Method of making a trihalosilane
a trihalosilane and trihalosilane technology, applied in the field of trihalosilane making, can solve the problems of limited methods and direct cost addition to these processes, and achieve the effect of less energy and more economical methods
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example 1
[0051]Re on carbon. In a flow reactor, about 0.6 g of catalyst, comprising 5.9% (w / w) Re on carbon, were loaded into a glass tube. Activation of the catalyst was performed with 10 sccm H2 at 450° C. for about 15 hours. The temperature of the reactor was decreased to 200° C. and the reaction was started by passing H2 through the MeSiCl3 bubbler. Samples were taken from the reaction stream and injected into a GC for analysis using an online switching valve. The reaction was run while varying the following conditions: reaction temperature, flow rate of hydrogen, and MeSiCl3 bubbler temperature. The catalyst activation and reaction were done without applying back pressure to the system. HSiCl3 was produced at the conditions and yield listed in Table 2 below.
[0052]
TABLE 2HSiCl3 production with Re on carbon.BubblerHSiCl3Temp.TimeH2CH3SiCl3TempYield(° C.)(min)(sccm)(sccm)(° C.)(%)500155102.128.32.4500300101.114.04.1500342100.50.26.0500390100.2−15.29.7500429300.5−14.75.6
example 2
[0053]Re and Pd on carbon. About 0.5 grams of catalyst, comprising 7.5% (w / w) Re and 0.2% (w / w) Pd both on carbon, were loaded into a flow reactor. The catalyst was treated with 20 sccm H2 flow at 500° C. for about 3 hours. After catalyst treatment, the temperature of the reactor was decreased to 300° C., and H2 and methyltrichlorosilane were introduced into the reactor tube by first passing the H2 through a bubbler containing methyltrichlorosilane and then into the reactor tube. The reaction temperature, pressure, flow rates, and flow ratios were varied to determine their affect on trihalosilane yield. Samples were periodically taken from the product stream and analyzed by GC. The analysis results and conditions are listed in Table 3.
[0054]
TABLE 3HSiCl3 production with Re—Pd on carbon.BubblerHSiCl3Temp.TimeH2CH3SiCl3PTempYield(° C.)(min)(sccm)(sccm)(psig)(° C.)(%)500108100.81.10.611.4600146100.81.11.516.5700187100.810.423.8700224100.31−15.434.2700270200.21.1−31.442.0700305100.136.5...
example 3
[0055]Re and Pd on carbon. In a flow reactor, about 0.5 g of catalyst, comprising 8.1% (w / w) Re and 1.0% (w / w) Pd both on carbon, were loaded into a glass tube. Activation of the catalyst was performed with 10 sccm H2 at 450° C. for about 15 hours. The temperature of the reactor was decreased to 400° C. and the reaction was started by passing H2 through a MeSiCl3 bubbler. Samples were taken from the reaction stream and injected into a GC for analysis using an online switching valve. The reaction was run while varying the following conditions: reaction temperature, flow rate of hydrogen, and MeSiCl3 bubbler temperature. The catalyst activation and reaction were done without applying back pressure to the system. HSiCl3 was produced at the conditions listed in Table 4 below.
[0056]
TABLE 4HSiCl3 production with Re and Pd on carbon supported catalyst.BubblerHSiCl3Temp.TimeH2CH3SiCl3TempYield(° C.)(min)(sccm)(sccm)(° C.)(%)50047102.126.16.560086102.227.08.6700121102.327.617.3700164100.98.0...
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