Distillation dilute systems

In dilute systems the logarithmic-mean insoluble-gas and nonvolatile-hquid concentrations approach unity, and Eq. (5-261) reduces to the dilute-system formula. For equimolar counter diffusion (e.g., binary distillation), these log-mean factors should be omitted. See Eq. (5-189). 

The equations that express the addition of individual resistances in terms of HTUs, applicable to either distillation and dilute systems or concentrated systems are ... 

It is easy to define the number of transfer units for equimolar counter-diffusion (distillation) and for dilute systems, when the mole fraction of the solute is so small that the... 

The result of a diminution in pressure is frequently that the azeotropic composition becomes richer in the low-boiling constituent. A reduced pressure may thus be reached at which the special point vanishes. As examples, the mixtures ethanol-water and water-phenol may be taken (see Fig. 226). By distilling dilute alcohol at 70 mm, absolute alcohol may be prepared without the use of anentrainer. The azeotropic point water-phenol is eliminated at 32 ram. The shift in the azeotropic point has been determined by Sheinker and Peresleni [45] for two other systems ... 

This equation shows that n for absorption is essentially the n for distillation plus a correction factor. The interfacial mole frac y i can be determined as shown in Figure 16-8B. The integral in Eq. (16-541 can then be determined graphically or numerically. For very dilute systems 1 - y is approximately 1 everywhere in the column. Then the correction factor in Eq. (16-541 will be approximately zero. Thus, n for dilute absorbers reduces to the same formula as for distillation. 

Off-Gas Treatment. Before the advent of the shear, the gases released from the spent fuel were mixed with the entire dissolver off-gas flow. Newer shear designs contain the fission gases and provide the opportunity for more efficient treatment. The gaseous fission products krypton and xenon are chemically inert and are released into the off-gas system as soon as the fuel cladding is breached. Efficient recovery of these isotopes requires capture at the point of release, before dilution with large quantities of air. Two processes have been developed, a cryogenic distillation and a Freon absorption. 

The sulfate ester hydrolysate is stripped to give a mixture of isopropyl alcohol, isopropyl ether, and water overhead, and dilute sulfuric acid bottoms. The overhead is neutralized using sodium hydroxide and refined in a two-column distillation system. Diisopropyl ether is taken overhead in the first, ie, ether, column. This stream is generally recycled to the reactors to produce additional isopropyl alcohol by the following equiUbrium reaction ... 

Extraction. Traditionally tea leaf is extracted with hot water either in columns or ketdes (88,89), although continuous Hquid soHd-type extractors have also been employed. To maintain a relatively low water-to-leaf ratio and achieve full extraction (35—45%), a countercurrent system is commonly used. The volatile aroma components are vacuum-stripped from the extract (90) or steam-distilled from the leaf before extraction (91). The diluted aroma (volatile constituents) is typically concentrated by distillation and retained for davoring products. Technology has been developed to employ enzymatic treatments prior to extraction to increase the yield of soHds (92) and induce cold water solubiUty (93,94). 

The ammonia-water absorption system was extensively used until the fifties when the LiBr-water combination became popular. Figure 11-103 shows a simplified ammonia-water absorption cycle. The refrigerant is ammonia, and the absorbent is dilute aqueous solution of ammonia. Ammonia-water systems differ from water-lithium bromide equipment to accommodate major differences Water (here absorbent) is also volatile, so the regeneration of weak water solution to strong water solution is a fractional distillation. Different refrigerant (ammonia) causes different, much higher pressures about 1100-2100 kPa absolute in condenser. 

Selectivity. The relative separation, or selectivity, Ot of a solvent is the ratio of two components in the extraction-solvent phase divided by the ratio of the same components in the feed-solvent phase. The separation power of a hquid-liquid system is governed by the deviation of Ot from unity, analogous to relative volatility in distillation. A relative separation Ot of 1.0 gives no separation of the components between the two liquid phases. Dilute solute concentrations generally give the highest relative separation factors. 

Methylsulfinyl carbanion (dimsyl ion) is prepared from 0.10 mole of sodium hydride in 50 ml of dimethyl sulfoxide under a nitrogen atmosphere as described in Chapter 10, Section III. The solution is diluted by the addition of 50 ml of dry THF and a small amount (1-10 mg) of triphenylmethane is added to act as an indicator. (The red color produced by triphenylmethyl carbanion is discharged when the dimsylsodium is consumed.) Acetylene (purified as described in Chapter 14, Section I) is introduced into the system with stirring through a gas inlet tube until the formation of sodium acetylide is complete, as indicated by disappearance of the red color. The gas inlet tube is replaced by a dropping funnel and a solution of 0.10 mole of the substrate in 20 ml of dry THF is added with stirring at room temperature over a period of about 1 hour. In the case of ethynylation of carbonyl compounds (given below), the solution is then cautiously treated with 6 g (0.11 mole) of ammonium chloride. The reaction mixture is then diluted with 500 ml of water, and the aqueous solution is extracted three times with 150-ml portions of ether. The ether solution is dried (sodium sulfate), the ether is removed (rotary evaporator), and the residue is fractionally distilled under reduced pressure to yield the ethynyl alcohol. 

Preparation of 2-Bromo-3-Hexyne A solution of 13B g of 3-hexyne-2-ol and 9 g of pyridine in 13B ml of anhydrous ether was treated with 175 g of phosphorus tribromide, added dropwise over a period of about 20 minutes at a temperature of about -10°C. The reaction mixture was permitted to come to room temperature while stirring for about 3 hours, and was then heated to refluxing for about 1 hour. After cooling, the reaction mixture was poured over about 50 g of crushed ice. A two-phase system formed, and the ether layer was separated, washed with dilute sodium bicarbonate solution, dried over anhydrous potassium carbonate and fractionally distilled. The 2-bromo-3-hexyne formed in the reaction was collected at 75°C at the pressure of 50 mm of mercury. 

E.coli recA y.luxCDABE strain were grown for 16-18 hours at 37°C in LB-broth in the presence of 20 pg/ ml of ampicillin. Immediately before the experiment the culture was diluted 1 20 by fresh culture medium and incubated until early log-phase. The grown biomass was mixed with AR solutions in final concentrations of ICfs, ICH n ICfs M, with used for their dilution with distilled water (control) and incubated for 60 minutes. The luminescence intensity of UV-irradiated E.coli recA lux and intact specimens were registered by plate bioluminometer LM OIT (Immimotech, Czech Rep.) in a real time. The number of viable cells was determined from the colony-forming units (CFU) on a surface of a LB-agar after the subsequent incubation within 24 hours at 37 °C. A quantitative estimation of an induction of the SOS-system calculated on formula... 

By contrast with nonazeotropic systems, for azeotropic systems there is a maximum reflux ratio above which the separation deteriorates16. This is because an increase in reflux ratio results in two competing effects. Firstly, as in nonazeotropic distillation, the relative position of the operating surface relative to the equilibrium surface changes to improve the separation. This is countered by a reduction in the entrainer concentration, owing to dilution by the increased reflux, which results in a reduction in the relative volatility between the azeotropic components, leading to a poorer separation16. 

---