO is nanocrystalline and preparation method thereof, belongs to field of inorganic nano-material preparation.
Background technology
In recent years, one-dimentional structure nano material is as nanometer rod, and nanotube, especially overlong nanowire obtains a wide range of applications.Such as, nano wire is owing to having high-specific surface area and excellent ionic conducting property makes it be widely used in the aspects such as lithium ion battery, gas sensor and photochemical catalysis.
Along with industrial expansion, dyestuff and heavy metal have become main environmental pollutant.Absorption method is simple due to it, less investment, and high efficiency and restorability have become a kind of effective decontamination method.Formic acid oxidation bismuth replaces haloid element poisonous in BiXO (X=Cl, Br, I) due to it by more green element (C, H and O), may become novel photocatalyst material and sorbent material.
It is raw material that the people such as formic acid oxygen bismuth has good photocatalysis performance, FangDuan adopt with Bismuth trinitrate, and DMF is as reactant, and water is as solvent, and at 120 DEG C, hydro-thermal obtains flower-shaped HCOOBiO; The people such as JinyanXiong are with sodium formiate and Bismuth trinitrate for raw material, and obtain HCOOBiO with N.F,USP MANNITOL, EG, DEG, TEG for solvent hydro-thermal at 150 DEG C respectively, obtained HCOOBiO is the flower-like structure that nanometer sheet assembling is formed.HCOOBiO prepared by above two sections of reports is flower-shaped or globosity, and in addition, document only reports photocatalysis performance, does not study the absorption property of its heavy metal ion and dyestuff.
Summary of the invention
The object of the present invention is to provide nanometer wire HCOOBiO nanocrystalline and preparation method thereof.
The technical solution realizing the object of the invention is: a kind of HCOOBiO of unique morphology is nanocrystalline, and described HCOOBiO is nanocrystalline is nanometer wire.
Utilize soft chemical method to prepare the nanocrystalline method of the above-mentioned HCOOBiO with unique morphology, comprise the following steps:
Step one: by Bi (NO 3) 35H 2o is dissolved in DMF;
Step 2: step one solution is placed in reaction kettle for reaction;
Step 3: reaction terminates rear washing, and namely to obtain nanometer wire HCOOBiO nanocrystalline.
Bi (NO in gained solution in step one 3) 35H 2o volumetric molar concentration is 0.033mol/L.
Temperature of reaction described in step 2 is 120 DEG C, and the reaction times is 6-24h.
The present invention has following remarkable advantage:
1, method is simple, without the need to adding any catalyzer and template, only uses DMF and Bismuth trinitrate two kinds of raw materials to obtain HCOOBiO nanocrystalline;
2, obtained HCOOBiO is nanocrystalline is overlength wire, and its winding can form reticulated structure, has larger specific surface area and pore structure, is conducive to the raising of its performance;
4, this dye sheet such as nanocrystalline heavy metal ion Cr (VI) and tropeolin-D reveals excellent absorption property, higher than the absorption property of flower-like structure 3 times, is expected to have good application in industrial wastewater treatment field.
Accompanying drawing explanation
Fig. 1 is that hydrothermal method of the present invention preparation has the nanocrystalline schematic flow sheet of the HCOOBiO of unique morphology.
Fig. 2 is that the TEM of the nanometer wire HCOOBiO that embodiment 1-3 obtains schemes ((a) embodiment 1; (b) embodiment 2; (c) and (d) embodiment 3).
Fig. 3 is that the present invention obtains nanometer wire 20mgHCOOBiO to different concns K 2cr 2o 7adsorptive capacity variation diagram ((a) K in time of solution and tropeolin-D 2cr 2o 7; (b) tropeolin-D).
Fig. 4 is TEM figure ((a) comparative example 1, (b) comparative example 2) of the flower-shaped HCOOBiO that comparative example 1 and comparative example 2 obtain.
Fig. 5 is that comparative example 2 obtains sample to K 2cr 2o 7the adsorptive capacity of solution and tropeolin-D in time variation diagram ((c) is K 2cr 2o 7solution, (d) is tropeolin-D).
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Composition graphs 1, the present invention utilizes DMF to have the nanocrystalline method of the HCOOBiO of unique morphology for solvent and reactant preparation, and its feature comprises the following steps:
Step one: by Bi (NO 3) 35H 2o is dissolved in DMF, wherein Bi (NO 3) 35H 2o volumetric molar concentration is 0.033mol/L;
Step 2: step one solution is placed in reaction kettle for reaction 6-24h, wherein temperature of reaction is 120 DEG C;
Step 3: reaction terminates rear washing, and namely to obtain nanometer wire HCOOBiO nanocrystalline.
Embodiment 1:
Step one: by 1mmolBi (NO 3) 35H 2o is dissolved in 30mlDMF;
Step 2: by the isothermal reaction in closed reactor of the solution of step one gained, temperature of reaction 120 DEG C, the reaction times is 6h;
Step 3: namely obtain nanometer wire HCOOBiO after product washing step 2 obtained nanocrystalline.
Shown in the transmission electron microscope picture 2 (a) of products therefrom, product defines nanometer linear structure.But nano wire is shorter, only about 2-5 μm.
Embodiment 2:
Step one: by 1mmolBi (NO 3) 35H 2o is dissolved in 30mlDMF;
Step 2: by the isothermal reaction in closed reactor of the solution of step one gained, temperature of reaction 120 DEG C, the reaction times is 12h;
Step 3: namely obtain nanometer wire HCOOBiO after product washing step 2 obtained nanocrystalline.
Shown in the transmission electron microscope picture 2 (b) of products therefrom, product is still nanometer linear structure, but length increases.
Embodiment 3:
Step one: by 1mmolBi (NO 3) 35H 2o is dissolved in 30mlDMF;
Step 2: by the isothermal reaction in closed reactor of the solution of step one gained, temperature of reaction 120 DEG C, the reaction times is 24h;
Step 3: namely obtain nanometer wire HCOOBiO after product washing step 2 obtained nanocrystalline.
Shown in the transmission electron microscope picture 2 (c) of products therefrom and (d), product is still nanometer linear structure, and length is longer.It is passed through to the K of different concns in Fig. 3 (a) 2cr 2o 7the adsorption experiment of solution and tropeolin-D finds: with K 2cr 2o 7the increase of concentration, the adsorptive capacity of sample increases gradually, and maximal absorptive capacity can reach 174mg/g; Also 93mg/g can be reached to the adsorptive capacity of tropeolin-D, and its adsorption rate is very fast, has reached in a basic balance during 30s.
When adopting the temperature of reaction of > 120 DEG C, form flaky nanometer structure.
Comparative example 1:
Step one: by 1mmolBi (NO 3) 35H 2o is dissolved in 5mlDMF, adds 25ml ethanol, stirs;
Step 2: by the isothermal reaction in closed reactor of the solution of step one gained, temperature of reaction 120 DEG C, the reaction times is 24h;
Step 3: namely obtain flower-shaped HCOOBiO after product washing step 2 obtained nanocrystalline.
Shown in the transmission electron microscope picture 4 (a) of products therefrom, product is the flower-like structure of nanometer sheet composition, substantially identical with bibliographical information structure.
Comparative example 2:
Step one: by 2mmolBi (NO 3) 35H 2o is dissolved in 30mlDMF;
Step 2: by the isothermal reaction in closed reactor of the solution of step one gained, temperature of reaction 120 DEG C, the reaction times is 48h;
Step 3: namely obtain flower-shaped HCOOBiO after product washing step 2 obtained nanocrystalline.
Shown in the transmission electron microscope picture 4 (b) of products therefrom, product is the flower-like structure of nanometer sheet composition, substantially identical with bibliographical information structure.Pass through K in Fig. 5 (c) and (d) 2cr 2o 7the adsorption experiment of solution and tropeolin-D finds: it is to K 2cr 2o 7adsorptive capacity be only 43mg/g, be only 1/4 of the nanometer linear structure adsorptive capacity of comparable sodium; It is only 37mg/g to the adsorptive capacity of tropeolin-D, is only 1/2 of the nanometer linear structure adsorptive capacity of comparable sodium.

Claims (7)

1. the HCOOBiO of a unique morphology is nanocrystalline, it is characterized in that described HCOOBiO is nanocrystalline and has nanometer wire microtexture.
2. the HCOOBiO of unique morphology according to claim 1 is nanocrystalline, it is characterized in that described nanocrystalline employing following steps preparation:
Step one: by Bi (NO 3) 35H 2o is dissolved in DMF;
Step 2: step one solution is placed in reaction kettle for reaction;
Step 3: reaction terminates rear washing, and namely to obtain nanometer wire HCOOBiO nanocrystalline.
3. the HCOOBiO of unique morphology according to claim 2 is nanocrystalline, to it is characterized in that in step one Bi (NO in gained solution 3) 35H 2the volumetric molar concentration of O is 0.033mol/L.
4. the HCOOBiO of unique morphology according to claim 2 is nanocrystalline, it is characterized in that the temperature of reaction described in step 2 is 120 DEG C.
5. the preparation method that the HCOOBiO of unique morphology is nanocrystalline, it is characterized in that adopting soft chemical method, its concrete preparation process is:
Step 1: by Bi (NO 3) 35H 2o is dissolved in DMF;
Step 2: step 1 solution is placed in reaction kettle for reaction;
Step 3: reaction terminates rear washing, and namely to obtain nanometer wire HCOOBiO nanocrystalline.
6. the preparation method that the HCOOBiO of unique morphology according to claim 5 is nanocrystalline, to is characterized in that in step 1 Bi (NO in gained solution 3) 35H 2o volumetric molar concentration is 0.033mol/L.
7. the preparation method that the HCOOBiO of unique morphology according to claim 5 is nanocrystalline, it is characterized in that the temperature of reaction described in step 2 is 120 DEG C, the reaction times is respectively 6-24h.
CN201410315980.4A 2014-07-03 2014-07-03 HCOOBiO nanocrystalline with unique morphology and preparation method therefor Expired - Fee Related CN105236480B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108786895A (en) * 2018-07-06 2018-11-13 兰州大学 BiOCOOH/g-C3N4Composite photo-catalyst and its preparation method and application
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
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

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WO2011033343A1 (en) * 2009-09-18 2011-03-24 Universidade De Aveiro Method for the preparation at low temperatures of ferroelectric thin films, the ferroelectric thin films thus obtained and their applications
CN103135224A (en) * 2013-03-25 2013-06-05 武汉工程大学 Preparation method for light-operated reversible wetting coating
CN103182293A (en) * 2013-04-01 2013-07-03 北京工业大学 Method for preparing manganese oxide nanowire by deposition on surface of natural porous diatomite

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN108786895A (en) * 2018-07-06 2018-11-13 兰州大学 BiOCOOH/g-C3N4Composite photo-catalyst and its preparation method and application
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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