Variable pressure distillation

A variable pressure oil pump was used in this distillation. Approximately 10 g of a volatile component, consisting mostly of hexamethyl-disiloxane, was obtained at room temperature (15 (in) before the forerun. The forerun contained the desired product and mineral oil from the n-butyllithium solution. The pot residue was about 5 g. The submitters find the disilyl compound thus obtained is contaminated with a trace amount of mineral oil and 4-6% of a vinylsilane, probably 2-methyl-l-trimethylsiloxy-3-trimethylsilyl-2-propene. This impurity becomes quite significant if the reaction medium is less polar than the one described (e.g., too much hexane from n-butyllithium is allowed to remain behind). The spectral properties of the desired product... 

A variable pressure pump is used for the distillation. The forerun consisted of mineral oil contaminant and product. The allylic alcohol is not very stable at room temperature but can be kept indefinitely in the refrig-... 

DISTILLATION. Assume that there are two components, so g = 2, = 2, and S = 1. Both components are found in both phases. There are four variables pressure, temperature, and the concentrations of component A in the liquid and vapor phases (the concentrations of component B are unity less those of component A). If the pressure is fixed, only one variable, e.g., liquid-phase concentration, can be changed independently and temperature and vapor-phase concentration follow. 

Let s consider a simple one-feed two-product distillation column. When examined as stand-alone item with a fixed feed, its control is typically a 5x5 multivariable problem. Among the five controlled variables three are for the basic inventory pressure, level in reflux drum and reboiler. The two remaining are for quality eontrol purity of distillate and bottom products. The five manipulated variables are distillate flow D, bottom product B, boilup V or reboiler duty Qr, condenser duty and reflux flow L. The combination of controlled and manipulated variables may lead to several control structures. Here we present some typical situations useful for dynamic simulation. 

Pressure is often considered the prime distillation control variable, Pressure affects condensation, vaporization, temperatures, compositions, volatilities, and almost any process that takes place in the column. An unsatisfactory pressure control often implies poor column control. Pressure is therefore paired with a manipulated stream that is most effective for providing tight pressure control. When the top product is liquid, this stream is almost always the condensation rate when the top product is vapor, this stream is almost always the top product rate (see Sec. 17.2.). 

If distillation is the choice of separator, then some preliminary selection of the major design variables must be made to allow the design to proceed. The first decision is operating pressure. As pressure is raised,... 

The most common alternative to distillation for the separation of low-molecular-weight materials is absorption. In absorption, a gas mixture is contacted with a liquid solvent which preferentially dissolves one or more components of the gas. Absorption processes often require an extraneous material to be introduced into the process to act as liquid solvent. If it is possible to use the materials already in the process, this should be done in preference to introducing an extraneous material for reasons already discussed. Liquid flow rate, temperature, and pressure are important variables to be set. 

The most common alternative to distillation for the separation of low-molecular-weight materials is absorption. Liquid flow rate, temperature, and pressure are important variables to be set, but no attempts should be made to carry out any optimization at this stage. 

Distillation columns are controlled by hand or automatically. The parameters that must be controlled are (/) the overall mass balance, (2) the overall enthalpy balance, and (J) the column operating pressure. Modem control systems are designed to control both the static and dynamic column and system variables. For an in-depth discussion, see References 101—104. 

Example 3 Calculation of TG Method The TG method will he demonstrated hy using the same example problem that was used above for the approximate methods. The example column was analyzed previously and found to have C -I- 2N + 9 design variables. The specifications to be used in this example were also hstedat that time and included the total number of stages (N = 10), the feed-plate location (M = 5), the reflux temperature (corresponding to saturated liquid), the distillate rate (D = 48.9), and the top vapor rate (V = 175). As before, the pressure is uniform at 827 kPa (120 psia), but a pressure gradient could be easily handled if desired. 

The problem presented to the designer of a gas-absorption unit usually specifies the following quantities (1) gas flow rate (2) gas composition, at least with respect to the component or components to be sorbed (3) operating pressure and allowable pressure drop across the absorber (4) minimum degree of recoverv of one or more solutes and, possibly, (5) the solvent to be employed. Items 3, 4, and 5 may be subject to economic considerations and therefore are sometimes left up to the designer. For determining the number of variables that must be specified in order to fix a unique solution for the design of an absorber one can use the same phase-rule approach described in Sec. 13 for distillation systems. 

While working in a plant, a troubleshooter read a pressure gauge daily for several weeks and only realized it was inaccurate when one day the blower was down. The gauge still read about normal operating pressure. Had this have been a distillation unit, it could have been more serious. In distillation service, pressure is a more important variable than in many other unit operations. Relative volatility is a function of pressure. Pressure, or more accurately delta-P, is the best indication of the tower hydraulics. 

In a 2-1. flask fitted with a total-reflux, variable-take-off distillation head is placed a solution of 53 g. (0.472 mole) of dihydroresorcinol (Note 1), 2.3 g. of -toluenesulfonic acid monohydrate and 250 ml. of absolute ethanol in 900 ml. of benzene. The mixture is heated to boiling and the azeotrope composed of benzene, alcohol, and water is removed at the rate of 100 ml. per hour. When the temperature of the distilling vapor reaches 78° (Note 2), the distillation is stopped and the residual solution is washed with four 100-ml. portions of 10% aqueous sodium hydroxide which have been saturated with sodium chloride. The resulting organic solution is washed with successive 50-ml. portions of water until the aqueous washings are neutral and then concentrated under reduced pressure. The residual liquid is distilled under reduced pressure. The yield of 3-ethoxy-2-cyclohexenone (Note 3), b.p. 66-68.5°/0.4 mm. or 115-121°/11 mm., Mq 1.5015, is 46.6-49.9 g. (70-75%). 

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