DE1519557A1 - High vacuum centrifugal still - Google Patents

Description

! Marriage to British Petroleum Company Limited,

Britannic House, / Pinsbury Circus, Iondon B.C. 2 / England,

High vacuum centrifugal stabilizer.

The invention relates to a high vacuum centrifugal still with a separately arranged cooler and a rotating evaporator, to which the liquid to be distilled is fed in a thin layer is β -

In such a known device, this spacing space is essentially free; the surface of the evaporator, the shape of a rotating disc have, so that the film-like distribution of the material to be distilled by centrifugal force comes about ₀ This known apparatus is suitable at pressures of 1 / U Hg for distillation of thermally inclement 'Good. In the known device, the material to be distilled is only heated for a short time. The distillate is condensed on the cooling surface and removed from the system} the undistilled residue is also cooled and removed

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According to the invention, a high vacuum ^ centrifugal distillation device is proposed with a separately arranged cooler and a rotating evaporator to which the liquid to be distilled is supplied in a thin layer, the evaporator having a plurality of distillation zones arranged one behind the other, the cooler a plurality of cooling zones arranged one behind the other has zones and these zones are arranged relative to one another in such a way that the distillate in each case one after the other a distillation zone, an evaporator zone and then this Eedistillat can be fed to a next distillation zone and the residue is discharged from each distillation zone is. Of this, the last distillation zone is so far

at
except when the distilled material is removed from the last cooling zone assigned to it "

According to a further embodiment of the invention, the surface of the evaporator and the cooler are preferred arranged in parallel.

The distance between the evaporator and cooling surfaces preferably approaches half the molecular free path of the vapor molecules at the operating pressure »This distance is preferably smaller than the free molecular path _β

The stills can be through rings or on the Surface of the evaporator "arranged wave-like elevations be delimited" Guide bodies, such as guide plates or guide shells, are specified attached to the surface of the cooler

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Preferably, the guide body on the cooling surface are inclined so that the condensed distillate from a Distillation zone under the action of gravity runs along the underside of an inclined guide body J and flows to the next distillation zone, i.e. each guide body is at one point on the cooler surface attached above the distillation zone and inclined so that the tip of the guide body is above the next see the following distillation zone (

One can easily use the undistilled J. Residue using the force of gravity with the help Remove the ducts that keep the evaporator in each Enforce the de-distillation zone and preferably on the outside Circumference of each distillation zone are arranged

The AU. the cooling surface arranged guide body j are preferably inclined as steeply as possible to j to take into account the geometrical mechanical limitation, which are given by &# n distance between the cooling and evaporator surface, furthermore by the height the rings defining the distillation zones and through; the angles of inclination of the evaporator and cooling surfaces; ■ • If the inclination of the condensate conduction is greater, the smaller the tendency of the condensed distillate to drip back into the eltine distillation zone.

The surface of the evaporator can be arranged horizontally his} «ie iataber preferably from the Hitte inclined upwards, the angle of inclination «ur

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The horizontal look enlarged with the diameter of the evaporator surface. The maximum practically acceptable diameter for the horizontal evaporator is in the order of magnitude somewhat more than 30 cm . If one lowers the rotation speed of the evaporator or the Flußgesohwindigkeit of the to be distilled good enlarged _t in such a way that there is still a continuous film is present on the surface of the evaporator but unfavorable conditions in the central region are generated, where the material thickness of layers forms. These difficulties can be avoided if the surface of the evaporator is inclined upward from the center and the centrifugal force on the circumference is smaller for a given surface area and for the speed of rotation in the case of an inclined plate compared to a horizontal blade * Even in a device, in which the evaporator surface has a diameter of less than about 50 cm, the inclination of the plates is still advantageous. In a small iaborgerät of 12.7 cm Durehmesser can the evaporator to tS> ° inclined to the horizontal to be "in a large distillation apparatus with a Durehmesser of 152 cm, the inclination angle may - B5 be ° to the horizontal, said medium correspondingly to intermediate sizes Angles belong «By tilting the surface of the evaporator in this way, you can put a thin film of the material to be distilled on the

keep the entire evaporator surface

The evaporator is preferably in the form of a circular disk formed, whereby individually known heating means can be provided for him. For example oil can circulate in this disk as heating fuel. Preferably, however, an electric Radiator arranged in the disc.

The area of each distillation zone is preferably equal to or greater than that of the subsequent ones Distillation zone, let the maximum areas in each case be determinative values duroh the amount of liquid determined in each zone. It is appropriate that the evaporator surface of each zone is immediate proportional to the amount of liquid in this zone would be, ao that the filling deoke and the time of admission remained constant over the entire evaporator surface.

The cooler (condenser) preferably also has take the shape of a disc and you can get any suitable Provide coolant for him. Preferably jtdooh a linriohtung available, which a flowing coolant, ss.B. Air, or especially water, through which Allow cooler to circulate.

In stills according to this invention, the material to be distilled is according to an embodiment fed to the center of the rotating evaporator surface, from where it under the action of centrifugal force in the form of a thin continuous film over the The surface of the first distillation zone spreads out

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Bas distillate we * in the first cooling or condensate "on" condenses and flows to the next distiller »one, with the undistilled Bucket and from the first Zone removed by suitable training of the system This process is carried out from zone to zone last zone repeated · Here the distillate is collected as the end product and the residue, iiie indicated above, removed accordingly. 3) 1 x off Collected residues from each zone may or may not be recirculated depending on whether it is necessary »a case of fractional distillation or whether a continuous separation of the distillate * and the liquor is necessary

In parts of this device, ¥ 0 it is necessary, by means of individually known means dia Temperatures, ss.B, with the help of thermocouples (Thermocouples) measure

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An object of success is based on the following Drawings explained which illustrate schematic embodiments.

Show Eif

Pig, Fig. 1 is a partially sectioned front view of the Distillation device with a horizontally arranged evaporator,

FIG. 2 shows a side view of the device according to FIG. 1.

According to FIGS. 1 and 2, the device has a glass container 1 with ayifia. molded channel 2 on the has a slight downward slope in the direction of the outlet valve 3. The drain valve can be used as a two-way tap be designed, which is designed so that the liquid entering via the upper line 4 either via the lower line 5 back to the container or via a drain line 6 to a container, not shown can flow «At the bottom of the container there is a pipe 7 for the Entry of the misappropriation goods and, if necessary, for the emptying of the device available. The container is provided with a lid 9 that is attached to it via a Rubber sleeve To is sealed. A connecting pipe 3 penetrates the cover 9 and is in the usual way with connected to a diffusion pump, which is supported by a rotating vacuum pump (not shown). Inside the container is a circular rotating evaporator 11 made of aluminum cast, in which a electric radiator is built in. Over a wave 14 is the evaporator 11 with a not shown Motor in connection. Connect electrical lines 15 the heating element 12 through the shaft with sliding rings, not shown, arranged outside the container *

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The shaft 14 is sealed on the cover 9 by a vacuum seal 15. The upper outer surface of the evaporator 11 is divided into ring zones with the aid of concentric rings 16a, b, c. Guide channels 17a, b, ο go through the evaporator at different circumferential locations in each annular zone. A circular cooler 18 is arranged above and parallel to the evaporator and is provided with a central opening through which the W ₆ IIe 14 is passed. They are Einfew. Outlet pipes 19, 2o are provided so that the cooling water can circulate in the cooler 18. Concentric cooling sockets 21a, b, c are provided on the underside of the cooler 18, so that condensation zones corresponding to the distillation zones of the evaporator are formed. The ends of the guide bodies or guide shells 21 protrude slightly beyond the upper ends of the associated rings 16, and the end of the last guide body runs out over the channel 2. At the bottom of the container 1 is. an oil pump 22 is present and driven by a shaft 23 which is itself enclosed in a tube 24 and passed through the cover 9 at a vacuum seal 25. That pipe 24 has a branch 26, the end 27 of which extends up to a point near the center of the evaporator 11. A residue on take it 28 is supported by the tube 24 and has a ball valve 29 at the bottom. The ball valve 29 is actuated by the plunger 3o, which penetrates a vacuum seal in the cover 9 and is connected to the ball valve 29 via a lever 31. A funnel 32 is provided under the evaporator 11 and is supported by the residue sensor 28.

The container 1 is at 1o / u mercury pressure or less evacuated and the material to be treated slowly introduced through the tube 7, with degassing at the same time of the good takes place. The feed pump 22 and the

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Evaporator 11 are set in & ang and the feed material kept in circulation via the evaporator. By The evaporator is heated in this phase of work supports degassing.

In the initial state, before evaporation takes place, the entire liquid to be evaporated goes in the form of a thin film over the inner ring ^ 16c and falls through the guide channel 17c due to gravity along the outer periphery of the inner distillation zone first into the funnel 32, then into the residue take it up 28 and finally on the bottom of the container 1p If the temperature of the evaporator rises, finds a first distillation, especially the one more? volatile constituents of the material take place and the vapors formed condense on the guide body 21o. That Condensate runs over the surface of the guide body and drips into the middle distillation zone near its inner circumference. This liquid goes as a thin film to the middle ring 16b and becomes heated. There is partial evaporation, mainly of the more volatile constituents, and these vapors condense on the central guide body 21b. The non-evaporated liquid of the middle distillation zone runs through the guide channels 17b along the outer circumference of this zone first into the funnel 352, then into the residue receiver 28 and finally to the bottom of the container 1. The steam condensate of the middle Diffuser flows along the surface of the latter and drips into the outer distillation zone in the area the inner circumference of the latter. This liquid flows to the outer ring 16a in the form of a thin film and is heated. Again a part is evaporated, mainly the multi-volatile components of the liquid and these vapors condense on the outer baffle 21a.

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The non-evaporated liquid of the outer distillation zone flows through the guide channels 17a around the outer circumference of this zone, first into the funnel 32, then into the residue receiver 28 and finally to the bottom of the container 1. The vapor condensate of the outer guide body runs downwards over its surface and drips into the channel 2. The distillate collected in the channel flows under the action of gravity to the upper line 4 and from here to the outlet valve 3 flows to container 1. If the temperature rises slowly and it reaches the predetermined value, the tap of the outlet valve is turned so that the distillate comes into the discharge line 6 and from here into the distillate receiver. The ball valve 29 is now preferably closed so that the residue is taken up in the container 28 * The distillation is continued until all of the supplied material has been pumped away from the lower part of the container 1 "If you wish, you can stop the distillation at this point in time" Is it However, if necessary, a number of successive distillation stages (fractional distillation ^) can be carried out one after the other, at higher temperatures in each case, the residue after the first distillation stage in the. Container remains. The procedure is then that the first distillate receiver is replaced by another after all the material supplied has been pumped away from the container 1. The ball valve 29 is opened so that the residue can flow to the bottom of the container. Uun the residue stillationsstufe forms the starting distillate for the next De- ^ which is carried out at elevated temperature. If the temperature conditions are uniform, the second distillate is collected in the distillate receiver, the second residue is recorded in the residue

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I collected 28. This process will continue for as long as necessary. If necessary, the distillation is "ended _9" the supplied energy is switched off, the device is cooled, the vacuum is released and the final residue flows from the residue receiver 28 into a sample container. The device can then be cleaned with a suitable solvent.

Another object of the invention emerges from the following drawings.

Ee seigern

Fig. 3 is a front view of an evaporator and a Coolers that have an inclined position.

Pig. shows a partially sectioned front view a modified device with the distillation zones of the evaporator extending from the circumference to the center. at In this embodiment, the material to be treated is an outermost distillation zone at a point close to the inner one Perimeter of the zone.

In this embodiment, the bowl-shaped guide bodies above each distillation zone are inclined downwards towards the center of the evaporator. Partial evaporation takes place in the outer distillation zone, mainly of the volatile constituents of the feed material. The steam condenses on the guide body above this zone and the condensate runs on the lower surface of the guide body to a channel 33a which is attached to the lower edge of the guide body along its entire circumference. The diameter of this channel is approximately the same as the ring separating the outer and middle distillation zones. The condensate drains from the gutter through a plurality of sron tubes 34a which distribute the liquid and lead around the inner circumference of the central distillation zone. 909834/1284

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The unevaporated part of the product flows in the form of a thin filff to the periphery of the outer distillation zone, then downwards through the duct 17a into the iriohter and then into the residue sensor 28 * Similarly, the material migrates from the middle distillation zone in the form of a thin one .Hirnes the zone periphery and there is an evaporation mainly the more ^ lüchtigen components instead * the non-evaporated T _e il flows through the Ijeitkanäie 17b through the evaporator into the funnel 32 and then into the Rückstandsaufnehmer 28 * the steam condenses on the iieitsohalen above the middle distillation zone and the condensate flows on the lower surface of the rider body to channel 33b * which runs around the entire circumference of the lower inde of the rider body * is attached * The diameter of this channel is approximately equal to the diameter of the ring; of the medium and separates innere.Destillierzonen * The liquid condensate flows now νοη of the channel by a plurality of tube% h starting from that result ^ / aind the distributed along the inner periphery of the inner distilling> zione "miftellen flowing the liquid in a similar manner In the inner distillation zone the out inform of a thin mimes ziiitt ^ onentimfangi, whereby an evaporation of the more volatile constituents takes place »The non-evaporated fur deö good flows through the cooling channels 17c» over the evaporator into the tCrehter 32 and from here ίιφβη residue receiver 28 »the Daöipf condenses on the Ϊιο it body above the inner evaporation zone, and the Köiidettsät flows into a channel on the lower surface of the part body-is. 351 which is formed between the groove 14 and dom ring % , whereby this ring forms the inner circumference of the inner dilution zone »The liquid condensate flows along the channel through a large number of ceilings 31 into the funnel 38 and from here into one in the ftsnauttg of the container 1 formed channel 39 «This liquid can either at the bottom of the container

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ters 1 carried away, or in an I) estillataufne: h $ er with * Using the two-way valve 3 are collected.

Another object of the invention is shown in FIG. 5 depicted, this figure being a partially custom Front view of an embodiment similar to Mg. 4 shows, however, the condensate trays "or conductive body are modified.

This design is initially similar to that of the Pig. 4 the material to be distilled is fed to the outer distillation zone at a point near the inner circumference of this zone. Good migrates in the form of a thin film to the circumference of the outer Destillatiönszone, wherein a T _e ilverdampfung, in particular & »of. more volatile constituents takes place. The non-evaporated portion flows downward through the guide channels 17a and ^ μΓοΙι the evaporator into the funnel and from here into the residue receiver 28, the steam formed condenses on the guide bowl above the outer distillation zone and .the steam from the inner part of this distillation zone condenses on Cooling plate 4o. The liquid formed runs off along its surface and is collected in a channel 41, which runs along the lower edge of the cooling plate around the entire circumference of the channel and is "fastened there. The diameter of the channel is slightly smaller than the diameter of the Ring separating the outer and middle distillation zones. From this channel the liquid flows off via a number of tubes 42 at points which are arranged around the inner circumference of the middle distillation zone _e stillierzone originating vapor condenses on the cooling plate 43 --The gefbüLdete liquid, running along the baffle to the trough-44 on the entire circumference of the KUhlbleohes at the bottom

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the latter is attached. The diameter of the channel is slightly smaller than the diameter of the ring that defines the outer circumference of the outer distillation zone. The liquid condensate drains from the groove through a plurality of tubes which direct the liquid to locations located along the inner periphery of the outer distillation zone. In the middle distillation zone the sut migrates in the form of a thin film to the outer periphery of the zone and partial evaporation takes place mainly from the several volatile constituents. The non-evaporated portion of the material runs through the guide channels 17b and the evaporator into the funnel 32 and from here into the residue receiver 28. The vapor formed condenses on the guide plate above the middle distillation zone and the steam from the inner part of this zone condenses on the cooling plate 46. The liquid formed runs off along this surface and is collected in the channel 47. This gutter is attached to the lower edge of the baffle over the entire circumference of the latter. The diameter of the channel is somewhat smaller than the diameter of the ring which separates the central and inner distillation zones. From this channel the liquid runs through a number of tubes 48 to locations which are arranged around the inner circumference of the inner de-stilling zone. The vapor originating from the outer part of the central distillation zone condenses on the guide plate 49. The liquid formed flows on this guide plate to the channel 4t, where the liquid of the <.leitb.leoh.s- 4o had also flowed off. In a similar way, the liquid flows from the inner distillation zone in the form of a thin film to the periphery of the zone and there is partial evaporation, mainly of the multi-liquid components ^ tatt ^ jDer niently evaporated 5? _e il des öut-it flows over the _,? iei-tkaaäle 17c into the evaporator, from here into the Triohtar 32 and then into the Rückatandnehmer - 909834/1 284 ^ ^^ ^; ^ ^{1C ^:;} ^ -

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The steam formed condenses on the baffle above the inner distillation zone and the steam originating from the inner bearing of the zone condenses on the cooling plate in a cooling bowl. The liquid formed runs along this surface into the channel 51, which is formed between the shaft 14 and the ring 36, this ring forming the inner circumference of the inner distillation zone * The liquid condensate flows from the channel via a plurality of tubes 52 into the funnel and from here to the chute 59, the invention in the W _a of the container 1 is formed 38th This liquid can either be collected at the bottom of the container or by switching the two-way valve 3 to a distillate receiver. The vapor from the outer part of the inner distillation zone condenses on the cooling plate S3. The liquid formed flows along this plate to the channel 47 »Where the liquid from the baffle 46 has also flowed off.

liner of the advantages of this particular arrangement in that the distillation by a certain degree is accompanied by the return current which the Örad der Separation will be increased * as a result of the fleflträft |

In addition, the D _a fiipfmöiekUle after leaving the upper surface of the · * evaporator of a force tangentialeh subjected. In general, the heavy molecules are moved further in the tangential trajectory than the small molecules, but? At the same time, the heavy molecules leave the evaporator further outside (later), since they evaporate later. The more volatile constituents therefore tend to collect in the inner zone, while the less volatile constituents tend to collect in the outer zone.

The device shown in Fig. 5 is created to that from the inner and outer zones of each individual

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Distillate collected distillate to be able to separate, so that an improved separation that on attributed to the above centrifugal effect is, comes about.

An embodiment "which provides both a rotating cooler and a rotating evaporator, is shown in Figure 6, which Figure shows a front view of the cooler and evaporator.

Here water or cooling liquid is supplied to the cooler via tubes which extend through the rotor shaft, in a known per se W _e ise the place between the cooling liquid supply and the rotor shaft is ABG-ediohtet. This particular embodiment is advantageous in that the condensed liquid can fall back less than before onto the surface of the evaporator before it reaches the lower edge of the baffle. This increases the rate of distillation.

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Claims (10)

1 ο high vacuum centrifugal distillation device with separate arranged cooler and rotating evaporator, which the liquid to be distilled in a thin Layer is supplied, characterized in that the • Evaporator (11) a plurality of arranged one behind the other Distillation zones (at 16a, b, c), the cooler (18) has a plurality of cooling zones arranged one behind the other (at 21a, b, o) and these zones are relative are arranged to each other in such a way that one after the other the distillate of a distillation zone (21o) a Evaporation zone (at 16c) and then this redistillate can be fed to a next distillation zone (at 21b) and the residue from each distillation zone (at 16a, b, c) is derived. . 2 β high vacuum centrifugal distillation device according to Claim 1, characterized in that the last cooling zone (at 21a) with a drainage channel or the like. (2) connected is. 3. Apparatus according to claim 1 and 2, characterized in that the surfaces of the evaporator and the Cooler are arranged in parallel. 4. Apparatus according to claim 1 and 2 or 3 _f, characterized in that the distance between the surface of the cooler and the evaporator is smaller than the mean, molecular free path of the vapor molecules at operating pressure. """ 909834/1284 VT- 5 · Device according to one of claims 1 to 4 »daduroh characterized in that the distillation zones are limited by rings (16c, 16b, 16a) or wave-shaped elevations on the surface of the evaporator and that the cooling zones by guide bodies arranged on the surface of the cooler, vie Leitsohalen or J "eit plates (21a, b, c) are given. 6. Device according to claim 51, characterized in that that the flat guide body downwards in the direction of the respective distillation zone of the evaporator are inclined * 7 · Device according to one of claims 1-6, characterized in that for the undistilled residue in each distillation zone the evaporator penetrating guide channels (17a, b, e), preferably aa outer circumference every distilling scene, are present 8. Device according to one of claims 1-7 »characterized in that the evaporator ^{surface is inclined upwards from the center by an angle between 15 and 85 €} to the horizontal. 9 · Device according to one of claims 1-8, characterized characterized in that there is an electric heater in the evaporator. 10. Device according to one of claims 1 - 9t thereby characterized in that the area of each distillation zone is at least equal to the area of the next following one Distillation zone is BAD OfHJGJNAL 909834/1284 11 · Terriohtung according to one of claims · 1 - 10 _9, characterized in that the evaporator serves as a cooling device for a flowing coolant _# ., ..-. '■ BATH 90983Λ / 128Λ ZO L e r s e i t e