Method for preparing two-dimensional ordered mesoporous nanosheet by inorganic salt interface induced assembling

A technology of inorganic salts and nanosheets, which is applied in nanotechnology, nanocarbon, inorganic chemistry, etc. for materials and surface science, and can solve the difficulty of assembling and modifying single-layer nanosheets, two-dimensional single-layer nanosheets involving less and other problems, to achieve the effect of simple assembly method, highly ordered pores, and good ethanol dispersibility

Active Publication Date: 2019-08-16
FUDAN UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, the method of synthesizing ordered mesoporous materials using inorganic salts as substrates has not been reported. There are few reports on the assembly of two-dimensional single-layer nanosheets by EICA technology, and it is difficult to realize the assembly and modification of single-layer nanosheets.

Method used

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  • Method for preparing two-dimensional ordered mesoporous nanosheet by inorganic salt interface induced assembling
  • Method for preparing two-dimensional ordered mesoporous nanosheet by inorganic salt interface induced assembling
  • Method for preparing two-dimensional ordered mesoporous nanosheet by inorganic salt interface induced assembling

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Embodiment 1

[0029] PEOs117 - b -PS 113 (Molecular weight 16700 g·mol -1 , 0.1 g) was dissolved and dispersed in 10.0 g THF solution, then 2.0 g phenolic resin precursor solution (20 wt%, containing 0.25 g phenol and 0.15 g formaldehyde) dissolved in THF was added, and magnetic stirring was continued at room temperature for 0.5 h to form a uniform transparent solution , pour a certain mixed solution into the inorganic salt NaCl solid crystal powder, perform suction filtration for 30-120 s (or centrifuge at 3000 rpm / 3 min) with a vacuum of 2 Calcined under protection for 3 h to decompose the template agent, the heating rate was 1 °C / min, after the product was cooled, it was washed with deionized water for 3-5 times to remove the NaCl template, and the obtained two-dimensional single-layer ordered mesoporous polymer nanosheets The pore size is 27 nm. If the calcination condition is adjusted to 600°C tube furnace with N 2 Calcined under protection for 3 h, with a heating rate of 1 °C / min,...

Embodiment 2

[0031] PEOs 117 - b -PS 113 (Molecular weight 16700 g·mol -1 or F127) and tetrabutyl titanate (TBOT, 0.2 g) were dissolved and dispersed in 10 mL THF solution, then concentrated hydrochloric acid (0.1 mL, 37%) and acetic acid (0.1 mL, 98%) were added, and magnetic stirring was continued at room temperature for 0.5 h, pour a certain mixed solution into the inorganic salt NaCl solid crystal powder, perform suction filtration for 30-120 s (or 3000 rpm / 3 min centrifugation) with a vacuum of 2 Calcined under protection for 2 h to decompose the template agent at a heating rate of 1 °C / min; then take out the solid in a muffle furnace and calcinate at 430 °C for 2 h in air at a heating rate of 1 °C / min, and use it after the product is cooled. Washed 3-5 times with deionized water to remove the NaCl template, the resulting two-dimensional monolayer ordered mesoporous TiO 2 The nanosheet pore size is 18nm.

Embodiment 3

[0033] PEOs 117 - b -PS 113 (Molecular weight 16700 g·mol -1 , 40 mg) and tetraethyl orthosilicate (TEOS, 0.2 g) were dissolved and dispersed in 4.0 g tetrahydrofuran solution, then 0.1 M hydrochloric acid (0.06 g) was added, and magnetic stirring was continued at room temperature for 0.5 h to form a uniform solution, and a certain amount of the mixed solution was poured into In the inorganic salt NaCl solid crystal powder, vacuum filter 2 Calcined under protection for 3 h to decompose the template agent at a heating rate of 1°C / min; then take out the solid in a muffle furnace and calcinate at 600°C for 2 h under air at a heating rate of 1°C / min, and use it after the product is cooled. Washed 3-5 times with deionized water to remove the NaCl template, the resulting two-dimensional single-layer ordered mesoporous SiO 2 The nanosheets have a pore size of 25 nm.

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Abstract

The invention belongs to the technical field of nanoporous materials, and concretely relates to a method for preparing a two-dimensional ordered mesoporous nanosheet by inorganic salt interface induced assembling. The method comprises the following steps: uniform diffusion and transfer of a target precursor solution in the crystal interface of an inorganic salt are achieved by vacuum suction filtration or low-speed centrifugation with the soluble inorganic salt as a substrate and an amphiphilic block copolymer as a template; a highly ordered monolayer mesoporous structure is formed by a solvent volatilization induced co-assembling technology; and gradient temperature-controlled Ostwald ripening promotes organic solvent volatilization and induces molding, and the template is removed under the protection of N2 to obtain the highly ordered monolayer two-dimensional mesoporous nanosheet material. The assembled nanosheet material has a large pore size and regular and ordered spherical porechannels; and the type of the precursor can be changed to synthesize a plurality of mesoporous metal oxides, metal simple substances and inorganic nonmetal nanosheets. The method of the invention hasthe advantages of simplicity, easily available raw material, universality to nanomaterials, and suitableness for amplified production.

Description

technical field [0001] The invention belongs to the technical field of nanoporous materials, and in particular relates to a method for preparing two-dimensional ordered mesoporous nanosheets through inorganic salt interface induced assembly. Background technique [0002] In recent years, with the rapid development of nanomaterials and nanotechnology, nanomaterials due to their unique size structure, stable physical and chemical properties, and special microscopic effects (such as small size effect, quantum size effect, interface effect, macroscopic quantum tunneling effect, etc.) ) and has been widely used in catalysis, sensing, adsorption, electrochemistry, bioseparation, drug sustained release, etc. (L. Wu, J. J.Willis, I. S. McKay, B. T. Diroll, J. Qin, M. Cargnello, C. J. Tassone, Nature. 548, 197 (2017); H. W. Liang, W. Wei, Z. S. Wu, X. Feng, K. Mullen, J. Am. Chem. Soc. 135, 16002 (2013), J. Zhang, T. Wang, P. Liu, Z. Liao, S. Liu, X. Zhuang, M. Chen, E. Zschech, ...

Claims

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Application Information

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IPC IPC(8): C01B32/15C01G23/053B82Y40/00C01B33/12C01F7/30C01G25/02C01G25/00C01F17/00C01F7/304
CPCC01B32/15C01G23/053B82Y40/00C01B33/12C01F7/30C01G25/02C01G25/00C01P2006/16C01P2004/20C01P2004/01C01F17/206C01B33/126C04B38/0022C04B2111/00008C01F7/304C01F17/235B82Y30/00C04B35/10C04B35/14C04B35/46C04B35/48C04B35/49C04B35/52C04B38/0054C01F17/32B32B18/00C01B33/113C01P2004/24
Inventor 邓勇辉柳亮亮邹义冬杨玄宇
Owner FUDAN UNIV
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