Method for preparing porous silicon material by using catalytic reaction of silicon and halogenated hydrocarbon
A porous silicon, unreacted technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of high cost, serious pollution, difficult to treat fluorine-containing wastewater, etc., and achieves simple process, clean preparation, and easy scale. The effect of chemical production
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Embodiment 1
[0036] Take 1g of commercial copper powder catalyst and 10g of silicon powder according to the required particle size and mix evenly, fill it in a fixed bed reactor, and pass in methylene chloride for reaction, wherein, the reaction temperature is 300°C, the pressure is 0.2MPa, and the space velocity of methylene chloride 100h -1 , after reacting for 10 hours, cool to room temperature, take out the solid residue, place it in a high-temperature furnace for calcination in air, the calcination temperature is 600°C, and the calcination time is 1 hour. Remove non-silicon impurities, wash twice with distilled water, filter, and dry in a drying oven at 120° C. for 2 hours to obtain a porous silicon material. 50% of the silicon is unreacted and transformed, and the porosity of the porous silicon material is 53% (the calculation method is: porosity=1-bulk density / true density). The gaseous product in the reaction process is condensed into a mixture of organosilicon monomers, which can...
Embodiment 2
[0045] Take 1g of commercial copper powder catalyst and 10g of silicon powder according to the required particle size, mix evenly, fill it in a fixed bed, and pass in methylene chloride for reaction, wherein the reaction temperature is 300°C, the pressure is 0.3MPa, and the space velocity of methylene chloride is 100h -1 , after reacting for 5 hours, cool to room temperature, take out the solid residue, place it in a high-temperature furnace for calcination in air, the calcination temperature is 600°C, and the calcination time is 1 hour. Remove non-silicon impurities, wash twice with distilled water, filter, and dry in a drying oven at 120° C. for 2 hours to obtain a porous silicon material. 60% of the silicon is unreacted and transformed, and the porosity of the porous silicon material is 41%. The pore distribution is measured according to the method of Example 1, and the pore diameter of the porous silicon material is 0.1 micron to 15 micron, mainly concentrated at about 3.3...
Embodiment 3
[0047] Take 1g of commercial copper powder catalyst and 10g of industrially pure raw silicon powder according to the required particle size, mix evenly, pack in a fixed bed, and feed in methylene chloride for reaction, wherein, the reaction temperature is 310°C, the pressure is 0.3MPa, and the air of methylene chloride is speed is 100h -1 , after reacting for 15 hours, cool to room temperature, take out the solid residue, place it in a high-temperature furnace for calcination in air, the calcination temperature is 600°C, and the calcination time is 1 hour. Remove non-silicon impurities, wash twice with distilled water, filter, and dry in a drying oven at 120° C. for 2 hours to obtain a porous silicon material. 10% of the silicon is unreacted and converted, and the porosity of the porous silicon material is 73%. The pore distribution is measured according to the method of Example 1, and the pore diameter of the porous silicon material is 0.01 micron to 8 micron, mainly concent...
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