US1587188A - Art of distillation - Google Patents

Description

June 1 1926. Y 1,587,188

J. SCHNEIBLE ART 0F DISTILLATIOII Filed'Dec. 27, 1920 5 Sheets-Shut l ART OF DISTILLATION Fed Dec. 27, 1920 www 5 Sheets-Shout 2 June 1 1926. p 1,587,188

J. SCHNEIBLE ART OF DISTILLATION Filed Dec. 27, 1920 5 Sheets-Sheet 3 zan Jane 1 1926. l

J- SCHNElBLE ART 0F DISTILLATION Filed Dec. 27, 1920 5 Sheets-Sheet 4 www.

June 1 1926. 1,587,188

J. SCHNEIBLE ART OF DISTILLATION Filed Dec. 27, 1920 5 Sheets-Sheet 5 ing? drawings, in which:

Patented June l, 1926.

UNITED STATES PATENT orFicE.

JOSEPH BCHNEIBLE, F CHICAGO, ILLINOIS.; BEATRICE SCHNEIBLE-INGBAM, ADMIN- ISTRALRIX OF SAID JOSEPH 'SCHNEIBL DECEASED, ABSIGNOB T0 CLAUDE D. SCHNIBLE, K. F. SCHREEEB, AND BENJAMIN B. SCHNEIDER, AS TRUBTEES UNDER THE NAME OF THE SCHNEIBLE TR'UT.

Am: on msfrrLLA'rIr.

Application led December 27, 1920. Serial No. 435,376.

The present ini-'eution relates to the art of distilling mixed liquids to effect the separation of one or more of the constituents thereof and will be fully understood from the following description, in which a. preferred method of practicing the inventionis set forth and illustrated by the accompanyig. 1 is an elevation, in part diagrammatic, illustrating in assem ly apparatus, for carrying out the invention;

Fig. 2 is a detail sectional view of dephlegmating plates of the distilling column;

Fig. 3 is a detail sectional view of e. half of a liquid collectinv and removing plate for use Within the conlumn;

Fig. 4 is a sectional view through reflux condenser plates of the distilling' column;

Fig. 5 is a sectional view through the head and some of the plates of the preheuter or heat exchanger, and

Fig. 6 is an elevation of a modified form of column, partially broken away.

Referring more particularly to Fig. 1 of the drawing, the numeral 10 indicates a column still, the construction of which is hereinafter described, mounted upon a suitable pedestal 11. The column still is preferablyr formed of sections or units, as-

` sembled in proper order upon the base or pedestal. The lowerinost unit is the collection chamher l2 in which distillation residue collects before withdrawal from the column. Above this is the still chamber or unit 13, which is surmounted by a number of like units, 14,. 14 forming a distilling und aidephlegmating column. At an intermediate point l5, the position of whlch is' determined :is hereinafter set forth, the liquid to be distilled is fed into the column. That portion of the column below the unit 15 muy hr designated as the distilling column, and the portion above as the dephlegmating .i ruloll' unit lli muy likewise be irrrrted :it un intermediate point as hereinafter described. A reflux condensing column li' sui-mounts the dephlegmating column` heinfJ` formed of units or sections 1&2 18 containing coils through which a cooling lurrlilun flows.

From the bonnet 19 of the column still vapors pass through pipe 2O into the dome or bonnet 21 of the condenser 22, cooled as hereinafter described. Condensate passes oli through pipe 23 und meter 24 and uncon clensed vapors are drawn ofi' through pipe 25 h a vacuum pump 26.

Tte residue from the column still passes out through pipe 27 and cooler 27* and is forced by pump 28 through pipe 29 into a preheater 30 at an intermediate point 3l. It travels upwardly through coils in the preheater, passing out at 32 throu h pipe 33 to cooler 34. The liquid to ie treated enters the preheater through pipe 35 and descends therethrough, being heated in the portionfof the preheater below the point 3l at which the residue from the still enters by means of steam admitted through pipe 36 and leaving through pipe 3T. The heated liquid passes from the preheater 30 through ipe 38 to the'column still at the point in icated 15.

In accordance with the present invention the column still is so constructed that the entire internal space thereof above the still or liquid heater pro er is substantially lilled with vapor and is ree from accumulations` of. li uid. rlvhe va )or space of the column may ence be readily saturated, for example, by a relatively immscible constituent of the mixture undergoing distillation and such a constituent may accordingly be separated or returned to the residual liquid, as desired. Thus, if a liquid such as beer or wine be distilled, and the column is so controlled that the constituents parsing olf as vapor contain more than 80% of alcohol, the higher boiling fusel oil, will readily and quickly saturate the internal space of the column with its vapors. Additional fusel oil will then be returned to the residue or may be collected, and removed by proper means, as more particularly hereinafter de. scribed.

A suitable construction of the column in accordance with the invention is illustrated by the detail sectional views in Fi 2, 3 und 4 of the drawings. The unitsl iriniug the dephlegmating column portion of the column still may be constructed as shown in Fig. 2. The units 14 are provided at their 'lected liquid from the column,

u per edges with external coupli flange riiigs 89 which form shoulders agei which the lower ed re of the next rin above rests. Each unit is provided internal y with u. oen trally downwiirdl' inclined baille rin 40 extending inward y from the woll o the unit. A cimcnvocinvex pliite 41 is mounted above the opening;r in each ring 40, upon spiral venes 42, the lower edges of which tit upon und are secured to the upper surfeces of the baille rings. effective in imparting a whirling movement to the va ors, and the siii-luces of the de- Hecting p utes :ind of the biilllc rings do not permit collection or accumulation of con densed liquids.

When it is desired to remove iin immiseible constituent present in a mixed liquid in small proportion, as, for exemple, fiisel oil from beers or wines, a cut-oil unit 16, so constructed as to immediately withdraw colis interposed at ii suitable point in tho colinnn between two of the units or sections 14. Thecollecting unit 16 is provided internally with ii centrally upwardly inclined collectingI ri 43 which extends inwardly and is piovide with nn iipwnrtely pro'ccting ihm e or rim 44 at its inner g w ich exten s slightly beyond the inner ge of the baille ring of the section or unit above. A pipe 45 taps the section 16 to driiin the col ecting ring 44 and carries the collected liquid to the receptacle 4G, in which the linmisciblo constituent (fusel oil, for example) separates from the remainder of the liquid nnd may be withdrawn through valved pipe 47. From the bottom of receptacle 46 it return pipe 48 lends liquid u wardly to a oint somewhat above the ou et pipe 47 an carries it into the unit 16, dischargin it ecntiniiously upon the deilcctor late 1 of the unit below after the proper liquid level has been established in receptacle 46. It is apparent that no accumulation of liquid upon the collecting ring 43 is possible.

In case it is not desired to collect the immiscible constituent a. vnlved lay-pass 49 is provided between the pipes 45 and 48 and valves 50 und 51 are provided in pi es 45 and 48 respectively to close them o when the by-pass is opened. With the b -pam open and valves 50 and 51 closed all iquid caught on collector-ring 43 is immediately discharged upon the next lower dellector lntc. without being permitted to accuiniiliile within the still.

The reflux condenser portion li' of the i-oliiniii still is pieferably mede up of iinit or sections 1S, thc construction of which is preferably ns shown in Fig. 4. These units :irc sich provided externiill `with o. coupling tliinge 52 and internally with iin in- 'iviirdtiv and downwardly inclined baille ring 53, :ibove which is arranged a. series of cir- 'llie venes 42- are of cular coils 54 having an inlet- 55 and outlet 56, both of which pass through suitable glands in .the wall of the iinit. A niiinbcr of depending spiral venes 57 iure seciiiixl to the balo rings 53 (except in the misc of ilic lowermo reflux condenser unit) and hy these vanes a concave-convex defini-.ting philo 58 is suspended iibove the coils of llic next. unit below. The form of the i'lcllccting plates and baille rings prevent iicciiiiiiihitioiis liquid and the spiriil venes 57 impart ii whirling movement to the vapors and liquids. The coils in successive be connected together by bends 59. The units making up the body of the condenser 22 are of similar construction to the units 418 of the iciliix condenser 17.

In Fig. 5 the construction of the units of the prelieating device is shown. Erich unit 60 is provided with o coupling flange 6I, and is provided internally with a downwiirdly and inwardly inclined biillle ring (l2. By means of brackets 63 n distributing philo 64 is supported above erich biilc ring plate 64 being provided with a central conccvo-convex portion 05, n series of openings 66 surrounding the central portion 65 und ii peripheral upturncd flange 67. A coil 68 is disposed in o sones of spiral turns below the portion of the plate 64 eontiiinin f the openings 66, the coils in adjacent unite being connected py the external pipo bends 69 (shown in i .1

In order that the invention may be fully understood, it will be described in detail in connection with' the distillation of a. fermented liquid such iis beer, consis'tii'ur iur 'cl of water and containing 3 to 4% oinlco io which is miscible in all pro ortions with tlic water, and about 0.02% o the higher fermentation prodiiet (fusel oil).

The beer to he treated passes through pipo 35 into the domo of the preheater 30, and travels downwardly therethrough, being heated in the upper portion of the rclieiiter by residue from the still, which is forced upwnrdl through the coils in the prchenter units an out through pipe 33. In the lower units of the preheater steam is used as ii heating medium,\ entering through pipe 36 and leaving through pipe 37. The preheated beer leaves the prelieater through ipe 38 and enters the column still at tie unit marked 15. A

The point of admission of the relicatcd beer und its temperature ure care ully roiitrnllcd in such incliner that. llie operation of thc column is iiot iiccted by its admission. In order to determine the proper point of admission of the beer thc chai'- :iccr of the liquid condensate within thc deplilegmating column is determined iit various points. n nd that point is selected for the admission of thc beer at which tho liquid condensate has substantially the suine iiiiidV units may composition or alcohol concentration as the beer. In general, this point may be determined by temperature and pressure observations, as the temperature at any point within a column constructed in accordance with this invention is substantially' the boiling point of the liquid at that point. The temperature of the preheated beer is brought to substantially the temperature in the colinbefore stated, the operation of the column,

is not affected. The still or heater unit, at the base of the still, is heated by steam entering through pipe 73, its outlet being through pipe 74. In order to maintain the proper conditions within the columnthe admission of steam is controlled to maintain a substantially constant temperature at an intermediate point in the distilling column of the column still above the heater A and above the point at which ebullition occurs, the controlling thermostat being at that Cpoint substantially constantly laved by the escendin liquids in the dephlegmating column. he numeral indicates the line from the thermostat which actuales control device 76 to control the steam admission valve 77. A recording thermometer 78 indicates and records the temperature prevailing at the point of control.

The temperature of the vapors escaping from the top of the column still are maintained constant by suitable control of the flow of cooling medium, for example, cold Water, to the coils of the reflux condenser which forms the top of the column still. This may be effected by controlling the supply valve 78 on the supply line 79 by means of the control device 80, governed by thermostat line 81 runningto the interior of the bonnet 17 of the column. The cooling medium (water) may be supplied directly to the reflux condenser from a suit- 'able source, or it may be forced, for example, by pump 82 upwardly through the coils in alcohol condenser 22, then through line 79 controlled by valve 78 into and downwardly through the coils of the reflux condenser 17, An inverted U-trap 83 in the exit line 82 maintains the liquid level in the cooling coils. The quantity of cooling medium required by the reflux con denser 17 is in excess of that required by the the valve 85 is close alcohol condenser 22, and hence the latter is provided with an ample supply when the feed of cooling medium is controlled in accordance with the requirements of the reflux condenser The vapor passages in the colunln are constructed of ample size to permit the free passage of the ascending vapors, which are concentrated to alcohol (by volume in the condensed liquid) or higher. The fusel oil vapors soon saturate the interior space of the column, and, if not collected by means of the cut-olf plate 16 at a oint in the column where the concentration 1s about 47% alcohol by volume in the condensed liquid, or slightly thereabove as hercinbe' fore described, arc returned lo the residue which leaves the still through pipe 27. The decrease in temperature through the column is regular and uniform and the temperature prevailing at any point therein is substantially the boiling point of the liquid reflux at that point. The proper point lfor the insertion of the cut ofi' plate may hence be readily determined in practice by temperature observations.

The desired absolute pressure throughout the device may be maintained by any suitable means, for example, the exhaust pump 26 connected to the vapor space in the lower portion of the condenser 22. Two lines connecting the pump 26 with the vapor pipe 25 are provided, one, 84, being provided with a valve of ordinary construe tion and the other 86 with a variable pressure check valve 87 by adjusting which the vapor pressure within the system may be readily controlled. In order to bring the system to the desired pressure conditions on starting the valve 85 may be opened, and when the working ressure is established and the valve 87 may be adjusted from time to time to maintain the Working pressure.

The pressure drop or gradient through the column is regular and uniform and is maintained at a point suliciently low to prevent carrying liquid reflux upwards through the column. In general, the operating conditions are so maintained that the pressure drop from the base of the column to the point where the alcohol vapors are removed is not greater than 1% inch of mercury.

To illustrate fhe Working conditions preveiling in the system yduring operation, with an absolute pressure of about 2.7 pounds per square inch at the top of the column and a condensate fromthe condenser 22 of 95% alcohol by volume, the pressure at the bottom of the column 1s 3 lbs. absolute per square inch, the temperature maintained at the still control point 75a is about 600 C., that at the bonnet 19 of the column still is about 39o C. and that prevailing at the point 15 where the beer is introduced iS about 59"C, The beer leaving the preheater is maintained at about this temperature. The pressure at the heater of the still is abolut 3.1 lhs. absolute pressure per square inc i.

In Figure 6 I have shown a modified form of construction of a column still in accordance with my invention, wherein means are provided in a single column for the production, rectitioation and withdrawal of the desired products of fractional distillation. In that figure, numeral 91 indicates a heater unit, through which the heating medium, such as steam, is supplied through pipe 92 and from which the heating medium is Withdrawn through pipe 93. Below the heater unit 91 is provided a unit 94 in which the residue of the distillation operation collects and from which it is withdrawn through pipe 95. 'lhe heater unit 91 is surmounted by a number of dephlegmating units 14 forming a distilling column 96 and a dephlegmating column 97. Between the distilling column 96 and the dephlegmatin polumn 9T a feed unit 15 is interpose into which fresh liquid is supplied through pipe 98. The fresh liquid is preheated in accordancewith the foregoing description of my process to a temperature substantially the same as the temperature within the column at the point at which it is supplied, this point being that at which the reflux liquid within the column has approximately the same composition as the fresh liquid supplied. At an intermediate point in the dephlegmating column 97, above the feed unit 15, a cubed plate 16 may be interposed. The liquid collected in this plate is immediately withdrawn through pipe 99 into the receptacle 100, where a separation of any immiscible constituent may take place. lhe separated immiscible constituent may be removed through discharge pipe 101 and the remaining liquid returned through pipe 102 to the cut-oft' unit. A by-pass 103 is provided between the pipes 99 and 102 for use in case it is not desired to effect the separation of an immiscible constituent.

Above the dephlegmating section 97 is a reflux condenser section 104, made up of reflux condenser plates 18, 18. At the top ol' the reflux condenser section is a cut-oli' unit 105, of construction similar to that of cut-olf unit 16, and the liquid collected therein is drained off through pipe 106 and cooling coil 10T to a suitable receptacle (not shown). Above the cut-olf plate 105 are placed a series of reflux condenser plates 18, 18, forming a rectifyng section 108, at the lop of which a cut-off plate 109 is inserted and the liquid collected there may be withdrawn through pipe 110 and cooling coil 111 to a suitable receptacle (not shown). Above the cut-olf unit 109 an additional rectifying condenser 108 may be placed, if

desired. The column is surmounted by a dome 112, which is provided with a vapor outlet 113, to which may be applied an exhaust pump, if desired.

A. cooling medium is supplied through pipe 114 to the upermost unit of the rectifying section 108, and descends through the coils therein, leaving through pipe 114. A cooling medium is likewise supplied through pipe 120a to the uppermost unit of the rectifying condenser 108, and descends through the coils in the units of the rectif ing and relluxing sections 108 and 104 to tie lowermoet unit thereof, out of which it passes through the inverted U-shaped pipe or trap 116,' the highest point ot' which is slightly above the uppermost cooling coil in the top unit of the rectifying section 108 of the column. A full column of cooling liquid in the coils is thereby assured.

'lhe supply of heat-infr medium to the heater unit 91 is controlled by means of vulve 117 and control device 118 to produce a constant temperature at a point in the distilling section 96 of the column below the point of introduction of fresh liquid as described in connection with the form of construction of Fig. 1. The supply of cooling medium to the rectifying and reflux condenser sections cf the column are, controlled by valve 120 and control device 121 to produce a constant temperature of the vapors in the column at the unit 105 Where rectified liquid is withdrawn therefrom.

In operating the column, for example, for the distillation of beer or Wine, the fresh beer is introduced into the column through pipe 98 at the feed unit 15 and descends through the distilling section 96 together with relluxed liquid. The vapors ascend through the column, in which, as has been` hereinbefore stated, no accumulation of refluxing liquid is permitted. If it is desired to remove fusel oil, this may be accomplished by means of the cut-off unit 16 as described in connection with the form of construction shown in Figure 1. The operation of the reflux condenser section 104 is controlled to produce a temperature in the column at the cut-off plate 105, such that the liquid collected there is alcohol of the desired concentration, for example, 190 proof. This control is effected by means of the control device 121, as above described. The liquid withdrawn at the unit 105 is substantially pure, being rectified by the action of the rectifying section 108 superposed upon it. If it is desired to recover the heads or lower boiling point products, this mayY be effected by means of the cut-off unit 109, by means of which the heads may be Withdrawn, having been previously rectified in the column. At the cut-olf plates 105`and 109 the liquids are withdrawn at substantially their boiling points and are consequently herein described in detail, results in aY marked uniformity of operation of the column, there being a very regular drop in temperature and also a very regular decrease in pressure throughout the column. The operating conditions are so controlled that this drop in pressure is not sufficient to cause liquid reflux to be carried through the column, and is preferably maintained below ythree-fourths of an inch between the cut-oil' plate 105 and the heater unit.

The specillc details of operation and construction which have been set forth are not intended to be rfgarded as limitations upon the scope of the invention except in so far as included in the accompanying claims.

I claim:

l. In a distilling apparatus, a unitary column construction comprising superposed heating, distilling and reflux condensing sections, means for supplying a heating inedium to the heater section, means for supplying a cooling medium to the reflux condensing section, means for regulating the supply of heating medium to the heater section by means of temperature indications in the distilling section, and means for regulating the supply of cooling medium to the reflux condensing section by the temperature ol the vapors issuing therefrom.

2. In a distilling apparatus, a unitary column construction comprising superposed heating, distilling and reflux condensing sections, means for supplying a heating medium to the heater section, means for supplying a cooling medium to the reflux condensing section, and means :for regulating the supply of heating medium to the heater section by means of temperature indications in the distilling section.

3. In a distilling apparatus, a unitary column construction comprising superposed heating, distilling and reflux condensing sections, means for supplying a heating-medium to the heater section, means for supplying a cooling medium to the reflux condensing section, means for regulating the supply of heating medium to the heater section by means of temperature indications in the distilling section, and means for controlling the pressure of exhaust of uncondensed gases from said column.

4. In a distilling apparatus, a unitary col umn construction comprising superposed heating, distilling, dephlegmating and reflux condensing sections, means for supplying a heating medium to the heating section thereof', means for controlling the supply of cooling medium to the reflux condensing section bri the temperature of vapors issuing therefrom, and means for controlling the pressure of exhaust of vapors from the column.

5. In a distilling apparatus, a unitary column construction comprising superposed heating, distilling, dephlegmaiing und reflux condensing sections, means for supplying a heating medium to the heating section, means for supplying a cooling medium to the reflux condensing section, means for controlling the supply of heating medium to the heating section by temperature indications in the distilling section, means for controlling the supply ol cooling,r medium to the reflux condensing section by the te1nperature of the vapors issuing therefrom, and means for regulating tlie'pressure of exhaust of uncondensed vapors from the colA umn.

6. In a distilling apparatus, a unitary col umn construction comprising superposed heating, distilling and reflux condensing sections, said sections being constructed to provide a continuous, uninterrupted vapor passage, means for supplying a heating ine dium to the heater section, means for supplying a cooling medium to the reflux condensing section, means ior regulating the supply of heating medium to the heater section by means of' temperature indications in the distilling section, and means for regulating the supply of cooling medium to the reflux condensing section by the temperature of the vapors issuing therefrom.

"7. In ia distilling apparatus, a unitary column construction comprising superposed heating, distilling and reflux condensing sections, said sections being constructed to proY vide a continuous, uninterrupted vapor passage, means for supplying a heating medium to the heater section, means for supplying a cooling medium to the reflux condensing Section, and means for regulating the, supply of heating medium to the heater section by means of temperature indications in the distilling section.

8. In a distilling apparatus, a unitary column construction comprising superposed heatinlg, distilling land;` reflux condensing sections, said sections being constructed to provide a continuous, uninterrupted vapor passage, means for supplying a heating medium to the heater section, means for supplying a cooling medium to the reflux condensing section, means for regulating the supply of heating medium to the heater section by means of temperature indications in the distilling section, and means for controlling the pressure of exhaust of uncondensed gases from said column.

9. In a distilling apparatus, a unitary column construction comprising superimposed heating, distilling, dephlegmating and reflux condensing sections, said sections being constructed to provide a continuous, uninterrupted vapor passage, means for supplying a heating medium to the heating section thereof, means for controlling the supply of cooling medium to the reflux condensing section by the temperature of vapors issuingr therefrom, and means for controlling the pressure of exhaust of vapors from the column.

l0. In a distilling apparatus, a unitary column construction comprising superposed heating, distilling, dephlegmating and reflux condensing sections, said sections being constructed to provide a continuous, uninterrupted vapor passa'ge, means for supplying a heating medium to the heating action, means for supplying a cooling medium to the refiux condensing suction, means for controlling the supply of heating medium to the heating section by temperature indications in the distilling section, means for controlling the supply of cooling medium to the reflux condensing seetion by the temperature of the vapors issuing therefrom, and means for regulating the pressure of exhaust of uncondensed vapors from the column.

11. In a dlstilling apparatus, a unitary column construction comprising superposed heating, distilling and reflux condensing sections, said sections being constructed to provide a continuous uninterrupted vapor passage, means for supplying a heating medium to the heating section, means for supplying cooling medium to the refiux condensing section and means for imparting rotating motion to the vapors in said vapor passage.

12. In a distilling apparatus, a unitary column construction comprising superposed heating, distiiling and reflux condensing sections, said sections being constructed to provide a continuous uninterrupted vapor passage, means for supplying a heating medium to the heating section, lneans for supplying cooling medium to the reflux condensing section and means for imparting rotating motion to the vapors in said vapor passage, means for regulating the supply of heating medium to the heating section by temperature indications in the distilling section, and means for controlling the supply of cooling medium to the reflux condensing section by the temperature of vapors issuing therefrom.

13. In a distilling apparatus, a unitary column construction comprising superposed heating, distilling, dephlegmating and reflux condensing sections, said sectlons being constructed to form a continuous, uninterrupted vapor passage through the column, means for producing a gradual temperature decrease from the heating section through the reflux condensing section of the column, and means for withdrawing reflux from said column without interrupting the vapor passage therethrough. 14. In a distilling apparatus, a unitary column construction comprising superposed heating, distilling, dephlegmating and reflux condensing sections, said sections being constructed to form a continuous, uninterrupted vapor passage through the column, means for supplying a heating medium to the heating section, means for supplying a cooling medium to the reflux condensing section, means for controlling the supply of heating medium to the heating section by temperature indications in the distilling section, means for controlling the supply of cooling medium to the reliux condensing section by the temperature of the vapors issuing therefrom, and means for withdrawing reflux from said column without obstructing the vapor passage therethrough.

15. In a distilling apparatus, a unitary column construction comprising superposed heating, distilling, dephlegmating and refiux condensing sections, means for supplying heating medium to the heating section, means for supplying a cooling medium to the reflux condensing section, means for controlling the supply of heating medium to the heating section by temperature indications 'in the distillin section, means for controlling the suppy of cooling medium to the reflux condensing section by the temperature of vapors issuing therefrom, means for feedin fresh liquid into the column at a point 1n the column where the composition of refluxed condensate has approximately the same composition as the fresh liquid, and melans -for withdrawing residue from the sti l.

16. In a distilling apparatus, a unitary column construction comprising superposed heating, distilling, dephlegmating and reflux condensing sections, means for supplying heating medium to the heating section, means for supplying a cooling medium to the reflux condensing section, means for controlling the supply of heating medium to the heating section by temperature indications in the distilling section, means for controlling the supply of cooling medium to the reflux condensing section by the temperature of the vapors issuing therefrom, means for preheating fresh li uid, means for introducing the preheated (lresh liquid into the column at a point Where the refluxed condensate has ap roximately the same composition as the resh liquid, and means for withdrawing residue from the heating section.`

17. In a distilling apparatus, a unitary column construction comprising superposed heating, distilling, dcphlegmating reflux condensing and rectifying sections, means for supplying cooling medium to the reflux condensing and rectifyingr sections, means for controlling the supply of cooling medium thereto by the temperature at the top of' the reflux condensing section, and means for withdrawing from the top of the rei'lux condensing section condensate formed in 4the rectif ing section.

18. In a istilling apparatus, a unitary column construction com rising superposed heating, distilling, dep legmating, reflux condensing and rectifying sections, said sections being constructed,to form an uninterrupted va or passage tl'irough the Leoluinn, means or supplyino` a cooling medium to the rectifying and retux condeiisinry sections, means for controlling the supp of cooling medium by the temperature o the vapors at the top of the refiux condensing section, and means for withdrawing'condensiitc formed in the rectifying section from, the top of the reflux condensing scction without interrupting the vapor .passage through the column.

19. In a distilling apparatus, a unitary column construction com rising superposed heating, distilling, dep legniating, reflux condensing and rectifying sections, said sec tions being constructed to rovide an uninterrupted vapor passage t rough the column, means tor supplying cooling medium to the reflux condensing section, means for controlling said supply of cooling medium by the temperature of the vapors of the top ol the reflux condensing section, means for controllingr the pressure of exhaust of uncondenserl ases from the column, and means for witdrawing from the top of the reflux condensing section liquid condensate formed in the rectifying section.

20. In a distilling apparatus, a unitary column construction comprising a superposed heating, distilling, dephlcgmating, retlux condcnsingand rectifying sections, said sections being constructed to provide an uninterrupted vapor passage throughthe column, means for supplying a heating medium to the heating section, means for controlling said supply of heating medium by tempera.- turc indications in the distilling Section, means for supplying cooling medium t0 the reflux condensing section, means for controlling said supply of cooling medium by the temperature of vapors at the to of the reflux condensing section, means or controlling the pressure of uncondensed-gases exhausted from the column, and means for withdrawing from the top of the reux minimiser liquid condensate formed in the rectify-'ing section without interrupting the riipor passage throuph the column.

2l. ln rombination, a column still, the inlornnl construction of which is such as to provide :in uninterrupted vapor assage thrrcllirougli. means for supplying iieating mediums only to lhe base of the column, niciins t'or supplying u cooling medium in the upper part of the column, means for controlling the pressure of uncondensed ,Jusos exhausted from the column and means l'nr controlling the heating and cooling meerature conditions within the the pressure drop in the coldiums by tem still to contro 'umn still.

22. In combination, a distilling system including a unitary column construction comprising superposed heating, distilling, dephlegmating and reflux condensing sections, means for supplying a heating medium to the heating section, means for supplying a cooling medium to the reflux condi-using section, means for exhausting uncomlensed ras and vapor from the system and ineensiol` controllin, the pressure drop in tho column including means for controlling the suppl)r of heating medium to the heating: section and of cooling medium to the rcllux condensing section by temperature indications within the column.

23: In n. clist-illing apparatus, a unitary column construction comprising supcrposiu! heatin'g, distilling, de hleginating und reflux condensing sections, t ie construction of sniil sections being such as to provide ii continu ous va or passage through the c olunin, means or supplying a heating medium to the heating section, means for supplying :i cooling medium to the reflux condensingr section, means fr controlling the prvssnw of exhaust of uncondensed vapors from thc column, and means for controlling the pressure drop in the column to produce u pres` sure drop of not over three-fourths inch between the heating section und thc top of the redux-condensing section, said means including means for controlling the supply ol heatin medium to the heating section and of coong medium to the reflux condensing section by temperature indications within the column.

24. In a distilling apparatus, a unitary column construction comprising superposeil heating, distilling, dephlegmating and rcflux condensing sections, a condenser for condensing vapors issuing from the reflux condensing section,mcans for controlling the pressure of uncondensed vapors issuing from the condenser, and means for controlling pressure drop within the column structure comprising means to control the temperature conditions therein.

25. The process of continuously distilling 'ailiqilid mixture which comprises heatingr a liquid mixture, conducting the evolvcil vapors in a continuous rising body, coolingr the rising vupor body to condense fractions thereof, cxhauslin'g unroinlcnsed gases from the rising viipor body, controlling the pri s sure of unconilcnscd gases exhausted from the Column of vapor and controlling the pressure drop in the va )or holly hycontrolling the icating of tlic liquid ini\turc und the cooling of the vapor body.

26. The process of continuously distilliiig a liquid iiiixtuie which coiiipi'iscs heating a liquid mixture, conducting the evolved lll) vapors in a continuous rising body, cooling the rising body to condense fractions thereof, removing condensed fractions of desired compositions Without interrupting the continuity of the vapor body, exhausting uncondensed gases from the column of vnpor, controlling the pressure of uncondensod gases exhausted from the column of vapor and producing T1 predeter'mined pressure drop in the vapor body by controlling the heating of the liquid mixture and the cooling of the vapor body.

27. The p'roeesss of continuously distilling a liquid mixture which com rises heating a liquid mixture, conducting t e evolved "er pors in a continuously rising body and impurting a rotating motion thereto, cooling the rising vapor body to condense fractions thereof, exhausting uncondensed gases from the column of vapor, controlling the pressure of uncondensed gases exhausted from the column of vapor, and controlling the pressure dro in the va or body by' controlling the heating of t e liquid mixture and the coolingy of the vapor body.

28. The process of continuously distilling u liquid mixture which Acomprises heatin a liquid mixture, conducting the evolve vapors in a continuous rising body, cooling the rising vapor body to condense fractions thereof, withdrawing and condensing vapors from the column of rising vapor maintaining a controlled exhaust pressure on the uucondensed gases, and controlling the ressurc drop in the vapor body by controllim.'` the heating of the liquidv mixture and the coolinv' of the vapor body.

29. he process of continuously distilling a liquid mixture which comprises heating n liquid mixture, condueting the evolved vapors in a continuous risnghbody and im parting a rotating motion t ereto, cooling the rising va or body to condense fractions thereof, with rawing and condensing vapors from the column of rising vapor, maintaining a controlled exhaust pressure on uncondensed gases, and controlling the res sure drop on the vapor body by contro ing the heating of the liquid mixture in the cooling of the vapor h ody.

JOSEPH SOHN EIBLE.

vapors in a continuous rising body, cooling the rising body to condense fractions thereof, removing condensed fractionsl ot' desired compositions without interrupting the continuity of the Vapor body, exhausting uncondensed gases from the column of vapor, controlling the pressure of uncondenscd gases exhausted i'roln the column of vapor and producing predetermined pressure drop in the vapor body by controlling the heating of the liquid mixture and the cooling of the vapor body.

27. The processs of continuously distilling a liquid mixture which comprises heating a liquid mixture, conducting the evolved vapors in a continuously rising body and imparting a rotating motion thereto, cooling the rising vapor body to condense fractions thereof, exhausting uncondensed gases from the column of vapor, controlling the pressure of uncondensed gases exhausted from the column of vapor, and controlling the pressure drop in the vapor body by controlling the eating of the liquid mixture and the cooling of the vapor body.

28. The process of continuously distilling a liquid mixture which comprises heating a liquid mixture, conducting the evolved vapors in a continuous rising body, cooling the rising vapor body to condense fractions thereof, withdrawing and condensing vapors from the column of rising vapor maintaining a controlled exhaust pressure on the uncondensed gases, and controlling the pressure drop in the vapor body by controlling the heating of the liquid mixture and the cooling of the vapor body.

29. The process of continuously distilling a liquid mixture which comprises heating a liquid mixture, conducting the evolved vapors in a continuous rising body and iinparting a rotating motion thereto, cooling the rising vapor body to condense fractions thereof, withdrawing and condensing vapors from the column of rising vapor, maintaining a controlled exhaust pressure on uneondensecl gases, and controlling the pressure drop on the vapor body by controllingr the heating of the liquid mixture in the cooling of the vapor body.

JOSEPH SCHNEIBLE.

Certiicate of Correction.

It is hereby certied that in Letters Patent No. 1,587,188, granted June 1, 1926, upon the application of Jose h Schneible, of Chicago, Illinois, for an improvement in The Art of Distillation, errors ap) grant and in the heading to the printe ear requiring correction as follows: In the specification, asslgnment, name of secondmentioned assignee, for K. F. Schrerer read K. F. Schreier, as shown by the records ofy assignments in this office; and that the said Letters Patent should be read with these corrections therein that the same may conform to the record oi the case in the Patent Office.

Signed and sealed this 17th day of August, A. 1926.

[SEAL] M. J. MOORE, Acting Uowwmasz'mwr of Patents; n

Certificate of Correction.

It is hereby certified that in Letters Patent No. 1,587,188, granted June l, 1926, upon the application of Jose h Schneible, of Chicago, Illinois, for an improvement in The Art of Dstillation, errors appear requiring correction as follows.: In the grant and in the heading to the printed specification, assignment, name of secondmentioned assignee, for K. F. Schrerer read K. F Schreier, as shown by the records ofV assignments in this oHice; and that the said Letters Patent should be read with these corrections therein that the same may conform to the record of the case in the Patent Office.

Signed and sealed this 17th day of August, A. D. 1926.

[SEAL] M. J. MOORE,

Acting Comissoner of Patents.

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