Ordered dual-mesoporous silica material and preparation method thereof
A silica and double mesoporous technology, applied in the field of mesoporous materials, can solve the problems of high process requirements, complex steps, poor order of pores, etc., and achieve the effects of good repeatability, simple process and high product structure stability.
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Embodiment 1
[0026] Dissolve 1.5g of P123 in 47mL of deionized water at a water bath temperature of 42°C, add phosphoric acid dropwise, adjust the solution to pH=2.0, and continue to stir vigorously for 6 hours to obtain a transparent liquid. Add 3.21g of ethyl orthosilicate to the liquid The ester was stirred vigorously at 42°C for 24 hours.
[0027] After filtration, the obtained solid was dissolved in 60 mL of 0.8 mol / L phosphoric acid solution, transferred to a stainless steel reaction kettle with a polytetrafluoroethylene liner, sealed, and allowed to stand at 120°C for hydrothermal reaction for 2 days.
[0028] The reactant was vacuum filtered, dried at 45°C, and calcined at 550°C for 7 hours to obtain a white product of ordered double mesoporous silica material.
[0029] figure 1 and image 3 They are the scanning electron microscope image and X-ray small angle scattering image of the product respectively, and through nitrogen adsorption characterization, it can be concluded that ...
Embodiment 2
[0031] Dissolve 1.0g of P123 in 35mL of deionized water at a water bath temperature of 37°C, add phosphoric acid dropwise, adjust the solution to pH=2.4, and continue to stir vigorously for 4 hours to obtain a transparent liquid. Add 1.17g of sodium silicate to the liquid, Stir vigorously at 37°C for 24 hours.
[0032] After filtration, the obtained solid was dissolved in 45 mL of 10 mol / L phosphoric acid solution, transferred to a stainless steel reactor with a polytetrafluoroethylene liner, sealed, and allowed to stand at 100°C for hydrothermal reaction for 4 days.
[0033] The reactants were vacuum filtered, dried at 65°C, and calcined at 500°C for 6 hours to obtain a white product of ordered double mesoporous silica material.
[0034] figure 2 , Figure 4 , Figure 5 and Image 6 They are the scanning electron microscope image, X-ray small-angle scattering image, nitrogen adsorption-desorption curve, and pore size distribution curve obtained by the BJH algorithm respe...
Embodiment 3
[0036] Dissolve 7.5g of P123 in 150mL of deionized water at a water bath temperature of 40°C, add phosphoric acid dropwise, adjust the solution to pH=1.8, and continue to stir vigorously for 3.5 hours to obtain a transparent liquid. Add 10.2g of sodium silicate to the liquid, Stir vigorously at 40°C for 24 hours.
[0037] After filtration, the obtained solid was dissolved in 160 mL of 7 mol / L phosphoric acid solution, transferred to a stainless steel reactor with a polytetrafluoroethylene liner, sealed, and allowed to stand at 100°C for hydrothermal reaction for 3 days.
[0038] The reactants were vacuum filtered, dried overnight at 65°C, and calcined at 550°C for 6 hours to obtain a white product of ordered double mesoporous silica material.
[0039] Characterization results: the length of the product is about 17 μm, the degree of order is very high, and it is double-pored, the pore sizes are 2.66nm and 7.8nm, and the specific surface area is 770m 2 / g, the pore volume is 0....
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