Specification reflux

In the example, the minimum reflux ratio and minimum number of theoretical plates decreased 14- to 33-fold, respectively, when the relative volatiHty increased from 1.1 to 4. Other distillation systems would have different specific reflux ratios and numbers of theoretical plates, but the trend would be the same. As the relative volatiHty approaches unity, distillation separations rapidly become more cosdy in terms of both capital and operating costs. The relative volatiHty can sometimes be improved through the use of an extraneous solvent that modifies the VLE. Binary azeotropic systems are impossible to separate into pure components in a single column, but the azeotrope can often be broken by an extraneous entrainer (see Distillation, A7EOTROPTC AND EXTRACTIVE). 

A number of simulations were carried out for different column configurations (number of stages and feed stage location) and for differing operation specifications (reflux ratio and bottom product rate). Only the specifications and results of our final simulation are reported here. 

Specifically, refluxing OSO4 with concentrated HBr for 2 h gives ... 

Thus the optimal reflux ratio for an appropriately integrated distillation column will be problem-specific and is likely to be quite different from that for a stand-alone column. 

Fractionation. Direct fractionation also can be used to remove dissolved water from LPG. The water-rich overhead vapor from the dryer fractionator is returned to the fractionator as reflux and the water phase is discarded. A dry LPG product that meets either propane or butane water specifications is produced as a ketde product from the fractionator. 

Resoles. Like the novolak processes, a typical resole process consists of reaction, dehydration, and finishing. Phenol and formaldehyde solution are added all at once to the reactor at a molar ratio of formaldehyde to phenol of 1.2—3.0 1. Catalyst is added and the pH is checked and adjusted if necessary. The catalyst concentration can range from 1—5% for NaOH, 3—6% for Ba(OH)2, and 6—12% for hexa. A reaction temperature of 80—95°C is used with vacuum-reflux control. The high concentration of water and lower enthalpy compared to novolaks allows better exotherm control. In the reaction phase, the temperature is held at 80—90°C and vacuum-refluxing lasts from 1—3 h as determined in the development phase. SoHd resins and certain hquid resins are dehydrated as quickly as possible to prevent overreacting or gelation. The end point is found by manual determination of a specific hot-plate gel time, which decreases as the polymerization advances. Automation includes on-line viscosity measurement, gc, and gpc. 

Condenser and eboiler AT. The losses for AT are typically far greater than those for reflux beyond the minimum. The economic optimum for temperature differential is usually under 15°C, in contrast to the values of over 50°C often used in the past. This is probably the biggest opportunity for improvement in the practice of distillation. A specific example is the replacement of direct-fired reboilers with steam (qv) heat. 

Simple analytical methods are available for determining minimum stages and minimum reflux ratio. Although developed for binary mixtures, they can often be applied to multicomponent mixtures if the two key components are used. These are the components between which the specification separation must be made frequendy the heavy key is the component with a maximum allowable composition in the distillate and the light key is the component with a maximum allowable specification in the bottoms. On this basis, minimum stages may be calculated by means of the Fenske relationship (34) ... 

While process design and equipment specification are usually performed prior to the implementation of the process, optimization of operating conditions is carried out monthly, weekly, daily, hourly, or even eveiy minute. Optimization of plant operations determines the set points for each unit at the temperatures, pressures, and flow rates that are the best in some sense. For example, the selection of the percentage of excess air in a process heater is quite critical and involves a balance on the fuel-air ratio to assure complete combustion and at the same time make the maximum use of the Heating potential of the fuel. Typical day-to-day optimization in a plant minimizes steam consumption or cooling water consumption, optimizes the reflux ratio in a distillation column, or allocates raw materials on an economic basis [Latour, Hydro Proc., 58(6), 73, 1979, and Hydro. Proc., 58(7), 219, 1979]. 

Process Unit or Batch Unit A process unit is a collection of processing equipment that can, at least at certain times, be operated in a manner completely independent from the remainder of the plant. A process unit normally provides a specific function in the production of a batch of product . For example, a process unit might be a reactor complete with all associated equipment (jacket, recirculation pump, reflux condenser, and so on). However, each feed preparation tank is usually a separate process unit. With this separation, preparation of the feed for the next batch can be started as soon as the feed tank is emptied for the current batch. 

However, the total number of equilibrium stages N, N/N,n, or the external-reflux ratio can be substituted for one of these three specifications. It should be noted that the feed location is automatically specified as the optimum one this is assumed in the Underwood equations. The assumption of saturated reflux is also inherent in the Fenske and Underwood equations. An important limitation on the Underwood equations is the assumption of constant molar overflow. As discussed by Henley and Seader (op. cit.), this assumption can lead to a prediction of the minimum reflux that is considerably lower than the actual value. No such assumption is inherent in the Fenske equation. An exact calculational technique for minimum reflux is given by Tavana and Hansen [Jnd. E/ig. Chem. Process Des. Dev., 18, 154 (1979)]. A computer program for the FUG method is given by Chang [Hydrocarbon Process., 60(8), 79 (1980)]. The method is best applied to mixtures that form ideal or nearly ideal solutions. 

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. 

When the feed composition oecomes enriched in water, as with Case B, the column profile changes drastically (Fig. 3S2b). At the same reflux and boil-iip, the column no longer meets specifications. The MIPK product is lean in MIPK and too rich in water. The profile now tracks generally up the left side of Region 11. Note also the dramatic change in the temperature profile. A pinched zone still exists... 

Regardless of the procedure used, certain initial steps must be taken for the determination or specification of certain product properties and yields based on the TBP distillation curve of the column feed, method of providing column reflux, column-operating pressure, type of condenser, and type of side-cut strippers ana stripping requirements. These steps are developed and ilhistrated with several detailed examples by Watkins (op. cit.). Only one example, modified from one given by Watkins, is considered briefly here to indicate the approach taken during the initial steps. 

To illustrate the use of these equations, consider a charge of 520 mol of an ethanol-water mixture containing 18 mole percent ethanol to be distilled at 101.3 kPa (1 atm). Vaporization rate is 75 moFh, and the product specification is 80 mole percent ethanol. Let L/V = 0.75, corresponding to a reflux ratio R = 3.0. If the system has seven theo-... 

In Distefano s method, Eqs. (13-149) to (13-161) are solved with an initial condition of total reflux at Lq equal to D R + 1) from the specifications. At t = 0, Lq is reduced so as to begin distillate withdrawal. The computational procedure is then as follows ... 

R = reflux ratio, g reflux/g product Tp = product temperature, °C Tp = saturated-feed temperature, °C Cp = specific heat of solid ciys-tals, cal/(g °C) and X = heat of fusion, cal/g. 

In light ends fractionation it is usually just as important to remove light material from the heavier cut as it is to keep heavy material out of the lighter cut sidestreams are seldom withdrawn. The desired purity (expressed as per cent of impurity) of the overhead and bottoms is determined by product specifications or by the requirements of subsequent processing units. To meet these purity requirements, higher reflux ratios and greater numbers of plates between cuts are required than in crude distillation units. 

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