Mesoporous high polymer or carbon/silicon oxide nano-composite material with three-dimensional pore canal structure and preparation method thereof

A technology of nanocomposite materials and three-dimensional channels, applied in the field of mesoporous nanocomposite materials and their preparation, to achieve strong operability, simplify the preparation process, and increase the effect of hydrophobic core

Inactive Publication Date: 2012-03-21
CHONGQING UNIV OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] So far, the use of PDMS-PEO as a template to synthesize porous materials is only reported by N. Husing in 2003, which used PDMS-PEO as a template to synthesize porous oxide Silicon material, but the literature did not characterize the pore structure and properties of the obtained material, that is, it cannot be confirmed that it has an ordered mesoporous structure
Moreover, the use of PDMS-PEO in the synthesis of mesoporous silica materials in this literature does not make much sense. Only when PDMS-PEO is used as a structure-directing agent to synthesize mesoporous carbon / silicon oxide nanocomposites or mesoporous carbon materials can its growth be brought into full play. Advantages such as skeleton stability and increased pore size

Method used

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  • Mesoporous high polymer or carbon/silicon oxide nano-composite material with three-dimensional pore canal structure and preparation method thereof
  • Mesoporous high polymer or carbon/silicon oxide nano-composite material with three-dimensional pore canal structure and preparation method thereof
  • Mesoporous high polymer or carbon/silicon oxide nano-composite material with three-dimensional pore canal structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1 Synthesis of Phenolic Resin Prepolymer

[0046] Melt 0.61g phenol at 40-42°C, add 0.13 g 20 wt% NaOH aqueous solution at this temperature and stir for 10 min, add 1.05 g 37wt% formaldehyde aqueous solution, raise the temperature to 70-75°C for 1 hour, cool down to room temperature, and use 0.6 mol / L HCl solution to adjust the pH value of the solution to 7.0, dehydration under vacuum and reduced pressure for 1 to 2 hours below 50°C. The obtained viscous liquid was dissolved in THF to prepare a 20 wt% solution for use.

Embodiment 2

[0047] Example 2 Preparation of As-made samples

[0048] Dissolve 1.0 g of F127 and 1.0 g of PDMS-PEO in 40.0 g of tetrahydrofuran (THF), and stir at 40°C for 10 min to obtain a uniform and transparent solution. Then add 10.0 g of the 20 wt % phenolic resin prepolymer prepared above ( M w <500) THF solution, stirred for 0.5h to obtain a homogeneous solution. Transfer the above solution to a petri dish, volatilize at room temperature for 5-8 h, and then place the petri dish in an oven at 100°C for 24 h to obtain a transparent orange-yellow film material. The above material was scraped off the Petri dish and ground into powder to obtain the As-made intermediate.

[0049] The triblock copolymer F127 in this example ( M w =12600, EO 106 -PO 70 -EO 106 ) was purchased from Aldrich, PDMS-PEO ( M w =3012, DMS 32 -EO 20 ) were purchased from Shenzhen Merrill Chemical Technology Co., Ltd., and other reagents were purchased from Shanghai Chemical Reagent Company. All reag...

Embodiment 3

[0050] Example 3 Preparation of three-dimensional ordered mesoporous polymer / silicon oxide and carbon / silicon oxide nanocomposites

[0051] Put the above-mentioned As-made intermediate in a tube furnace for calcination under the protection of nitrogen gas, calcine at 400°C for 3 hours to obtain a three-dimensional ordered mesoporous polymer / silicon oxide nanocomposite material, and calcinate at 900°C for 2 hours to obtain a three-dimensional ordered mesoporous Porous carbon / silicon oxide nanocomposite material; during the firing process, when the temperature is below 600°C, the heating rate is set to 1°C / min, and when the temperature is above 600°C, the heating rate is set to 5°C / min . The samples calcined at 400°C under nitrogen atmosphere are marked as MP-CS-400N, and the samples calcined at 900°C under nitrogen atmosphere are marked as MP-CS-900N.

[0052] According to the adjustment of various material types, dosage ratios, process parameters, etc. in the present invent...

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Abstract

The invention discloses a mesoporous high polymer or carbon / silicon oxide nano-composite material with a three-dimensional pore canal structure. The mesoporous high polymer or carbon / silicon oxide nano-composite material is prepared by mixing PDMS-PEO (Polydimethylsiloxane-Poly Ethylene Oxide) and F127 serving as mixed structure directing agents and a phenolic resin performed polymer Resol serving as a carbon source precursor and reacting to obtain an As-made intermediate, and calcining, wherein crystal diffraction peaks of 110, 200, 211, 220, 310, 222 and 321 are shown in the small angle X ray scattering (SAXS) map of the As-made intermediate, and the q value ratio of the diffraction peaks is shown in the specifications. The specific surface area of the mesoporous carbon / silicon oxide nano-composite material with a three-dimensional cubic Imm pore canal structure is 650-1,600m<2> / g, the pore volume range is 0.45-0.63 cm<3> / g, the pore size is 5.0-6.2 nanometers, and the stability of a mesoporous material framework is up to 900 DEG C. The high polymer or carbon / silicon oxide nano-composite material provided by the invention is particularly suitable for the fields of super capacitor electrode materials, adsorbents, catalyst carriers, separation of biomolecules, gas-sensitive materials, optoelectronic devices, hydrogen storage and the like.

Description

technical field [0001] The invention relates to the technical field of new nanometer materials, in particular to a three-dimensional cubic Im m Mesoporous nanocomposite material with channel structure and its preparation method. Background technique [0002] Ordered mesoporous materials are porous materials with regular pore structures and pore diameters ranging from 2 to 50 nm, which are assembled through the interface interaction between organic and inorganic substances based on surfactant molecular aggregates as templates. Mesoporous materials have the following superior characteristics: ①Long-range, that is, mesoscopic horizontal structure and orderly pore structure; ②The pore size distribution is narrow, and the pore size can be continuously adjusted; ③By optimizing the synthesis conditions or post-processing, it can have good thermal stability. and certain hydrothermal stability; ④ extremely high specific surface area, up to 1000~1500 m 2 / g; ⑤The particles have ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02
Inventor 刘玉荣
Owner CHONGQING UNIV OF ARTS & SCI
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