Preparation method of regular octahedral bismuth fluoride material

A technology of regular octahedron and bismuth fluoride, which is applied in chemical instruments and methods, inorganic chemistry, bismuth compounds, etc., can solve problems such as inability to obtain fluorination, energy consumption, environmental pollution, and expensive products, so as to avoid energy waste and protect The effect of simplifying the environment and preparation method

Active Publication Date: 2016-07-27
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This type of reaction is time-consuming, energy-consuming and environmentally polluting, so the product is expensive
In addition, bismuth (III) ions in bismuth nitrate pentahydrate were chelated by mannitol to precipitate bismuth hydroxide in alkaline solution, and bismuth hydroxide was stirred in HF solution for 12 hours to undergo a solid-liquid reaction to form BiF 3 The method is theoretically feasible, but the actual yield is very low, there are many impurities and the product is unstable
[0004] Chinese invention patent (CN101212050A) discloses a preparation method of bismuth fluoride cathode material for lithium secondary batteries, which specifically includes dissolving bismuth salt in acetic acid solution to prepare bismuth salt acetic acid solution, adding a surfactant; and preparing soluble fluoride salt or HF ethanol at the same time aqueous solution to obtain a mixed solution of alcohol and fluorine; mix the two solutions at 0-45°C to obtain BiF 3 The precipitate was then filtered, washed and dried to obtain BiF 3 products, but this preparation method cannot obtain bismuth fluoride with specific morphology
Therefore, at present, there is no report on the synthesis technology of octahedral bismuth fluoride materials at room temperature.

Method used

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  • Preparation method of regular octahedral bismuth fluoride material
  • Preparation method of regular octahedral bismuth fluoride material
  • Preparation method of regular octahedral bismuth fluoride material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 0.485gBi(NO 3 ) 3 ·5H 2 O was dissolved in 19ml of deionized water, and 1ml of HNO was added 3 , configured as a bismuth nitrate solution with a concentration of 50mM; dissolve 0.42gNaF in 80ml of deionized water, add 2gPVP, and configure a sodium fluoride solution with a concentration of 0.125M; add the bismuth nitrate solution to the sodium fluoride solution, and stir After uniformity, let stand for reaction for 5 days; wash the obtained precipitates with deionized water and absolute ethanol three times respectively, and dry in a blast drying oven at 60° C. for 12 hours to obtain octahedral bismuth fluoride materials.

[0041] Carry out X-ray diffraction analysis to regular octahedral bismuth fluoride material, the result is as follows figure 1 As shown, the prepared bismuth fluoride has a single composition, belongs to the face-centered cubic crystal system (JCPDS51-0944), has a space group of Fm3m, and has high crystallinity.

[0042] SEM analysis of octahedral ...

Embodiment 2

[0044] 0.485gBi(NO 3 ) 3 ·5H 2O was dissolved in 19ml of deionized water, and 1ml of HNO was added 3 , configured as a bismuth nitrate solution with a concentration of 50mmol / L; dissolve 0.42gNaF in 80ml of deionized water, add 0.5gPVP, and configure a NaF solution with a concentration of 0.125mol / L; add the bismuth nitrate solution to the sodium fluoride solution After mixing evenly, let it stand at 25°C for 5 days; wash the obtained precipitates with deionized water and absolute ethanol three times respectively, and dry them in a blast drying oven at 60°C for 12 hours to obtain octahedral fluorine bismuth material. Scanning electron microscope analysis was carried out to the obtained product, such as Figure 5 As shown, it consists of octahedral micro-nano structures, and the octahedral structure has a single, uniform and regular pattern.

Embodiment 3

[0046] 0.485gBi(NO 3 ) 3 ·5H 2 O was dissolved in 19ml of deionized water, and 1ml of HNO was added 3 , configured as a bismuth nitrate solution with a concentration of 50mmol / L; dissolve 0.42gNaF in 80ml of deionized water, add 3gPVP, and configure a NaF solution with a concentration of 0.125mol / L; add the bismuth nitrate solution to the sodium fluoride solution , stirred evenly and left to react at 25°C for 5 days; the obtained precipitates were washed three times with deionized water and absolute ethanol respectively, and dried in a blast drying oven at 60°C for 12 hours to obtain octahedral fluorinated bismuth material. Scanning electron microscope analysis was carried out to the obtained product, such as Image 6 As shown, it consists of octahedral micro-nano structures, and the octahedral structure has a single, uniform and regular pattern.

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Abstract

The invention relates to a preparation method of a regular octahedral bismuth fluoride material. The method comprises the following steps: (1) dissolving bismuth fluoride into deionized water, adding concentrated nitric acid and preparing a bismuth nitrate solution with the molar concentration of 45-55mM; (2) dissolving sodium fluoride into the deionized water and adding polyvinylpyrrolidone to prepare a sodium fluoride solution with the molar concentration of 37.5-125mM; (3) adding the bismuth nitrate solution to the sodium fluoride solution, carrying out standing reaction at 20-30 DEG C to obtain a sediment, wherein the volume ratio of the bismuth nitrate solution to the sodium fluoride solution is 1 to (3.5-4.5); and (4) filtering, washing and drying the sediment obtained in the step (3) to obtain the regular octahedral bismuth fluoride material. According to the preparation method, the regular octahedral bismuth fluoride material can be synthesized by one-step reaction; the cost is saved; the environment is protected; and the product is high in purity, uniform and regular in shape and size, and beneficial to large-scale mass production in future.

Description

technical field [0001] The invention relates to a preparation method of bismuth fluoride, in particular to a preparation method of a regular octahedral bismuth fluoride material. Background technique [0002] In recent years, Bi-based compounds have attracted attention due to their special layered structures and appropriate bandgap widths. As a metal fluoride cathode material, BiF 3 High storage capacity is achieved through reversible switching reactions. Although BiF 3 Its mass specific energy is only 905Wh / kg, but its volume specific energy is as high as 7170Wh / l. BiF 3 As a typical ionic compound, it can be doped with carbon and silver to make the positive electrode material of the secondary battery, and can make full use of all the valence of the material, so that the electrode process has more exchange electrons, high battery voltage and energy. density and other advantages, with more in-depth research on it, BiF 3 It will become a promising anode material for a n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G29/00
CPCC01G29/00C01P2002/72C01P2004/03C01P2004/41C01P2004/61C01P2006/80
Inventor 叶苗苗李建张土乔刘小为
Owner ZHEJIANG UNIV
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