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The yields of the methyl trifluoroacetate product observed in this present work were less than those obtained in other batch autoclave works, which employed only 4 ml of liquid phase, compared with 50 ml in this study. Furthermore, an encouraging initial product formation rate of ca. 40 mol/m3 h, quickly decreased after the first hour, and came to an apparent end after only 2 h. This observation had not been reported previously.
Work performed in a semi-continuous porous tube reactor (300 ml of re-circulating liquid phase) also showed the same reaction characteristics as in the batch reactor. Thus, the deteriorating product formation rate cannot be attributed to gaseous reactant depletion (batch operation). The results suggest problems associated with catalyst instabilities, e.g. with the previously elucidated Wacker chemistry. 相似文献
Control of the process and selection of process conditions require knowledge of the temperatures within the die. Temperature gradients exist because of the high heating rate and because of variations of density and electrical resistivity of the medium due to the presence of the part. Direct measurement of temperature with thermocouples or other conventional means is impractical because of the high temperatures, high currents, and high pressures that are involved. Therefore, a computer model was developed to predict temperature as a function of time and applied voltage for any location in the die. The computer model is composed of three parts: a geometrical model to approximate the density and resistivity variations in the medium, a finite-element model to calculate the rate of resistive heating within each element, and a finite-difference model to calculate the temperature distribution based on solution of the heat-transfer equations. Predicted temperatures have been shown to be in excellent agreement with measurements, and numerical simulation provided encouraging consistency and reasonably accurate predictions of temperature profiles within the die. The model demonstrated the feasibility of a new process to achieve simultaneous application of pressure and heat to powder densification in Electroconsolidation. 相似文献