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Publication
_________________________________________________________________
Number GB401484A
i»?
Title
_________________________________________________________________
EN Title Improvements in or relating to the fractional distillation of
volatile liquids and to other processes of contacting immiscible
fluids of different densities
Abstract
_________________________________________________________________
Fluids of different densities are passed in opposite directions
through a rotating spiral conduit of progressively increasing radius,
the lighter fluid being introduced at the outer end and caused to
travel in the direction of the inner end, and the heavier fluid being
caused to travel in the direction of increasing radius by the action
of centrifugal force.
The spiral conduit may be flat or conical, and a number of flat spiral
conduits may be arranged side by side on a common spindle.
The process may be employed for the fractional distillation of liquids
such as crude petroleum , or the absorption of constituents of gases
or liquids by other liquids, or for effecting reaction between liquids
of different densities, such as sulphuric acid and alcohol or oil.
As shown in Fig.
2, vapours from a boiling liquid contained in a still are passed up a
vertical pipe 32 and a space 35 to the outer end of a conical spiral
tube 25 rotating at high speed about a vertical axis.
The vapour passes up the tube 25 to a chamber 17 and from there into a
stationary pipe 46.
After passing through a stationary reflux condenser, the remaining
constituents of the vapour are condensed and collected.
Condensate from the stationary condenser is returned through a pipe 52
to pipe 46 and the spiral 25.
The condensate entering and formed within the spiral is prevented from
blocking the passage of the vapour by means of centrifugal force which
urges it to the outer side of the tube and along the spiral in the
direction of increasing radius.
It finally leaves the lower outer end of the spiral and passes down
the stationary tubes 38, 32 to the still.
The conical spiral tube 25 is supported by a conical shell 11 with
baseplate 12 and downwardly tapering portion 13.
Mercury seals 36, 53 are provided between the stationary and rotating
parts of the apparatus.
When the apparatus is at rest, the mercury in the seals flows back
into the annular troughs 40, 55.
As shown in Fig.
4, vapours from a boiling liquid in a still 77 pass up a tube 76,
along a radial tube 75 to the outer end of a flat-spiral tube 60.
They pass through the spiral
vertically, through a chamber
stationary vertical pipe 99.
to
in
the inner end, which is upturned
a stuffing box and then up a
The spiral tube with its insulating casing 62, and the still 77 are
rotated at high speed by means connected with the pulley 67.
Condensate
the outer
pump.
forming in the apparatus is urged by centrifugal force to
end of the spiral 60 and to the chamber 178 of a diaphragm
The chamber 178 is provided with ball check-valves.
Operation of the pump causes the condensate to flow along a tube 195
which passes radially to the tube 76 and then downwardly through it
into the still.
A pulley 193 causes rotation of a sleeve 190 and cam 189 at a lower
speed than that of the casing 62.
A
piston 187 is thus caused to reciprocate with a frequency
corresponding to the difference in speed of the two pulleys.
Pulsations are communicated to the bellows 183 and the condensate is
forced along the pipe 195.
The apparatus shown in Fig.
9, comprises a number of rotating spiral tubes 102, apparatus is used
for contacting two liquids, a separating chamber is secured to the
pipe 114.
The heavier liquid is withdrawn from the bottom through an outlet
provided with a float-operated valve.
As shown in Figs.
14 and 15, two similar heating vessels 130 are fixed at opposite sides
of a rotating table 128 which also supports a flat spiral tube 125.
The vessels 130 are heated electrically.
Vapours of disc form, mounted in a casing 105 on a hollow shaft 103.
Vapour or light liquid is passed under pressure through the inlet 114
into the outer ends of the spiral tubes 102 through which it passes in
countercurrent to condensate or heavy liquid.
It is led away through the pipe 111.
Heavy fluid may be supplied at
through the perforated pipe 112.
the
interior of the spiral tubes
When the enter the outer end of the spiral 125 through inlets 132, 133
and pass in countercurrent to condensate which is urged by centrifugal
force towards the outer end of the spiral and the vessels 130.
From the inner end of the spiral, the vapours pass up an axially
disposed vertical tube 138 and then into a stationary still head 143.
The tube 138 may be cooled by air which is supplied through the pipe
144 to the jacket 142.
The tube 138 is tapered in order that centrifugal force may assist
gravity in urging the condensate towards the bottom and into the
spiral tube.ALSO: Fluids of different densities are passed in opposite
directions
through
a rotating spiral conduit of progressively
increasing radius, the lighter fluid being introduced at the outer end
and caused to travel in the direction of the inner end, and the
heavier fluid being caused to travel in the direction of increasing
radius by the action of centrifugal force.
The spiral conduit may be flat or conical, and a number of flat spiral
conduits may be arranged side by side on a common spindle.
The process may be employed for the fractional distillation of liquids
such as crude petroleum , or the absorption of constituents of gases
or liquids by other liquids, or for effecting reaction between liquids
of differrent densities, such as sulphuric acid and alcohol or oils.
As shown in Fig.
2, vapours from a boiling liquid contained in a still are passed up a
vertical pipe 32 and a space 35 to the outer end of a conical spiral
tube 25 rotating at high speed about a vertical axis.
The vapour passes up the tube 25 to a chamber 17 and from there into a
stationary pipe 46.
After passing through a stationary reflux condenser, the remaining
constituents of the vapour are condensed and collected.
Condensate from the stationary condenser is returned through a pipe 52
to pipe 46 and the spiral 25.
The condensate entering and formed within the spiral is prevented from
blocking the passage of the vapour by means of centrifugal force which
urges it to the outer side of the tube and along the spiral in the
direction of increasing radius.
It finally leaves the lower outer end of the spiral and passes down
the stationary tubes 38 and 32 to the still.
The conical spiral tube 25 is supported by a conical shell 11 with
base plate 12 and downwardly tapering portion 13.
Mercury seals 36, 53 are provided between the stationary and rotating
parts of the apparatus.
When the apparatus is at rest, the mercury in the seals flows back
into the annular troughs 40, 55.
As shown in Fig.
4, vapours from a boiling liquid in a still 77 pass up a tube 76,
along a radial tube 75 to the outer end of a flat-spiral tube 60.
They pass through the spiral
vertically, through a chamber
stationary vertical pipe 99.
to
in
the inner end, which is upturned
a stuffing box and then up a
The spiral tube with its insulating casing 62, and the still 77 are
rotated at high speed by means connected with the pulley 67.
Condensate
the outer
pump.
forming in the apparatus is urged by centrifugal force to
end of the spiral 60 and to the chamber 178 of a diaphragm
The chamber 178 is provided with ball check-valves.
Operation of the pump causes the condensate to flow along a tube 195
which passes radially to the tube 76 and then downwardly through it
into the still.
A pulley 193 causes rotation of a sleeve 190 and cam 189 at a slower
speed than that of the casing 62.
A
piston 187 is thus caused to reciprocate with a frequency
corresponding to the difference in speed of the two pulleys.
Pulsations are communicated to the bellows 183 and the condensate is
forced along the pipe 195.
The apparatus shown in Fig.
9, comprises a number of rotating spiral tubes 102, of disc form,
mounted in a casing 105 on a hollow shaft 103.
Vapour or light liquid is passed under pressure through the inlet 114
into the outer ends of the spiral tubes 102 through which it passes in
counter-current to condensate or heavy liquid.
It is led away through the pipe 111.
Heavy fluid may be supplied at
through the perforated pipe 112.
the
interior of the spiral tubes
When the apparatus is used for contacting two liquids, a separating
chamber is secured to the pipe 114.
The heavier liquid is withdrawn from the bottom through an outlet
provided with a float-operated valve.
As shown in Figs.
14 and 15, two similar heating vessels 130 are fixed at opposite sides
of a rotating table 128 which also supports a flat spiral tube 125.
The vessels 130 are heated electrically.
Vapours enter the outer end of the spiral 125 through inlets 132, 133
and pass in countercurrent to condensate which is urged by centrifugal
force towards the outer end of the spiral and the vessels 130.
From the inner end of the spiral, the vapours pass up an axially
disposed vertical tube 138 and then into a stationary still head 143.
The tube 138 may be cooled by air which is supplied through the pipe
144 to the jacket 142.
The tube 138 is tapered in order that centrifugal force may assist
gravity in urging the condensate towards the bottom and into the
spiral tube.
Description
_________________________________________________________________
lSecond Edition l
PATENT SPECIFICATION s Application Date: Oct 13, 1932 No 28,597/32 41
Complete Specification Accepted: Nov 16, 1933.
COMPLETE SPECIFICATION.
Improvements in or relating to the Fractional Distillation of Volatile
Liquids and to other Processes of Contacting Immiscible Fluids of
Different Densities.
I, WALTE Ri, JOSE Pl PODBIELNIAK, a Citizen of the United States of
America, of Medical Arts Building, Tulsa, Oklahoma, United States of
America, do hereby declare the nature of this invention and in what
manner the same is to be performed, to be particularly described and
ascertained in and by the following statement:This invention deals with the art of fractional distillation of
volatile fluids, and provides a novel method and apparatus for
fractional
distillation,
either on a commercial scale or for
analytical processes, of fluids having constituents of different
boiling points, for contacting liquids and gases and for contacting
liquids of different densities for adsorption or reaction purposes.
In operations such as these, effective and thorough interchange and
contact
is
important
Thus,
in the commercial or laboratory
distillation of liquid mixtures having constituents or fractions of
various boiling points, it is frequently desirable or essential to be
able to fractionate the mixture with such closeness as to isolate
constituents in substantially pure state.
For
example, in the distillation of petroleum crude or other mixtures
of similar complexity of composition, it is frequently desirable to
fractionate the crude into constituents ranging to volatility from the
lightest to the heaviest, with such sharpness of separation that the
fractions or cuts will consist of the constituents of the mixture in
substantially pure conditions, or of compounds which together have a
very close boiling range.
-In prior fractionating apparatus, when it is attempted to separate
the fractions or constituents of comparatively higher boiling point
and higher molecular weight, whether in petroleum or other complex
mixtures, insurmountable difficulties have been encountered such as
prevent precise fractionation and isolation of the higher boiling
point constituents, due chiefly to the increasing complexity of
isomerai Cpounds for any lPrice i Fsice t 5 given boiling range, and
because of the extreme closeness in boiling point of many of these
heavier constituents In order to approximate close fractionation of
such mixtures by the usual types of fractionat 5 a ing apparatus,
extremely high or long fractionating columns are required.
However, even these fail to accomplish the separation of the heavier
fractions with the desired closeness when such frac 60 tions reach the
higher boiling ranges and complexity of molecular structure In so far
as I am aware, the separation of the heavier fractions having boiling
points within a range of about 60 C, 65 cannot be accomplished by
fractionating equipment heretofore employed, whether in laboratory or
commercial scale distillation It may be stated that from an analytical
standpoint, it is desirable to 70 determine the exact composition of
petroleums and other similar complex mixtures, and to be able to carry
the
analysis
of the mixture composition through the heaviest
constituents which it may 75 contain.
It is a primary object of this invention to provide a method and
apparatus for fractional distillation that will enable all volatile
mixtures to be separated into 80 their pure constituents, or single
compounds, or into fractions having an extremely close boiling point
range which may be as low as say 1 or less And the invention is
intended to provide fur 85 ther an apparatus for accomplishing such
close fractionation without the requirement for large and complicated
equipment.
In order to attain precise fractionation 90 of the heavier-and more
complex fractions of, for example, petroleum crudes, there would be
required a fractionating column of impracticably great length or
height, since in theory the closeness of fractiona 95 tion will depend
upon the intimacy and time of contact between the liquid and gaseous
phases An ideal column which would accomplish perfect separation
between the constituents of a mixture, 45 1,484 would be one of
infinite length, of infinitesimal diameter, and one which holds at any
one time an infinitesimal quantity of liquid and vapor Although the
theoretical requirement of infinitesimal liquid or vapor holdup is of
primary importance in batch distillation, since the quantitative
separation of complex mixtures is carried out in batch distillation,
-in any case minimum liquid and irapor holdup is a practical advantage
in decreasing the size of the equipment.
Aside from the difficulty, inconvenience, and expense involved in
constructing fractionating columns of length substantially greater
than those now in use, such construction is made impossible by the
fact that in the usual fractionating column, gravity is relied upon to
cause the liquid or reflux to flow downward and countercurrently to
the ascending vapor within the column Hence, the usual fractionating
column must be vertical and given such dimensions and the vapor
velocity limited that the vapor will not hold up the liquid flow or
cause the liquid to be entrained by the vapor stream Also sufficient
clearance between plates of the column must be allowed in order to
avoid priming, and this alone may necessitate building a fractionating
column of very great length.
Because heretofore gravity has been relied upon to bring about
countercurrent flow of the reflux liquid with the vapor, a limit has
been reached as to the efficiency which such apparatus may have, and
engineering and economical standpoints have prevented building columns
of much greater length The same considerations have entered into the
construction of gas and liquid contact devices, such as absorption
columns, and of devices for effecting reaction between liquids of
different densities, as between oil and sulphuric acid .
The present invention departs from the usual methods and apparatus for
fractional distillation in that instead of causing the reflux to flow
by gravity, I bring about countercurrent flow by centrifugal force,
taking advantage of the difference in specific gravity of the fluids
involved, for example, of the reflux and the vapor.
By the aid of centrifugal force, the reflux or heavier fluid may be
caused to flow rapidly through a fractionating column or tube of small
diameter, thereby reducing the amount of liquid and vapor held (O in
the column to a minimum, and without interference by the vapors of
lighter kind, since bv virtue of the differences in specific gravities
of the two fluids, they are caused to follow -counter-current paths.
W 5 Also the centrifugal force may be made to overcome very much
greater interferences " or pressure drops than would be possible with
gravity alone.
According to the invention, therefore, I provide a process for
contacting immis 70 cible fluids of different densities in which the
heavier fluid is introduced at the inner end of a conduit constructed
as a curve with progressively increasing radius and rotating about a
central axis at a 75 speed sufficient to cause an effective flow by
centrifugal action, and the lighter fluid is forced to flow through
the conduit in counter-current to the heavier fluid.
Where this process is used for distillation 6 o it will be understood
that instead of the heavier fluid or reflux being introduced at the
inner end of the conduit it may be formed partly or even wholly by
condensation within the conduit itself 85 The invention also comprises
an apparatus for carrying out the above process comprising a conduit
in the form of a spiral curve of progressively increasing radius
mounted for rotation about the 90 axis of the spiral, means for
causing fluid to pass through the conduit from the outer to the inner
end thereof, and means for admitting another fluid of greater density
to
the inner end of the conduit during the 95 flow of the
first-mentioned fluid By constructing the fractionating column in
accordance with these principles the entire column may be built in an
extremely compact form, and may be of practically 100 any desired
length without involving prohibitive construction A close approach to
the ideal column characterised hereinabove is therefore made possible
by the invention in that the column may be made 105 of great length
and capable of great capacities, and the reflux and vapor may be put
through the column at high rates regardless of the column diameter.
Hence,
greater
efficiency
is
attained
in 110 bringing about close
fractionation,
than
heretofore used.
can
be
attained
by
fractionating
equipment
It
is to be distinctly understood that the invention broadly
contemplates the 116 use of centrifugal force in effecting intimate
and extended contact of a liquid with a gas or vapor or another liquid
of heavier specific gravity for a wide variety of purposes For
example, it may be 120 used for the absorption or reaction of
constituents of gases with liquids or for immiscible liquids of
different specific gravity with each other to secure reaction, as
alcohol and sulphuric acid 125 In the drawing I show various types of
construction embodying the invention.
It will be understood that the invention in its broader aspects is not
limited to details of the particular constructions 130 401,4841
401,484 shown herein:
In the accompanying drawing:
Figure 1 is a general view, diagrammatic in parts, illustrating a
device embodying the invention, the insulating layer about the
fractionating tube coil being omitted to more clearly illustrate the
arrangement and mounting of the tube; Fig 2 is a broken vertical
contracted sectional view of the fractionating apparatus on enlarged
scale; Fig 3 is a sectional view on line 3-3 of Fig 2 on a reduced
scale; Fig 4 is a vertical sectional view of the modified form of
apparatus in which the coil is formed as a fiat spiral instead of a
spiral helix, as in the form of Fig 1; Fig 5 is an enlarged sectional
view of a detail of the pump mechanism of Fig 4; Fig 6 is a detail
sectional view, showing the lower mounting of the device of Fig 4; Fig
7 is a detail sectional view on the line 7 of Fig 6; Fig 8 is a detail
sectional view showing the upper mounting of the device of Fig 4; Fig
9 is a view of a modified form of countercurrent contact device in
multiple disk form; Fig 10 is a vertical sectional view on line 10 of
Fig 11; Fig 11 is a view on a reduced scale showing the device of Fig
9 in connection with a still or other vaporizing device; Fig 12 is a
view on reduced scale, showing the device of Fig 9, adapted for the
treatment of immiscible liquids in a countercurrent contact operation;
Fig 13 is a detail sectional view of the separating chamber of the
device shown in Fig 12; Fig 14 is a view of a modified form of
construction in horizontal section on line 14-14 of Fig 15; and Fig 15
is a vertical sectional view of the form of construction illustrated
in Fig 14.
Referring first to Figs 1 and 2, numeral 10 designates the centrifugal
fractionating apparatus which comprises a rotatable mounting or body
11 comprising a vertical shell, which may be of conical shape as
indicated, or at any rate so designed that both liquid and vapor
throughout the bulk of the coil length are continually forced along
the desired direction by centrifugal force The shell 11 is supported
on a circular plate 12 which is supported on a circular, hollow,
downwardly tapering base 13, which may conveniently be made as a
single casting, the lower reduced tubular portion 13 a of the base is
journaled in suitable bearings, conventionally indicated at 14 and 15,
bearing 14 serving as a vertical support for the rotating parts Shell
11 has at its 7 Q upper end a tubular extension 16 which provides an
inner chamber 17 closed at its lower end by plate 18 Tubular extension
16 is journaled in a suitable bearing 19 Any other suitable mechanical
75 arrangements may be provided for supporting and journaling the tube
supporting structure at its upper and lower ends.
The supporting structure may be rotated by any suitable drive means,
such as by 80 pulley 20 keyed to the lower tubular portion 13 a of the
base and driven from motor 21 by way of gears 22, pulleys 23 and belt
24.
Mounted on the supporting structure 85 exteriorly of shell 11 is a
spirally wound fractionating tube or " column " 25, which opens at its
lower end 25 a through the bottom plate 12 into the interior 26 of the
base 13, and at its upper end at 25 b 90 through the wall of shell 11
into chamber 17 Although for purposes of illustration I show a
fractionating tube coil having a comparatively small number of turns,
the apparatus may be built so as to accom 95 modate a coil of very
great length and consisting of a correspondingly great number of turns
In order to maintain the proper temperature and equilibrium conditions
in the tube, the coil is prefer 100 ably thermally insulated with a
layer 27, of suitable thermal insulating material as shown in Fig 2;
and since in operation the coil is revolved at a high rate of speed,
the insulation may be protected 105 by enclosing it within a suitable
sheath 28 It may be stated at this point that the fractionating tube
diameter may be but a fraction of the diameter required for the usual
vertical fractionating 110 column capable of corresponding throughout,
because of the centrifugal action maintaining the liquid and gaseous
phases
in separate paths of flow, as will more fully appear
hereinafter 115 Heated vapors to be subjected to rectification and
fractionation in the spiral tube or column may be taken from any
suitable source; for example, as shown in Fig 1, a still 30 containing
the liquid 120 mixture to be fractionated, such as petroleum crude,
the liquid being heated and evaporated in the still as by means of
steam coil 31 Vapors are conducted from still 30 through line 125 32
which extends upwardly through the lower sleeve portion 13 a of the
rotatable base 13 to a point somewhat below plate 12 Pipe 32 may be
regarded as a stationary vapor inlet to the fractionat 130 ing
apparatus In order to prevent fluid leakage from the interior space 26
within base 13 around the inlet pipe 32 at such times as the liquid
seal between the fractionating tube and pipe 32 may be ineffective,
the pipe may be caused to fit more or less snugly within the elongated
sleeve 13 a.
Carried on the upper end of pipe 32 is a circular plate or vane 34
which is spaced at 35 a suitable distance from plate 12 The outer
periphery of vane 34 projects within an annular liquid sealchamber or
recess 36 formed between plate 12 and the upper flanged portion 13 b
of the base A suitable number of pipes or conduits 38, two being
shown, extend from pipe 32 at a suitable distance below its upper end,
to l openings 39 located in plate 34 a radial distance from the center
thereof corresponding to the radial distance of the lower open end 25
a of the fractionating tube Assuming the tubular coil to be rotated in
the direction indicated by arrow A in Fig 3, tubes 38 are preferably
given at their upper ends a curvature as indicated at 38 a, so that
the tubes will extend substantially in the diagonally downward path
which the liquid discharged from the lower end of the fractionating
tube tends to follow, due to the rotation of the tube.
Within base 13 and directly below flange 13 b is an annular trough 40
which, when the apparatus is stationary, contains a suitable sealing
fluid, preferably mercury Filling and drain plugs 41 and 42 are
provided in the side and hot-tom respectively of the mercury trough.
As the apparatus is rotated, the mercury within trough 40 is caused by
centrifugal action to rise along the outer wall of the trough, and
when the apparatus is rotated at operating speed, the mercury will be
displaced from the trough into the annular seal chamber 36 to the
position indicated at 43 Preferably the outer wall of the trough will
be curved as at 44 in order to permit smooth flow of the mer cury into
the sealing chamber The provision of a mercury seal joint of the
character shown between the stationary inlet pipe 32 and the rotating
fractionating tube is of particular advantage in that the parts of the
seal are entirely free from wear, as distinguished from the usual type
of stuffing box within which a compressed packing is used Furthermore,
owing to the great centrifugal force holding the mercury in the liquid
seal chamber, the mercurv will not become displaced to one side of the
sealing vane 34 even by extremely high differential pressure at
opposite sides of the vane.
The vapors passing out of the upper end of the fractionating tube into
the chamber 17 are conducted through a stationary outlet line 46,
supported by bracket 47, 70 to the reflux condenser 48, wherein the
heavier fractions of the vapors may be condensed by a suitable cooling
fluid introduced to the condenser through line 49 and discharged
through line 50 The 75vapors from the reflux condenser are conducted
through line 51 to suitable con, densing means, not shown The refi-4 x
condensate from the condenser 48 is -returned through line 52 to the
vapor outlet 80 line 46, from which the reflux passes into chamber 17
and into the fractionating tube.
A mercury seal, indicated at 53 and similar in principle to the
hereinabove 85 described lower seal, is provided between the upper
rotating extension 16 of the supporting structure and the stationary
outlet pipe 46 The seal 53 comprises a hollow housing 54 consisting of
a lower 90plate 55 joined at 56 to tubular portion 16, and an upper
plate 57 having a reduced diameter sleeve portion 58 which may be
fitted more closely to pipe 46 in order to close off the escape of any
vapors that 95 may be in the housing at such times as the mercury seal
may be broken Mounted on the outlet pipe is a circular plate or vane
60 which forms a barrier between opposite sides of the mercury seal in
the 100 same manner as the lower vane 34 The bottom 55 of housing 54
may be cupped as at 55 a, in order to accommodate sufficient mercury
to effect the seal Upon rotation of the housing to operating speed,
105the mercury rises to the position indicated at 61, thereby sealing
between the spaces within the housing above and below the vane, and
causing the flow of vapors from chamber 17 to pass into the outlet
-line 110-In the operation of the apparatus, the vapors from still 30
pass upwardly through the stationary pipe 32, the major portion of the
vapors flowing through the upper portion 32 a of the inlet into space
115 35, although some of the vapors may be conducted into that space
through the conduits 38 The vapors then pass into the lower end 25 a
of the fractionating tube and upwardly through the tube into 120
chamber 17 and the outlet line 46 leading to the reflux condenser As
previously stated, the reflux is returned through the outlet to
chamber 17, from whence it flows downwardly through the fractionat
125ing tube and counter-currently to the descending vapors, into space
35 Due to -its greater specific gravity, the reflux liquid in space 35
is maintained at the outside of the opening 25 a so as not -to 130
401,484 is such that distillation curves plotted to represent the
range through which distillation is carried, will indicate, in the
case of separation of constituents comprising single compounds,
successive con 70 densates each of substantially constant boiling
point and between which a well defined change in boiling point will
appear And in the separation of constituents having a predetermined
boiling 75 range, the fractional condensates will be found to conform
substantially precisely to such boiling range, without overlapping
between the successive cuts.
In Figs 4 to 8, a modified form of 80 ' apparatus is illustrated, as
particularly adapted to a distillation operation, in which the
countercurrent treatment tube is formed as a flat spiral.
In this form of construction, the tube, 85 formed as a flat spiral 60,
is surrounded by insulating material 61 and encased in a generally
disk-like casing 62, mounted for rotation about a vertical axis On its
lower side, the casing 62 is provided 90 centrally with a vertical,
depending cylindrical tubular bearing member 63 which passes through
the journal 64 supported on the frame 64 a The cylindrical tube 63 is
mounted in the journal 64 in a suit 95 able bearing 65, and acts as a
tubular drive shaft Its lower end is closed and is provided with
exterior threads as indicated at 66 in Fig 6 A drive pulley 67 is
secured to the cylindrical shaft 100 member 63, as by a set screw.
On its upper side the casing 62 is likewise provided centrally with a
cylindrical tube member 68 serving as a shaft member and projecting
upwardly through the 105 journal 69, being mounted in a bearing
therein.
The inner end of the coil spiral 60 is directed upwardly from the
center of the coil and from that point the tube portion 11 (72
projects
upwardly
through the tubular shaft member 68, being
surrounded within the latter by a packing of a suitable insulating
material, such as asbestos, designated 73 This central 115 tube
constitutes the outlet for the lighter fluid or uncondensed vapor
passing out of the coil.
At its outer end, the tube forming the coil or spiral is curved
downwardly, as 120 (at 74, and from this point is carried as the tube
75 radially within the easing 62 and opens into the central tube 76
which passes downwardly through the cylindrical shaft member 63, being
surrounded 125 within the latter by the insulating packing 73 a, which
may be of asbestos or other suitable material The tube 76 constitutes
the inlet to the spiral for lighter fluid or vapor 130 interfere with
the flow of vapors into the fractionating tube Liquid in space 25
passes downwardly through conduits 38 and line 32 to the evaporator.
The countercurrently flowing reflux and vapors in the fractionating
tube, by centrifugal action and by the progressively increasing radius
of curvature of the tube, are caused to flow in separate paths, the
reflux, by virtue of its higher specific gravity, being forced to flow
along the outside interior wall of the tube in the direction of
increasing radius of curvature, and the vapors to follow a path at the
inside
of the reflux Thus, the two phases are maintained in
countercurrent flow with the result that a high capacity of flow
through the tube is secured without causing the previously mentioned
phenomena of priming, or in other words without causing reflux liquid
to be picked up and carried by the vapor stream The liquid and vapors
are maintained in intimate and extended heat exchange, the inner
surface of the liquid stream is in direct contact with the vapors
Furthermore, entrained matter and heavier constituents in the vapors
are thrown to the outside of the vapor stream and in contact with the
reflux,
so
that the heaviest constituents of the vapors and
entrainment carried thereby is brought into most intimate contact with
the reflux The most advantageous speed of rotation of the column may
vary, but I may state that satisfactory results have been attained
revolving the column at a rate of from 1600 to about 4000 R P M.
Since
the
reflux and vapors are maintained in their respective paths
of flow by centrifugal force, the column or fractionating tube may be
of practically any length desired, or of reduced diameter, the
increased resistance to countercurrent flow being insignificant as
compared with the centrifugal force acting to maintain the tube or
column in operation.
By proper control of the reflux, the composition of the vapors passing
through the outlet line 51 to the final condensers may be controlled
so that the condensate will consist, if desired, of one constituent of
the mixture being evaporated, and in substantially its pure state; or
the condensate may consist of an extremely close cut fraction, the
boiling range of which may be as low as within 10 C or less.
The heavier liquid constituents returned from the fractionating tube
to the still may be revaporized and the various fractions or
constituents subsequently obtained as final condensate in the order of
their decreasing volatility, as separation of the mixture of the
constituents proceeds The efficiency of the apparatus 401,484 In Figs
4 to 8 inclusive, the device is illustrated as used in fractional
condensation of the vapors from a still or heating device The still
may suitably be a i vessel of cylindrical shape, designated 77, the
mouth of which is internally threaded so that it can be screwed to the
shaft member 63, the tube 76 then communicating with the interior of
the vessel and receiving vapors therefrom The vessel 77 and its
contents are heated by any suitable means, for example, by the
surrounding electrical resistance heating furnace 78 In operation, the
casing 62 with the coil spiral 60 and the associated parts, including
the cylindrical tubular shaft members 63 and 68 and the heated vessel
77 are rotated at a suitable speed to bring the desired centrifugal
force 2 Q into play, say from 1000 to 4000 R P M.
Vapors from the vessel 77 rise through the tube 76 and pass through
the radial tube portion 75 to the outermost turn of the coil, through
which they pass countercurrent to the reflux liquid, provided as
hereinafter described Uncondensed vapors pass out from the inner coil
of the spiral 60 through the tube 72.
To provide for the return of relfux condensate from the tube to the
distilling vessel 77, at the end of the outer turn of the coil 60,
where it turns downwardly at 74 and is connected with the radial tube
75, a liquid outlet tube 176 is provided, which extends radially
outward to the valve casing 177 of a pump device, suitably of the
diaphragm type The valse casing, which is connected to the outer wall
of the casing 62, is provided centrally with a chamber 178 with which
the liquid inlet line 176 communicates.
It discharges through the line 179, as hereinafter set forth In the
inlet and outlet valves, ball check valves 180 are provided and are so
arranged as to be seated by centrifugal force during operation of the
device From the chamber 178 in the pump casing there is provided a
short conduit 181 extending radially through the periphery of the
casing 62) and terminating in the interior of a suitable diaphragm,
for example, the metallic bellows member 183 The latter is completely
encased in a chamher 184, which communicates through the pipe 185 with
the interior of the pump cylinder 186, within which there is provided
the reciprocable piston 187.
The latter is operated through piston rod 188 by means of the
eccentric 189, suitably formed of two spaced disks formed on or
secured to the sleeve 190 journaled on the tubular shaft member 63,
the disks being formed with flanges 191 directed toward each other and
spaced at their lips to provide a peripheral opening through which the
piston rod 188 passes On the inner side of the flanges, rollers 192
are secured to the piston rod 188, these rollers riding on the inner
70 faces of the flanges 191 The sleeve 190 together with the eccentric
189 are rotated with respect to the tubular drive shaft 63 of the disk
62 by means of the pulley 193, driven by any suitable drive 75 member
In operation, the sleeve 190 and the eccentric 189 are driven at a
rate of speed different from that at which the casing 62 and the tube
spiral contained therein are driven, the differ 80 ence determining
the number of reciprocations given the pump piston 187 Thus, if the
tube spiral is driven at a rate of 1800 R P M and the pulley 193 and
eccentric 189 are driven at a rate of 1650 85 R.P M, the pump piston
187 will be reciprocated 150 times per minute The reciprocation of the
piston 17 is communicated to the liquid filling the diaphragm chamber
184 and the conduit 185 90 and causes a corresponding contraction and
expansion of the diaphrag u bellows 183, thereby communicating the
movement to the liquid reflux contained in the pump chamber 178 By the
action 95 of the ball valves 180, the reflux, forced out of the tube
spiral through the line 176 into the pump chamber, is forced out
through the conduit 179 and passes through the radial tube 193, which
enters 100the central vapor conduit 76 and passes actually downward
therethrough, as shown at 196, the reflux return tube terminating
somewhat below the opening of the vapor tube 76 The reflux or heavier
105 liquid discharged from the tube spiral by centrifugal force is
thus returned to the heating vessel 77.
The vapors discharged from the inner end of the tube spiral through
the line 110 72 enter a chamber 97 in a stuffing box 98, from which
they pass out through the stationary tube 99 mounted in a sleeve in a
bracket 101 supported from the frame 64 a 115 The operation of the
device will be readily understood from the preceding description of
the form shown in Figs 1 to 3 inclusive The tube spiral, with its
casing 62, is rotated at a predeter 120 mined speed, the distilling
vessel 77 being rotated therewith The contents of the distilling
vessel 77, in normal operation, are disposed against the sides of the
vessel, and not at the bottom as 125 in ordinary operation of
stationary stills.
The contents of the distilling vessel are heated and the vapors given
off passed through the line 76 and the line 75, entering the tube
spiral 60 at its outer 130 6 401 481 through the tube 112, enters the
tube spirals, and passes through them countercurrent to the vapors,
effective fractionation being secured in the tube spirals.
Reflux and condensate is thrown out of 70 the tube spirals into the
chamber within the easing 105, and descends through the pipe 114 into
the still 116.
It
will be readily apparent that the apparatus may be shown
substantially as 75 illustrated in the preceding Figures for the
absorption of constituents of gases or vapors by absorptive or
reactive liquids, the absorption or reaction liquid being supplied
through the line 112 and the 80 vapors to be treated being supplied
through the inlet line 114.
In Figs 12 and 13, the modification of Figs 9 and 10 is shown in
connection with apparatus for the treatment of a 85 lighter by a
heavier liquid, for example, as in the treatment of oils with
sulphuric acid to remove constituents of the former.
In
this
method
of
utilization, the casing communicates through its
inlet 114 90 with an elongated chamber 118, to which the lighter
liquid to be treated is supplied through the line 119 The light liquid
is forced under pressure up into the casing 105 and into the tube
spirals which 95 it traverses, leaving through the central hollow
shaft 103 and the outlet pipe 111, the latter terminating in a cap 120
through which the line 112 enters The treated light liquid is
withdrawn through 100 the line 121 The heavy liquid used in the
process is supplied through the line 112, enters the tube spirals, and
passes through them countercurrent to the light liquid, by the action
of the centrifugal force de 105 veloped on rotation of the tube
spirals.
The desired chemical action between the heavy and light liquids takes
place, and the used heavy liquid is discharged into the casing 105
setting through the 110 opening 114 into the chamber 118 In the latter
separation of the heavy and the light liquids takes place, the heavier
liquid descending to the bottom and discharging through the line 122,
provided 115 with the float controlled valve 123.
In Figs 14 and 15 I have shown a modified form of apparatus in which
the tube or column is likewise formed as a flat spiral, and in which
the
120 vessel or vessels containing the liquid subjected to
distillation are directly connected with the spiral column.
In this form of construction the flat spiral tube 125 is, for
convenience, 125 mounted on a plate or disk 126 of wood, or material,
known under the Registered Trade Mark " Bakelite " or other suitable
material, and the spiral tube and mounting plate are packed in heat
insu 1301 end They traverse the tube spiral countercurrent to reflux
liquid or absorption liquid, which may be supplied through the pipes
99 and 72 The reflux liquid is forced to travel outwardly through the
spiral
against
the
vapors
by
centrifugal
force, effective
fractionation or absorption of constituents of the vapors being
secured in the spiral On reaching the outer end of the spiral, liquid
is forced to enter the conduit 176, from which it is withdrawn into
the pump chamber 178 and forced through the reflux or liquid return
line 195 back through the line 196 into the distilling vessel.
In Figs 9 and 10 I have shown a modified form of the apparatus, more
particularly adapted for commercial installation.
In this form of construction, the individual tube spirals 102, each in
disk form, are mounted on a hollow shaft 103, being suitably held in a
position, as by a frame 102 a The shaft 103 passes through trunnions
104 of a stationary cylindrical casing 105 At their inner ends the
tube spirals open, as indicated at 106, into the interior of the shaft
103.
The outer ends of the tube spirals open directly into the interior of
the casing 105, as indicated at 107.
The hollow shaft 103 is closed at one end, 108, and at its other end
passes through a stuffing box 109 in the casing trunnion 104 and
enters a stuffing box provided at the end of the stationary outlet
pipe 111 A smaller relatively stationary liquid supply pipe 112 passes
through the vapor outlet pipe 111 and the hollow shaft 103, being
closed at its end and provided with perforations 113 for that portion
of its length opposite the openings of the tube spirals 102.
The operation of the device of Figs.
9 and 10 will be readily apparent Vapors or light liquid entering the
casing, for example, through the inlet pipe 114 under suitable
pressure are forced into the spiral tubes 102 and traverse them
countercurrent to heavier fluid or liquid.
Liquid may be supplied at the interior of the tube spirals through the
pipe 112.
The device of Figs 9 and 10 is illustrated in Fig 11 in its
application to a distillation process, the casing 105 being mounted by
means of brackets 115 on the still 116 M and the inlet 114 of the
casing being secured to the vapor outlet 117 from the still Vapors
from the still enter the casing 105, and are forced to traverse the
tube spirals 102 as hereinbefore described, the spirals being rotated
at a suitable speed to secure the desired centrifugal force effect,
say 1000 to 4000 R P M Reflux liquid is supplied 401,484 L lating
material,
such as asbestos, in a by centrifugal force Reflux
condensate casing formed by upper plate 127, lower formed in the
delivery tube 138 is forced plate 128 and the cylindrical ring 129 to
travel in the direction of enlarging The lower plate 128 is extended
beyond diameter and hence finds its way into the the ring 129 and on
it are mounted the inner end 140 of the tube spiral 125 70 opposed
balanced vessels or kettles 130, Having now particularly described and
of generally toroidal shape, which com ascertained the nature of my
said invenmunicate by the liquid level balancing tion and in what
manner the same is to
Claims
_________________________________________________________________
tube 131 The balanced vessels commu be performed, I declare that what
I claim nicate with the outer turn of the spiral is 75 tube 125 at 132
and 133 respectively It
1 A process for contacting immiscible will be noted that the liquid
level balanc fluids of different densities, in which the ing tube 131
opens into the vessels 130 heavier fluid is introduced at the inner at
their outer peripheries and the commu end of a conduit constructed as
a curve nicating tubes 132 and 133 at their inner with progressively
increasing radius and 80sides, as in rotation, liquid present in
rotating about a central axis at a speed the kettles is thrown to the
outer side by sufficient to cause an effective flow by centrifugal
force centrifugal action, and the lighter fluid The assemblage of the
kettles, tube is forced to flow through the conduit in spiral and
associated parts is mounted on countercurrent to the heavier fluid 85
the hollow, rotatable shaft 134 supported
2 A process of fractional distillation by bearings 135 and 136 and
driven by in which vapour from a heated liquid is pulley 137 from any
suitable source of caused to enter the outer end of a curved power
Within the hollow shaft 134 is conduit of progressively increasing
radius mounted the delivery tube 138 which and rotating about a
central axis and is 90 projects beyond the upper end of shaft cooled
in its passage through the conduit 134 and rotates therewith The in so
that constituent parts are condensed, terior tubular cavity 139 in
delivery the condensates being forced by centritube 138 is conical in
form, enlarging fugal action to flow in the reverse direcslightly from
its upper end, which is tion through the conduit 95 open, to its lower
end 139 a which is
3
Apparatus
for
carrying
out
the
proclosed The inner end of tube
spiral 125 cess claimed in claim 1 or claim 2, comis bent inwardly at
140 and opens into prising a conduit in the form of a spiral delivery
tube 138 at about its lower end curve of progressively increasing
radius The interior of shaft 134, surrounding mounted for rotation
about the axis of 100 the delivery tube 138 is packed with suit the
spiral, means for causing fluid to pass able heat insulating material
141, such through the conduit from the outer to as asbestos, slag
wool, or the like the inner end thereof, and means for adThe portion
of the delivery tube 138 mitting another fluid of greater density
extending beyond shaft 134 is surrounded to the inner end of the
conduit during 105 by a stationary mantle or sleeve 142 the flow of
the first mentioned fluid. mounted on the casing of bearing 135
4 Apparatus as claimed in claim 3
provided which the spiral conduit
143, into which inner end a tube
138 opens The sleeve 142 of the
110 is spaced from the delivery
suitable cooling medium may
in At the top of sleeve 142 there is
joins at its a collecting still head
which lies in the axis delivery tube
spiral, and is adapted to be rotated
tube 138 and therewith. air or other
5 Apparatus as claimed in claim 3 or be forced into the space between
the two claim 4, in which the conduit is in the by means of inlet pipe
144, discharging form of a conical spiral curve. through openings 145
If desired, a
6 Apparatus as claimed in claim 3 or 115 cooling or reflux liquid may
be supplied claim 4, in which the conduit is in the in the delivery
conduit, to aid in cooling form of a flat spiral curve. the vapors and
supplement the reflux con
7 Apparatus as claimed in claim 6, in densate formed therein and in
the, spiral which the conduit as a whole is composed In operation, the
shaft 134 carrying the of a number of smaller flat spiral conduits 120
tube spiral and associated parts is rotated arranged side by side on a
spindle at a suitable speed, say 1000 to 2500 common to all. R.P M The
vessels 130, previously
8 Apparatus as claimed in claims 3, charged with the desired quantity
of a 6, or 7, in which the spiral conduit is mixed liquid to be
fractionated, are enclosed in a casing, the outer end of 125 heated,
as by resistance coils 146 con the conduit opening into the casing,
and nected in series and to the slip rings 147 means being provided
for passing a liquid and 148 The vapors pass inwardly into the inner
end of the conduit, for through the tube spiral 125 countercur
removing the liquid from the casing after rent to reflux, which is
forced outwardly it has been discharged from the open end 130 401,484
401,484 of the conduit, for admitting a gas, vapor or liquid into the
casing, and for maintaining a drop of pressure between the interior of
the casing and an outlet for the gas, vapor or liquid leading from the
inner end of the conduit.
9 The process of fractional distillation substantially as described.
10 Apparatus for contacting immiscible fluids of different densities,
substantially as described.
11 Apparatus for contacting immiscible fluids of different densities,
substantially as shown in the accompanying drawings.
12
in
The products of distillation when produced by the process claimed
claims 1, 2 and 9. Dated this 13th day of October, 1932. WALTER
JOSEPH PODBIELNIAK. Per Boult, Wade and Tennant, 111/112, Hatton
Garden, London, E.C 1, Chartered Patent Agents. 15. Abing-don: Printed
for Hls allajesty's Stationery Office by Burgess and Son. lft 8031 T
-125/2 i 1937 l
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