Патент USA US2136966код для вставки
Nov. 15, 1938. A. c. CARUS f MANUFACTURE OF QUINONE ‘ >§§Rs“ ‘Filed Sept. 25, 1956 2,136,966‘; Patented Nov. 15, 1938 2,136,966 - UNITED STATES‘ ‘PATE NT OFFICE 02,136,966 _ ‘MANUFACTURE or QUINONE Alwin C. Cams, La Salle, Ill., assignor to Oarus Gh?mical Company, Inc., avcorporation oi’ Illi no _ Application September 25‘, 1936, Serial No. 102,609 3 Claims. (Cl. 202-46) r.‘E'nis method relates to the manufacture of quinone and other like substances in which the product is distilled from a reaction mass with steam. UK ' ’ The distillation of quinone and other 'or-. ganic bodies by steam distillation has long been practiced, but in the preparation of qui none and certain other organic materials by steam there is a tendency for the quinone to con 10 dense and form a cake in the condenser which eifectively blocks the distillation operation. ture may be such as is obtained by oxidizing aniline with manganese compounds. Distillate passes off through the line It into the condenser 5, the mouth 6 of the line I being within the body of water 1 in the condenser. The water is circulated through the line l2 by the pump I3 into the extraction vessel l5, wherein a layer of solvent is maintained. A cooling coil ['6 may be supplied therein for cooling the solvent. The arrangement shown is for a solvent heavier than 10 It has now been discovered that this di?iculty ‘water, but where a lighter ‘solvent is used the may be overcome providing the concentration of flow may be reversed. The washed water passes through the line I‘! controlled by the valve l8 the quinone in the water condensate is kept be and back to the condenser 55.‘ , 15 low saturation, and preferably well below satura A vacuum is maintained within the condenserv - tion to such an extent that no cake is formed. 5 by the pump Ill, both for the purpose of facili This result may be accomplished by condensing tating the evaporation of quinone in the still and the steam in an excess of water which is con also to cool the water within the condenser by stantly refreshed, followed by subsequent re 20 moval of the quinone from this water'.. From the boiling. The boiled water is condensed within - standpoint of economy, however, it is preferred the re?ux condenser IS. A line 20, controlled by 20 to recirculate the water, and this is particularly ' valve 2|, may lead from the solvent vessel I4 to the condenser tubes and may be employed to true because it is impossible to completely re move the quinone therefrom. Preferably, this wash out the condenser of quinone, if necessary, by circulating some of the washed water there 25 result is accomplished by removing the water through. The valves IB and 2| may be kept before it has become concentrated or saturated with quinone and removing the quinone, or some partially open, if desired, to maintain a higher pressure in the vessel H than in the condenser 5. of it, from the water by contact with a water im This system has the advantage that the solvent miscible quinone solvent, separating the water 30 therefrom and returning it to the condenser. need not be subjected to a high vacuum under .As an example of this invention, quinone is ‘ which it would evaporate and be lost, or would 30 distilled from a reaction mixture by the use of have to be recovered in part through an expen sive recovery system. A low boiling solvent is steam and preferably under a vacuum, for ex 7 ample, such as to produce a temperature of the desirable in the subsequent recovery of the quinone.‘ The chamber 15 may even be under 35 » order of 60 to 80° C. and the distillate condensed in water from which the quinone is removed with pressure if desired. Thus, very low boiling sol a quinone solvent so that the quinone content of the water is kept so low that there will be no blocking of the condenser and no cake will be 40 formed on the pipe leading into the water. This result may be accomplished by discharg ing the quinone vapors beneath a body of water _Which is then circulated rapidly into another chamber and then passing it through or in con~ tact with a solvent, and returned to the con vents may be employed. The water in the condenser 5 should be kept slightly acid to prevent decomposition of qui none. The water may be cooled by vacuum in duced evaporation. ‘ Any water immiscible solvent may be employed, but preferably it should be one having a high 40 vapor pressure'wherever heat or a high vacuum is employed. ' The quinone may then‘ be recovered readily The rapidity of circulation ‘and the volume of from the solvent and the water. Water are, of course, adjusted so that caking is The invention is, of course, applicable to any entirely or substantially prevented. These ad other compound, organic or inorganic, which justments will, of course, also depend upon the _ has a tendency to cake in the condenser, and solubility of quinone in the solvent. 50 which is volatile with steam. densing vessel. ‘ " The invention is illustrated diagrammatically in the drawing, in which i represents a still con- ‘ taining a reaction mixture 2 into which steam 65 may be supplied by the line 3. The reaction mix The foregoing detailed description has been given for clearness of understanding only and no unnecessary limitations should be understood therefrom, but the appended claimsshould be 2 2,136,966 ' construed as broadly as permissible in view of the prior art. I claim: 1. The method of distilling a. quinone which comprises volatllizlng the quinone with steam, condensing the vapors in a body of water in the substantial absence of an organic solvent for the quinone, and continuously extracting the qulnone from the water by circulation of the 10 water through a body of solvent to maintain the’ concentration of the quinone therein at a point so low that it will not form a cake in the con denser. 2. The method as set forth in claim 1, in which the water is cooled by maintenance of a vacuum thereon. 3. The method as set forth in claim 1 in which the quinone is benzoquinone. ' ALWIN' c. CARUS.