US1292676A - Rectifying process and apparatus. - Google Patents

Description

E. A. BARBET.

RECTIFYING PROCESS AND APPARATUS. APPLICATION FILED MAR. 6. 19:4.

1,292,676. Patented Jan. 28,1919.

Fig. 1

4 SHEETS-SHEET I.

Witnesses." I In. nt

Attorney.

E. A. BARBET.

RECTH-"YING PROCESS AND APPARATUS. APPLICATION FILED MAR. 6, 1914.

1 ,292,676. Patented Jan. 28, 1919.

4 SHEETSSHEET,2.

17 3 33; zzl/ i Z 001/ i f L swtorney.

E. A. BARBET.

RECTIFYING PROCESS AND APPARATUS.

APPLICATION FILED MAR. s. 1914.

1 ,292,676. Patented J an. 28, 1919.

Fig.2.

. 4 SHEETS-SHEET 3- Attorney.

me A I E. A. BARBETV RECTIFYING PROCESS AND APPARATUS.

APPLICATIONIILEDMAILG,19H.

Patented Jan. 28,1919.

4 SHEETS-SHEET 4.

srA;-s ATENT orFIoE- e'mm Aucusrm BARBET, or PARIS, FRANCE, ASSIGNOR 'ro socmri: E. BARBIE-T &

FILS & CIE., 0F PARIS, FRANCE.

' :mzorrrrnve rnocnss AND APPARATUS.

I; vTo itma'y concern? I "Beit known that I, EMILE Aueus'rrn BAR- BET,' a citizen of the French Republic, re-

lowing is a specification. w

The present invention relates to an improvedmethod of obtaining alcohol from fermented liquids containing the same, such as wine or from alcohol containing distillates at will, and to an apparatus for use in connection with said method, said method and apparatus operatingwith a maximum economy of steam and producing completely purified alcohols from fermented musts.

In the accompanying drawing, Figures 1 and 1, show a side elevation of a complete apparatus for carrying out' my improved process in which the interior construction of .certain parts is shown diagrammatically.

Fig. 2 shows the apparatus of Figs. 1 and I 1 in the arrangement used for operating on a, which it enters. through phlegms, assubsequently described, parts not operating being eliminated for the sake of clearness. v

Fig. 3 is a vertical section, an

Fig. at is a plan view of a differential steam regulator, which may be employed in connection with the apparatus shown in Figs; 1 and 2.

' Referring to be treated is first heated in a heat exchanger pipe a by the Waste heat from the exhaustlng column m, which enters through pipe a and leaves through pipe (1 and then passes by pipe I), provided with a valve b into the upper part of the preliminary distilling column 0. Steam is admitted by opening the valve 6 into the bottom of the column a. The vapor generator-both by the preheating in a and the heating in c, which liberates the products more volatile than alcohol together with a small amount of the alcohol, then passes. by pipe e into the first rectifier F, containing cooled plates f, and uncooled plates 9. The vaporous products not condensed by the cooled plates f, pass through pipe 71 to a condenser 11- in which they are condensed and the condensate is returned through pipe 6 to the upper part of the first rectifier, the condensed forerunnings being extracted at a 'test gage; The plates f are Figs. 1, 1 and 2, the wine to.

' 0 Specification-of Letters Patent. Patented J an, 28, 1919,

Application filed March 6, 1914. Serial No. 822.953.

maintained at a re ulated temperature, by means ofa cooling uid circulating between these plates and the refrigerator h, flowing to the cooled plates through pipe h and returning through pipe It. If desired the condenser 71 may be omitted, if sufiicient cooling is efl'ected by the cooling plates f. The lower portion of the rectifier is heated by means of steam introduced through valve h and pipe k and controlled by the differential regulator 1' The liquid condensed by the plates flows downwardly through the column and out through the pipe n to the main rectifyin column to be described further on. The llquid from the bottom of the column 0, which still contains the greater portion ofthe alcohol, passes by pipe Z, into the upper part of the exhausting column m, steam being admitted to the bottom of this column by the pipe 0', the vapor from the top of the column passing through the pipe 72, into the main rectifying column, at the point 9, located below the level at which the pipe n enters.

In the main rectifying column Q, the plates 1", in the upper part of the column are cooled by means of a cooling fluid circulating between these plates and the refrigerator s and pipes s and 8 while the lower plates 9, g and g are not cooled. Steam is admitted into the main rectifying column Q, through valve .2 and pipe a and regulated by the differential regulator 7' receiving pressure through pipes r and 1' and additional steam may 'be introduced from 0 through the pipe and valve (1, into the bottom of the column.

The wash from the bottom of the main rectifying column passes through pipe a into the preheater a fdrthe preheating of condensates from various other sources which are introduced to the first rectifying column F through pipe a, at the level 9. The outlet for said wash is through pipe a From a point :0, located near, but not at thetop of the. main rectifyin column Q, where the vapors richest in alco ol exist, the vapors are drawn ofi' to a condenser and cooler y, and from this the purified alcohol is obtained, ready for shipment.

, The other vapors from the top of the main rectifying column pass through pipe t to condenser u, in which they are condensed, the liquid passing through pipe u either to the main rectifying column Q, at a point a short distance above "the level m, or

through the trap o, pipe to to the level 9 of the first rectifier F. In practice I prefer to divide a condensate in the condenser u, andconvey a portion of the same to the first rectifier and another portion to the main rectifier.

The lower plates g and g of the main rectifying column Q, are intended for the removal of the alcohol'from the condensate obtained in the first rectifier F, and also from the refluxes coming from the upper plates 1". There is no necessity of cooling the plates 9 and g;

' The impurities of the tails which are less volatile are in these circumstances retained in the lower portion of the column. The alcoholic degree increases to a maximum under the eifect of'the condensation produced by each plate 0". Finally in the uppermost parts of the column traces of the forerunnings products which may stillbe present, concentrate under the eflect of they redistil- .lations whichare produced on these cooling plates 1*.

i If it is desired to treat condensates from.

distilling columns, generally known in the art as phlegms, connection between the two plate columns 0. and m is closed, by interposing solid disks at the joints e and p. Moreover the steam valves 0 and e are closed and the steam valves d and f are opened phlegm rectifier of the usual kind, which is for greater clearness illustrated in Fig. 2 by eliminating the elements of the apparatus .made idle as above recited.

If it is desired to treat wine directly the converse operations are effected, namely steam is allowed to pass through the joints 0' and p by removing the solid disks, steam valves 0 -and e are opened, (5 and f closed, and h opened and t and r are opened, in order to cause the operation of the difi'ercntial regulators j'and j,1of which the construction and operation will be more fully described hereinafter.

In order to successfully operate, the hourly output for bad tasting products should be the sameas for good tasting products, in the two different manners of operating on these condensates or wines. The internal pressure existing at the plate g of the first rectifier F,

and at theplate I of the main rectifier Q should be constant. This condition will be obtained by "forming upon these plates, the respective pressure outletsfor the two steam regulators (Z and '0. While these two steam iaigulators would be sufiicient for treating column condensates or phlegms only, since The there is only one heating to control, namely for the first rectifier or the main rectifier, the same does not apply when treating wines, because then each apparatus includes two supplies of heating steam. The regulators d and 0 control the steam admission at the bottoms of columns 0 andm. Another means must be provided for controlling the steam inlet at the bottom of g and g, and it must be effected in a manner which will not be dependent upon the continued fluctuations or variations of the operations of regulators d and o. This calls for the addition of two difierential regulatorsj and j, which are alike, and are more fully illustrated in Figs. 3 and 4.

This apparatus comprises two superposed compartments 1 and 2. The lower compartm'ent receives through a pipe 4: the pressure of the base of the apparatus (g for the purifier and g for the rectifier) the upper compartment, instead of communicating with the atmosphere, as do the regulators (l and 0, communicates through a tube 3 with the plate (g or g respectively), that is to say with the columns at the levels which receive the vinous alcoholic vapors of the columns 0 and m where the regulators d and 0 tap the pressure for their operation.

Between 9 and g, (likewise between 9 and 9) there is a difference in pressure of 0.30 meters to 0.40 meters (expressed in values of acolumn of water), due to the mixing of the vapors with the liquid on the suc cessive plates. The necessary difference in pressure between these two levels having been determined once for all, the regulator is set to maintain exactly this difference.

If the pressure increases, for instance, at the plate g, this momentary excess of pressure acts in the upper compartment of j, causesthe level of the water to drop and therefore the float falls, thus opening a little more the steam valve p, and reestablishing to its normal point, .the difference in pressure-between g and g.

Thus any pressure may be obtained for the operation of columns 0 and 121. without any attention to the heating of g and Q2 being required. They are automatically con- 1-15 trolled by the-difi'erentialregnlator which maintains the diflerence in pressure between 9 and g and between 9 and Q constant.

In this regulator, the two compartments 1 and 2, instead of being superposed, may be side by side.

Almost all wine distilling columns effect a certain concentration of their alcoholic distillates. It rarely occurs that condensates are produced below 60 C, and sometimes even 9092 C. are attained. This concentration results in an appreciable decrease of the bad odor of the condensate, discharging the most acrid and' less volatile products, into the distillers wash.

Inwine rectifiers of the kind shownin Figs. 1 and 1, ithas been endeavored. not to produce, at the top of the exhausting column m, any species .turn,-for the following reasons 1. To render the exhaustion more easyand less expensive in steam.

/2. To prevent the formation of malodorous ,thers by the combinationsfof the acids, of

{the wine with alcohol, a 'henomenon which greater the alco- I 'is the'more pronounced. t e holic strength of the wine.

The wine leaving the purifier or prelimi-..

nary distilling column .0 'is' boiling "and is poorer by that quantity of alcoholic vapor which has'passed to the purifier fg and has not reentered the wine but has been conducted'through n to the rectifier.-

The. vapors which are liberated at the top 'of m are therefore relatively poor in alcohol, and consequently rich' in wash odors.

The compound rectifier for wines and con densates which. is shown in Figs. land 1,

I is particularly suitable for the continuous rectification of the inethylic alcohol which is so diflicult to purify.

The apparatus is also applicable to all diificult separations of bodies which boilat different temperatures, and are miscible in all proportions, for instance, for'the rectification of acetonated products of forerun ning, for the separationof sulfuric ether and alcohol, etc.

' The purity of the alcohol depends. above all, upon the efliciency of the plates and,

from this point of view, there is nothing more x v eflicient than -cooled athermanous plates.

elements as liquid.

For treating wines, the apparatus operates well as a direct rectifier; the vapor liberated by the wine permits of the complete utilization of its heat units. in order to boil the liquid on the upper concentrating and rectifying plates; in the majority of the apparatus actually in use, the alcoholic vapor of the wine is condensed with a total loss of heat units and is treated in the subsequent WhatI claim is: a v 1; A process for continuously producing concentrated alcohol from fermented alcoholic'liquids which comprises heating the liquid sufiiciently to drive off the first runnings as vapors and rectifying said first runnings by fractional condensation, heating the liquid 'fromwhich the first runnings have been removed sufficiently .to vaporize all the alcohol contained therein, rectifying. the alcoholic vapors thus produced together with the alcoholic condensate from the rectification of the vaporized first running's, and withdrawing separately the alcohol condensate from the rectification of the combined alcoholic vapors.

'2. A process of continuously obtaining of' alcoholic condensate re-L .column and connect ons fo/r alcohol from a fermented liquid containing the same" which. comprises preliminarily heating the. "liquid, again heating the liquid,

to a temperaturednsuflicient to vaporize more than a small portion of the alcohol contained therein, Withdrawing together the vapors-generated in said two heatings,'fracti-onally condensing said vaporsby cooling and re-heatingand re-condensing the heavier condensates therefrom, exhausting the liquid thus deprived. of its lightervapors by heating thesame, fractionally condensing the vapors produced by said heating by.,coo1;

ing, re-heating and fraction'ally condensing ltherewith the heavier condensate therefrom and re-heating and fractionally condensing the condensate from the first-mentioned fractional condensation, withdrawing the combined alcoholic vapors from the lastmentioned condensation, withdrawing .the

uncondensed vapors, condensing the same and returning at least a portion ofthe condensate for re-heating and condensation to extract'the alcohol contained therein.

3. An apparatus for distilling fermented alcoholic liquids co'inprising a preheater for .said liquid, means for distilling o'fi'='vapors lighter than alcohol from said-liquid', a rectifier for rectifying the vapors tliu's produced and separating alcoholic vapors therefrom,

means for distilling. off alcoholic vapors from the liquid from which lighter vapors have been removed, and rectifying means for rectifying together saidalcoholic vapors. and the alcoholic condensate from the first distillation, and means for independently removing the alcoholic condensate there.- from. 4. An apparatus for distilling fermented musts and the like, comprising a preheater for the liquid, a preliminary distilling column, means for conducting, liquid fromv the preheater to the upper part of said column,

an inlet for conducting heating fluid to the bottom of said column, a first rectifier comprising cooled plates in the upper portion thereof and plates in the lower portion thereof, means for admitting vapors from ling column to the upper portion of said column, of which the plates .in the upper portion are cooled, means for delivering a heating fiuld to the lower endof said main rectifying column, connections for delivering thecondensate from the first rectifier to an intermediateportion of the main rectifying column, at a, P {1t above the bottom of the cooled plates, connections for introduc preliminary distilling column, means for conducting the liquid from the pre-heater to the upper part of said column, and means for introducing a heating liquid to the lower part thereof, a first rectifier, cooling means associated with the upper portion of said 1 rectifier, and heating means associated with ing distilling column,

the lower portion thereof, means for withdrawing vapors from the upper part of said column and introducing them into an intermediate portion of sa1d rectifier, an exhaustand means for conveying the liquid from said preliminary distilling column to the exhausting distilling column, a main rectifying column, means for cooling the upper portions of said main rectifying column, and means for heating the lower portion of said rectifying column, means for introducing the vapors from said exhausting column to an intermediate portion of said main rectifying column, means for introducing the liquid from said'preliminary rectifying column to a level in said main rectifying column above that at which the vapors from said exhausting distilling column are .introduced, an alcohol condenser, and means for conducting alcohol vapors from the upper portion of said main rectifying column thereto, a separate condenser, and means for conducting vapors from the top of said main rectifying column to said separate condenser, and means for re-introducing the condensate therefrom at a level above that at which the alcohol vapors are withdrawn.

6. An apparatus for continuously distilling fermented alcoholic'liquids comprising means for removing the first runnings of head vapors from said liquids and means for fractionally condensing alcoholic vapors the liquid from which the first runnings have been removed to remove the alcohol therefrom as vapor, means for rectifying together the alcoholic condensate from the first runnings and the last mentioned alcoholic vapors, and means for removing separately the rectified alcohol.

7 In an apparatus for continuously producing alcohol from fermented liquids, a distilling column, a rectifying column provided at its lower portion with heating means and at its upper portion with cooling means, a conduit for leading vapors from said distilling column to the rectifying colthe heating point and the point of admission of said vapors. 8. An apparatus ling fermented alcoholic liquids comprising a preheater for said liquids, a distilling column for distilling ofi vapors lighter than alcohol from said liquid, means for introd'ucing steam into said distilling column, a rectifying column provided at its lower portion with means for introducing steam to heat the same, a conduit for leading vapors from said distilling column into the rectifying column at a point above the point of introducing steam and regulators controlled by the pressure at said point of introduction of vapors for determining the admission of. steam to said distilling column and said rectifying column respectively. I

9. An apparatus for continuously distil- -1ing fermented alcoholicliquids comprising a preheater for said liquid, a distilling column for distilling ofi vapors lighter than alcohol from said liquid, a rectifier for rectifying the vapors thus produced and separating alcoholic vapors therefrom, a second distilling column for distilling ofi' alcoholic vapors from the liquid from which lighter vapors have been removed, means for introducing steam into the lower portion thereof for heating the same, and a final rectifying column for rectifying together said alcoholic vapors and the alcoholic condensate from the first distilling column, said final rectifying column being provided. with means for introducing said alcoholic vapors aIt intermediate points thereof, means for introducing steam into said final rectifying column at a lower point in said column, and regulators controlled by the pressure at intermediate points of said final rectifying column for determining the admission of heating steam to the second distilling column for v continuously distiland the final rectifying column respectively.

10. Am apparatus fOr distilling fermented alcoholic liquld-scomprisin a preliminary d1st1ll1ng column for disti ling ofl vapors lighter than alcohol from said liquid, a recfrom sa1d first runnings, means for heating tifier for rectifying the vapors thus produced and separating alcoholic va ors therefrom by condensation, a conduit lieing provided between said distilling column and said rectifying column for conducting the Vapors to the latter, a second distilling column for distilling'ofl alcoholic vapors from the liquid from which the lighter vapors have been removed, a final rectifying column for rectifying together said alcoholic vapors and the alcoholic condensate from the first rectifying column, a conduit being provided between the second distilling column and the final rectifying column for the, passage of the alcoholic vapors and a further conduit between the first rectifying column and the final rectifyingcolumn for passage of the alcoholic condensate, and means for closing 011' the conduits between each distilling column and the corresponding rectifying column, whereby the distilling columns are completely segregated from the system.

11. An apparatus for distilling fermented alcoholic liquids comprising a preliminary distilling column for distillin ofi' vapors lighter than alcohol from said liquid, a recti er for rectifying the vapors thus produced and separating alcoholic vapors therefrom by condensation, a conduit being provided between said distilling column and said rectifying column for conducting the vapors to the latter, a second distilling column for distilling ofi alcoholic vapors from the liquid from which the lighter vapors have been removed, a final rectifying col- 1 umn for rectifying together said alcoholic vapors and the alcoholic condensate from the first rectifying column, a conduit being provided between the second distilling column and the final rectifying column for the passage of the alcoholic vapors and .a further conduit between the first rectifying column and the final rectifying column for passage of the alcoholic condensate, means for closing off the conduits between each distilling column and the corresponding rectifying column, whereby the distilling columns are completely segregated from the system, pipes for supplying steam to each of said distilling columns and rectifying columns, difierential regulators operated by variations in pressure between different points in the rectifying columns to control the'supply of steam to the rectifying columns, regulators, each controlled by the pressure at a. point in one of the rectifying columns, to control the su ply of steam to the distilling columns, an means for cutting out the difierential regulators from the system and causing the other regulators to control the steam supply to the rectifying columns when the distilling columns are se' egated from the system.

n testimony, whereof I afiix my signature in presence of two witnesses.

EMILE AUGUSTIN BARBET.

Witnesses HANSON C. Coxn, RENE Tmnuo'r.

Images