US910440A - Process of distilling glycerin. - Google Patents

Process of distilling glycerin. Download PDF

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Publication number
US910440A
US910440A US43640608A US1908436406A US910440A US 910440 A US910440 A US 910440A US 43640608 A US43640608 A US 43640608A US 1908436406 A US1908436406 A US 1908436406A US 910440 A US910440 A US 910440A
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steam
glycerin
condenser
still
distilling
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US43640608A
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Frank J Wood
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Marx & Rawolle
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Marx & Rawolle
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S203/00Distillation: processes, separatory
    • Y10S203/11Batch distillation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Description

F. J. WOOD. PROCESS OF DISTILLING GLYOERIN. APPLICATION FILED JUNE 3,1908.
91 0,440. Patented Jan. 19, 1909.
00L 0 WATER UNITED STATES rarnNT OFFICE.
FRANK J. woon, or NEW YORK, N. Y. Assic'NoR 'ro MARX &'RAW61.ILE, of saw some, Y
. A CORPORATION or NEW YORK.
rnocnss or msrmtme assassin.
Specification of Letters Patent.
Patented Jan. is, 1969.
Application filed. June 3, 1908. Serial No. 430,406. I
To all whom. it. may cmcem:
Be it} known that I, FRANK J. Woon, of New York, in the county of- Kings and State of New York, have invented certain new and useful Improvements in- Processes of Distilling Glycerin; and I do hereby declare the following to be a full, clear, and exact description of the invention, such as will enable others skilled in the art to which it ap ertains to make and use the same.
1y present invention contemplates steps in the process of distillin glycerin consisting of returning to the still part of the steam from which the glycerin vapors have been condensed, condensing the balance of the steam, and introducing a fresh supply of steam into the jet returning to the still, the
- live steam replacing the quantity of steam condensed and filling the additional oflice of maintaining the circulation through the circuit.
The invention relates primarily to the distillation of glycerin containing impurities and fatty acids which emit;v foul odors in vaporizing.
In Letters Patent No. 881,525 issued on my application March 10, 1908, and in an application for patent filed August 13, 1907, I have set forth aprocess, and shown appropriate means, of distilling glycerin having in view a saving inthe consumption of steam necessary to distil a given quantity of glycerin. The idea present in both the patent and application referred to is the multiple effect of a singleste'am supply, that is, conducting a single et of steam successively to a plurality of stills and condensing the glyca erm from each distillation.
The present invention seeks to effect economy of steam, not by conducting the single column to a plurality of stills, but by returning the steam to a single still after the glycerin vapors have been condensed. The presence of the impurities and fatty acids, however, and the objectionable odor which they emit when vaporized, would render it unpracticable to' continue using the same steam in the still as this steam would carry a large portion of these vapors with it, they not being condensed with the glycerin, and this objectionable element'in the steam would obviously be increased as the distilling continued. To avoid this, and atthe same time utilize re eatedly the column of steam, I provide or condensing a portion of the steamcarrying vapors of the fatty acids or other impurities and adding to the circuit a supply of live steam equivalent to the amount condensed.
In the accompanying drawing I have shown in conventional arrangement apparatus appropriate for carrying out the process, the figure being an elevation,- partly in vertical section.
Referring to the drawing, 1 designates the still and 2' the glycerin condenser. '3 is the steam'condenser; 4 the evaporator; 5 the boiler and 6 the vacuum pump. All of these parts are or may be of any preferred construction and the application for patent above referred to shows and describes in detail substantially the same form of still, condensers, etc. The still is shown equipped with an interior annular ledge 7 affording a central passage 8 and having a steam inlet 9 beneaththe ledge and a glycerin inlet 10 above the ledge, the steam and glycerin being designed to enter the still in tangential lines of direction so as to cause them to whirl about and unite, thus eifectively insuring their physical association. The normal level of glycerin in the still is indicated at 12 and the, glycerin is forced by a pump 13 into an initial heater 14 prior to its introduction into the still at 10, a pipe 15 conducting steam to the heater from the boiler.
The glycerin condenser 2 is shown pro' vided with a hot water space 16 through which extend vertical tubes 17 the normal level of the hot Water in this condenser being indicated at 18. A pipe 19 is shown co'n'- necting the still to the glycerin condenser. The condensed glycerin is collected in, and removed from, the receptacle 20 beneath the condenser. From this receptacle a pipe 21 is shown leading to the steam condenser 3, a branch 22 thereof extending into the still. 23 is a steam nozzle leading from pipe 15 and opening into pipe 22.
The steam condenser 3 is, or may be, of substantially the same construction as the glycerin condenser except that it is supplied with cold water as by a pipe 24. From the distillate receptacle 25 in the bottom of the steam condenser a pipe 26 connects the latter to the water space of the evaporator 4 while a pipe 27 connects the steam space of the evaporator with the space above the water level 18 of the glycerin condenser. steam space of the evaporator is also shown in communication with'pipe 15 by a ipe 28, the latter having a throttle or reutting valve 29. This valve reduces the pressure from that of the boiler to about atmospheric as that is suificient for evaporating the sweet .water of low specific gravity as it comes down from the condenser 3.
The pressure in the steam space of the evaporator being about atmospheric the pressure in the hot water condenser 2 will also be about the same, the size of ipe 27 being ample to take all the flow of steam from the condenser without back pressure.
30 is a condenser in communication with the evaporator and having an outlet 31 leading to a sewer.
The vacuum pump 6 is shown in communication with the system for the purpose of reducing the pressure as well understood in the art.
In carrying out the rocess performed by the apparatus describe the steam from the boiler passing through pipes 15 and 23 enters the still and combines with the previously heated glycerin and the combined vapors pass to the glycerin condenser and through the tubes thereof. These tubes are surrounded by a body of hot water which is at a temperature sufficiently high to maintain the steam but low enough to condense the glycerin vapors so that the glycerin accumulates in the receptacle 20 and may be drawn oif. The steam, carrying with it the vapors of the impurities and fatty acids, passes into pipe 21. A portion of this steam will enter the steam condenser 3 through the reduced passage way thereto, while the balance of the steam will pass through pipe 22 and back into the still. Before its entrance into the still, however, this steam encounters the jet of live steam issuing from the nozzle 23 and consequently the steam supply is increased proportionately to the loss itmay have occasioned by the quantity which passes to the steam condenser. Thus the steam jet 23 supplies new steam and prevents the undue accumulation of gases from the impurities-and fatty acids in the glycerin and also maintains the circulation between the still and the glycerin condenser.
The water of condensation collected in the receptacle 25 passes through pipe 26 to the evaporator 4. The steam space of this evaporator which is at about atmospheric pressure is being supplied with live steam through pipe 28 reduced to atmospheric pressure by the throttle valve 29. I provide means for economizing in the amount of steam necessary to furnish "the evaporator by connecting its steam space by pipe 27 with the s ace in the lycerin condenser above the evel of the ot water therein. When the glycerin condenses by passing through the tubes 17 it gives upl so much heat to the water surrounding t ese tubes that this water readily boils and the steam thus generated is available for use in the evaporator or in other ways. from evaporator 4 are condensed at the conoenser 30, the cold water supply pine 24 being shown in communication with both of the condensers 30 and 3. This evaporator is normally operated with a vacuum in the liquor space, established by connection 32, and atmospheric pressure in the steam s ace. I am aware that distilling processes ave heretofore been known in which the fluid mingled with the element distilled is returned to the still and its use repeated. This is true in the distillation of hydrocarbons by the action of air. But to repeat the .use of a steam column in distilling glycerin it is essential that a portion of the steam be removed from the circuit and condensed owing to the accumulating entrainment of impure vapors, as previously expla ned, and also that the volume of the steam column be maintained by adding a quantity equal to that condensed.
I claim as my invention 1. The process of distilling glycerin consisting of supplying to the still a portion of the steam from which the glycerin vapors of aprevious distillation have been condensed, and adding live steam to the steam supply.
2. The process of distilling glycerin consisting of condensing a portion of the steam from which the glycerin va ors of a previous distillation have been con ensed, supplying the balance of the steam to the still, and adding live steam to the steam supply.
3. The process of distilling glycerin consisting of maintainin a circuit for a steam supply between a still and a glycerin condenser, condensing the glycerin vapors while maintaining the steam, condensing a portion of the steam, returning the balance of the steam throu h the circuit into the still, and introducing ive steam into the circuit in the path from the glycerin condenser to the still.
4.. The process of distilling glycerin consisting of condensing a portion of the steam from which the glycerin vapors of a previous distillation have been condensed, sup lyin the balance of the steam to the still an evaporating the water of condensation.
5. The process of distilling glycerin consisting of combining steam and glycerin, condensing the glycerin in a hot water condenser, generating steam by the heat given off by the glycerin in its condensation, maintaining the steam during the condensation of the glycerin, returning a portion of the steam to the still, condensin the balance of the steam and evaporating the water of condensation by the action of the steam generated in the condensation of the lycerin.
6. In a process of distilling glycerin, the steps of condensing the glycerin vapors in a hot water condenserin the presence of a The vapors vacuum, the water space of the condenser specification in the presence of two subscribbeinghunder atmospheric pressure, conductd ing witnesses. ing t e sweet water to an evaporator, an conducting to the steam space of the evap-- v FRANK WOOD 5 orator steam generated in the water space Witnesses:
of the glycerin condenser. GEORGE MAcIN'rosH, J r.,
In testimony whereof, I have signed this JOHN C; SHIELDS.
US43640608A 1908-06-03 1908-06-03 Process of distilling glycerin. Expired - Lifetime US910440A (en)

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