Simple Column Design

Simple Distillation. In this category, we include the separation of ideal or slightly non-ideal mixtures that do not form azeotropes, based on the differences in the relative volatilities of components. A simple column designates a device that separates one or several feeds in only two products top distillate and bottoms. Complex columns are can deliver more than two products. In this category we include columns with side-streams, columns equipped with auxiliary devices, as prefractionators, side-strippers and side-rectifiers, as well as thermally integrated columns. 

FIGURE 6 14 Feasible sharp split simple column designs at (a) minimum reflux and (b) above minimum reflux. 

Consider first the design of distillation systems comprising only simple columns. These simple columns employ ... 

It is thus recommended that in a first pass through a design, thermal coupling should not be considered. Rather, simple columns should be used until a first overall design has been established. Only when the full heat-integration context has been understood should thermal coupling be considered. 

Establish simple sequences. Using methods described in Chap. 5, sequences of simple columns with low overall vapor load are established. Consideration should not be restricted to the single sequence with the lowest overall vapor load, since many factors need to be considered in finally arriving at the best design. 

As pointed out in Chap. 5, replacing simple columns by complex columns tends to reduce the vapor (and heat) load but requires more of the heat to be added or removed at extreme levels. This means that the introduction of complex columns in the design might prejudice heat integration opportunities. Thus the introduction of complex distillation arrangements needs to be considered simultaneously with the heat integration. This can be carried out manually with some trial and error or using an automated procedure such as that of Kakhu and Flower. ... 

A more quantitative and lengthy method, but still very useful for checking of the type required here is the Smith-Brinkley method (Reference 5). It uses two sets of separation factors for the top and bottom parts of the column for a fractionator or reboiled absorber and one overall separation factor for a simple absorber. The method is tailor-made for analysis of a column design or a field installed column. The Smith-Brinkley method starts with the column parameters and calculates the resulting product compositions unlike other methods that require knowing the compositions to determine the required reflux. 

It is important to appreciate that, in all aspects of column evaluation and column design in GC, the compressibility of the mobile phase must be taken into account or serious enors will be incurred. Either equation (13) or (15) can be employed but, as already stated, equation (13) is recommended as the more simple to use. 

Finally, the speed of response of the detector sensor and the associated electronics once played an important part in optimum column design. The speed of response, or the overall time constant of the detector and associated electronics, would be particularly important in the analysis of simple mixtures where the analysis time can be extremely short and the elution of each peak extremely rapid. Fortunately, modern LC detector sensors have a very fast response and the associated electronic circuits very small time constants and, thus, the overall time constant of the detector system does not significantly influence column design in contemporary instruments. The instrument constraints are summarized in Table 2... 

Jedrzejewski and Taylor [408] have evaluated microbore pSFC-PB-MS. Microbore separations can take full advantage of the simple DFI design, and are still being pursued. Packed-column SFC-MS was recently reviewed [13]. The two techniques, cSFC and pSFC, are complementary compounds in complex mixtures may be more easily identified with cSFC-MS, while pSFC-MS may be more suitable for target component analysis. 

The curves represent a plot of Log.(/V),(Reduced Plate height)against Log.(v), (Reduced Velocity). The lower the Log.(/7) curve versus the Log.(v) curve the better the column is packed. At low velocities the (B) term dominates and at high velocities the (C) term dominates as in the Van Deemter equation. The best column efficiency is achieved when the minimum is about 2 particle diameters and thus, Log (.ft) Is about 0.35. The minimum value for (H) as predicted by the Van Deemter equation has also been shown to be about two particle diameters. The optimum reduced velocity is in the range of 3 to 5 that is Log.(v ) takes values between 0.3 and 0.5. The Knox equation is a simple and effective method of examining the quality of a given column but, as stated before, is not nearly so useful In column design due to the empirical nature of the constants. 

It is seen that the optimum flow-rate increases rapidly as the separation becomes less difficult and, in fact, there is a flow-rate change that extends over three orders of magnitude. Again the trend in column design becomes more apparent, simple separations are carried out on short, wide columns, packed with relatively large particle and operated at at high flow-rates. 

For single separation duty, Bernot et al. (1991) presented a method to estimate batch sizes, operating times, utility loads, costs, etc. for multicomponent batch distillation. The approach is similar to that of Diwekar et al. (1989) in the sense that a simple short cut technique is used to avoid integration of a full column model. Their simple column model assumes negligible holdup and equimolal overflow. The authors design and, for a predefined reflux or reboil ratio, minimise the total annual cost to produce a number of product fractions of specified purity from a multicomponent mixture. 

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