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Nanometer material with controllable particle sizes and silicon dioxide hollow spheres and method for preparing nanometer material

A technology of silica and nanomaterials, applied in the direction of silica, silica, nanotechnology for materials and surface science, etc., can solve the problem of unfavorable macromolecular object transportation and packaging, small pore size of silica hollow spheres, Problems such as emulsion template instability, to achieve the effect of good industrial application prospects, cheap raw materials, and low surfactant dosage

Active Publication Date: 2016-10-26
山东济清科技服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN102583400A has prepared mesoporous silica hollow spheres by sol-gel / emulsion method, and the formed emulsion oil droplets are used as templates of hollow structures, and this emulsion template is extremely unstable (emulsion is a thermodynamically unstable system), and The pore size of the prepared silica hollow spheres is small, which is not conducive to the transportation and encapsulation of macromolecular objects. In addition, some materials need to be calcined twice, which destroys the structure of the hollow spheres to a certain extent.

Method used

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  • Nanometer material with controllable particle sizes and silicon dioxide hollow spheres and method for preparing nanometer material
  • Nanometer material with controllable particle sizes and silicon dioxide hollow spheres and method for preparing nanometer material
  • Nanometer material with controllable particle sizes and silicon dioxide hollow spheres and method for preparing nanometer material

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Embodiment 1

[0032]Add 0.04g CTAB and 1.50g PVP to the mixed solution composed of 20mL ethanol and 30mL deionized water in turn, stir at 30°C and 500rpm for 1h to obtain solution A; at room temperature, 1.20g TEOS was ultrasonically dispersed In 7mL of cyclohexane solution, under constant stirring, quickly add to solution A, continue to stir for 0.5h to form mixed solution B; add 0.7mL of ammonia water with a mass concentration of 27% to mixed solution B, and continue to stir at 30°C React for 2 hours to obtain solution C; transfer the mixed solution C to an autoclave, put the autoclave in an oven, and cool the autoclave to room temperature after solvothermal reaction at 180°C for 24 hours; centrifuge the obtained precipitate, wash it, and 60 After drying at ℃ for 10h, calcining at 550℃ for 5h in a box-type calciner to obtain the final product SiO 2 hollow ball.

[0033] FESEM ( figure 2 a) It can be clearly observed that the morphology of the sample is a sphere with a particle size of ...

Embodiment 2

[0035] Add 0.04g CTAB and 1.50g PVP to the mixed solution composed of 20mL ethanol and 30mL deionized water in turn, stir at 30°C and 500rpm for 1h to obtain solution A; at room temperature, 1.20g TEOS was ultrasonically dispersed In 7mL of cyclohexane solution, under constant stirring, quickly add to solution A, continue to stir for 0.5h to form mixed solution B; add 0.7mL of ammonia water with a mass concentration of 27% to mixed solution B, and continue to stir at 30°C React for 2 hours to obtain solution C; transfer the mixed solution C to an autoclave, put the autoclave in an oven, and cool the autoclave to room temperature after solvothermal reaction at 200°C for 24 hours; centrifuge the obtained precipitate, wash it, and After drying at ℃ for 10h, calcining at 550℃ for 5h in a box-type calciner to obtain the final product SiO 2 hollow ball.

[0036] FESEM ( figure 2 b) It can be clearly observed that the shape of the sample is a sphere with a particle size of 220-270...

Embodiment 3

[0038] Add 0.04g CTAB and 1.50g PVP to the mixed solution composed of 20mL ethanol and 20mL deionized water in turn, stir at 30°C and 500rpm for 1h to obtain solution A; at room temperature, ultrasonically disperse 1.20g TEOS In 8mL of cyclohexane solution, under constant stirring, quickly add to solution A, continue to stir for 0.5h to form mixed solution B; add 0.7mL of ammonia water with a mass concentration of 27% to mixed solution B, and continue to stir at 30°C React for 2 hours to obtain solution C; transfer the mixed solution C to an autoclave, put the autoclave in an oven, and cool the autoclave to room temperature after solvothermal reaction at 200°C for 24 hours; centrifuge the obtained precipitate, wash it, and After drying at ℃ for 10h, calcining at 550℃ for 5h in a box-type calciner to obtain the final product SiO 2 hollow ball. The particle size range of the prepared silica hollow sphere is 260-320nm, the shell thickness is 20nm, and the pore diameter is 12nm. ...

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Abstract

The invention discloses a nanometer material with controllable particle sizes and silicon dioxide hollow spheres and a method for preparing nanometer material. TEOS (tetraethyl orthosilicate) is used as an organic silicon source, CTAB (cetyl trimethyl ammonium bromide) is used as a structure directing agent, water, ethyl alcohol and cyclohexane are used as solvents, and PVP (polyvinyl pyrrolidone) is used as a stabilizer. The method includes carrying out heat reaction by the aid of the solvents to form precursors of the SiO2 hollow spheres; calcining the precursors and removing organic matters so as to obtain the SiO2 hollow spheres. The nanometer material and the method have the advantages that the silicon dioxide hollow spheres prepared by the aid of the method are excellent in dispersibility and have the adjustable particle sizes (of 220-430 nm), large pore diameters (of 10-12 nm) and uniform shell thicknesses, and cavities are large and can be used for storing large quantities of guest molecules; the nanometer material is high in chemical stability and packaging capacity and can be widely applied to the fields of enzymatic catalysis, substance adsorptive separation and the like; the method includes simple synthesis processes, is clean and is free of pollution and low in cost, and preparation procedures are good in repeatability.

Description

technical field [0001] The invention belongs to the field of inorganic material science, in particular to a silicon dioxide hollow sphere nano material with controllable particle size and a preparation method thereof. Background technique [0002] In recent years, mesoporous silica has attracted widespread attention in the field of nanomaterials science because of its large specific surface area and pore volume, good thermal stability, adjustable pore size, controllable morphology, and cytotoxicity. It has broad application prospects in the fields of macromolecular adsorption and separation, enzyme catalysis, chemical sensors, drug controlled release, and environmental protection. However, its capacity space is limited, and silica hollow spheres not only have the advantages of mesoporous silica, but also the hollow part inside can accommodate a large number of guest molecules or large-sized molecules, which has become a research hotspot of many scholars. [0003] At present...

Claims

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Application Information

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IPC IPC(8): C01B33/18B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B33/18C01P2004/03C01P2004/04C01P2004/34C01P2004/64
Inventor 周国伟王丹丹刘作花郑玉洁
Owner 山东济清科技服务有限公司
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