Azeotrope evaporation

Polyethers such as monensin, lasalocid, salinomycin, and narasin are sold in many countries in crystalline or highly purified forms for incorporation into feeds or sustained-release bolus devices (see Controlled-RELEASE technology). There are also mycelial or biomass products, especially in the United States. The mycelial products are generally prepared by separation of the mycelium and then drying by azeotropic evaporation, fluid-bed driers, continuous tray driers, flash driers, and other types of commercial driers (163). In countries allowing biomass products, crystalline polyethers may be added to increase the potency of the product. 

Since non-bound or non-coordinated nucleophiles are even more reactive, crown-ethers [138] and cryptands (polyaminoethers) [139,140] have been used to chelate the alkali metal cations, notably the potassium ion of K[ F]F. This allows the [ F]fluoride anion to be less tightly paired with the cation and therefore to be more reactive, which has been coined the naked ion effect. In practice, the crown-ether (e.g. 18-crown-6) or better the polyaminoether Kryptofix-222 (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane) is added to the aqueous K[ F]F/K2C03 solution which is then concentrated to dryness [139,140]. The complex (KP FIF-K ) can be further dried, if needed, by one or more cycles of addition of dry acetonitrile and azeotropic evaporation. 

To prevent the nitration reactors from coofing, the reaction should be carried out adiabatically. The process developed by Du Pom uses the heat of reaction for the azeotropic evaporation of benzene and water. Unfortunatdy, this variant is very costly in terms of investments. 

The aeidified sanples vete extracted with ediyl eftier twica The extract was dried by azeotropic evaporation with ethand, HPLC and spectrcxnetric analyses veie performed as rqorted previously (Sok Kim, 1990),... 

The reactor effluent, containing 1—2% hydrazine, ammonia, sodium chloride, and water, is preheated and sent to the ammonia recovery system, which consists of two columns. In the first column, ammonia goes overhead under pressure and recycles to the anhydrous ammonia storage tank. In the second column, some water and final traces of ammonia are removed overhead. The bottoms from this column, consisting of water, sodium chloride, and hydrazine, are sent to an evaporating crystallizer where sodium chloride (and the slight excess of sodium hydroxide) is removed from the system as a soHd. Vapors from the crystallizer flow to the hydrate column where water is removed overhead. The bottom stream from this column is close to the hydrazine—water azeotrope composition. Standard materials of constmction may be used for handling chlorine, caustic, and sodium hypochlorite. For all surfaces in contact with hydrazine, however, the preferred material of constmction is 304 L stainless steel. 

The situation becomes more complicated when the reaction is IdneticaUy controlled and does not come to complete-chemical equilibrium under the conditions of temperature, hquid holdup, and rate of vaporization in the column reactor. Venimadhavan et al. [AIChE J., 40, 1814 (1994)] and Rev [Jnd. Eng. Chem. Res., 33, 2174 (1994)] show that the existence and location of reactive azeotropes is a function of approach to equilibrium as well as the evaporation rate. 

Sodium di(ethylhexyl)sulfosuccinate (Aerosol-OT) [577-11-7] M 444.6. Dissolved in MeOH and inorganic salts which ppted were filtered off. Water was added and the solution was extracted several times with hexane. The residue was evaporated to one fifth its original volume, benzene was added and azeotropic distillation was continued until no water remained. Solvent was then evaporated. The white solid was crushed and dried in vacuum over P2O5 for 48h [El Seoud and Fendler J Chem Soc, Faraday Trans I 71 452 /9751. 

The occurrence of such azeotropes clearly restricts the degree to which aqueous solutions of HX can be concentrated by evaporation. However, they do afford a ready means of obtaining solutions of precisely known concentration in the case of hydrochloric acid, its azeotrope is particularly stable over long periods of time and has found much use in analytical chemistry. 

To a stirred and refluxing solution of 40 parts of benzene and 35 parts of dimethylformamide (both solvents previously dried azeotropically) are added successively 1.6 parts of sodium hydride and 7.7 parts of Ct-(2,4-dichlorophenyl)imidazole-1-ethanol, (coolingon ice is necessary). After the addition is complete, stirring and refluxing is continued for 30 minutes. Then there are added 7.8 parts of 2,6-dichlorobenzyl chloride and the whole is stirred at reflux for another 3 hours. The reaction mixture is poured onto water and the product 1-[2,4-dichloro-/3 (2,6-dichlorobenzyloxy)phenethyl] imidazole, is extracted with benzene. The extract is washed twice with water, dried, filtered and evaporated in vacuo. The bese residue is dissolved in a mixture of acetone and diisopropyl ether and to this solution is added an excess of concentrated nitric acid solution. The precipitated nitrate salt is filtered off and recrystallized from a mixture of methanol and diisopropyl ether, yielding 1-[2,4-dichloro- (2,6-dichlorobenzyl-oxv)phenethyl] imidazole nitrate melting point 179°C. 

The latex can be concentrated by different means. One method consists of heating the latex under vacuum conditions to remove excess water and organic solvent by evaporation. In the case of an organic solvent forming azeotrope with water, the final concentration may be higher and the temperature of the treatment can be reduced. Using the concentrating treatment, the polymer content in the latex can be increased to 70% and the water content can be reduced to 2%. 

A solution of quinoline 1-oxide (0.29 g, 2 mmol) in cyclohexane (1 L) was dehydrated by azeotropic distillation in the reaction vessel. The solution was purged with dry N2 and irradiated with a Hanau high-pressure Hg lamp. The resulting solution was evaporated and the residue was extracted with a little cyclohexane. The insoluble part contained carbostyril (3). The cyclohexane extract was evaporated and the residue purified by short-path distillation at 50°C/0.1 Torr yield 0.174g (60%) moisture-sensitive oil. 

Inasmuch as methyl nitrate is very sensitive to mechanical action, it was found much safer to use it in methanol soln. Such solns, called Myrol, may be obtained directly in the methyl nitrate manufg process, since all that is necessary is to use an excess of methanol. One of the most suitable solns proved to be an azeotropic mixt consisting of about 75% methyl nitrate and 25% methanol. This mixt has a bp of 57.5°. Myrols contg at least 25% methanol will not evaporate to leave 100% methyl nitrate... 

B. 5-Hexynal. To a solution of 5.60 g. (0.050 mole) of 2,3-epoxycyclohexanone in 120 ml. of benzene in a 500-ml. round-bottomed flask is added 10.82 g. (0.051 mole) of trans-1 -amino-2,3 diphenylaziri-dine.2 Initially, after brief swirling at room temperature, the reaction mixture is a colorless, homogeneous solution however it rapidly turns yellow and cloudy due to separation of water. After 2 hours the benzene and water are removed as an azeotrope under reduced pressure on a rotary evaporator with the bath maintained at approximately 30°. The resulting crude mixture of diastereomeric hydrazones weighs 15.4 g. (Note 7) and is subjected directly to the fragmentation reaction (Note 8). 

The limitations of the reaction have not been systematically investigated, but the inherent lability of the aziridines can be expected to become troublesome in the case of epoxyketones which are slow to form hydrazones. The use of acid catalysis is curtailed by the instability of the aziridines, particularly the diphcnylaziridine, in acidic media. Because of their solvolytic lability, the hydrazones are best formed in inert solvents. A procedure proven helpful in some cases is to mix the aziridine and the epoxyketone in anhydrous benzene, and then to remove the benzene on a rotary evaporator at room temperature. Water formed in the reaction is thus removed as the azeotrope. This process is repeated, if necessary, until no carbonyl band remains in the infrared spectrum of the residue. 

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