Patent US2. 61. 01. Extractive distillation process. Sept. DROUT, JR EXTRACTIVE DISTILLATION PROCESS Filed April 1, 1. LLAno. N. J.,asslgnor to Standard 0. Development Company, a corpo- . This application is a . Patent application Serial. No. In particular the invention . It is another object of this invention to provide a novel and improved process for thepnrifica'tion of alcohols, particularly alcohols of . In'each of the . above mentioned applications the appropriate solvent suitable for the separation, e. Howeverrtheprocess . The invention is particularly applicable tothose distillations where the overheadseparates into two . The non- solvent phase of the distillateisextracted with theisolven- t and theresultinglextract isrefluxed torthe extractive distillationxcolumn. Jtds an : obiectcf this inventionzthereforeto atoms produced by the reaction of mono- olefins, by removing therefrom impurities both water- : soluble . I Theserand other objects of . Henetofore, isuchalcohols were obtained only in very poor yields and'at high cost by repeated reprovide a process for the purification of organic fractionations of partially refined alcohols. Traces of sulfur 1 compounds, boiling over a wide range up to 2 vol. Vialine Jean Paul, 34, married a. Now the full shameful weight of U.S./elite. Via Line is a food supplement that helps reduce weight through suppressing the appetite. Ngo agriculturalproduction: weather,sosandcroos vanKeuenandJ. Modelling o agriculturalproduction: weather,soilsandcrops H.vanKeulenandJ.Wolf. Promotes weight loss With anti-stress function Helps improve emotional well-being Up to 6 cm loss on thigh area Optimized Assimilation technology 30-pc lozenges per box. B. Operation at elevated temperature and pressure greatly broadens the solubility range of secondary butanol and secondary amyl alcohol. For example, at 1. C. Secondary amyl alcohol is completely miscible with water. Another method of' enhancing the solubility of secondary butanol and sec- pentanol is the addition of low molecular weight'oxygenated compounds, such as low molecular weight therefrom by decantation. The latest Tweets from VIA Line (@VIALineRedGold). Via Line is a revolution in weight loss strategy: it is 100% natural! Flickr photos, groups, and tags related to the 'Herbert Vogel' Flickr tag. Additional polymer oil impurity, particularly a portion of the higher boiling fractions thereof, concentrates in the column at a point near the alcohol feed plate upon contact of the crude alcohol feed with the internal aqueous reflux. This concentration of polymer oil occurs near the alcohol feed plate; A stream containing the polymer concentrate is removed from theldistillation column at this point and the polymer. In this manner practically all the odor- producing con- ,taminants are removed from the alcohol. The dilute aqueous alcohol product obtained as botalcohols. In the case of sec- pentanol, acetone may be employed as a solubilizer. The distillation tower is operated without the conventional external reflux of part or all of the total distillate condensate. Instead the column distillate is condensed and the non- solvent phase of the distillate is extracted with the extractive distillation toms from the distillation zone and containing between - 9. The product is far superior in odor to any alcohol obtained by any of the purification - methods known to the art. December 3. 1, 1. As described in said application with reference to alcohol purification optimum quality alcohol can be obtained by operating the extractive distillation column with no external reflux. However, if the number of plates in the extractive distillation column is small enough so that excessive alcohol loss from the top of the column occurs then the selective reflux principle of this invention is recommended. This selective reflux is obtained in the case of alcohol purification by water extratcing the non- aqueous phase of the condensed distillate and refluxing the re sulting extract in whole or in part to the extractive distillation zone. The feed line i is locatedat: a point preferablyk above the midsection . BOth plate in a : 4. Water is fed to the tower in considerable amounts through line 3. The water is fed to the top or near the top of the tower but always above the alcohol feed plate. To obtain the desired separation of the impurities from the alcohol, themixtureis' subjected- to a continuous fractional distillation in column 2; The'water introduced in sufficiently large quantity at the upperp'art of thetower effectively modifies the relative volatilities of the organic compounds being separated, and distillation : of. For contimious eflicient operation, the water must be added continuously . The .: feed stream may he preheated to a temperature close to that of the internal liquid reflux under equilibrium boiling conditions at . Fat Burner; Appetite Suppressant; Metabolism Booster; Draining; Joint Pain; Natural. Make up; Nail Care; Skin Care; Face care; Eye care; Lip care; Hair. Saffron Extract Benefits: 6 Reasons Why Dr. The preheated alcohol feed stream may be liquid, partially vaporized or completely vaporized when introduced into the fractionation column. Vapors of the organic compounds introduced as a feed stream pass upwardly through the distillation zone in contact with descending internal liquid reflux under equilibrium reboiling and refluxing conditions. Due to the fact that water, considerably in excess of the amount of water distilled, iszintroduced to mix with the condensate near theitop ofithe distillation . Jthe. Contrasted therewith in normal rectification of al cohols from an aqueous yfeed, thewater concention diminishes rapidly toward the limiting water concentration - of- the aqueous azeotropes in the vapors ascending the distillation; column. With adequate water concentration in the internal reflux for effecting the separation, the alcohol to be isolatedfiin the aqueous bottoms is dissolved in the aqueous internal reflux that reaches the bottom of the distillation column. Inthe decanterthe condensate separates into two phases, namely, an aqueous- phase 1 and an organic phase 6. The organic phase is'lead via line t to an extraction zone!) entering at a pointatthe midsectionthereof. In the extraction zone the organic phase is countercurrently extracted with water entering at a point- near the top of the extraction zone via line I0. In the extraction zone the materials separate into a raflinate phase consisting of hydrocarbons . This- phase is withdrawn via line H. The aqueousextract phase is withdrawn via line 1. It. It is alsowpossibleito return the reflux in whole 0 inlpartxthroughsolvent'ffeed line. IB. In this event the solvent feediline 3. It : should 'bep bo'rne in mind that in 'somedistillations, for example; in which ahydrocarbonsolvent is employed as an extractive distillation solvent the upper phase would be the solvent phase while the lower phase would be the non- solvent phase. In any event it is the non- solvent phase of the condensated distillate which is extracted in the extraction zone whichiis returned tothe distillation zone as reflux. This alcohol is recovered by extraction of the overhead organic phaseand isreturned tothe distillation zone togetherwith the aqueous phase of the condensed distillate. A sidestream containing this polymer oil concentrate is removed from the column and the polymer . This 'sidestream l. SI'Bl'Il. OVBd from the column at a point below the crude alcohol feed plate, but preferably at a point immediately below the alcoholieedplate. This stream is withdrawn at a point near the alcohol feedplate or slightly belowthe alcohol feed plate; In the decanter the stream separates into an upper polymer oil phase 2. The latter is returned to the tower via- line 3. Part of the aqueous bottoms is withdrawn from line l. SI for heating by indirect or direct heat exchange with a heating medium such as live steam, and returned via line 3. In column IS the aqueous alcohol is concentrated to the desired level up to the 9. The remaining propyl oil,'if any, contained in the aqueous alcohol is removed from the concentrating column in a 'sidestream I! Some remaining traces of light material, if any, and alcohol are removed overhead via line 1. If desired, this overhead may be recycled to the feed to the extractive distillation zone. Part of the condensate may be refluxed to the top of the column via line 2. Excess Water may be removed from the system via line 2. Although the dilute aqueous alcohol solution from the distillation zone has been described as concentrated by fractional distillation, other means of concentration may be employed, such as solvent extraction. For obtaining satisfactory results on a practical scale the preferred range is 8. I Under steady conditions in the extractive distillation zone, the internal reflux, having adequate water concentration for accomplishing the separation of the wide- boiling impurities, tends to have a nearly constant water concentration in a preferably homogeneous liquid phase at each plate, and the high water concentration is approximately uniform in the internal reflux below the alcohol feed plate. This internal reflux in flowing from the top to the bottom of tower becomes richer in the alcohol while the other impurities of the feed become distilled overhead. In the distillation process the mol per cent water in the total overhead from the extractive distillation column will vary with the operating conditions and with the nature of the. The aqueous bottoms removed from the extractive distillation zone will contain approximately 7. The overhead from the extractive distillation zone upon condensation and cooling separates into two phases, . An Engler distillation of a typical organic phase, resulting from the purification of isopropanol reveals that the initial boiling point lies between not- A portion 4. It is evident from the results obtained that the'water employed within the limits specified, increases the efiective vapor pressures of the impurities relative to the vapor pressure of the alcohol being purified, thus allowing the impurities to pass overhead from the distillation zone. Although it is preferable not to have any plates in the tower above the water feed plate, it is possible to carry out the separation with a limited number of plates above the water feed plate. However, this number should be held to a minimum. In this regard the impurities are removed in a' manner similar to that described for the isopropanol system. The following are approximate typical compositions of some of the crude aqueous alcohols which may be treated according to this purification process: CRUDE ETHYL Ancorron 8. B. 2. 5- 5 weight per cent colloidal carbon CRUDE SECONDARY BUTYL ALCOHOL 7. Balance water and other impurities CRUDE SECONDARY AMYL ALCOHOL- S 5. For- secondaryamyl alcoholssufiicientqwater.
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