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
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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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