5811 5815.output

* GB786219 (A)
Description: GB786219 (A) ? 1957-11-13
Improvements in grinding mills
Description of GB786219 (A)
PATENT SPECIFICATION
786,219 Date of Application and filing Complete Specification: May 4,
1955.
No 12954/55.
Application made in Italy on May 6, 1954.
Complete Specification Published: Nov 13, 1957.
Index at Acceptance:-Class 59, A 2 (C: F: G).
International Classification:-BO 2 c.
COMPLETE SPECIFICATION
Improvements in grinding mills I, CAMILLO BARGERO, an Italian citizen,
of 7, Piazza S Francisco, Casale Monferrato, Italy, do hereby declare
the invention, for which I pray that a patent may be granted to me,
and the method by which it is to be performed, to be particularly
described in and by the following statement:-
This invention provides a grinding mill of the type comprising an
elongated cylindrical drum rotating about a horizontal axis, a
plurality of radial partitions within the drum extending
longitudinally over the whole length of the latter and defining a
plurality of longitudinally extending main 1 S chambers of circular
sector-shaped crosssection, grinding bodies in said chambers, an inlet
opening at one end of the drum for charging the material to be ground
and associated with one of said main chambers, an outlet opening at
the other end of the drum for discharging the material ground and
associated with at least one of the remaining main chambers, and means
connecting said main chambers therebetween in order to allow conveying
the material being ground from said inlet opening towards said outlet
opening of the drum, characterised in that the said connecting means
comprise arcuate channels arranged externally of the outer periphery
of the drum and communicating with two successive main chambers
through openings provided in the outer peripheral wall of the said

drum.
In order that the invention may more readily be understood, certain
embodiments of the same will now be described with reference to the
accompanying diagrammatical drawings, wherein:
Figure 1 is a side elevation of an embodiment of a grinding mill
according to the present invention.
Figures 2, 3 and 4 are transverse sections on the lines II-II, III-III
and IV-IV respectively of Figure 1 lPrice 3 s 6 d l Figure 5 is an
enlarged perspective view of one end of the grinding mill shown in
Figure 1; Figure 6 is a side elevation of a modified grinding mill
construction provided with four chambers; Figure 7 is a part sectional
view corresponding to Figure 6; Figure 8 is a longitudinal section
taken on line VIII-VIII of Figure 6; Figures 9 and 10 are transverse
sections taken on lines IX-IX and X-X respectively of Figure 6; Figure
11 shows a modification of Figure 6; and Figures 12 to 14 are
transverse sections taken on lines XII-XII, XIII-XIII and XIVXIV
respectively of Figure 11.
Referring to Figures 1 to 5, the grinding mill shown comprises a
cylindrical drum 1 closed at its ends, except for openings 22, 23 for
the inlet and outlet of the material; the drum carries a gear wheel 24
by which it is rotated.
The drum 1 is subdivided into three longitudinally extending circular
sectorshaped main chambers A, B and C of an angular width of about 108
, 90 and 1620 respectively, in which the material is successively
ground to the desired fineness by grinding bodies, e g balls, enclosed
within the chambers.
The material is fed to the first main chamber A through the opening 22
by a screw which is not shown on the drawing, the finely ground
material being discharged from the third main chamber C through the
opposite opening 23.
The grinding mill is rotated in the direction shown by the arrow 28,
and the continuous supply of material through the outlet opening 22
causes the longitudinal travel of the material within the successive
grinding chambers, this taking place in main chamber A from the inlet
22 towards the outlet 23, in main chamber B in the opposite so
direction and in main chamber C in the same direction as in main
chamber A.
Chambers A and B communicate with each other at the end of the
grinding mill near the outlet opening 23 and at its central portion,
for the passage of the material which has undergone the first grinding
step.
This communication is established through grids 25 provided in the
casing of main chamber A, each grid giving access to an external
arcuate channel 26 ending in an opening 27 for discharging the

material into chamber B. An annular chamber 30 is arranged about the
drum at the end of the grinding mill near the inlet opening 22 A grid
29 is provided within the chamber 30 in the wall of the main chamber
B, together with a transverse partition 31 and a sieve 32.
The material issuing from main chamber B through the grid 29 reaches
the sieve 32.
The insufficiently ground portions are not passed by the apertures of
the sieve and are returned through an external conduit 33 to main
chamber A for further grinding, while the fine material which is
passed by the sieve 32 is retained by the outer wall of the annular
chamber 30 and is discharged through an opening 34 into the fine
grinding main chamber C.
The intermediate external arcuate channel 26 directly conveys any
material which has been sufficiently ground in the first main chamber
A to the second main chamber B without the material travelling
uselessly through the remainder of the first main chamber, thereby to
avoid any clogging and to improve the output of the grinding mill.
In the grinding mill construction shown in Figures 6 to 10, the drum 1
is subdivided lengthwise into four sector-shaped main chambers In the
main chambers A and B the first and second grinding steps respectively
are carried out, the angular widths of these main chambers being 1080
and 90 respectively The two main chambers C serving for fine grinding
are each 810 wide.
A helical conduit 40 and a plurality of arcuate channels 41 are
provided around the drum 1, the channels 41 being arranged at
intermediate positions and at the end near the outlet opening for the
material A sieve 42 is arranged within each arcuate channel 41, a grid
43 being provided within the channel 41 adjacent to the main chamber
A.
The material having undergone a first grinding step is passed by the
grid 43 and reaches the sieve 42 Its coarser portions are conveyed
towards opening 44 by which they are discharged into the main chamber
B in which they undergo a second grinding step The finer portions
passed through this sieve are conveyed along the helical conduit at
the front end of which they are discharged through two openings 45
into either main chamber C for fine grinding.
A grid 46 is provided at the end of main chamber B near the inlet
opening 22 to allow the material which has travelled through the whole
of main chamber B to 71 reach either main chamber C through the
openings 45 A chamber 47 forming an annular channel is provided around
the grid 46.
In the modified construction shown in 7 Figures 11 to 14, the grinding
mill is subdivided into four sectors as in the previously described
construction The drum includes three arcuate channels 50 spaced along

the length of the grinding mill and enclosing 8 ( grids 51 in the wall
of main chamber A through which the material which has been
sufficiently ground can escape and pass through openings 52 to the
next main chamber B 8 ' The central portion of the drum also includes
an arcuate channel 53 and an external helical conduit 54 ending at the
front end near the inlet opening 22.
A sieve 55 and a grid 56 in the wall of the 9 ( main chamber B are
arranged within the arcuate channel 53 The material passed by the grid
56 which is too coarse for the meshes of the sieve 55 is returned
through an opening 57 to the main chamber B for Go further grinding,
while the material passed by the sieve 55 is conveyed by the helical
conduit 54 towards the inlet end of the grinding mill and admitted
through openings 58 into either main chamber C for fine l OC grinding.
My improved grinding mill is simple in construction and has a high
output for a low power consumption.
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* 5.8.23.4; 93p
* GB786220 (A)
Description: GB786220 (A) ? 1957-11-13
Improvements in or relating to the manufacture of insulated electric cables
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The EPO does not accept any responsibility for the accuracy of data
and information originating from other authorities than the EPO; in
particular, the EPO does not guarantee that they are complete,

up-to-date or fit for specific purposes.
PATENT SPECFICATION
Inventor: -JOHN STANLEY WADDINGTON.
Date of filing Complete Specification: May 4, 1956.
Application Date: Mlay 5, 1955 No 13109/55.
(Patent of Addition to No 749, 288, dated Feb 11, 1955).
Index at Acceptance:-Class 36, A( 1 B 3: 5 16).
International Classification -H Oib.
COMPLETE SPECIFICATION.
Improvements in or relating to the Manufacture of Insulated Electric
Cables.
We, BRITISH INSULATED CALLENDER'S CABLES LIMITED, a British Company,
of Norfolk House, Norfolk Street, London, W.C 2, do hereby declare the
invention, for which we pray that a patent may be granted to us, and
the method by which it is to be performed, to be particularly
described in and by the following statement:-
This invention relates to the manufacture of electric cables of the
kind comprising one or more conductors each having a dielectric of
fibrous insulating material impregnated with an insulating oil or
compound.
Usually the dielectric is built up of paper and for convenience of
description such cables will hereinafter be termed "impregnated paper
insulated cables" whether the dielectric is built up of paper or other
fibrous insulating material, either natural or synthetic.
In the manufacture of impregnated paper insulated cables, the cable
core comprising one or more insulated conductors is usually dried in a
sealed tank with the aid of heat and vacuum It is then either
impregnated in the tank and afterwards taken out and sheathed or, in
the case of an oil-filled cable, is removed from the tank after being
dried, then sheathed and finally impregnated.
In the Complete Specification of our copending Patent Application No
749,288 there is described and claimed an improved process of
impregnated paper insulated cable manufacture which comprises drawing
the cable core into a metal tube in which the core is a loose fit and
converting the tube into a closed container for the core as by sealing
off the ends of the tube, drying the enclosed cable core under vacuum
with the aid of a high frequency electric field applied to the
dielectric, impregnating the dried lPrice 3 s 6 d l core within the
tube and reducing the crosssection of the tube to form a sheath for
the impregnated cable core.
The present invention provides a process 45 of impregnated paper
insulated cable manufacture which is a modification of the process of

the aforesaid Application and comprises extruding an oversized metal
sheath on to the cable core and converting the sheath into 50 a closed
container for the core as by sealing off the ends of the tube, drying
the enclosed cable core under vacuum, impregnating the dried core
within the oversized sheath and reducing the cross-section of the
sheath to 55 fit the core either tightly or with a small clearance.
The oversized sheath extruded around the core may be of lead or a lead
alloy or of aluminium or other suitable ductile metal 60 Vacuum drying
of the enclosed cable core may be effected with the aid of a high
frequency electric field applied to the dielectric or by generating
heat in the core conductor (or conductors) and/or in the sheath by 65
passing a heavy low voltage current therethrough or by a combination
of both dielectric loss and resistance heating methods.
For this purpose the oversized sheath with its core may be run on to a
drum or into a 70 pan which may be heated by steam or other means to
reduce the amount of dielectric loss and/or resistance heating that
would otherwise be necessary Alternatively where it is preferred to
avoid bending the core 75 within its sheath before the core has been
dried or before it has been both dried and impregnated, as the
sheathed core leaves the extrusion press or machine it may be drawn
into a long straight tubular jacket which 80 may be heated by steam,
electrical resistance heating or in any other convenient manner.
Price 250 7869220 786,220 the sheathed core itself preferably being
heated also in any one or more of the ways above described.
For heating the core of a single core cable by dielectric loss
heating, the high frequency field may be applied in various known
ways, for instance by coupling a high frequency generator between the
core conductor and the oversized metal sheath In that case the core
dielectric is preferably screened, the screen being in contact with
the wall of the oversized metal sheath, In the case of a multi-core
cable, the generator may be coupled between each two core conductors
in turn or a number of generators corresponding to the number of cores
can be used and connected across each core conductor and its
dielectric screen Alternatively a multi-phase generator may be used of
which the output terminals are respectively coupled to the respective
core conductors of the cable.
The frequency of the high frequency current fed to the cable will be
chosen having regard on the one hand to ensuring adequate heating of
the dielectric and on the other to the avoidance of standing waves
along the length of the cable which would result in non-uniformity of
drying We prefer to use a blast spark gap oscillator producing high
frequency damped oscillations, the inductance and the capacitance of
the tuned circuit of which are arranged to give damped high frequency
oscillations of several hundred kilocycles per second.

Where dielectric loss heating is employed, the cooling effect of the
conductor on the neighbouring part of its dielectric may be avoided by
resistance heating the conductor by passing a heavy low voltage direct
current through it, the source of direct current supply being isolated
from the high frequency generator by means of chokes having a high
impedance at the frequency of the high frequency heating current For
corresponding reasons supplementary heating of the oversized metal
sheath may also be carried out in a similar way In the latter case,
where the drying operation is carried a O out when the cable core and
its sheath are in a coiled state, successive turns may be insulated
from one another if necessary.
Impregnation of the dried cable core within its oversized metal sheath
may be carried out with or without supplementary heating of the
conductor or of the sheath and with or without a degree of dielectric
loss heating of the dielectric, as may be found desirable to maintain
the cable core at the required impregnating temperature.
The required reduction in cross-section of the oversized metal sheath
may be carried out in any suitable way-for instance by a swaging,
rolling or drawing operation in one or more stages or by a combination
of any two or all of such operations Since the reduction in
cross-section of the oversized metal sheath results in a diminution in
the cubical capacity of the sheath even though the reduction may be
accompanied by an 70 elongation of the sheath, care must be taken to
avoid a build-up of pressure within the sealed sheath during the
operation of reducing its cross-section to make it fit the cable core
tightly or with a small clearance 75 as may be required, by providing
means, for instance pressure release valves, at the rear end of the
sheath for the escape of impregnating oil or compound Care must be
exercised to keep the local increase of pres SI) sure in the vicinity
of the sinking die or other cross-section reducing means within
permissible limits by carrying out the reducing operation at such a
speed that, having regard to the viscosity of the oil or com 85 pound
at the temperature at which reduction is effected, the oil or compound
can flow rearwardly as fast as required The keeping of this local
increase of pressure within permissible limits is assisted if the
reduction 90 in cross-section of the sheath is effected by fluting it
This may be done by passing it through a group of fluting rolls each
of which rotates a fixed axis at right angles to the cable axis to
impart a flute extending 95 parallel to the cable axis or by passing
it through a group of fluting rolls which rotates about the cable axis
so that each roll of the group imparts to the sheath a helically
extending flute having a long pitch length 100 Alternatively, a
reduction in cross-section of the sheath may be effected by
corrugating it by forming in its wall one or more helically extending

grooves of short pitch Such fluting or corrugating results in the
forma 105 tion of a number of longitudinally or helically extending
channels between the cable core and the wall of the sheath and thus
involves a considerably smaller diminution in the cubical capacity of
the sheath than is 110 involved when reducing its cross-section by
drawing it through a sinking die.
From what has been stated in the preceding paragraph it will be
appreciated that the invention is especially suitable for the manu 115
facture of oil-filled cable, that is cable in which the impregnant is
an oil of which the viscosity at normal working temperatures is such
as to permit ready flow along the cable and into or out of expansion
chambers In 120 cables of this type the risk of a local buildup of
pressure at the sheath reducing means is small The invention may also
be applied however to the manufacture of cables impregnated with
compounds which at working 125 temperatures of the cable are viscous
or highly viscous liquids or even plastic solids, provided that at the
temperatures at which the oversized metal sheath is reduced in
cross-section, such compounds are liquids 130 current therethrough,
and after impregnating 65 the dried core in situ within the oversized
sheath, reducing the cross-section of the sheath to fit the core
either tightly or with a small clearance, wherein the oversized sheath
with its core is run On to a drum or into a 70 pan which drum or pan
is heated by steam or other means to reduce the amount of dielectric
loss and/or resistance heating that would otherwise be necessary.
A process of manufacturing impreg 75 nated Daner insulated cable by
extruding an oversized metal sheath on to a cable core consisting of
one or more insulated conductors and converting the sheath into a
closed container for the core and drying the en 80 closed cable core
under vacuum by applying a high frequency electric field to the
dielectric and/or by generating heat in the core conductor (or
conductors) and/or in the sheath by passing a heavy low voltage 85
current therethrough, and after impregnating the dried core in situ
within the oversized sheath, reducing the cross-section of the sheath
to fit the core either tightly or with a small clearance, wherein the
core is dried 90 whilst the oversize sheath containing it is in a
straight tubular jacket which may be heated by steam, electrical
resistance heating or in any other convenient rmanner.
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* GB786221 (A)
Description: GB786221 (A) ? 1957-11-13
Improvements in or relating to the steering of freight trucks
786,221 Date of Application and filing Complete Specification: May 16,
1955.
No 14036/55.
Application made in France on May 31, 1954.
Index at Acceptance:-Class 79 ( 5), H( 5: 24).
International Classification:-B 62 d.
Improvements in or relating to the steering of freight trucks We,
SOCIP Tt M I C (MECANIQUE INDUSTRIE CHIMIE), a Body Corporate duly
organized according to the French laws, of 40, rue du Colis 6 e,
Paris, Seine, France, do hereby declare the invention for which we
pray that a Patent may be granted to us, and the method by which it is
to be performed, to be particularly described in and by the following
statement:-
The invention relates to freight trucks, operated singly or in a
train, each truck being adapted to be pushed or drawn in one or the
other direction and so arranged that when it is coupled to other
similar trucks it will pass very substantially on the wheel tracks of
the preceding truck, even in case of frequent and sharp changes in
direction, or when the trucks effect turns having a very small radius
of curvature.
The invention consists of freight truck adapted to be pushed or drawn
either singly or in a train of trucks identical to said truck,
comprising a pair of coupling pins, these pins being arranged on the
central longitudinal axis of said truck, one pin at the front and the
other at the rear, a coupling rod pivotally connected to the front
coupling pin of the truck and adapted to be pivotally connected to the

rear coupling pin of a preceding truck, two wheels having a fixed
common axis which is coincident with the transverse plane of symmetry
of the truck and positioned between the aforesaid coupling pins, at
least one swivelling front wheel, a connection bar rotatable
integrally with said front wheel, means by which the orientation of
said bar and therefore of said front wheel is tied to that of the
coupling rod associated therewith, whereby the axis of said front
wheel will constantly pass substantially through the intersection of
the plane normally to, and centrally of, the coupling rod with the
transverse plane of symmetry of the truck, said connection bar being
releasable at will from the coupling lPrice 3 s 6 d l rod to enable
said front wheel to castor freely when said freight truck is used
singly.
The position of this slide relative to the coupling rod and the
connection bar, whereby the relevant swivelling wheel will be steered
according to the angular position of the coupling rod with respect to
the longitudinal axis of the truck, may be readily determined by means
of a simple geometrical construction as described hereinafter.
Now it has been found that by securing the slide to the connection bar
so that the distance between this slide and the vertical axis about
which the swivelling wheel is mounted be constant, or by so fixing
this slide on the coupling rod that the distance from the slide to the
point of attachment of the coupling rod to the truck be constant, the
orientation of this swivelling wheel while being adequate for a given
angular setting of said coupling rod will remain substantially
adequate for any other orientation of this coupling rod.
Therefore, either of these solutions or any other intermediate
solutions may be applied in the practice.
Preferably, the connection bar is of the retractable type, one or the
other end thereof being releasable so as to avoid interfering with the
free swivelling movement of the corresponding pivoting wheel when the
truck is not coupled.
The attached drawing forming part of this specification illustrates
diagrammatically by way of example one form of embodiment of this
invention: In the drawing:Figure 1 is a plan view from below showing a
truck constructed according to the present invention.
Figure 2 is an explanatory diagram.
The truck illustrated in the drawing comprises beneath its platform 1
a pair of wheels 2, 3 having a common fixed axis coincident with the
transverse plane of symmetry of the truck; another pair of wheels 4, 5
are carried by offset shells 6, 7 adapted to swivel about vertical
axes located on the longitudinal plane of symmetry of the truck.
With this known arrangement the truck may be pushed or propelled in
either direction and its front and rear swivelling wheels will take

automatically the desired orientation so as to follow the selected
path, the offset pivoting shell facilitating this orientation or
proper angular setting of the steering wheels which is such that the
axes of the wheels 4, 5 must constantly intersect each other on the
axis of the intermediate wheels 2, 3 at the momentary centre of
curvature I of the path followed by the truck.
The truck also comprises a coupling rod 8 pivotally mounted on a
vertical pin 9 and a pin 10 adapted to be pivotally conected to the
outer end of the coupling rod of another similar truck; the swivelling
shell 6 is rigid with a connection bar 11 carrying at its outer end a
slide 12 consisting in the example illustrated of a fork adapted to
receive the coupling rod between its arms.
When the truck is pushed in one or the other direction the coupling
rod 8 and connection bar 11 are disconnected from each other to enable
the swivelling wheels 4, 5 to take automatically the orientation
corresponding to the direction in which the truck is to be propelled;
preferably, the coupling rod 8 and connection bar 11 are retractable
to avoid interfering with the truck operation at the uncoupled end
thereof.
The steering diagram of Fig 2 shows the momentary centre of curvature
I of the truck when the latter is driven along a curve.
This centre I is located at the intersection of the plane passing
through the centre of, and normally to, the coupling rod 8, with the
axis of rotation of the wheel 4 adjacent to this coupler rod, and also
with the transverse plane of symmetry of the truck 1 which is
coincident with the common axis of the wheels 2, 3; with this diagram
it is possible to determine the length 1 of the connection bar, i e
the distance between the slide 12 and the swivel axis 13 of the offset
swivelling shell carrying the corresponding wheel 4, on the one hand,
and the distance 1 ' between this slide 12 and the axis of rotation 9
of the coupling rod 8.
When these distances have been determined, according to the form of
embodiment illustrated in Fig 1, the length 1 between the slide 12 and
its centre of pivoting 13 is determined and to this end the slide 12
may be secured to the outer end of the connection bar 11 According to
an alternative embodiment, the fixed length may be the distance 1 '
between the slide 12 and the centre of pivoting 9 of the coupling rod
8; in this case the slide 12 is secured on the coupling rod 8 and
adapted to slide along the connection bar 11.
In fact, experience teaches that with either of these solutions almost
perfect results may be achieved, and when a plurality of similar
trucks are coupled together each truck will pass very substantially on
the tracks of the 70 preceding truck, irrespective of the angle of
steering.

Obviously, the wheels 2, 3 prevent the side-skidding of the truck and
the rear wheel will be steered automatically in the 75 direction
adapted to cause its axis to intersect the momentary centre I; the
line drawn at right angles to the coupling rod 8 ', of the following
truck 1 ', will also pass substantially through the momentary centre
of rotation I, 80 and consequently the axes of the different wheels of
this following truck will also pass through this centre I.
Although from the purely geometrical standpoint this solution is only
approximate, 85 practical embodiments thereof have given very
satisfactory results and shown substantial improvements over those
obtained up to now with trucks designed to be coupled by two, three or
more to form trains of trucks 90 for transporting freight or luggages.
Of course, the form of embodiment described and shown herein is given
by way of example only and many modifications may be brought thereto
Thus, notably, the 95 rear wheel may be dispensed with if desired, and
on the other hand one or the other of the swivelling wheels of the
arrangement may be replaced by several swivelling wheels 100
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* GB786222 (A)
Description: GB786222 (A) ? 1957-11-13
Improvements relating to potters' jiggers and like rotating devices for
shaping or treating pottery ware
PATENT SPEFICATlON
Date of filing Complete Specification: May 14, 1956.
Application Date: May 18, 1955 No 14289 /55.

Index at Acceptance lass 87 ( 1), C 4.
International Classification:-CO 4 b.
COMPLETE SPECIFICATION.
Improvements relating to Potters' Jiggers and like Rotating Devices
for Shaping or Treating Pottery Ware.
I, WILLIAM HANCOCK, of "Mooifields",
Moss Hill, Stockton Brook, Stoke-on-Trent, in the County of Stafford,
a British Subject, do hereby declare the invention, for which I pray
that a patent may be granted to me, and the method by which it is to
be performed, to be particularly described in and by the following
statement:-
The present invention has relation to potters' jiggers and like
rotating devices for shaping or treating pottery ware and has for its
object to generally improve and modernize such devices whereby their
efficiency shall be increased and their life and utility prolonged.
According to the present invention a metal head comprising a circular
disc like body, a central bearing for the upright driving spindle and
an upright peripheral flange is provided with an external covering of
plastic such as poly-vinyl chloride to give a yielding or cushioning
protective surface.
The cavitous wall of the head is of conical or inwardly tapering
formation to accommodate a plastic mould having a tapering or conical
male formation on its underside with a wedge action.
In order that the invention may be clearly understood and readily
carried into practice reference may be had to the appended explanatory
drawings in which:The Figure illustrates in vertical sectional
elevation a rotary metal head and mould constructed according to the
present invention.
In a convenient embodiment of the present invention the head a of the
device is constructed of metal to a circular disc-like formation
having a central boss a' on its underlPrice 3 s 6 d 1 side through
which the vertical bore passes for attachment to the driving spindle.
Externally this boss a' is slightly coneshaped or tapered and the
disc-like part a is provided with an upwardly directed peripheral
flange a the inner face as of which is cone-shaped or tapered In this
invention this metal rotating jigger head a is covered externally with
a substantial layer of plastic ' such as poly-vinyl chloride or the
like by dipping or other similar operation and this plastic layer
constitutes a cushioning surface for any article brought into contact
therewith and also gives a very clean finish and appearance.
A plastic mould b is employed having on its underside a tapering
conical formation b' which will wedge into the tapering socket part a'
of the rotatable head a and this mould may overhang the sides of the
rotating member a as at b' so that it can be easily manipulated by the

fingers and has in fact a cavity on its upper side with a further
tapering wall b' and an annular shoulder having a slightly inclined
upper face b' according to whether it is to support plate, saucer or
the like for treatment.
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* GB786223 (A)
Description: GB786223 (A) ? 1957-11-13
Improvements in and relating to the manufacture of organic chemical
compounds
A high quality text as facsimile in your desired language may be available
amongst the following family members:
FR1139576 (A) US2811486 (A)
FR1139576 (A) US2811486 (A) less
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The EPO does not accept any responsibility for the accuracy of data
and information originating from other authorities than the EPO; in
particular, the EPO does not guarantee that they are complete,
up-to-date or fit for specific purposes.
786 o 223 4 r g i ' Date of Application and filing Complete
Specification: June 9, 1955.

No 16677/55.
Application made in United States of America on June 9, 1954.
Index at acceptance:-Classes 1 ( 1), F 4 C; and 2 ( 3), CIEWK( 2: 3;
8), CMF 1 (A 3: C 4: C 5: C 6: D 2:
D 3).
International Classification:-B Olj C 07 b.
Improvements in and relating to the Manufacture of Organic Chemical
Compounds We, Ko DAK LIMITED, a Company registered under the Laws of
Great Britain, of Kodak House, Kingsway, London, W C 2 (Assignees of
WILBERT JEPTHA HUMPHLETT), do hereby declare the invention for which
we pray that a patent may be granted to us, and the method by which it
is to be performed, to be particularly described in and by the
following statement: -
This invention relates to processes for the manufacture of chemical
compounds and to apparatus for carrying out such processes.
Many organic reactions are well known from the standpoint of the
chemistry involved and the reactants, reaction proportions, reaction
conditions and the like have been worked out with great particularity
within the bounds of known processes for effecting chemical reactions
using known apparatus.
While such chemical reactions thus proceed quite satisfactorily in
laboratory operations, it is often difficult to effectively carry out
the reactions on a commercial scale with high yields and high reaction
rates and without objectionable side reactions, decomposition and the
like which reduce yields and necessitate extensive product
purification.
In the laboratory, it is customary to effect chemical reactions by
discontinuous or batch processes and usually such reactions are
translated into plant scale operations using similar batch processes
This poses many problems because of the large capacity equipment which
is needed, the problem involved in heating and cooling large volumes
of reactants, the long reaction times necessary for economical yields
with the attendant opportunities for unwanted side reactions and
decomposition and the difficulty in controlling or adjusting the
reaction conditions except from batch to batch Many chemical reactions
are equilibrium reactions which can be driven to completion as regards
one reactant only by the use of large excesses of the other reactant
or reactants Because of capacity limitations and economic factors it
is not feasible to use the required excess necessary for substantially
complete conversion and the use of an excess of one reactant in batch
operations makes the subsequent product recovery more difficult and
costly.

Attempts have been made to carry out such reactions continuously by
progressively mixing the reactants in a flowing stream and effecting
the reaction progressively with a progressive removal of the resulting
reaction mixture containing product Although such continuous addition
and withdrawal does obviate some of the heating and cooling problems,
such processes are essentially flowing batch processes and hence are
called continuous batch processes If the batch process reaction is
equilibric in nature the continuous process reaction will also be
essentially equilibric in nature and the continuous batch processes do
not result in higher yields or higher reaction rates The recovery of
product from the equilibrium reaction mixtures involves the same
problems as in the true batch processes with the exception that the
recovery can be carried out continuously rather than waiting until the
entire reaction has been effected The yield per volume of reactants is
usually little if any better than in a true batch process and it is
necessary to process large volumes of reactants Such continuous batch
processes have found greatest utility in polymerization reactions or
the like in which equilibrium considerations are usually not a factor
and where the product can be coagulated continuously and separated
mechanically.
It is desirable, however, to provide a simple and straightforward
process for effecting such common chemical processes as condensation,
addition and halogenation, particularly where the reaction involves an
equilibrium reaction in continuous and progressive fashion using
simple apparatus of low capacity but high throughput rates in which
process, equilibrium factors are largely overcome, that is, conversion
of at least one reactant and preferably all reactants is substantially
complete in much shorter times than is possible with batch reactors of
the same capacity in terms of yield per unit time and in which, where
this necessary, large excesses of one of the reactants can be used
during the reaction without having to process large volumes of
material to recover the product.
According to the present invention there is provided a process for the
production of a chemical compound comprising reacting together at
least two reactants of different volatilities in a column packed to
provide a multiplicity of tortuous constricted paths and collecting
said compound from the lower end of said column-said process being
characterised in that a liquid comprising said two reactants or the
reactant of lower volatility flows downwards through said column while
the vapour of a solvent for said two reactants or the vapour, in
excess, of the reactant of higher volatility respectively flows
upwards through said column, the temperature of the column being
adjusted so that the two reactants or said reactant of lower
volatility and said chemical compound remain substantially in the

liquid state and said solvent or said reactant of higher volatility
remains substantially in the vapour state while passing through said
column, and in that the proportions of said two reactants flowing
through said column are adjusted so that said reactants or reactant
flowing downwards react substantially completely to form said chemical
compound.
The present invention is applicable for use in carrying out any of the
well-known chemical reactions involving a wide variety of reactants In
particular, the invention is concerned with effecting reaction wherein
at least two of the components of the reaction system have different
volatilities In general the process of the invention is adapted for
continuously and progressively effecting chemical reaction in
counterflowing liquid-vapour streams between components of a reaction
system including at least two components of substantially different
volatilities.
In one embodiment of the present invention, designated a tangential
reaction system, cyclic flow of the reactant of higher volatility is
combined with an inline flow of the reactant of lower volatility,
whereby the reactant which has essentially linear flow is almost
completely converted to the desired product, and wherein the reaction
time and the rate of inline flow of the reactant are related By inline
flow or linear flow of reactant or reactants is meant that the
reactant or reactants are passed through the reaction zone only once
to achieve substantially complete conversion to product.
In such processes of the invention, a continuous circulation of the
reaction component of relatively high volatility in cyclic fashion is
established by progressively vaporizing such component in a vaporizing
zone, continuously passing the vapours thus being generated from the
vaporizing zone upwardly through a re 70 action zone defined within a
packed column which is effective to cause the vapours to flow through
a multiplicity of tortuous constricted fluid passages, progressively
condensing the vapours emerging from the reaction zone after 75
passage therethrough, and progressively returning the condensate to
the vaporizing zone for revaporization Thus, one of the components of
the reaction system continually circulates in a cyclic system; and, as
will appear 80 hereinafter, this cyclically circulating component is
usually one of the reactants entering into the actual chemical
reaction but can be a solvent serving as the reaction vehicle With
this component circulating continuously in 85 cyclic fashion, a
reactant of relatively lower volatility is continuously and
progressively introduced into the reaction system at the top of the
reaction zone and is caused to flow downwardly in liquid form through
the fluid 90 passages in the reaction zone countercurrent to the
upflowing vapours Chemical reaction is effected in the counterflowing

streams and the reaction product flowing to the bottom of the reaction
zone is progressively withdrawn 95 either into a suitable receiver
below the reaction zone or out of the reaction system entirely.
The reactant of relatively low volatility thus undergoes essentially
inline flow from the 100 top to the bottom of the reaction zone where
it is withdrawn in chemically converted form.
This inline flow of one reactant combined with cyclic flow of another
component with a common area of counterflow through the 105 reaction
zone thus prescribes a reaction system which geometrically resembles a
circle and tangent, and the reaction systems of this invention have
therefore been named tangential reaction systems based on the flow of
110 the components during the process.
During the process of the invention, the reaction zone is maintained
at a temperature which is effective to maintain the upflowing vapours
in vapour form but which is ineffec 115 tive to cause substantial
vaporization of the less volatile reactant in the downflowing liquid
or of the product formed by the reaction.
The amount of reactant introduced at the top of the reaction zone for
downward flow is 120 correlated with the amount of product formed and
being withdrawn from the bottom of the reaction zone whereby the
conversion of this reactant is substantially complete When the
upflowing vapours are one of the actual re 125 actants, as is usually
the case, the flow of vapours is adjusted so that there is a large
excess of the vapours over the amount used in the reaction This tends
to drive the reaction to completion as regards the down 130 786,223
end below the normal liquid level in reservoir 17 A vent 19 opens out
of the lower end of condenser 16 for venting non-condensable gases to
the atmosphere.
The vaporizer assembly 13 desirably com 70 prises the reservoir 17 in
which the more volatile component is vaporized, and a suitable heater
20 for effecting continuous vaporization A stoppered inlet 22 permits
introduction of material being vaporized into 75 the apparatus as
necessary to maintain the supply of this component during the
reaction.
Column 10 and vapour inlet tube 12 are provided with a suitable
heating means such as the ribbon heater 23 which is wound 80 around
inlet tube 12 over its entire length and around column 10 at least
from the region of vapour inlet tube 12 to vapour outlet conduit 14 A
feed reservoir 24 adapted to hold a charge of reactant is mounted at
the 85 top of column 10 and opens into column 10 through orifice 25
for continuous gravity flow of reactant into the packed column The
flow rate from reservoir 24 into column 10 is adjusted by means of
valve 27 90 The lower end of column 10 opens into product receiver 28
whereby product is progressively and continuously withdrawn from the

reaction zone by gravity A withdrawal tube 29 provided with a suitable
valve 30 95 is arranged for withdrawing product from receiver 28.
In operating the apparatus illustrated in the accompanying drawing, a
relatively volatile component which is either a reactant or a 100
reaction solvent is charged into reservoir 17 and progressively
vaporized by heater 20 whereby a continuous flow of vapours into
column 10 through tube 12 is established.
Heater 23 is energized sufficiently to main 105 tain the reaction zone
in column 10 between inlet 12 and outlet 14 at a temperature effective
to maintain the vapours in vapour form.
The stream of vapours passes upwardly through the multiplicity of
tortuous con 110 stricted fluid passages formed by the packing 11 in
column 10 and exit through outlet conduit 14 The vapours emerging from
the column are continuously condensed in condenser 16 and flow
downwardly through con 115 duit 18 back into reservoir 17 for
revaporization Any non-condensable gases entrained in the vapour
stream are vented from the apparatus at 19.
When a continuous circulation of the vola 120 tile component in the
cyclic system has been established, the inline counterflow of the less
volatile component is begun by opening valve 27 from reservoir 24 The
less volatile component, in liquid form, flows downwardly 125 through
the tortuous constricted passages in the packing countercurrent to the
upflowing vapours whereby the desired reaction is effected The
temperature in the reaction zone is adjusted so that the downflowing
liquid 130 flowing reactant by displacing the equilibrium.
Once this flow of excess vapours is established, the vaporized
material is then also replenished at the rate the vapours enter into
chemical reaction and hence substantially complete conversion of both
reactants being added is accomplished Thus, when the reaction is
established and the relative rates adjusted, the process can be
carried on indefinitely with high conversions in short time and with
good uniformity of product.
Because the vapours circulate through the system, they provide the
required excess for shifting the reaction equilibrium without giving
large volumes of reaction mixture from which the product must be
recovered.
Instead the product is obtained in high concentration, and in many
cases, in sufficient concentration and purity for use without further
purification.
The present invention also provides apparatus particularly adapted for
carrying out chemical reactions of the equilibrium type in tangential
reaction systems In general, the apparatus comprises a packed column
through which upflowing vapours are channeled from a suitable
vaporizer assembly to a vapour outlet at the top of the reaction zone

which leads the vapours to a downwardly directed condenser from which
the condensed vapours are returned to the vaporizer assembly for
revaporization A suitable reservoir for the less volatile reactant is
arranged for progressive and continuous feed into the top of the
packed column and means are provided at the bottom of the packed
column for collecting product.
Apparatus of the present invention is illustrated in the accompanying
drawing which is a view in elevation, partly broken away and in
section.
Referring particularly to the drawing, a generally vertically disposed
tubular column 10, which can be constructed of glass or inert metal,
is filled with an inert packing material, such as glass helices as
indicated at 11 The nature of the packing is not critical and any of
the well-known column packing materials can be used such as variously
sized glass helices, glass beads, Berl saddles and similar packings
such as are commonly used in the distillation column art and which
permits fluid and vapour passage through the column along tortuous
constricted channels A vapour inlet tube 12 is arranged for channeling
vapours from a vaporizer assembly 13 into a lower zone of column 10 A
vapour outlet conduit 14 opens out of an upper zone of column 10 for
channeling vapours from column 10 into a downwardly directed condenser
16 Condenser 16 in turn is connected for gravity flow of condensate
into the reservoir 17 of vaporizer assembly 13 by means of condensate
conduit 18, the conduit 18 extending into reservoir 17 a sufficient
distance to 786,223 and product formed therefrom are not substantially
vaporized during travel through the reaction zone under gravity The
product formed is continuously removed by gravity from the reaction
zone into receiver 28.
The relative rates of introduction of the counter-flowing components
can then be adjusted by adjusting valve 27 from feed reservoir 24 and
by adjusting the vaporization rate in vaporizer assembly 13 The time
necessary for passage of the downflowing liquid through the packed
column will depend upon a number of factors including the viscosity of
the liquid at the reaction temperature, the length of the column and
the type of packing By a suitable correlation of these factors and the
proportions of reactant, it is often possible to effect substantially
complete reaction of the downflowing reactant in a single passage
through the reaction zone This completeness of reaction is also
assisted by employing the upflowing vapours in large excess whereby
the reaction equilibrium is shifted toward complete reaction of the
downflowing component Once the proper correlation of conditions is
achieved, the process can be maintained by progressive addition of
reactants at the rate of product withdrawal and substantially complete
conversion is continuously achieved.

The process embodying the invention is applicable for a variety of
chemical reactions including condensation, addition, and halogenation
In one of the embodiments of the present invention, a normally solid
material is melted and flowed downwardly in molten condition while
vapours of another reactant are passed upwardly countercurrent to the
downflowing melt A typical example of this type of reaction is the
formation of acid chlorides of normally solid fatty acids, as for
example those containing up to 18 carbon atoms Thus, for example,
palmitic, oleic or stearic acids can be flowed downwardly through the
packed column in liquefied form while thionyl chloride vapours are
passed upwardly through the column Reaction occurs in the few minutes
necessary for any increment of the fatty acid to pass downwardly
through the column, and a highly concentrated acid chloride of
excellent quality is continuously withdrawn from the bottom of the
column.
In another type of reaction, a solution of the less volatile reactant
is passed downwardly countercurrent to the upflowing vapours The
solution can consist of the less volatile reactant dissolved in
product obtained from the reactant, or in a suitable inert high
boiling solvent or in some of the more volatile reactants When crude
reaction product is used as solvent, any unreacted components in the
product get another chance to react and there is no large-scale
purification necessary to separate product from solvent as is the case
with an inert solvent In many cases, the solvent for the less volatile
reactant can actually have the same composition as the upflowing
vapours In this way the solvent also acts as a reactant and any
unreacted 70 portion tends to vaporize off in the lower zones of the
column and join the vapour stream.
Two normally liquid materials of different volatility can also be used
as counterflowing reactants Thus the normally liquid lower 75 fatty
acids or substituted fatty acids can be chlorinated by upflowing
thionyl chloride vapours One of the most interesting processes
embodying the invention involves the use of an inert solvent, suitable
as a reaction vehicle, 80 as the vaporised component which is
continuously circulated in cyclic fashion and a mixture of the actual
reactants is flowed downwardly through the column countercurrent to
the vapours acting as reaction 85.
vehicle Excellent reactions are effected in this way using reactants
which normally are reacted in solvent media In this embodiment where
the reaction vehicle is introduced into the reaction zone in the form
of vapour flow 90 ing in countercurrent to the reactants, the improved
reaction obtained may depend on improved heat transfer, stripping of
the downflowing liquid or mixing in the downflowing liquid or on more
than one of these factors 95 The small amount of condensed vapour also

assists in the downward flow of the reactants.
Some reactions are facilitated by the use of a suitable catalyst and
the catalyst can be introduced with the downflowing liquid, or, 100 if
relatively volatile, can be vaporized and included in the upflowing
vapour stream The latter condition is particularly advantageous since
the catalyst circulates continuously and does not contaminate the
product 105 The invention is illustrated but not limited by the
following Examples:EXAMPLE 1.
A mixture of 200 rml of thionyl chloride and 2 ml of quinoline was
charged into the 110 vaporizer reservoir of apparatus such as is
illustrated in the drawing The mixture was heated until a continuous
circulation of thionyl chloride was established, with the packed
column (containing 1/8 inch glass helices) 115 being maintained at a
sufficiently high temperature to keep the thionyl chloride vapours
from condensing in the column A solution of 2,4-di-tert amyl
phenoxyacetic acid (m p.
123-125 C) in four times its weight of 120 warm 2,-di-tert amyl
phenoxyacetyl chloride was progressively introduced at the top of the
column The rate of formation of crude product from a column 50 cm long
and 2 cm.
in diameter was 70 grams per hour The 125 product receiver was heated
with a heating mantle to continuously boil out entrained thionyl
chloride The crude product after being heated under reduced pressure
to remove all entrained thionyl chloride represented a 98 % 130
786,223and 9 4 parts by volume of water was progressively introduced
at the top of the column.
The reaction product withdrawn from the bottom of the column was
diluted with 200 volumes of water and acidified with 11 volumes of
concentrated hydrochloric acid.
After standing for one hour, the precipitate which formed was filtered
off, dried and recrystallized from 10 volumes of ligroin to give a 91
% yield of white crystals melting at 158 C This process, whidh forms a
valuable coupler for use in photographic applications, is represented
by the following equation:
yield of crude product which contained only about 1 % of free acid by
infrared determination This crude product was then distilled at
143-146 C and 2 mm pressure to give a nearly water-white product in a
final yield of 85 % based on the acid.
EXAMPLE 2.
A continuous circulation of acetone in the cyclic system was
established and then a solution of 10 parts by weight of 2,4-di-tert
amyl phenoxyacetyl chloride, 7 parts by weight of 2 amino 4,6 dichloro
5-methyl phenol hydrochloride, 8 3 parts by weight of dimethylaniline,
62 parts by volume of acetone OH C N HC 1 CH 3 3, Cl OCH2 COC 1 C 5 H

11 C 6 H 5 N(CH 3)2 OH 5 l cl HC COH 20;j C 34 C 5 H 11 + C 6 H 5 N(CH
3)2 H Cl Cl ( 2 ',4 '-di-tert-amyl-phenoxy)-acet-(
2-hydroxy3-5-dichloro-4-methyl)anilide The yield rate from a column 23
inches long and 1 inch outside diameter was 40 grams per hour.
EXAMPLE 3.
The preparation of palmitoyl chloride by a batch reaction usually
involves reactant contact times of 9-10 hours, and it is necessary to
subject the product to vigorous purification in order to obtain
light-coloured product In contrast to this, 50 grams of molten
palmitic acid was progressively passed downwardly through the packed
column of the apparatus of this invention countercurrent to thionyl
chloride vapours The palmitic acid was added at the rate of 120 grams
per hour A theoretical yield of palmitoyl chloride was obtained
showing no trace of unreacted palmitic acid with the time of passage
through the column being about 5 minutes for each increment of acid
Thionyl chloride entrained in the product was readily removed by
heating on a steam bath under reduced pressure The product was of
sufficiently light colour for many uses without distillation A single
distillation gave a water-white distillate of palmitoyl chloride
boiling at 110-115 ' C at 25 microns pressure.
EXAMPLE 4.
A continuous circulation of acetic acid was established through the
cyclic system A solution of 7 8 parts by weight of 1 P(
21,41,61trichlorophenyl) 3 m aminobenzamido-5pyrazolone and 6 2 parts
by weight of 2,4di-tert amyl phenoxyacetyl chloride in 75 volumes of
acetic acid was progressively added to the top of the packed column
and was converted to an amide, 1-l 21,41,61-trichlorophenyll 3-l -( 2
',4 '11-di-tert -amyl-phenoxyacetamido)-benzamidol -5-pyrazolone,
useful as a colour coupler, during passage through the column The
crude product was collected at the rate of 60 grams per hour from a
23inch column of 100 mm inside diameter.
Similarly, improved results are obtained with other reactions useful
in the art The size of the apparatus employed, of course, can be
varied depending on the desired volume to be processed.
The invention thus provides improved processes for effecting chemical
reactions continuously at high reaction rates with high yield of
product in which the conversion of at least one of the reactants is
substantially complete, while avoiding long contact times, the
necessity for large capacity reactors and other objectionable features
of batch and continuous batch processes.
The apparatus of the present invention can be operated continuously to
produce chemical reaction products of excellent uniformity over
prolonged periods of time without attention except for maintaining a
continuous supply of the reactants to replace the reactants used up in

the process.
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