Extractors

The extractor consists of a glass cylinder A, terminating at the base in the open tube B. Fused within the top of A as shown is another tube C, having a small hole D blow n in the side a fine glass tube leads from the base of C, rises about two-thirds of the height of the cylinder to E, and then returns past F into the open tube B. 

Note. In the older types of Soxhiet extractor, an external tube ran from B up to the top of C for conveying the ascending column of hot vapour. This type had the disadvantage not only of being more easily broken, but also that the condensed liquid in C received very little heat, and therefore the extraction, being carried out by the lukewarm solvent, was usually very slow. 

If the outlet of the siphon tube at the bottom of the Soxhlet apparatus is well plugged with cotton wool so that no finely-divided bariuna hydroxide can pass into the flask, the barium hydroxide may be placed directly into the extractor until the latter is three-quarters full the remaining space is filled with glass wool. 

A continuous ether extractor (see Figs. II, 44, 1-2) gives more satisfactory results. 

A solution of 2,3-dimethylindole (145 g, 1 mol) in dry dioxan containing hydroquinone (100 mg) was treated with JV,JV,JV-trimethylbenzylammonium ethoxide (5 ml of a 40% solution in MeOH) and warmed to 35 C. Freshly distilled acrylonitrile (150 ml, 2.5 mol) was added at a rate such that the temperature did not rise above 40°C. The solution was then stirred overnight and diluted with 10% aq. acetic acid (11). The solution was extracted with CH Clj and the extract was washed with water and dried (MgS04). extract was then mixed with silica gel (800 g) and the solvent removed in vacuo. The silica was placed in a Soxhlet extractor and extracted with cyclohexane. The extract deposited the product as colourless needles (125 g, 63% yield). 

Extra coarse 170-220 Filtration of very coarse materials. Gas dispersion, gas washing, and extractor beds. Support of other filter materials. 

Many continuous extractions involving solid samples are carried out with a Soxhiet extractor (Figure 7.18). The extracting solvent is placed in the lower reservoir and heated to its boiling point. Solvent in the vapor phase moves upward through the tube on the left side of the apparatus to the condenser where it condenses back to the liquid state. The solvent then passes through the sample, which is held in a porous cellulose filter thimble, collecting in the upper reservoir. When the volume of solvent in the upper reservoir reaches the upper bend of the return tube, the solvent and any extracted components are siphoned back to the lower reservoir. Over time, the concentration of the extracted component in the lower reservoir increases. 

Plot of extraction efficiency versus pH of the aqueous phase for the liquid-liquid extractor of the molecular weak acid in Example 7.16. 

In a solid-phase extraction the analytes are first extracted from their solution matrix into a solid adsorbent. After washing to remove impurities, the analytes are removed from the adsorbent with a suitable solvent. Alternatively, the extraction can be carried out using a Soxhlet extractor. 

Several standard methods for the quantitative analysis of food samples are based on measuring the sample s mass following a selective solvent extraction. For example, the crude fat content in chocolate can be determined by extracting with ether for 16 h in a Soxhlet extractor. After the extraction is complete, the ether is allowed to evaporate, and the residue is weighed after drying at 100 °C. This analysis has also been accomplished indirectly by weighing a sample before and after extracting with supercritical GO2. 

A schematic of the MGCC process is shown in Figure 9. The mixed Cg aromatic feed is sent to an extractor (unit A) where it is in contact with HF—BF and hexane. The MX—HF—BF complex is sent to the decomposer (unit B) or the isomerization section (unit D). In the decomposer, BF is stripped and taken overhead from a condensor—separator (unit C), whereas HF in hexane is recycled from the bottom of C. Recovered MX is sent to column E for further purification. The remaining Cg aromatic compounds and hexane are sent to raffinate column E where residual BE and HE are separated, as well as hexane for recycle. Higher boiling materials are rejected in column H, and EB and OX are recovered in columns I and J. The overhead from J is fed to unit K for PX separation. The raffinate or mother Hquor is then recycled for isomerization. 

Fig. 9. Xylenes separation via Mitsubishi Gas—Chemical Co. HF-BF extraction—isomerization process (107). A = extractor B = decomposer C = separator D = isomerization reactor E = heavy ends tower F = raffinate tower G = separator H = light ends fractionator ...

Acrylic Acid Recovery. The process flow sheet (Fig. 3) shows equipment and conditions for the separations step. The acryUc acid is extracted from the absorber effluent with a solvent, such as butyl acetate, xylene, diisobutyl ketone, or mixtures, chosen for high selectivity for acryUc acid and low solubihty for water and by-products. The extraction is performed using 5—10 theoretical stages in a tower or centrifiigal extractor (46,61—65). 

Fig. 38. Caustic purification system a, 50% caustic feed tank b, 50% caustic feed pumps c, caustic feed preheater d, amonia feed pumps e, ammonia feed preheater f, extractor g, trim heater h, ammonia subcooler i, stripper condenser j, anhydrous ammonia storage tank k, primary flash tank 1, evaporator reboiler m, evaporator n, caustic product transfer pumps o, purified caustic product cooler p, purified caustic storage tank q, ammonia stripper r, purified caustic transfer pumps t, overheads condenser u, evaporator v, evaporator vacuum pump w, aqueous storage ammonia tank x, ammonia scmbber y, scmbber condenser 2, ammonia recirculating pump aa, ammonia recycle pump. CW stands for chilled water.

Interfacial Mass-Transfer Coefficients. Whereas equiHbrium relationships are important in determining the ultimate degree of extraction attainable, in practice the rate of extraction is of equal importance. EquiHbrium is approached asymptotically with increasing contact time in a batch extraction. In continuous extractors the approach to equiHbrium is determined primarily by the residence time, defined as the volume of the phase contact region divided by the volume flow rate of the phases. 

There are certain limits to how far b can be increased and d can be reduced however, if the contact time in a weU-mixed extractor can be maintained at several minutes, it can usually be assumed that equiUbrium between the exit phases is attained, justifying the use of the equiUbrium stage concept represented by Figure 1 and equation 1. 

Dual solvent fractional extraction (Fig. 7b) makes use of the selectivity of two solvents (A and B) with respect to consolute components C and D, as defined in equation 7. The two solvents enter the extractor at opposite ends of the cascade and the two consolute components enter at some point within the cascade. Solvent recovery is usually an important feature of dual solvent fractional extraction and provision may also be made for reflux of part of the product streams containing C or D. Simplified graphical and analytical procedures for calculation of stages for dual solvent extraction are available (5) for the cases where is constant and the two solvents A and B are not significantly miscible. In general, the accurate calculation of stages is time-consuming (28) but a computer technique has been developed (56). 

Holdup and Flooding. The volume fraction of the dispersed phase, commonly known as the holdup can be adjusted in a batch extractor by means of the relative volumes of each Hquid phase added. In a continuously operated weU-mixed tank, the holdup is also in proportion to the volume flow rates because the phases become intimately dispersed as soon as they enter the tank. 

The earliest large-scale continuous industrial extraction equipment consisted of mixer—settlers and open-spray columns. The vertical stacking of a series of mixer—settlers was a feature of a patented column in 1935 (96) in which countercurrent flow occurred because of density difference between the phases, avoiding the necessity for interstage pumping. This was a precursor of the agitated column contactors which have been developed and commercialized since the late 1940s. There are several texts (1,2,6,97—98) and reviews (99—100) available that describe the various types of extractors. 

Fig. 10. Economic operating range of extractors. Superscripts a and b are constants.

Eor design of a large-scale commercial extractor, the pilot-scale extractor should be of the same type as that to be used on the large scale. Reflable scale-up for industrial-scale extractors still depends on correlations based on extensive performance data collected from both pilot-scale and large-scale extractors covering a wide range of Hquid systems. Only limited data for a few types of large commercial extractors are available in the Hterature. 

Commercial Extractors. Extractors can be classified according to the methods appHed for interdispersing the phases and producing the countercurrent flow pattern. Eigure 11 summarizes the classification of the principal types of commercial extractors Table 3 summarizes the main characteristics. 

Types of extractor General features Fields of industrial appHcation... 

Fig. 12. Unagitated column extractors (a) spray column (b) packed column and (c) perforated-plate column.

The simple box-type mixer—settler (113) has been used extensively in the UK for the separation and purification of uranium and plutonium (114). In this type of extractor, interstage flow is handled through a partitioned box constmction. Interstage pumping is not needed because the driving force is provided by the density difference between solutions in successive stages (see Plutoniumand plutonium compounds Uraniumand uranium compounds). 

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