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Preparation method for template-free synthesis of phosphoric acid microspheres

An antimony phosphate microsphere, template-free technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as cumbersome preparation methods, achieve simple preparation process, large-scale synthetic product yield, and good dispersibility Effect

Active Publication Date: 2015-08-19
LINGNAN NORMAL UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

[0003] Pena et al. and Melnikov et al. did not prepare antimony phosphate micro-nanomaterials with a three-dimensional hierarchical structure, but Li et al. prepared microspheres composed of nanoparticles with a hollow structure through a template method. The preparation method is relatively cumbersome. The microstructure of the product is a hollow microsphere composed of nanoparticles with a zero-dimensional structure
At present, there is no report on the preparation of antimony phosphate micro-nanomaterials with a three-dimensional hierarchical hollow structure composed of one-dimensional nanorods without using any template.

Method used

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  • Preparation method for template-free synthesis of phosphoric acid microspheres
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  • Preparation method for template-free synthesis of phosphoric acid microspheres

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Embodiment 1

[0034] A preparation method for template-free synthesis of antimony phosphate microspheres, comprising the steps of:

[0035] S1. Dissolve 1.5mmol antimony potassium tartrate in 60ml ethylene glycol, stir until completely dissolved. Then add 20mmol of phosphoric acid, stir for 30 minutes and mix well.

[0036] S2. The mixed solution obtained in S1 was transferred to a 100ml stainless steel reaction kettle lined with polytetrafluoroethylene, placed in a dry box, and reacted at 180°C for 8 hours. Then cool naturally to room temperature, rinse the obtained precipitate three times with deionized water and absolute ethanol, centrifuge, and dry in a vacuum oven at 80°C for 12 hours to obtain antimony phosphate flower-shaped hollow microspheres.

[0037] The X-ray diffraction figure of the antimony phosphate product that makes is shown in figure 1 , the position and intensity of each diffraction peak in the figure are consistent with the standard diffraction card monoclinic antimon...

Embodiment 2

[0040] A preparation method for template-free synthesis of antimony phosphate microspheres, comprising the steps of:

[0041] S1. Dissolve 1mmol antimony potassium tartrate in 60ml ethylene glycol and stir until completely dissolved. Then add 12mmol of phosphoric acid, stir for 30 minutes and mix well.

[0042] S2. The mixed solution obtained in S1 was transferred to a 100ml stainless steel reaction kettle lined with polytetrafluoroethylene, placed in a dry box, and reacted at 180°C for 8 hours. Then cool naturally to room temperature, rinse the obtained precipitate three times with deionized water and absolute ethanol, centrifuge, and dry in a vacuum oven at 80°C for 12 hours to obtain antimony phosphate flower-shaped hollow microspheres.

[0043] The SEM and TEM images of the antimony phosphate product are shown in image 3 (A) and 3(B), showing that the antimony phosphate product is a flower-like microsphere with a hollow structure and a relatively uniform shape and size, w...

Embodiment 3

[0045] A preparation method for template-free synthesis of antimony phosphate microspheres, comprising the steps of:

[0046] S1. Dissolve 1.5mmol antimony potassium tartrate in 60ml ethylene glycol, stir until completely dissolved. Then add 20mmol of phosphoric acid, stir for 30 minutes and mix well.

[0047] S2. The mixed solution obtained in S1 was transferred to a 100ml stainless steel reaction kettle lined with polytetrafluoroethylene, placed in a dry oven, and reacted at 150°C for 8 hours. Then cool naturally to room temperature, rinse the obtained precipitate three times with deionized water and absolute ethanol, centrifuge, and dry in a vacuum oven at 80°C for 12 hours to obtain antimony phosphate flower-shaped hollow microspheres.

[0048] The scanning electron micrograph of the antimony phosphate product that makes is shown in Figure 4 , showing that the antimony phosphate product is a flower-like microsphere with a hollow structure and a relatively uniform shape ...

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Abstract

The invention belongs to the technical field of inorganic nanometer materials and particularly discloses a method for template-free synthesis of phosphoric acid microspheres. The method specifically comprises the following steps of (S1) dissolving antimony potassium tartrate and phosphoric acid into a solvent to form a mixed solution, (S2) conducting solvo-thermal reaction on the obtained mixed solution and performing cooling, washing, centrifugal separationand drying to obtain a product, wherein the solvent is ethylene glycol or glycerol. The method adopts cheap and easily-obtained raw materials, and a large amount of phosphoric acid microspheres which is good in dispersity and even in shape and size, consists of namo rods and are of hollow structures are synthesized. The average diameter of the prepared phosphoric acid microspheres ranges from 1.3 microns to 2.5 microns, and the prepared phosphoric acid microspheres are expected to be widely applied in the fields of photocatalysis, lithium ion batteries and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic micro-nano materials, in particular to a preparation method for template-free synthesis of antimony phosphate microspheres. Background technique [0002] It is well known that the physical and chemical properties of inorganic nanomaterials are strongly dependent on their morphology, size, and microstructure due to the interrelationship between structure and properties. In recent years, inorganic micro-nano functional materials with controllable size and shape, especially with nanostructures as basic units (such as zero-dimensional nanoparticles, one-dimensional nanowires, nanorods and nanotubes, and two-dimensional nanoplates, nanosheets ) composed of micro-nano materials with a three-dimensional hierarchical structure have attracted great interest and attention because of their novel optical and electrical properties due to the advantages of both nanoscale and microscale. In add...

Claims

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Application Information

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IPC IPC(8): C01B25/37B82Y30/00
Inventor 马琳许丽梅周晓平徐旭耀
Owner LINGNAN NORMAL UNIV
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