US1452617A - Process of and apparatus for distilling liquids - Google Patents
Process of and apparatus for distilling liquids Download PDFInfo
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- US1452617A US1452617A US450998A US45099821A US1452617A US 1452617 A US1452617 A US 1452617A US 450998 A US450998 A US 450998A US 45099821 A US45099821 A US 45099821A US 1452617 A US1452617 A US 1452617A
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- vapors
- condenser
- glycerine
- water
- still
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D19/00—Recovery of glycerol from a saponification liquor
Definitions
- This invention is an operating device for use in connection with means for imparting 1 movement to a sliding sash.
- M improvement is directed, more particularl y, to the member for effecting the man- 2 ual operation of the sash adjuster, and to the means whereby said member is mounted for service within the car body.
- the object is to provide an operating member which is not affected by the jar and vibration inherent in the movement of the vehicle, and the parts of which operating member are interchangeable with corresponding parts of similar operating members, which interchangeability of parts enables the operating member to be assembled and mounted with ease and facility.
- my invention embodies a base member provided with a bearing and with an o ening for the reception of a reliaft actuator having a handle and a bushing unitary one with the other, said bushing being provided with an annular groove and being mounted for free rotative' movement within said bearing, a retainer 4 occu ying the opening to the base member and fittin in the groove for precluding endwise disp acement of said bushing, and a collar fitted to the base member in co-operative relation to the retainer so as to confine 4 it in the opening and prevent displacement under the jar or vibration of the vehicle and to prevent said retainer from dropping out of osition by the operation of the device.
- F lgure 3 is an elevation of the base member detached
- I Figure 4 is a detail perspective view of one form of retainer.
- the base member A is a single piece provided with a boss (5 extending outwardly from the face plate a. Said member is adapted for fixed attachment to the car body interiorly thereof, and to this end, the face plate 1s provided with a desired number of apertures I) through which screws 6 pass so as to be embedded in the car body, see F igure 1.
- the boss of said base member is externally threaded for a part of its length, as at a, and said boss is provided also with an opening d extending through said male threaded part 0, said opening being shown in the form of a slot, see Figures 2 and 3.
- the base member A is a fixed part of the operating device, and the boss a serves as a hearing within which is rotatably mounted a member of the shaft actuator.
- Said shaft actuator comprises a bushing B and a crank handle C, the same being of umtary construction by casting said parts in one piece or by uniting the bushing and the crank handle in fixed permanent relation.
- the bushing is provided with an axial opening e of angular or square form in cross section, the external diameter of said bushing corresponding substantially to the internal diameter of the boss a, whereby the ly within the boss so as to substantially pre dlude all lost motion or idle play while at the same time the bushing is free to rotate within the boss.
- the length of the bushing is equal substantially to the thickness of the face plate and the length of the boss, whereby in assem bling the shaft actuator relatively to the base member the face of the crank handle is in abutting relation to the end of the boss, whereas the inner end face of the bushing is flush, or substantially so, with the inner face of the face plate, see Figure 1.
- My invention relates to a process of, and.
- y invention may be considered as in some respects an improvement upon that disclosed in Patent #774171 ranted November 8, 1904, to William E. (xarrigues, in which is disclosed a process of distilling liq- I uids such as glycerine in which the water vapors carried over with the distilling liquid in a previous distillation are re-evaporatedi at less than atmospheric pressure.
- the steam so produced is superheated by transfer of heat thereto from the vapors of the distilling liquid, this latter. being condensed at least in part as it gives up steam, and the steam is mjected into the body of liquid to be distilled to aid in the evaporation of the liquid in the still.
- I can control the amount its heat to the of glycerine which it is possible to obtain in the form of dynamite grade glycerine, by Sub ectmg the uncondensed glycerine vapors and water vapors mixed therewith, to a cool-' ing medium at a stage of the recess subsequent to that in. which the gl pors pass through the superheater condenser and thereafter condensing the remaining va-' pors at a dili'erent point, to form the sweet water which is then progressed to the evaporator in a continuous rocess.
- Fig. 1 represents. a diagrammatic 'sidefelevation of thee paratus' included in my invention and used or pra'ctising my improved process certain parts being shown in section, and
- P ig. 2 is ;a similar view of a portion of the apparatus, on
- the still 1 5f. any suitable form contains the raw product .such as crude g1 cerine which may be antomatically fed into the still as required. It may be heated by any suitable means such as the steam coil 2 raw liquid. The still may additionallybe heated by any external source of heat in the usual manner.
- the raw product such as crude g1 cerine which may be antomatically fed into the still as required. It may be heated by any suitable means such as the steam coil 2 raw liquid. The still may additionallybe heated by any external source of heat in the usual manner.
- a pipe 3 to carry the superheated steam or vapors'which areto be n ected into the raw material in the artly immersed in the still to aid the distillation of the same.
- a spider 4 At the'lower end of pipe 3, there is preferably rovided a spider 4 provided with a numher of perforations or openings throu h which the superheated vapors pass into t e crude liquid.
- a lurality of s ider arms are provided whiclgare prefera 1 closed at the ends but may be left open if esired.
- the water vapors produced in evaporator 5 pass upwardly by pipe 6 into the superheater condenser 7 which may be rovided with a series of tubes 8 and b heater condenser there is a transfer of heat from the vapors of the distilling liquid which pass upwardly from still 1 through pipe 10, to the water vapors which have entered the superheater condenser from pipe 6.
- the water vapors may pass through the tubes 8 and the vapors of the distilling liquid pass around the tubes 8 or vice versa.
- the water vapors pass through the tubes 8 while the vapors of the distilling liquid pass around the tubes.
- the water vapors are considerably cooler than the vapors of the distilling liquid as will be explained more full hereinafter. Accordingly the vapors of t e distilling liquid are partly condensed and the .Water vapors are superheated. These superheated water vapors pass out of the superheater condenser by pipe connection 11 which carries the same into-the still, the superheated water vapors then continuing downwardly through the pipe connection 3 to a point near the bottom of the crude liquid in the still.
- the ta or receiver 12 is connected by pipe connection 13 to the bottom of the superheater condenser 7.
- a pipe connection 14 extends upwardly from receiver 12 and connects with the upper portion of a. condenser 15 which I term a cooler condenser, which is connected at the bottom by pipe 16 with its receiver 17.
- a pipe connection 18 extends upwardly from receiver 17 to a connection shown at 19 with a third condenser 20 which latter is connected at the bottom by pipe 21 with a receiver 22.
- Receiver 22 is connected at the bottom by pipe 23 with the evaporator 5.
- a concentrator 24 is adapted to receive distillates collected in receivers 12 and 17. These receivers may be connected by couplings 25 and 26, with the pipe 27' leadmg to the concentrator as shown.
- concentrator 24 per portion of concentrator 24 is shown as connected'by pipe 28 with the connection 19 leading into the upper portion of condenser 20.
- a vacuum pump 29 is connected I receiver 22 which latter is connected by.
- the evaporator 5 is heated by suitable means, such for example as the coil 31 shown as mounted within the same. This coil may be heated by the passage therethrough of exhaust steam from the coil 2 within still 1, the exhaust end of coil 2 being connected to the entrance end of coil 31 by pipe connection 32. Evaporator 5, mi ht, of course, be heated by any other suitab e means such for example as steam supplied directly from a boiler or b the exhaust steam from the pump 29. ith the construction shown in the drawings, the coil 2 in the still may contain condensed water at its lower end. If that is so this water is under high pressure until it passes the throttle valve 33 which is located between the outlet of coil 2 and the inlet of coil 31. After the water condensed in the still coil passes throttle valve 33 the water is under less pressure and a part of the same flashes into steam which is available for heater purposes in the evaporator.
- suitable means such for example as the coil 31 shown as mounted within the same. This coil may be heated by the passage therethrough of exhaust steam from the coil 2 within still 1,
- the crude glycerine is fed au tomatica ly into the still to which external heat is preferably applied.
- Air is now exhausted from the entire apparatus by means I of vacuum pump 29.
- Evaporator 5 contains water or is filled with so-called sweet water from a previous distillation. As stated, this is heated. by any suitable means, preferably by the submerged coil 31.- Under the reduced pressure existing in the apparatus the sweet water in the evaporator boils easily and the vapor passes out throu h pipe 6 into the superheated condenser 7.
- the baflle plates 9 being preferably provided to cause the vapors to follow a circuitous path as they pass around the condenser tubes.
- the sweet water vapors-act as a condensing medium and a part of the glycerine will accordingly be condensed in the superheater condenser 7.
- the amount of glycerine so condensed is controlled by the amount of the comparatively cool 'vapors rising from the evaporator. If the amount of comparatively cool vapors is increased, the amount of glycerine condensed .is increased, and if the amount of comparatively cool vapor'is decreased'the amount to distill over through the pipe connection 10 as stated.
- pipe connection 3 extends downwardly through the still from the top thereof in the arrangementshown so that the steam contained in pipe 3 is still further superheated by the vapors of the distilling glycerine as they pass upwardly;
- Condenser 15 preferably contains a series of cooling tubes through which water passes, being admitted to the tubes through pipe 34 and passing out'of the condenser by pipe 35.
- the rate at which the cooling water flows through the condenser may be regulated Jo valve 36.
- Most of the glycerine which as remained uncondensed is condensed at this point together with a part of the water vapors, the condensed glycerine and water dropping into receiver 17 from which this condensate passes through connections 26 and 27 to concentrator 24 where the glycerine is to be concentratedto form .the finished product.
- cerine passes from receiver 17 throu liligonis preferably a surface condenser the tubes of which may be cooled by water.
- the water vapor. which passes into this condenser through connection 19 contains some glycerine as stated-togetherwith certain impu rities such as fatty acids and trimethylene-' glycol. All of these vapors are condensed in condenser 20 to form the liquid which is known as sweet water.
- glycerine remaining in the evaporator is then removed and constitutes a finished product or may be further purified by redistillation.
- a trap 38 is referably interposed in the path by which the'vapors of distilling liquids pass from the still into superheater 7
- the vapors rising through pipe 10 usually carry certain impurities suspended therein such assalt which may be mechanically separated from the vapors by interposing baflle plates-or the like in the path of the vapors.
- pipe 10 enters trap 38 at one side thereof, the connection from the trap to the superheater taking the form of a pipe 39 which connects the top of the trap with the top of the superheater.
- Pipe 39 extends downwardly into the trap and is provided at its lower .end'with a portion 40 preferably of a conical section the lower end of which is covered by a perforated :plate or screen 41.
- the impurities mentioned such as salt are stopped by this screen and; drop through pipe 42, back into the still.
- the object in providing the tapered section 40' is to permit the cross sectional area of the openings in screen 41 to be approximately the same as that of the I pige 39 above tapered section 40. 7
- he concentrator 24 is preferably provided with a heating coil 43. Means are also preferably provided for introducing open steam into the lower part of concentrator 24, a steam pipe 44 being illustrated as leading into the concentrator in which it is provided with perforations,
- this substance may be distilled from the concentrated solution of glycerine containing this impurity, by injecting open steam through the perforated coil 44 which is located below the level of the liquor in the concentrator.
- the concentrated glyc'erine solution in the concentrator tests 1256 in specific gravity at 155 (3.
- the impurity of lower specific gravity may be distilled off through pipe 28 into condenser 20 with open steam as stated and there may be obtained in the concentrator a finished glyce rine of dynamite grade with a specific gravity of 1.262 or more at 154 C.
- the glycerine is condensed from a lower grade of crude glycerine it is necessary to allow the impurities carried by the same to pass beyond the cooler condenser 15 into the condenser 20.
- the amount of vapor which is condensed in condenser 15 is somewhat less than ,in the distillation of the high grade crude-product and accordingly the condneser 15 will be supplied with a smaller amount of cooling Water, by reducing the opening through valve 36.
- the crude product contains 5% of impurities for example, I consider it good practice to condense approximately 48% of the glycerine in condenser 7 and 43% in condenser 15, the remaining 4% of the glycerine remaining in the sweet water.
- a vacuum pump connected to said evaporator, a superheater condenser, a cooler condenser, connections for passing water vapors from said evaporator through said superheater condenser and into said still, means Y for passing vapors of distilling liquid from said still through said superheater condenser, to superheat said water vapors and partly condense said liquid vapors, means for passing the'uncondensed liquid vapors into said cooler condenser, to condense a further fraction of said liquid vapors, a third condenser, connected to said cooler condenser for condensing water vapor uncon'densed in said first two condensers, connections for leading condensed liquid from said superheater andcooler condensers to said concentrator. and a connection for leading condensed-water from said third condenser to said evaporator.
- distilling apparatus the combination of a still having an opening at the top thereof, an evaporator, a vacuum pump connected to said evaporator, a superheater condenser, a connection for passing water vapors from said evaporator through said superheater condenser and into the top of said still, said connection extending downwardly through the still and having openings at the lower end thereof, below the liquid level in the still, a connection for passing vapors of distilling liquid from said opening at the top of said still through said superheater condenser, to superheat said water vapors and partly condense said liquid vapors,
- distilling apparatus the combination of a still having a heating coil therein and a pair of openings in the top thereof, an evaporator having a heatin' coil therein, connected to the exhaust en of said first mentioned coil, a1 superheater. condenser, a vacuum pump connected to said evaporator, connections for passing water vapor said evaporator through said superheater condenser and into saidstill through one of said openings, and connections for passing vapors of distilling liquid from the other of said. openings in said still through said superheater condenser.
- distilling apparatus the combination of a still, an evaporator, a vacuum pump connected to said evaporator, a superheater condenser, a second condenser, receivare connected with said condensers, means for regulating the supply of-tcooling fluid of said second condenser, connections for passing water vapors from said evaporate! through said superheater condenser into 1d still and for passing vapors of distillingliquid from said still into said superheater condenser, a connection from the receiver of said superheater condenser to said second condenser, and means for passing fluid not condensed in said two condensers to said evaporator.
- distilling apparatus the combination from of a still, an evaporator, a vacuum pump connected thereto, a superheater condenser, a second condenser, a concentrator, connections for passing water. vapors from. said evaporator through said superheater condenser into said still and for passing vapors of distilling liquid from said still into said superheater condenser, means for passing liquid condensed in said twocondensers into said concentrator, means for passing fluid not condensed in said two condensers into said evaporator, and means for fractionating the distilled liquid in said concentrator.
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Description
- 35 tainer, a s
LOUIS ROTH, OF NEW YORK, N. Y., ASSIGNOR TO STERLING BRONZE COMPANY, OF
NEW YORK, N. Y., A CORPORATION OF NEW YORK.
OPERATING MEANS FOR SASH ADJUSTERS.
Application flled December 16, 1921. Serial a. 522,868.
To all whom it may concern:
Be it known that 1, Louis ROTH, a citizen of Austria-Hungary, residing at the city of New York, county of Bronx, and State of New York, have invented a certain new and useful Operating Means for Sash Adjusters, of which the following is a specification.
This invention is an operating device for use in connection with means for imparting 1 movement to a sliding sash.
As is well known, it is customary in some makes or styles of automobiles to employ a sash (one or more) in the body of the car for closing a window opening, and it is 1 usual, also, to associate with said sash appropriate means of one form or another for raising and lowering the same.
M improvement is directed, more particularl y, to the member for effecting the man- 2 ual operation of the sash adjuster, and to the means whereby said member is mounted for service within the car body.
The object is to provide an operating member which is not affected by the jar and vibration inherent in the movement of the vehicle, and the parts of which operating member are interchangeable with corresponding parts of similar operating members, which interchangeability of parts enables the operating member to be assembled and mounted with ease and facility.
To these ends my invention embodies a base member provided with a bearing and with an o ening for the reception of a reliaft actuator having a handle and a bushing unitary one with the other, said bushing being provided with an annular groove and being mounted for free rotative' movement within said bearing, a retainer 4 occu ying the opening to the base member and fittin in the groove for precluding endwise disp acement of said bushing, and a collar fitted to the base member in co-operative relation to the retainer so as to confine 4 it in the opening and prevent displacement under the jar or vibration of the vehicle and to prevent said retainer from dropping out of osition by the operation of the device.
gther functions and advantages of the invention will appear from the annexed description taken in connection with the drawin s, whereinigure 1 is a view partly in elevation and partly in vertical section of my operating means for a sash adjuster.
' bushing is fitted snu Figure 2 is a transverse section in the plane of the dotted line 22 of Figure 1.
F lgure 3 is an elevation of the base member detached, and I Figure 4 is a detail perspective view of one form of retainer.
The base member A is a single piece provided with a boss (5 extending outwardly from the face plate a. Said member is adapted for fixed attachment to the car body interiorly thereof, and to this end, the face plate 1s provided with a desired number of apertures I) through which screws 6 pass so as to be embedded in the car body, see F igure 1. The boss of said base member is externally threaded for a part of its length, as at a, and said boss is provided also with an opening d extending through said male threaded part 0, said opening being shown in the form of a slot, see Figures 2 and 3. The base member A is a fixed part of the operating device, and the boss a serves as a hearing within which is rotatably mounted a member of the shaft actuator.
Said shaft actuator comprises a bushing B and a crank handle C, the same being of umtary construction by casting said parts in one piece or by uniting the bushing and the crank handle in fixed permanent relation. The bushing is provided with an axial opening e of angular or square form in cross section, the external diameter of said bushing corresponding substantially to the internal diameter of the boss a, whereby the ly within the boss so as to substantially pre dlude all lost motion or idle play while at the same time the bushing is free to rotate within the boss. The length of the bushing is equal substantially to the thickness of the face plate and the length of the boss, whereby in assem bling the shaft actuator relatively to the base member the face of the crank handle is in abutting relation to the end of the boss, whereas the inner end face of the bushing is flush, or substantially so, with the inner face of the face plate, see Figure 1.
It is important to preclude accidental separation of the shaft actuator from the. base member, thus overcoming relative displacement of the parts by the jar and vibration of the vehicle. In my invention, this function is attained by a retainer D cooperating with the bushing of the shaft actuator. As shown, the retainer is in the Apr. 24, 1923.
W. E. SANGER PROCESS OF AND APPARATU S FOR DI STILLING LIQUIDS Filed March 9, 1921 2 Sheets-Sheet 2 .lll llllllllrllllfll 7471/47/14?! 11/6 .alIv
(EH tom Envemtoz WALTER. E. SANGER, OF'NEWeYOBK, N. Y., ASSIGNOR '10 WILLIAM GIGUE comm, 1110., OF NEW'YORK, N. Y., A. CORPORATION OF NEW YORK.
PROCESS DEW APPARATUS FOR DISTILLING LIQUIDS.
Application filed March 9, 1921. Ser1a1 No. 450,998.
To all whom it may concern:
Be'it known that I WALTER -E. SANGER, citizen of the United btates, and resident of New York, in the county of New York and State of New York, have invented certain new and useful Improvements in Processes of and Apparatus for Distillin Liquids, of whichthe following is a spec' cation.
My invention relates to a process of, and.
apparatus for distillin liquids, and the same is particularl well a apted for use in connection with iquids which show. a tendency to partially decompose when distilled directly or alone at normal pressure. Such liq- ="uids are distilled -in a partial vacuum, whereby the boiling point of the liquids is lowered in accordance with the degree of exhaustion. My improved process is particularly adapted for use in distillin crude lyceri'ne but it is not limited to such use. l he improved apparatus which is comprised within my invention is particularly adapted for practisin the process described herein.
y invention may be considered as in some respects an improvement upon that disclosed in Patent #774171 ranted November 8, 1904, to William E. (xarrigues, in which is disclosed a process of distilling liq- I uids such as glycerine in which the water vapors carried over with the distilling liquid in a previous distillation are re-evaporatedi at less than atmospheric pressure. The steam so produced is superheated by transfer of heat thereto from the vapors of the distilling liquid, this latter. being condensed at least in part as it gives up steam, and the steam is mjected into the body of liquid to be distilled to aid in the evaporation of the liquid in the still.
In the actual practise of glycerine distillation in accordance with't e disclosure of the patent a comparatively small amount of glycerine is actually condensed in the superheater in which the vapors of the distillin liquid give up heatto the water vapors whic are subsequently injected into the still. Ac-
cordingly there was a considerable amount of glycerine which was carried along to the evaporator in the form of a dilute glycerine solution called sweet water.' This sweet water had to be vconcentrated and again distilled in order to make the glycerine content thereof effective in the form of dynamite glycerine or the like.
I have found that I can control the amount its heat to the of glycerine which it is possible to obtain in the form of dynamite grade glycerine, by Sub ectmg the uncondensed glycerine vapors and water vapors mixed therewith, to a cool-' ing medium at a stage of the recess subsequent to that in. which the gl pors pass through the superheater condenser and thereafter condensing the remaining va-' pors at a dili'erent point, to form the sweet water which is then progressed to the evaporator in a continuous rocess. I'find that by the use of this additional condensing step, and by suitably regulating the supply of comparatively cool water vapors in the superheater condenser and of the cooling me-- cien'cy is obtained in a process of the character generally referred to above.
, In orderthat a better understanding of ycerine va- 'dium in the condenser next beyond the sumy invention may be had, attention is hereby directed to the accompanying-drawings forming part of this application and illustrating one embodiment of my invention. In the drawings, Fig. 1 represents. a diagrammatic 'sidefelevation of thee paratus' included in my invention and used or pra'ctising my improved process certain parts being shown in section, and
P ig. 2 is ;a similar view of a portion of the apparatus, on
an enlarged scale.
s Referring to the drawings, the still 1 5f. any suitable form contains the raw product .such as crude g1 cerine which may be antomatically fed into the still as required. It may be heated by any suitable means such as the steam coil 2 raw liquid. The still may additionallybe heated by any external source of heat in the usual manner.
Inside thestill there isqa pipe 3 to carry the superheated steam or vapors'which areto be n ected into the raw material in the artly immersed in the still to aid the distillation of the same. At the'lower end of pipe 3, there is preferably rovided a spider 4 provided with a numher of perforations or openings throu h which the superheated vapors pass into t e crude liquid. Preferably a lurality of s ider arms are provided whiclgare prefera 1 closed at the ends but may be left open if esired.
In the apparatus shown in the drawings the evaporator 5, which is suitably heated,
is adapted to evaporate water, such as the sweet water which has been obtained by condensing the water vapors carried over with the vapors of the distilling liquid in a previous distillation. The water vapors produced in evaporator 5 pass upwardly by pipe 6 into the superheater condenser 7 which may be rovided with a series of tubes 8 and b heater condenser there is a transfer of heat from the vapors of the distilling liquid which pass upwardly from still 1 through pipe 10, to the water vapors which have entered the superheater condenser from pipe 6. The water vapors may pass through the tubes 8 and the vapors of the distilling liquid pass around the tubes 8 or vice versa.
In the apparatus shown in the drawings the water vapors pass through the tubes 8 while the vapors of the distilling liquid pass around the tubes. The water vapors are considerably cooler than the vapors of the distilling liquid as will be explained more full hereinafter. Accordingly the vapors of t e distilling liquid are partly condensed and the .Water vapors are superheated. These superheated water vapors pass out of the superheater condenser by pipe connection 11 which carries the same into-the still, the superheated water vapors then continuing downwardly through the pipe connection 3 to a point near the bottom of the crude liquid in the still.
To describe briefly the other chief a paratus shown in the drawings, the ta or receiver 12 is connected by pipe connection 13 to the bottom of the superheater condenser 7. A pipe connection 14 extends upwardly from receiver 12 and connects with the upper portion of a. condenser 15 which I term a cooler condenser, which is connected at the bottom by pipe 16 with its receiver 17. A pipe connection 18 extends upwardly from receiver 17 to a connection shown at 19 with a third condenser 20 which latter is connected at the bottom by pipe 21 with a receiver 22. Receiver 22 is connected at the bottom by pipe 23 with the evaporator 5.
A concentrator 24 is adapted to receive distillates collected in receivers 12 and 17. These receivers may be connected by couplings 25 and 26, with the pipe 27' leadmg to the concentrator as shown. The upe plates 9. In the super-' esser:
per portion of concentrator 24 is shown as connected'by pipe 28 with the connection 19 leading into the upper portion of condenser 20. A vacuum pump 29 is connected I receiver 22 which latter is connected by.
pigs 23 to the evaporator 5 as noted above. he evaporator 5 is heated by suitable means, such for example as the coil 31 shown as mounted within the same. This coil may be heated by the passage therethrough of exhaust steam from the coil 2 within still 1, the exhaust end of coil 2 being connected to the entrance end of coil 31 by pipe connection 32. Evaporator 5, mi ht, of course, be heated by any other suitab e means such for example as steam supplied directly from a boiler or b the exhaust steam from the pump 29. ith the construction shown in the drawings, the coil 2 in the still may contain condensed water at its lower end. If that is so this water is under high pressure until it passes the throttle valve 33 which is located between the outlet of coil 2 and the inlet of coil 31. After the water condensed in the still coil passes throttle valve 33 the water is under less pressure and a part of the same flashes into steam which is available for heater purposes in the evaporator.
Assuming that, for instance, glycerine is to be re uired, the crude glycerine is fed au tomatica ly into the still to which external heat is preferably applied. Air is now exhausted from the entire apparatus by means I of vacuum pump 29. Evaporator 5 contains water or is filled with so-called sweet water from a previous distillation. As stated, this is heated. by any suitable means, preferably by the submerged coil 31.- Under the reduced pressure existing in the apparatus the sweet water in the evaporator boils easily and the vapor passes out throu h pipe 6 into the superheated condenser 7. flare it passes through the tubes 8 and is superheated by the vapor of glycerine and steam which pass upwardly from the still through pipe 10 and passes around the condenser tubes 8, the baflle plates 9 being preferably provided to cause the vapors to follow a circuitous path as they pass around the condenser tubes.
As the sweet water vapor which passes upwardly from the evaporator is saturated steam produced in a vacuum, its temperature is considerably below 212 F. The vapors coming from the still, however, have a temperature of about 325 F. the heat of the still being so regulated as to maintain these, vapors at about that tem erature. Accordingly there is a great di erence in temperature between the hot glycerine and steam vapors coming from the still and the sweet water vapor coming from the evaporator.
Accordingly the sweet water vapors-act as a condensing medium and a part of the glycerine will accordingly be condensed in the superheater condenser 7. The amount of glycerine so condensed is controlled by the amount of the comparatively cool 'vapors rising from the evaporator. If the amount of comparatively cool vapors is increased, the amount of glycerine condensed .is increased, and if the amount of comparatively cool vapor'is decreased'the amount to distill over through the pipe connection 10 as stated.
It will be noted that the pipe connection 3 extends downwardly through the still from the top thereof in the arrangementshown so that the steam contained in pipe 3 is still further superheated by the vapors of the distilling glycerine as they pass upwardly;
through the still on their .way to the pipe connection 10. The 'superheating ofthe steam which is injected into the crude glycerine in the still is thereforepartly accomplished in the still itself and partly in the superheater condenser 7 The. part of the glycerine which is condensed in condenser 7 drops into the receiver 12 from which it passes through pipe 27. into the concentrator 24.- :Most of the water vapor which is carried along with a the glycerine vapor does not condense in the superheater condenser but passes along together with the remaining uncondensed glycerine through pipe 14 into the surface condenser 15, which I term the cooler condenser.
Condenser 15 preferably contains a series of cooling tubes through which water passes, being admitted to the tubes through pipe 34 and passing out'of the condenser by pipe 35. The rate at which the cooling water flows through the condenser may be regulated Jo valve 36. Most of the glycerine which as remained uncondensed is condensed at this point together with a part of the water vapors, the condensed glycerine and water dropping into receiver 17 from which this condensate passes through connections 26 and 27 to concentrator 24 where the glycerine is to be concentratedto form .the finished product.
The remaining uncondensed water vapor, with a small percentage of uncondensed glynection 18 into the condenser 20.
cerine, passes from receiver 17 throu liligonis preferably a surface condenser the tubes of which may be cooled by water. The water vapor. which passes into this condenser through connection 19, contains some glycerine as stated-togetherwith certain impu rities such as fatty acids and trimethylene-' glycol. All of these vapors are condensed in condenser 20 to form the liquid which is known as sweet water. This drops into receiver 22 from which'it passes through pipe 23 into the evaporator, from which the water vapors againrise and circulate through the system in the manner described whereby a continuous circulation is created and a continuous process 1s obtained.
' The small quantity of glycerine passing over with the water vapor gradually accuniulates in theevaporator 5. When the accumulation is Sufficient to justlfy it,-a valve,
such as the valve 37, is closed, stopping the feed of sweet water to the evaporator until 'the water therein has been evaporated. The
glycerine remaining in the evaporator is then removed and constitutes a finished product or may be further purified by redistillation. l
A trap 38 is referably interposed in the path by which the'vapors of distilling liquids pass from the still into superheater 7 The vapors rising through pipe 10 usually carry certain impurities suspended therein such assalt which may be mechanically separated from the vapors by interposing baflle plates-or the like in the path of the vapors. In the construction illustrated, pipe 10 enters trap 38 at one side thereof, the connection from the trap to the superheater taking the form of a pipe 39 which connects the top of the trap with the top of the superheater. Pipe 39 extends downwardly into the trap and is provided at its lower .end'with a portion 40 preferably of a conical section the lower end of which is covered by a perforated :plate or screen 41. The impurities mentioned such as salt; are stopped by this screen and; drop through pipe 42, back into the still. The object in providing the tapered section 40'is to permit the cross sectional area of the openings in screen 41 to be approximately the same as that of the I pige 39 above tapered section 40. 7
he concentrator 24 is preferably provided with a heating coil 43. Means are also preferably provided for introducing open steam into the lower part of concentrator 24, a steam pipe 44 being illustrated as leading into the concentrator in which it is provided with perforations,
If by any cause an impurity such as trimethylene-glycol is run'into the concentrator with the glycerine, this substance may be distilled from the concentrated solution of glycerine containing this impurity, by injecting open steam through the perforated coil 44 which is located below the level of the liquor in the concentrator. If, for example, the concentrated glyc'erine solution in the concentrator tests 1256 in specific gravity at 155 (3., the impurity of lower specific gravity may be distilled off through pipe 28 into condenser 20 with open steam as stated and there may be obtained in the concentrator a finished glyce rine of dynamite grade with a specific gravity of 1.262 or more at 154 C.
,Itis thought that the operation of my process will be clear from the above. If the crude glycerine which is to be distilled is a comparatively high grade product, nearly half of the same may be condensed in the superheater condenser 7 and an equal fraction in the surface condenser 15. Thus, in actual practice about 48% of the glycerine in such a case is usually condensed in condenser 7 and 48% in condenser 15, the remaining 4% of the glycerine passing on and into evaporator 5 in the sweet water. In this operation the cooling water is caused to pass through condenser 15 at a comparatively high rate.
If the glycerine is condensed from a lower grade of crude glycerine it is necessary to allow the impurities carried by the same to pass beyond the cooler condenser 15 into the condenser 20., The amount of vapor which is condensed in condenser 15 is somewhat less than ,in the distillation of the high grade crude-product and accordingly the condneser 15 will be supplied with a smaller amount of cooling Water, by reducing the opening through valve 36. If the crude product contains 5% of impurities for example, I consider it good practice to condense approximately 48% of the glycerine in condenser 7 and 43% in condenser 15, the remaining 4% of the glycerine remaining in the sweet water.
' It will, of course, be obvious that my proc ess is not limited in itsapplicability to the distillation of 'glycerine, but that the same may be used in distilling or fractionating other liquids which are distilled by steam or water vapors and particularly such liquids which show a tendency to partially decompose when distilled directly or alone at normal pressure.
It should be noted that my invention is not limited strictly to the various detailshof the process and of the apparatus which have been particularly described hut that the same is as broad as is indicated by the accompanying claims. "-3- What I claim is. 1. In distillingapparatus, the combination of a still, a concentrator, an evaporator,
a vacuum pump connected to said evaporator, a superheater condenser, a cooler condenser, connections for passing water vapors from said evaporator through said superheater condenser and into said still, means Y for passing vapors of distilling liquid from said still through said superheater condenser, to superheat said water vapors and partly condense said liquid vapors, means for passing the'uncondensed liquid vapors into said cooler condenser, to condense a further fraction of said liquid vapors, a third condenser, connected to said cooler condenser for condensing water vapor uncon'densed in said first two condensers, connections for leading condensed liquid from said superheater andcooler condensers to said concentrator. and a connection for leading condensed-water from said third condenser to said evaporator.
2. In distilling apparatus, the combination of a still having an opening at the top thereof, an evaporator, a vacuum pump connected to said evaporator, a superheater condenser, a connection for passing water vapors from said evaporator through said superheater condenser and into the top of said still, said connection extending downwardly through the still and having openings at the lower end thereof, below the liquid level in the still, a connection for passing vapors of distilling liquid from said opening at the top of said still through said superheater condenser, to superheat said water vapors and partly condense said liquid vapors,
means for condensing the water vapors carried with said liquid vapors and means for passing the condensed water to said evaporator.
3. In distilling apparatus, the combination of a still having a heating coil therein and a pair of openings in the top thereof, an evaporator having a heatin' coil therein, connected to the exhaust en of said first mentioned coil, a1 superheater. condenser, a vacuum pump connected to said evaporator, connections for passing water vapor said evaporator through said superheater condenser and into saidstill through one of said openings, and connections for passing vapors of distilling liquid from the other of said. openings in said still through said superheater condenser.
4. In distilling apparatus, the combination of a still, an evaporator, a vacuum pump connected to said evaporator, a superheater condenser, a second condenser, receivare connected with said condensers, means for regulating the supply of-tcooling fluid of said second condenser, connections for passing water vapors from said evaporate! through said superheater condenser into 1d still and for passing vapors of distillingliquid from said still into said superheater condenser, a connection from the receiver of said superheater condenser to said second condenser, and means for passing fluid not condensed in said two condensers to said evaporator.
5. In distilling apparatus, the combination from of a still, an evaporator, a vacuum pump connected thereto, a superheater condenser, a second condenser, a concentrator, connections for passing water. vapors from. said evaporator through said superheater condenser into said still and for passing vapors of distilling liquid from said still into said superheater condenser, means for passing liquid condensed in said twocondensers into said concentrator, means for passing fluid not condensed in said two condensers into said evaporator, and means for fractionating the distilled liquid in said concentrator. I
' 6. ,The process of distilling glycerine which comprises, creating water vapors from the sweet water at less than atmospheric pressure, superheating the same by the heat of the vapors of the distilling glycerine, injecting the superheated water vapors into the glycerine to be distilled, partly condensing the glycerine vapors by transfer of heat as the Water vapors are superheated, subjecting' the uncondensed glycerine vapors and water vapors mixed therewith to a cooling medium at a difl'erent point, and so regulating the cooling medium in accordance with the grade of the glycerine treated as to there condense nearly all the remaining glycerine, collecting the glycerine condensed at the two points mentioned passing the remaining vapors to another point and there condensing them.
7. The process of distilling glycerine which comprises creating water vapors from the sweet water at less than atmospheric pressure, superheating the'same by the heat of the vapors of the distilling glycerine, injecting the superheated water vapors into the glycerine to be distilled, partly condensing the glycerine vapors by transfer of heat as the water vapors are superheated, subjecting the uncondensed glycerine vapors and water vapors mixed therewith to a cooling medium at a different point and so regulating the cooling medium in accordance with the grade of the glycerine treated as to there condense nearly all the remaining glycerine, passing the remaining vapors to another point and there condensing them, passing the condensed sweet water to the point at which the sweet water is to be evaporated at less than atmospheric pressure, and collecting the glycerine which has been condensed at the two points mentioned.
8. The process of distilling liquids which show a tendency to partially .deco'mpose when distilled directly-or alone at normal pressure, which comprises, creating water vapors at less than atmospheric pressure, superheating the same by the heat of the vapors of such distilling liquid and thereby condensing a part of said liquid vapors, in jecting the superheated water vapors into the crude liquid to be distilled, subjecting the uncondensed vapors of the distillin liquid to a cooling medium at a point di erent from that at which the first part of said vapors was condensed, so regulati the flow of said cooling medium in accor ance with the condition of the liquid treated, as to condense nearly all the remaining liquid at said second point, and collecting the fractions of condensate. i
9. The process of distilling liquids which show a tendency to partially decompose when distilled directly or alone at normal pressure, which comprises, creating water vapors at less than atmospheric pressure, superheating the same by the, heat of the vapors of such distilling li uid, and thereby condensing a part of said iquid vapors, injecting the superheated water vapors into the crude liquid to be distilled, subjecting the uncondensed vapors of the distilling liquid to a cooling medium at a point difi'erent from that at which the first part of said 'vapors was condensed, causing the flow of said water vapors at the-point where they receive heat from the vapors of the distilling liquid to proceed at a desired rate, and regulating the flow of said cooling medium at the said different point to determine the proportion of liquid condensed at .each point, collecting the fractions of condensate, and progressing the remaining vapors, to the point at which the water vapors at less than atmospheric pressure are created.
Signed at New York, in the county of New York and State of New York, this 8th day of March, A. D. 1921.
' -WALTER E. SANGER.
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