Pressure distillation reflux ratio

Vaporizer and condenser pressures Distillation pressures Distillation reflux ratios Evaporator pressures Number of evaporator stages Reactor conversion Recycle flowrates... 

KOH (15 gl 1), and then the supernatant is fractionally distilled (reflux ratio 20 1) in the presence of freshly activated molecular sieves to collect the fraction boiling at 117.2 °C (760mmHg). The fraction collected is further fractionated from sodium metal. All distillations should be carried out under nitrogen. The purified solvent is stored in a sealed reservoir to prevent contamination of C02 and water and dispensed by dry argon or nitrogen pressure. Care should be taken in handling en, because it is toxic. 

Trifluoroethanol [5n] This solvent is strongly acidic and the major impurities are water and trifluoroacetic acid. In its purification, it is dried over potassium carbonate anhydride for a night and then subjected to fractional distillation (reflux ratio 10 1) under atmospheric pressure, the middle fraction being collected. 

Remark 2 The separators are sharp and simple distillation columns (i.e., sharp splits of light and heavy key components without distribution of component in both the distillate and bottoms one feed and two products). The operating conditions of the distillation columns (i.e., pressure, temperature, reflux ratio) are fixed at nominal values. Hence, heat integration options are not considered, and the hot and cold utilities are directly used for heating and cooling requirements, respectively. 

Distillation column with top vapour recompression heat pump The flow diagram of the top vapour recompression scheme is shown in Fig. 2. The top column outlet stream is compressed with compressor to raise its temperature and promoting its energy content to be more usable. When the top column pressure is 21.6 bar, the temperature is increased from 81 to 139.9 C and also the pressure is increased from 21.6 to 52.6 bar. The compressor polytropic efficiency was assumed to be 70%. After the compressor, the heat exchanger allows transfer of the energy of this stream to boil up the bottom column outlet stream. With the same top column pressure and reflux ratio as before, the compressor outlet stream is condensed and cooled to 109.2 C, while the bottom column outlet stream is partially boiled. 

No attempt should be made to optimize pressure, reflux ratio, or feed condition of distillation in the early stages of design. The optimal values almost certainly will change later once heat integration with the overall process is considered. 

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]. 

Example 8 Calculation of Rate-Based Distillation The separation of 655 lb mol/h of a bubble-point mixture of 16 mol % toluene, 9.5 mol % methanol, 53.3 mol % styrene, and 21.2 mol % ethylbenzene is to be earned out in a 9.84-ft diameter sieve-tray column having 40 sieve trays with 2-inch high weirs and on 24-inch tray spacing. The column is equipped with a total condenser and a partial reboiler. The feed wiU enter the column on the 21st tray from the top, where the column pressure will be 93 kPa, The bottom-tray pressure is 101 kPa and the top-tray pressure is 86 kPa. The distillate rate wiU be set at 167 lb mol/h in an attempt to obtain a sharp separation between toluene-methanol, which will tend to accumulate in the distillate, and styrene and ethylbenzene. A reflux ratio of 4.8 wiU be used. Plug flow of vapor and complete mixing of liquid wiU be assumed on each tray. K values will be computed from the UNIFAC activity-coefficient method and the Chan-Fair correlation will be used to estimate mass-transfer coefficients. Predict, with a rate-based model, the separation that will be achieved and back-calciilate from the computed tray compositions, the component vapor-phase Miirphree-tray efficiencies. 

Pj = pure component vapor pressure, mm Hg R = reflux ratio (liquid returned to column)/(distillate drawoff) subscripts indicate number of plates, Rjnin... 

Figure 9-50. HETP and pressure drop data for a typical distillation system. Packing equivalent to X-200 (8 strands), stainless steel. System methylcyclohexane and toluene. Reflux Ratio 100%. Column Diameter 18 inches. Packed Height 5 feet. Used by permission ACS Industries, Inc., Separation Technology Division, Bull. B-129 (1992).

In the distillation column example, the manipulated variables correspond to all the process parameters that affect its dynamic behavior and they are normally set by the operator, for example, reflux ratio, column pressure, feed rate, etc. These variables could be constant or time varying. In both cases however, it is assumed that their values are known precisely. 

It is proposed to use an existing distillation column, which is fitted with a dephlegmator (reflux condenser) which has 200 vertical, 50 mm i.d., tubes, for separating benzene from a mixture of chlorobenzenes. The top product will be 2500 kg/h benzene and the column will operate with a reflux ratio of 3. Check if the tubes are likely to flood. The condenser pressure will be 1 bar. 

To solve Equation 9.50, start by assuming a feed condition such that q can be fixed. Saturated liquid feed (i.e. q = 1) is normally assumed in an initial design as it tends to decrease the minimum reflux ratio relative to a vaporized feed. Liquid feeds are also preferred because the pressure at which the column operates can easily be increased if required by pumping the liquid to a higher pressure. Increasing the pressure of a vapor feed is much more expensive as it requires a compressor rather than a pump. Feeding a subcooled liquid or a superheated vapor brings inefficiency to the separation as the feed material must first return to saturated conditions before it can participate in the distillation process. 

A distillation column uses a partial condenser as shown in Figure 9.19. Assume that the reflux ratio and the overhead product composition and flowrate and the operating pressure are known and that the behavior of the liquid and vapor phases in the column is ideal (i.e. Raoult s Law holds). How can the flowrate and composition of the vapor feed to the condenser and its liquid products be estimated, given the vapor pressure data for the pure components. Set up the equations that need to be solved. 

Example 11.2 Using the Underwood Equations, determine the best distillation sequence, in terms of overall vapor load, to separate the mixture of alkanes in Table 11.2 into relatively pure products. The recoveries are to be assumed to be 100%. Assume the ratio of actual to minimum reflux ratio to be 1.1 and all columns are fed with a saturated liquid. Neglect pressure drop across each column. Relative volatilities can be calculated from the Peng-Robinson Equation of State with interaction parameters assumed to be zero (see Chapter 4). Determine the rank order of the distillation sequences on the basis of total vapor load for ... 

Two heat-sensitive organic liquids of an average molecular mass of 155 kg/kmol are to be separated by vacuum distillation in a 100 mm diameter column packed with 6 mm stoneware Raschig rings. The number of theoretical plates required is 16 and it has been found that the HETP is 150 mm. If the product rate is 5 g/s at a reflux ratio of 8, calculate the pressure in the condenser so that the temperature in the still does not exceed 395 K (equivalent to a pressure of 8 kN/m2). It may be assumed that a = 800 m2/m3, /x = 0.02 mN s/m2, e = 0.72 and that the temperature changes and the correction for liquid flow may be neglected. 

Thermodynamics and mass transfer. Operating pressure, number of plates and reflux ratio in the distillation column temperature profile in the column equilibrium conditions in the reactor... 

Heat Requirement of the Process. Heat is required for vaporization in the extractive distillation column, and for the reconcentration of magnesium nitrate solution. Overall thermal effects caused by the magnesium nitrate cancel out, and the heat demand for the complete process depends on the amount of water being removed, the reflux ratio employed, and the terminal (condenser) conditions in distillation and evaporation. The composition and temperature of the mixed feed to the still influence the relative heat demands of the evaporation and distillation sections. For the concentration of 60 wt% HNO3 to 99.5 wt% HNO3 using a still reflux ratio of 3 1, a still pressure of 760 mm Hg, and an evaporator pressure of 100 mm Hg, the theoretical overall heat requirement is 1,034 kcal/kg HNO3. 

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