A kind of preparation method of micro-nano hierarchical pore structure calcium carbonate hollow microspheres

A calcium carbonate, graded pore technology, applied in the direction of calcium carbonate/strontium/barium, chemical instruments and methods, calcium/strontium/barium compounds, etc., can solve weak force, difficult to control calcium carbonate crystal morphology, poor compatibility and other problems, to achieve the effect of strong force, excellent structural characteristics and good compatibility

Active Publication Date: 2019-10-25
CENT SOUTH UNIV
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  • Description
  • Claims
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Problems solved by technology

[0007] Technical scheme of the present invention uses CaCl 2 and Na 2 CO 3 As the reaction raw material, polyvinylpyrrolidone (PVP) and sodium dodecylsulfonate (SDSN) are used in combination as a template to obtain calcium carbonate crystals through chemical precipitation reaction, and the calcium carbonate crystals are self-assembled to obtain calcium carbonate hollow microspheres The precursors, PVP and SDSN, have good compatibility with calcium carbonate crystals and strong interaction force, which can well control the growth of calcium carbonate crystals, and finally obtain a hollow calcium carbonate with a micro-nano hierarchical pore structure with good morphology. Microspheres; overcome the defects that the calcium carbonate crystal morphology is difficult to control due to the weak force and poor compatibility between the existing template agent and the inorganic material shell

Method used

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  • A kind of preparation method of micro-nano hierarchical pore structure calcium carbonate hollow microspheres
  • A kind of preparation method of micro-nano hierarchical pore structure calcium carbonate hollow microspheres
  • A kind of preparation method of micro-nano hierarchical pore structure calcium carbonate hollow microspheres

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Embodiment 1

[0033] Accurately weigh 1.11gCaCl 2 And dissolve it in a beaker with 100mL distilled water, stir evenly to prepare CaCl 2 solution; accurately weigh 2.12gNa 2 CO 3 And dissolve it in a beaker with 200mL distilled water, stir evenly to prepare Na 2 CO 3 solution; accurately weigh 2.72g SDSN and dissolve it in a beaker with 100mL distilled water, stir evenly to prepare SDSN solution; weigh 0.4g PVP and 100mL CaCl respectively 2 solution, 200mLNa 2 CO 3 The solution is mixed and stirred well. Under the conditions of reaction temperature of 50°C and magnetic stirring, 100 mL of CaCl 2 / PVP mixed solution dropwise into the SDSN solution, and after stirring for 30min, 200mLNa 2 CO 3 / PVP solution, dropwise added to CaCl 2 / PVP / SDSN mixed solution, control the rate of addition, so that the addition time is 1h, after the reaction, continue to stir for 4h, then filter the reaction product after standing for 12h; wash the precipitate with distilled water and absolute ethanol f...

Embodiment 2

[0035] Accurately weigh 1.11gCaCl 2 And dissolve it in a beaker with 100mL distilled water, stir evenly to prepare CaCl 2 solution; accurately weigh 2.12gNa 2 CO 3 And dissolve it in a beaker with 200mL distilled water, stir evenly to prepare Na 2 CO 3 solution; accurately weigh 2.72g SDSN and dissolve it in a beaker with 100mL distilled water, stir evenly to prepare SDSN solution; weigh 0.8g PVP and 100mL CaCl 2 solution, 200mLNa 2 CO 3 The solution is mixed and stirred well. Under the conditions of reaction temperature of 50°C and magnetic stirring, 100 mL of CaCl 2 / PVP mixed solution dropwise into the SDSN solution, and after stirring for 30min, 200mLNa 2 CO 3 / PVP solution, dropwise added to CaCl 2 / PVP / SDSN mixed solution, control the rate of addition, so that the dropping time is 0.5h; after the reaction is over, continue to stir for 2h, then filter the reaction product after standing for 24h; wash the precipitate with distilled water and absolute ethanol for 3 ...

Embodiment 3

[0037] Accurately weigh 1.11gCaCl 2 And dissolve it in a beaker with 100mL distilled water, stir evenly to prepare CaCl 2 solution; accurately weigh 2.12gNa 2 CO 3 And dissolve it in a beaker with 200mL distilled water, stir evenly to prepare Na 2 CO 3 solution; accurately weigh 3.27g SDSN and dissolve it in a beaker filled with 100mL distilled water, stir evenly to prepare SDSN solution; weigh 0.4g PVP and 100mL CaCl 2 solution, 200mLNa 2 CO 3 The solution is mixed and stirred well. Under the conditions of reaction temperature of 50°C and magnetic stirring, 100 mL of CaCl 2 / PVP mixed solution dropwise into the SDSN solution, and after stirring for 30min, 200mLNa 2 CO 3 / PVP solution, dropwise added to CaCl 2 / PVP / SDSN mixed solution, control the rate of addition, so that the addition time is 1h, after the reaction, continue to stir for 3h, and then filter the reaction product after standing for 24h; wash the precipitate with distilled water and absolute ethanol for...

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Abstract

The invention discloses a preparation method of hollow calcium carbonate microspheres of micro-scale and nano-scale pore structures. The method includes the steps of dropwise adding a calcium chloride / polyvinylpyrrolidone (CaCl2 / PVP) mixed solution to a sodium dodecyl sulfonate (SDSN) solution at a constant stirring speed, dropwise adding a sodium carbonate / polyvinylpyrrolidone (Na2CO3 / PVP) mixed solution to the SDSN solution to react, standing, conducting ageing, washing and drying an obtained product, and calcining the product at a high temperature to obtain the hollow calcium carbonate microspheres. According to the method, morphology of the hollow calcium carbonate microspheres of the micro-scale and nano-scale pore structures can be controlled; the hollow calcium carbonate microspheres which are uniform in size distribution and comprise micro-scale pores and nano-scale pores at the same time can be obtained, and the method is simple, efficient, mild in reaction condition and capable of meeting the requirement for industrialized production.

Description

technical field [0001] The invention relates to a preparation method of calcium carbonate hollow microspheres with micro-nano hierarchical pore structure, and belongs to the technical field of preparation of inorganic nano functional materials. Background technique [0002] As a functional material, micro-nano hierarchical porous structure materials have always been one of the frontier research fields of material science because of their special optical, electrical, magnetic, catalytic and mechanical properties. The micro-nano hierarchical pore structure material refers to a core-shell structure material with hierarchical pores that forms micron-scale cavities inside the material and nanopores on the surface of the material. The hierarchical structure is usually composed of nanoparticles assembled with each other. Micro-nano hierarchical pore structure materials have the characteristics of low density, large specific surface area, good stability, and good surface permeabilit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F11/18
CPCC01F11/183C01P2002/72C01P2004/03C01P2004/04C01P2004/50C01P2004/61C01P2006/16
Inventor 邹俭鹏杨洪志肖平潘一峰
Owner CENT SOUTH UNIV
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