Solvent Recovery

A major item of equipment in an extraction process is the solvent-recovery plant which is usually a distillation unit. It is not normally essential to remove all the raffinate from the solvent as this will be recycled through the system. In some processes the more difficult problem will be to remove all the solvent from the raffinate because of the value of the solvent and problems which might arise from contamination of the product.

Distillation may be achieved in three stages:

1. Evaporation, the removal of solvent as a vapour from a solution.

2. Vapour-liquid separation in a column, to separate the lower boiling more volatile component from other less volatile components.

3. Condensation of the vapour, to recover the more volatile solvent fraction.

Evaporation is the removal of solvent from a solution by the application of heat to the solution. A wide

Micro Distillation Column
Fig. 10.28. Diagram of a batch distillation plant with a tray or perforated-plate column.

range of evaporators is available. Some are operated on a batch basis and others continuously. Most industrial evaporators employ tubular heating surfaces. Circulation of the liquid past the heating surfaces may be induced by boiling or by mechanical agitation. In batch distillation (Fig. 10.28) the vapour from the boiler passes up the column and is condensed. Part of the condensate will be returned as the reflux for counter-current contact with the rising vapour in the column. The distillation is continued until a satisfactory recovery of the lower-boiling (more volatile) component(s) has been accomplished. The ratio of condensate returned to the column as reflux to that withdrawn as product is, along with the number of plates or stages in the column, the major method of controlling the product purity. A continuous distillation (Fig. 10.29) is initially begun in a similar way as with a batch distillation, but no condensate is withdrawn initially. There is total reflux of the condensate until ideal operating conditions have been established throughout the column. At this stage the liquid feed is fed into the column at an intermediate level. The more volatile components move upwards as vapour and are condensed, followed by partial reflux of

Vapour

Condenser

Condenser

Cooling water inlet

Vapour

Distillate

Cooling water inlet

Condenser

Cooling water outlet

Tray or perforated -plate

Rectifying-section

Inlet for-mixture

Stripping-section

Distillate

, Distillation column

Vapour

Heating

Heating

Evaporator (re-boiler)

Bottoms product

Fig. 10.29. Diagram of a continuous distillation plant with a tray or perforated-plate column.

the condensate. Meanwhile, the less volatile fractions move down the column to the evaporator (reboiler). At this stage part of the bottoms fraction is continuously withdrawn and part is reboiled and returned to the column.

Counter-current contacting of the vapour and liquid streams is achieved by causing:

(a) vapour to be dispersed in the liquid phase (plate or tray column),

(b) liquid to be dispersed in a continuous vapour phase (packed column).

The plate or tray column consists of a number of distinct chambers separated by perforated plates or trays. The rising vapour bubbles through the liquid which is flowing across each plate, and is dispersed into the liquid from perforations (sieve plates) or bubble caps. The liquid flows across the plates and reaches the reboiler by a series of overflow wiers and down pipes.

A packed tower is filled with a randomly packed material such as rings, saddles, helices, spheres or beads. Their dimensions are approximately one-tenth to one-fiftieth of the diameter of the column and are designed to provide a large surface area for liquid-vapour contacting and high voidage to allow high throughput of liquid and vapour.

The heat input to a distillation column can be considerable. The simplest ways of conserving heat are to preheat the initial feed by a heat exchanger using heat from:

(a) the hot vapours at the top of the column,

(b) heat from the bottoms fraction when it is being removed in a continuous process,

(c) a combination of both.

Since it is beyond the scope of this text to consider the distillation process more fully the reader is therefore directed to Coulson and Richardson (1991).

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