Preparation method and application of catalyst used in hydrogenation of silicon tetrachloride
A technology of silicon tetrachloride and catalyst, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, silicon organic compounds, etc., can solve the problems of low catalytic efficiency and achieve high catalytic efficiency
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[0011] A preparation method for a catalyst for the hydrogenation of silicon tetrachloride, comprising:
[0012] Mix the pretreated cuprous chloride and silicon powder in a stirred bed reactor, and heat the reaction under hydrogen; the pretreatment refers to adding cuprous chloride to silicon tetrachloride, stirring and heating, and filtering Dry under protective gas.
[0013] The average particle size of the cuprous chloride is preferably 2-7 μm.
[0014] Wherein, the molar ratio of silicon tetrachloride to cuprous chloride is preferably 1:1-2:1. This can not only ensure the sufficient dispersion of cuprous chloride, but also avoid wasting too much silicon tetrachloride and affecting the subsequent treatment.
[0015] Wherein, the stirring and heating in the pretreatment is well known to those skilled in the art. In the present invention, the temperature is preferably controlled at 40-50° C., the stirring speed is 60-300 rpm, and the stirring and heating time is 20-40 minute...
Embodiment 1
[0046] Liquid SiCl 4 CuCl with an average particle size of 2 μm was added into the stirred reactor at a molar ratio of 1:1, and it was heated to 40° C. and fully stirred for 20 minutes. After filtering, the filtered CuCl was heated to 80° C. and dried for 10 min under the condition of blowing nitrogen gas.
[0047] Dried CuCl and metallurgical grade silicon powder (silicon purity: 98%) with an average particle size of 190 μm were added to the stirred bed reactor and mixed, and CuCl accounted for 0.75% of the mass of the silicon powder. The added amount of metal powder aluminum in the stirred bed reactor is 1wt% of CuCl. The above mixture was heated to 280° C. for 50 min under the condition of feeding hydrogen. Prepare copper-silicon alloy catalyst A1.
[0048] SiCl 4 and H 2 After heating to 400°C, it is charged into a gas mixing device with a molar ratio of 1:2 for pre-mixing to form a mixed gas. Add the mixed gas and catalyst A1 into the fluidized bed reactor, keep the...
Embodiment 2
[0053] Liquid SiCl 4 CuCl with an average particle size of 4 μm was added into the stirred reactor at a molar ratio of 1.5:1, and it was heated to 45° C. and fully stirred for 30 minutes. After filtering, the filtered CuCl was heated to 90° C. and dried for 30 minutes under the condition of blowing nitrogen gas.
[0054] Dried CuCl and metallurgical grade silicon powder (silicon purity: 98.5%) with an average particle size of 200 μm were mixed into the stirred bed reactor, and CuCl accounted for 1% of the mass of the silicon powder. The addition amount of metal powder zinc in the stirred bed reactor is 5wt% of CuCl. The above mixture was heated to 350° C. for 70 min under the condition of feeding hydrogen. Prepare copper-silicon alloy catalyst A2.
[0055] SiCl 4 and H 2 After heating to 450°C, it is charged into a gas mixing device with a molar ratio of 1:4 for pre-mixing to form a mixed gas. Add the mixed gas and catalyst A2 into the fluidized bed reactor, keep the rea...
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