Agitator Evaporator

Evaporator, agitated falling-film, s.s. heat surface area, 3-6 m 0.55... 

Evaporative Process. Two methods of conducting the separation and recycle process have been investigated. According to the first method, the process is arranged in such a manner that only evaporators (agitated, wetted-wall type) are needed for the various separation steps. 

Before withdrawing a sample it is necessary to agitate it, even if it is a gas, and eventually heat the sample being careful to stay below temperatures which could cause evaporation of the lighter components. 

Epichlorohydrin (1 mol) was added dropwise over a period of 1.5 h to a solution of 2.2 mol of sodium acetylide in 1.5 1 of liquid ammonia. During, as well as for a period of 1.5 h after, the addition the temperature of the mixture was kept at about -45°C. The cooling bath was removed after this period and the mixture was agitated vigorously for another 3 h. The thermometer and vent were removed, and 75 g of powdered ammonium chloride v/ere added in 2-g portions with vigorous stirring. The atimonia was allowed to evaporate. 

A mixture of 100 ml of water and 0.10 mol of methylthioallene (see Chapter IV, Exp. 23) was placed in the flask and 24 g of sodium periodate were added in five portions at intervals of 4 min. The mixture was agitated vigorously and the temperature was kept between 25 and 30°C by occasional cooling. After 1 h twenty extractions with 10-ml portions of chloroform were carried out. The combined extracts were dried (without previous washing) over magnesium sulfate. Removal of the chloroform by evaporation in a water-pump vacuum gave the reasonably pure (> 9i%) le... 

Benzoylindoline (223 g, l.Omol) was dissolved in CH2CI2 (2.23 1) and Mn02 (261 g, 3.0 mol. Diamond"Shamrock grade M) was added. The mixture was heated at reflux and agitated for 18 h. The reaction mixture was filtered and the solid washed with hot CH2CI2 (200ml). Evaporation of the solvent left 7-benzoylindole. 

In production, anhydrous formaldehyde is continuously fed to a reactor containing well-agitated inert solvent, especially a hydrocarbon, in which monomer is sparingly soluble. Initiator, especially amine, and chain-transfer agent are also fed to the reactor (5,16,17). The reaction is quite exothermic and polymerisation temperature is maintained below 75°C (typically near 40°C) by evaporation of the solvent. Polymer is not soluble in the solvent and precipitates early in the reaction. 

This procedure may result in a concentration of cumene hydroperoxide of 9—12% in the first reactor, 15—20% in the second, 24—29% in the third, and 32—39% in the fourth. Yields of cumene hydroperoxide may be in the range of 90—95% (18). The total residence time in each reactor is likely to be in the range of 3—6 h. The product is then concentrated by evaporation to 75—85% cumene hydroperoxide. The hydroperoxide is cleaved under acid conditions with agitation in a vessel at 60—100°C. A large number of nonoxidising inorganic acids are usehil for this reaction, eg, sulfur dioxide (19). 

Lime Soda. Process. Lime (CaO) reacts with a dilute (10—14%), hot (100°C) soda ash solution in a series of agitated tanks producing caustic and calcium carbonate. Although dilute alkaH solutions increase the conversion, the reaction does not go to completion and, in practice, only about 90% of the stoichiometric amount of lime is added. In this manner the lime is all converted to calcium carbonate and about 10% of the feed alkaH remains. The resulting slurry is sent to a clarifier where the calcium carbonate is removed, then washed to recover the residual alkaH. The clean calcium carbonate is then calcined to lime and recycled while the dilute caustic—soda ash solution is sent to evaporators and concentrated. The concentration process forces precipitation of the residual sodium carbonate from the caustic solution the ash is then removed by centrifugation and recycled. Caustic soda made by this process is comparable to the current electrolytic diaphragm ceU product. 

Fig. 2. Flow sheet of lecithin producing unit. Crude soybean oil is heated in the preheater, 1, to 80°C, mixed with 2% water in the proportion control unit, 2, and intensively agitated in 3. The mixture goes to a dweUing container, 4, and is then centrifuged after a residence time of 2—5 min. The degummed oil flows without further drying to the storage tanks. The lecithin sludge is dried in the thin-film evaporator, 6, at 100°C and 6 kPa (60 mbar) for 1—2 min and is discharged after cooling to 50—60°C in the cooler, 8. 9 and 10 are the condenser and vacuum pump, respectively.

Purification Processes. Separation of neutral and polar Hpids, so-called deoiling, is the most important fractionation process in lecithin technology (Fig. 3). Lecithin is fluidized by adding 15—30% acetone under intensive agitation with acetone (fluidized lecithin acetone, 1 5) at 5°C. The mixture goes to a separator where it is agitated for 30 minutes. The agitator is then stopped and the lecithin separates. The oil micella is removed and the acetone evaporated. After condensation the acetone is returned into the process. 

Manufacture is either by reaction of molten sodium with methyl alcohol or by the reaction of methyl alcohol with sodium amalgam obtained from the electrolysis of brine in a Castner mercury cell (78). Both these methods produce a solution of sodium methylate in methanol and the product is offered in two forms a 30% solution in methanol, and a soHd, which is a dry, free-flowing white powder obtained by evaporating the methanol. The direct production of dry sodium methylate has been carried out by the introduction of methanol vapors to molten sodium in a heavy duty agitating reactor. The sohd is supphed in polyethylene bags contained in airtight dmms filled in a nitrogen atmosphere. 

FIG. 11-25 Overall heat-transfer coefficients in agitated-film evaporators. 

Economic and process considerations usually dictate that agitated thin-film evaporators be operated in single-effect mode. Veiy high temperature differences can then be used many are heated with Dowtherm or other high-temperature media. This permits achieving reasonable capacities in spite of the relatively low heat-transfer coefficients and the small surface that can be provided in a single tube [to about 20 m" (200 ft")]. The structural need for wall thicknesses of 6 to 13 mm (V4 to V2. in) is a major reason for the relatively low heat-transfer coefficients when evaporating water-like materials. 

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