US1372880A - Distilling and purifying apparatus for volatile liquids - Google Patents

Distilling and purifying apparatus for volatile liquids Download PDF

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US1372880A
US1372880A US115634A US11563416A US1372880A US 1372880 A US1372880 A US 1372880A US 115634 A US115634 A US 115634A US 11563416 A US11563416 A US 11563416A US 1372880 A US1372880 A US 1372880A
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distilling
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Henry A Hills
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G7/00Distillation of hydrocarbon oils

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  • cleaning fluid such as gasolene, benzin, and the like
  • This invention relates to an Y"improved process and apparatus for purifying volatiley cleaning fluids such as gasolene preferably ⁇ with the aid of steam.
  • volatiley cleaning fluids such as gasolene preferably ⁇ with the aid of steam.
  • foaming may be avoided by agitating the fluid inthe still sufficiently violently to prevent the accumulation o-f scum at the surface.
  • the fluid is preferably agitated in a vertical plane so that anyA scum on the surface ⁇ is drawn down and mixed with the body of the fluid. e rlhis agiy of the fluid and mix it therewith.
  • Another object of this invention to construct a disti-lling and purifying apparatus for volatile cleaning fluids embracing a still for heating the fluid by steam coils, and at the .same time violently agitating thev same by direct application. of steam tothe fluid tation not only prevents foaming, but also and subsequently condensing and passing the same through a separator, after which the fluid is passed through a water separator or filter to remove remaining traces of moisture and other impurities possibly existing therein.
  • lt is also an object of this invention to construct a distilling and purifying apparatus for fluids comprising a still, condensing means, separating mechanism to cause separation of the moisture from the condensed distilled fluid, and an imp-roved fil-y tering device" to remove remaining traces of moisture and impurities from the fluid.
  • llt is finally an object of this invention to construct a simple, practical, and highly efficient distilling and purifying apparatus to receive a dirty and impure fluid and after passage through the apparatus discharging the same as ⁇ a clear and highly purified ⁇ product.
  • the invention (in a preferred form) is i used in my apparatus.-
  • Fig. 6 is 'a horizontal section taken ⁇ therethrough with parts shown in elevation.
  • F ig. 7 is a longitudinal section on line Of 6.
  • l T Fig. 8 is a detail sectiontaken on line 8 8 of Fig.,5.
  • Fig. 9 is 'a detail view ofthe steam inlet nozzle.l y i As shown in the drawings;
  • the reference numeral 1 indicates as a whole the still, which, as shown, consists of an upright cylinder provided with a conical cover or end 2, into which an outlet pipe .3, is connected. Said cylinder 1, is provided with a sloping bottom 4, into which a drain or outlet pipe 5, is provided as well as a valved inlet pipe 5a, near the upper end thereof; said outlet pipe v5, beingl provided with a controlling valve 6. Mounted in the lower end of the. still 1, is a steam coil 7,
  • valve 9 the inlet'to which from a supply pipe 8 is controlled by a valve 9,'and the outlet from which is controlled by a valve 10. Also connected intothe supply pipe 8, is a valve .11, controlling the flow through a nozzle 12,
  • Said nozzle 12 is shown l-indetail .in Fig. 9, and consists of a reducing cou# -inner or near end.
  • the steam passing through this nozzle is'adapted to draw fluid through the holes 12d and project it forcibly and rapidly across the still.
  • This fluid strikes against the upper part of the inclined bottom 4 of the still and is thereby deflected upward so that such fluidis caused to circulatev in a substanti ally Vertical plane to draw down the scum on the surface of the fluidand keep the latter thoroughly agitated-.. .
  • the lparticles of dirt suspended in the fluid strike the wall of the still above the nozzle.. anda large proportion thereof falls vertically downward along such wall directly toward the outlet pipe 5.
  • a condenser 13 comprising an upright cylinder open at its up- .per end, and at its lower end provided with a crown sheet or plate 14, beneath which is a conical bottom '15.
  • a series of upright tubes 16 Connected sealingly throughy said crown sheet 14, are a series of upright tubes 16, which, at their upper ends, communicate through a plate 17, on which a conical top ⁇ or cover 18, is riveted, brazed, or otherwise secured, and into which said pipe 3, from the still 1, ⁇ is connected.
  • a distributing screen or plate 19, is mounted in said cover member 18, to distribute the contents flowing into the condenser from the pipe 3, to the various tubes 16.
  • An inlet pipe 20, is connected into the lower end of the cylinder 13, to admit a flow of cooling water to surround the condensing tubes 16, and an outlet pipe 21, is provided at a convenient point at the upper end of said cylinder 13.
  • An outlet pipe 22, is connected in the conical bottom 15, of the condenser to ⁇ receive'thc condensed distillates, and said pipe leads into a T into which a Vent pipe 23, is connected, as well as a pipe 24, leading to a separator 25, designed to separate the moisture from the volatile fluid.
  • Said separator 25, consists of a rectangular tank with a plurality of vertical longitudinal baffles 26, therein, as clearly shown in Figs. 6 and 8, so arranged that the mixture of fluid entering into the tank through.
  • a glass or sight chamber 33 Connected “on the fluid outlet pipe 27 is f a glass or sight chamber 33, and leading therefrom is a pipe 34, which communicates into a filter 35.
  • Said filter isshown in detail in Figs. 2 and 3, and, as shown, consists of a cylindrical casing or drum with detachable heads or ends 36 and 37 thereon.
  • the head 37 has fitted thereto a ring or annulus 38, which fits over one end of the drum 35, and saidrespective heads or ends 36 and 37 are clamped to one another on said drum 35, by means of long rods or bolts 39.
  • annulus or ring 38 is provided with an inwardly convergent circular flange 40, and mounted thereon is a filtering element consisting of inner and outer frusto-conical sleeves 41 and 42, respectively, with a layer of fabric therebetween, and another similar filtering element 43, is mounted on an inwardly convergent flange 44, formed on the head 37.
  • a stay rod or bolt 45 is threaded under the inner side of the head 37, and projects longitudinally within the drum 35, to afford a support for the ends of said frusto-conical filter elements.
  • a sight glass chamber 46 Connected into the head 36, to communicate with the interior of the drum 35, is a sight glass chamber 46, provided with a discharge pet cock 47, and similarly connected into the annulus 38, is a sight glass receptacle 48, provided with a petcock 49, said latter receptacle adapted to receive impurities passing through the first filter element 41-42, ⁇ and checked in their passage by the filter element 43.
  • ⁇ Another sight glass receptacle 50 provided with a pet cock 51, is connected through the head 37, of the drum, communicatingA with the interior of the filter element 43, so that by means of said receptacles water or other impurities collected at the-different stages in l the filter may be detected and drained off fromtime to time, as desired.
  • a discharge pipe 5,2 is connected through the head 37, ofthe filter, from which the finally purified fluid is drawn off.
  • the horizontal nozzle 12 serves also by the introduction .of steam therethrough, to set up a Violent swirling motion to the contents ⁇ of the still, this agitation contributing largely to the effectiveness of operation as well as the efficiency or economy, as all the possible heating effect of thev coils and jet is utilized. Furthermore due to the construction of the steam inlet nozzle 12, pounding action within the still due-to the steam jet is obviated, said nozzle operating as an injector todraw the of the tank during the tortuous passage ofv the contents of the separator toward "thel volatile fluid outlet pipe 27.
  • the water outlet pipe 28 extends to near the bottom of the interior of the tank 25, a certain amount of water is alwaysvtrapped therein and may be drained ofi' through the l 30, and outlet pipe 32, at a lower level than the oil within the tank due to the differencev in specific gravities ⁇ of the water and oil. rlhe vent pipe 31, prevents a siphon' effect taking place. through the outlet pipe 28, and discharge pipe 32, for the water.
  • a still a steam heating coil therein, a discharge orifice adjacent one side of the vertical wall of the still, a bottom sloping downwardly from the opposite wall of the still toward said orifice and an aspirating nozzle, said nozzle being supplied with steam from the same source as the heating coil andv positioned substantially vertically above the discharge orifice and'directed toward the sloping bottom of the still for supplying steam under pressure into the, still and alsomaintaining a circulatlon of r the liquid therein.

Description

H. A. HILLS.
DISTILLING AND PURIFYING APPARATUS FOR VOLATILE LIQUIDS.
)Patented Man 299 19211.
2 SHEETS-SHEEI l.
APPLICATION FILED AUG. 18, 1916- H. A. HILLS.
DISTILLING AND FURIFYING APPARATUS FOR VOLATILE LIQUIDS.
APPLICATION FILED AUG- 18, 1916.
Mmm/ed Mar. 2&1921.
uNTTan sTaTes TeaTeNT Acritics,
` HENRY'A. HILLs-or GRAND RAPIDS, MICHIGAN..
DIsTILLINe ANn'PUItIFYINefAPPARATUs FOR VOLATILE LIQUIDS. .I
' irri-assai.y
T all whom t may concern:
Be it known that I, HENRY A. HILLS, a citizen of the United States,`- and a resident of the city of Grand Rapids, in the county of Kent and State of Michigan, have invented certain new and useful Improvements in Distilling and Purifying Appara tus for Volatile Liquids; and I dohereby declare that the following is a full,rclear,-
and exact description of the same, reference being had to the accompanying drawings, and` to the numerals of reference marked thereon, which form a part of thisrspecifica tion.
A ,considerable amount of cleaning fluid, such as gasolene, benzin, and the like, `is used in cleaning' establishments, and of course in using ylarge quantities of the saine it is necessarykto recover and purify thel for delicate `cleaning operations.
fluid so that the same may be used over again practically any number of times. Va-
`rious types of apparatus have been designed and constructed for the purpose of purifying the fluid after use, involving distillation and filtration of the same, but in general the apparatus has proved inefficient, and -of course, unless a highly purified fluid is re-` covered, it is difficult to again use the fluid rl`here have been variousdefects in the forms of apparatus used inthe past. vln the first place when the gasolene or other liquid contains a considerable amount of impurity foaming takes place which results, in mechanically carrying over into the condenser l the impurities which rise tothe surface of the liquid in the form of scum and which form the envelop around the bubbles in the froth or foam produced. Further these prior fo-rms of construction employed excessive quantities of steam vand the water condensed from such steam was only partially removed from the condensed gasolene or other liquid.
One of the methodsiused inw distilling the Afluid is known as the dry process, that is, heating the fluid by means of steam coils, butthis method, if used alone, is ineflicient, due tothe fact that steam at lrelatively high pressure'is necessary to secure the desired heat for the purpose, and also for the reason that certain foreign ymatter may render this treatment impractical because of foaming. Another method, known asthe lwet process of distillation, is o-ne wherein steam is blown through the duid to distil the same,
Specification of Letters iaten't.
passingover therewith to the condenser, and mechanisms are then necessary to separate the moisture or water from the condensed fluid. This method has heretofore been imperfect in results owing tothe fact that-the steam introduced merely lifted the vfroth formed at the surface of the fluid over into the condenser instead of breaking up or avoiding the formation of a. froth. Fur-L rammed. Maase, aaai. Application filed Augusty 18, 1916. Serial No. 115,634.
ther, it has heretofore'involved a great waste H of steam, and required a condenser of large capacity to condense thelinterinixed Asteam and volatihzed fluid. vIn such machines,
separation of all the ywater there-from was thought to be impractical. Y
This invention relates to an Y"improved process and apparatus for purifying volatiley cleaning fluids such as gasolene preferably `with the aid of steam. I have vfound that foaming may be avoided by agitating the fluid inthe still sufficiently violently to prevent the accumulation o-f scum at the surface. `For this purpose the fluid is preferably agitated in a vertical plane so that anyA scum on the surface `is drawn down and mixed with the body of the fluid. e rlhis agiy of the fluid and mix it therewith.
Another object of this invention to construct a disti-lling and purifying apparatus for volatile cleaning fluids embracing a still for heating the fluid by steam coils, and at the .same time violently agitating thev same by direct application. of steam tothe fluid tation not only prevents foaming, but also and subsequently condensing and passing the same through a separator, after which the fluid is passed through a water separator or filter to remove remaining traces of moisture and other impurities possibly existing therein. l i
lt is also an object of this invention to construct a distilling and purifying apparatus for fluids comprising a still, condensing means, separating mechanism to cause separation of the moisture from the condensed distilled fluid, and an imp-roved fil-y tering device" to remove remaining traces of moisture and impurities from the fluid.
Itis also an object of this invention to construct a high efficiency still for volatile fluids constructed to utilize heating steam coils' together with means for introducing a jet of steam directly into the fluid.
' It is furthermore an important object of this invention to construct an apparatus utilizing both the d ry and wet distilling systems and provided with an improved aI-,
rangement of separatingand filtering devices to purify the distilled fluid.
llt is finally an object of this invention to construct a simple, practical, and highly efficient distilling and purifying apparatus to receive a dirty and impure fluid and after passage through the apparatus discharging the same as `a clear and highly purified` product.
The invention (in a preferred form) is i used in my apparatus.-
Fig. 6 is 'a horizontal section taken` therethrough with parts shown in elevation.
F ig. 7 is a longitudinal section on line Of 6., l T Fig. 8 is a detail sectiontaken on line 8 8 of Fig.,5.
Fig. 9 `is 'a detail view ofthe steam inlet nozzle.l y i As shown in the drawings;
The reference numeral 1, indicates as a whole the still, which, as shown, consists of an upright cylinder provided with a conical cover or end 2, into which an outlet pipe .3, is connected. Said cylinder 1, is provided with a sloping bottom 4, into which a drain or outlet pipe 5, is provided as well as a valved inlet pipe 5a, near the upper end thereof; said outlet pipe v5, beingl provided with a controlling valve 6. Mounted in the lower end of the. still 1, is a steam coil 7,
the inlet'to which from a supply pipe 8, is controlled by a valve 9,'and the outlet from which is controlled by a valve 10. Also connected intothe supply pipe 8, is a valve .11, controlling the flow through a nozzle 12,
withinV the still, which is adapted to introduce steam directly into the fluid within the:
still. Said nozzle 12, is shown l-indetail .in Fig. 9, and consists of a reducing cou# -inner or near end. The steam passing through this nozzle is'adapted to draw fluid through the holes 12d and project it forcibly and rapidly across the still. `This fluid strikes against the upper part of the inclined bottom 4 of the still and is thereby deflected upward so that such fluidis caused to circulatev in a substanti ally Vertical plane to draw down the scum on the surface of the fluidand keep the latter thoroughly agitated-.. .The lparticles of dirt suspended in the fluid strike the wall of the still above the nozzle.. anda large proportion thereof falls vertically downward along such wall directly toward the outlet pipe 5. Mounted adjacent the still 1, is a condenser 13, comprising an upright cylinder open at its up- .per end, and at its lower end provided with a crown sheet or plate 14, beneath which is a conical bottom '15. Connected sealingly throughy said crown sheet 14, are a series of upright tubes 16, which, at their upper ends, communicate through a plate 17, on which a conical top` or cover 18, is riveted, brazed, or otherwise secured, and into which said pipe 3, from the still 1, `is connected.
A distributing screen or plate 19, is mounted in said cover member 18, to distribute the contents flowing into the condenser from the pipe 3, to the various tubes 16. An inlet pipe 20, is connected into the lower end of the cylinder 13, to admit a flow of cooling water to surround the condensing tubes 16, and an outlet pipe 21, is provided at a convenient point at the upper end of said cylinder 13. An outlet pipe 22, is connected in the conical bottom 15, of the condenser to` receive'thc condensed distillates, and said pipe leads into a T into which a Vent pipe 23, is connected, as well as a pipe 24, leading to a separator 25, designed to separate the moisture from the volatile fluid. Said separator 25, consists of a rectangular tank with a plurality of vertical longitudinal baffles 26, therein, as clearly shown in Figs. 6 and 8, so arranged that the mixture of fluid entering into the tank through. the
inlet pipe 24, jis constrained to take a tortuous passage around said baflle -plates toward a fluid outlet pipe 27. The water outlet pipe 28 extends into the separator and downwardly close to the bottom thereof, as
shown in Figs. 7 and 8, and leads outwardly from said tank 25, at a sli htly lowerl level than the outlet pipe 27 onneoted on the side of the tank 25, is a glass gage 29, to indicate the position of the water level within the separator.. As clearly shown, said outlet pipe 28, communicates into a 'l' 30, hav
ing a long uprightventpipe 31, connected therein, as well as a discharge pipe 32, theout through the discharge pipe 32.
Connected "on the fluid outlet pipe 27 is f a glass or sight chamber 33, and leading therefrom is a pipe 34, which communicates into a filter 35. Said filter isshown in detail in Figs. 2 and 3, and, as shown, consists of a cylindrical casing or drum with detachable heads or ends 36 and 37 thereon. The head 37 has fitted thereto a ring or annulus 38, which fits over one end of the drum 35, and saidrespective heads or ends 36 and 37 are clamped to one another on said drum 35, by means of long rods or bolts 39. .Said annulus or ring 38, is provided with an inwardly convergent circular flange 40, and mounted thereon is a filtering element consisting of inner and outer frusto-conical sleeves 41 and 42, respectively, with a layer of fabric therebetween, and another similar filtering element 43, is mounted on an inwardly convergent flange 44, formed on the head 37.
A stay rod or bolt 45, is threaded under the inner side of the head 37, and projects longitudinally within the drum 35, to afford a support for the ends of said frusto-conical filter elements. Connected into the head 36, to communicate with the interior of the drum 35, is a sight glass chamber 46, provided with a discharge pet cock 47, and similarly connected into the annulus 38, is a sight glass receptacle 48, provided with a petcock 49, said latter receptacle adapted to receive impurities passing through the first filter element 41-42, `and checked in their passage by the filter element 43. `Another sight glass receptacle 50, provided with a pet cock 51, is connected through the head 37, of the drum, communicatingA with the interior of the filter element 43, so that by means of said receptacles water or other impurities collected at the-different stages in l the filter may be detected and drained off fromtime to time, as desired. A discharge pipe 5,2, is connected through the head 37, ofthe filter, from which the finally purified fluid is drawn off. A
The operationis as follows: The fluid .for distillation and purification is introduced into the still or cylinderv 1,
through the valved pipe 5a, and steam .is
' then admitted through the heating coil 7', by opening the valves 9 and 10. 'The utilization of the steam coil, as well as the direct vintroduction of steam through the nozzlel `12, into the fluid for heating the same.
effects an economical operation of the still,
for the reasonthat by vusing a combination of the dry and wet method of distillation.
a much less volume of steam (is used than in either the dry or wet methods. 'll-he steam coil is utilized to bring the contents of the still to the vaporization p0int, and after vaporiz'ation has been set up the wet steam is introduced through the nozzle 12, directly into the fluid to prevent the formation of froth and aid\the distillation, and it is obvious that by proper manipulation of the valves controlling the respectivesteam supplies to the still, the most efficient oper-- ation for various conditions may -be obtained. The horizontal nozzle 12, serves also by the introduction .of steam therethrough, to set up a Violent swirling motion to the contents`of the still, this agitation contributing largely to the effectiveness of operation as well as the efficiency or economy, as all the possible heating effect of thev coils and jet is utilized. Furthermore due to the construction of the steam inlet nozzle 12, pounding action within the still due-to the steam jet is obviated, said nozzle operating as an injector todraw the of the tank during the tortuous passage ofv the contents of the separator toward "thel volatile fluid outlet pipe 27. Due to the fact that the water outlet pipe 28, extends to near the bottom of the interior of the tank 25, a certain amount of water is alwaysvtrapped therein and may be drained ofi' through the l 30, and outlet pipe 32, at a lower level than the oil within the tank due to the differencev in specific gravities`of the water and oil. rlhe vent pipe 31, prevents a siphon' effect taking place. through the outlet pipe 28, and discharge pipe 32, for the water. ri`he positi`on of the outlet pipe 27, for the'volatile fluid is such 115 with respect to the position or height of the water outlet, that'regardless of Ythe quantity of water Within the tank 25, the Huid rislng to set up a flow of the fluid outwardly throughV the water outlet pipe 2.8, and of course the outflow of water is automatic, only occurring when the .quantity in the tank 25, reaches Ian amount suflicient `to 125 cause a rise in the level of the water to set` up a flow outwardly through the discharge pipe'therefor. l
, 'lihe-l separated volatile fluid leaving by the outlet pipe 2 7, enters the sight glass-130 chamber 33, and from there passes into the filter 35, wherein any traces of suspended moisture or other impurities are liltered out, and the volatile Huid leaving by the pipe 52, 1s entirely pure and clear. The
vent pipe 23, connected into the T which connects the pipes 22 and 24, from the condenser into the separator, acts to prevent lan augmentation orv lowering of pressure otherwise than necessitated by the prior art.
I claim as my invention: l. In a still having a sloping bottom, a vapor outlet at the top and a liquid inlet,
v the combination of a nozzle adjacent the bottom of the still having its discharge opening directed against said bottom, said nozzle` having a sleeve surrounding and spaced therefrom to provide an annular chamber around thenoz'zle, and an opening f 1,372,880 j l at the rear end of said chamber for supplying fluid by suction through the chamber simultaneously with the exhaust from the nozzle.
2. In an apparatus of the class described, a still, a steam heating coil therein, a discharge orifice adjacent one side of the vertical wall of the still, a bottom sloping downwardly from the opposite wall of the still toward said orifice and an aspirating nozzle, said nozzle being supplied with steam from the same source as the heating coil andv positioned substantially vertically above the discharge orifice and'directed toward the sloping bottom of the still for supplying steam under pressure into the, still and alsomaintaining a circulatlon of r the liquid therein.
In testimony whereof I have hereunto subscribed my subscribing witnesses.
HENRY A. HILLS.
Witnesses:
CHARLES W. HILLS, Jr. EARL M. IIARDINE.
name in the presence of two`
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2531547A (en) * 1946-09-09 1950-11-28 Phillips Petroleum Co Apparatus for washing oils with an immiscible wash liquid
US2763372A (en) * 1952-01-17 1956-09-18 Indiana Commercial Filters Cor Means for separating a two-phase liquid
US2929463A (en) * 1954-07-23 1960-03-22 Senogas Corp Apparatus for salvaging vapor gas from hydrocarbon liquids
US4356791A (en) * 1978-06-06 1982-11-02 The Diversey Corporation Filter device and filter element for use therein
US4946559A (en) * 1987-11-03 1990-08-07 Oy Santasalo-Sohlberg Ab Removal of dissolved volatile impurities from liquid
US20030178349A1 (en) * 2002-03-25 2003-09-25 Bacon Edward Dudley Down pipe filter

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2531547A (en) * 1946-09-09 1950-11-28 Phillips Petroleum Co Apparatus for washing oils with an immiscible wash liquid
US2763372A (en) * 1952-01-17 1956-09-18 Indiana Commercial Filters Cor Means for separating a two-phase liquid
US2929463A (en) * 1954-07-23 1960-03-22 Senogas Corp Apparatus for salvaging vapor gas from hydrocarbon liquids
US4356791A (en) * 1978-06-06 1982-11-02 The Diversey Corporation Filter device and filter element for use therein
US4946559A (en) * 1987-11-03 1990-08-07 Oy Santasalo-Sohlberg Ab Removal of dissolved volatile impurities from liquid
US20030178349A1 (en) * 2002-03-25 2003-09-25 Bacon Edward Dudley Down pipe filter

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