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Mesoporous-macroporous multilevel ordered monodisperse micron sphere and preparation method thereof

A technology of monodispersion and microspheres, applied in the field of materials, can solve the problems of poor monodispersity of particles, unsuitable for chromatographic packing, large size, etc., and achieve the effect of uniform size, easy to obtain raw materials, and simple method

Inactive Publication Date: 2013-01-02
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The size of the primary particles used by the author in this paper is relatively large, the particle size of MCM-41 is between 400-1000 nm, and the particle size of MCM-48 is between 200-700 nm, so the size of the final multi-level ordered microspheres is Also larger, between 10-25 microns, so not suitable for use as a conventional liquid chromatography packing material
[0005]2008, Kuroda K. research group (C. Urata, Y. Yamauchi, Y. Aoyama, J. Imasu, S. Todoroki, Y. Sakka, S. Inoue, K. Kuroda, J. Nanosci. Nanotechno., 2008, 8(6): 3101-3105) assembled nano-mesoporous materials into micron-sized spherical particles by spray drying method, and on the particles At the same time, it has 3 nm mesopores and 15-20 nm interparticle pores. Unfortunately, the monodispersity of the particles is not very good (distributed between 200 nm and 3.5 μm), so it is not suitable for use as a chromatographic filler

Method used

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  • Mesoporous-macroporous multilevel ordered monodisperse micron sphere and preparation method thereof
  • Mesoporous-macroporous multilevel ordered monodisperse micron sphere and preparation method thereof
  • Mesoporous-macroporous multilevel ordered monodisperse micron sphere and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 Preparation of nano-mesoporous materials

[0026] Mix 64 mL of water, 10.5 mL of ethanol, and 10.4 mL of 25 wt% cetyltrimethylammonium chloride aqueous solution at room temperature and stir for 10 min. Then, in this solution, 4.1 mL of triethanolamine was added, and further stirred until all the triethanolamine was dissolved.

[0027] Take 20 mL of the above solution, heat it to 60°C, and add 1.5 mL of tetraethyl orthosilicate dropwise to the solution while stirring, the dropping time is controlled within 2-3 min, and the stirring is continued for 10 min after the dropwise addition is completed.

[0028] The sample prepared by the above method was centrifuged, the supernatant was discarded, and the precipitate was immediately dispersed in deionized water, sonicated for 1 min, and washed twice.

[0029] Disperse 0.1 g of the sample in 10 mL of template removal solution (1 mL of concentrated hydrochloric acid + 9 mL of ethanol). After ultrasonic treatment for...

Embodiment 2

[0030] Example 2 urea-formaldehyde / SiO 2 Synthesis of Composite Microspheres

[0031]The nano-mesoporous material obtained above was dispersed in 10 mL of distilled water to obtain a colloidal solution of nano-mesoporous particles, and the pH of the solution was adjusted to 2 with 1 M HCl. Add 10% (v / v) absolute ethanol, add 3 g of urea under constant stirring, and then add 6 g of formaldehyde aqueous solution after it is completely dissolved, stir rapidly for 5 min, stop stirring and keep at 15 °C React for 1 h. Then add a large amount of water and stir quickly to terminate the reaction, pour the mixed solution into a large beaker and let it stand, and the composite microspheres will settle at the bottom of the beaker. After the obtained precipitate was washed with ethanol and water twice, ethyl acetate was used to remove water azeotropically. The scanning electron microscope image of the obtained material is shown in figure 2 .

Embodiment 3

[0032] Example 3 Synthesis of Mesoporous-Macroporous Hierarchical Ordered Microspheres

[0033] Synthesis of mesoporous-macroporous hierarchically ordered microspheres: The composite microspheres obtained in the previous step were vacuum-dried at 160°C for 1 h, and then calcined in a nitrogen atmosphere by temperature programming in a muffle furnace. The setting procedure of the muffle furnace is as follows: from room temperature to 180 °C for 180 min, from 180 °C to 240 °C for 300 min, at 240 °C for 60 min, at 240 °C to 260 °C for 120 min, and at 260 °C for 60 min, 260 °C It takes 120 minutes from ℃ to 300℃, 300 minutes from 300℃ to 600℃, and 180 minutes at 600℃. The scanning electron microscope image of the obtained material is shown in image 3 with Figure 4 .

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Abstract

The invention belongs to the field of materials, and particularly relates to a mesoporous-macroporous multilevel ordered monodisperse micron sphere and a preparation method thereof. The method includes: using a nanoscale mesoporous molecular sieve obtained by means of hydrothermal synthesis as a multilevel structure construction unit, obtaining a silicon dioxide / urea resin composite micro sphere through the PICA (polymerization-induced colloid aggregation method), performing azeotropic dewatering, and removing urea resin through high-temperature calcinations to prepare the mesoporous-macroporous multilevel ordered monodisperse micron sphere. Dimension of the micron sphere can be adjusted by adjusting usage and proportion of urea and formaldehyde and the pH of solution. The multilevel ordered monodisperse micron sphere prepared by the method is uniform in size and has wide application to adsorption, separation and the like.

Description

technical field [0001] The invention belongs to the technical field of materials, in particular to a mesoporous-macropore multi-level ordered monodisperse microsphere and a preparation method thereof. Background technique [0002] Due to their large specific surface area and pore volume, uniform pore size, regular and orderly pore structure, controllable morphology, and surface functionalization, mesoporous materials have been widely used since they were reported in 1992. A very active research field, with broad application prospects in separation science, catalysis, environmental protection, synthesis of nanomaterials, etc. Nano-mesoporous materials are a class of materials that control the macroscopic size of the resulting mesoporous materials to <100 nm. Nano-mesoporous materials have received more and more attention in recent years, and have been used as carriers for protein transport inside and outside cell membranes, gas Min Bragg mirrors, assembling multilevel ord...

Claims

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Application Information

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IPC IPC(8): C01B33/158B01J20/20B01J20/30B01J13/02
Inventor 张祥民雷杰李伟红
Owner FUDAN UNIV
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