5196 5200.output

* GB785603 (A)
Description: GB785603 (A) ? 1957-10-30
Sintering machines
Description of GB785603 (A)
PATENT SPECIFICATION
Inventor: HAROLD EARL ROWEN7 f i B y Date of Application and filing
Complete Specification: Sept 3, 1952.
No 22191/52.
> Complete Specification Published: Oct 30, 1957.
Index at acceptance:-Class 82 ( 1), 08 H.
International Classification:-C 22 b.
COMPLETE SPECIFICATION
Sintering Machines We, Ma DOWELL COMPANY INC, a corporation, organized
and existing under the laws of the State of Ohio, United States of
America, of 3203 West 711st Street, Cleveland, 2, Ohio, United States
of America, 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 a continuous sintering machine of the type
in which the pallets which carry the grates pass in continuous
succession over one or more windboxes.
In sintering machines of the above type the pallets are guided by
rails in an upper reach over the open upper ends of;a windbox or
windboxes, then pass over a "dead plate" which seals the pallets to
prevent passage of air The pallets 'are then guided by curved pants of
the rails to a lower reach extending below the windboxes to the
opposite end of the sintering machine, whereupon they are raised to
the upper reach, loaded with the material to be sintered, and again
pass over the windboxes.
As the pallets pass from the upper reach and about the curved rails,
they are inverted and their burden or load of sintered material is
permitted to drop out of them As each pallet passes onto and about the
curved porItions of the rails it slides by gravity through a short

space;and strikes the preceding pallet so as to, jar or jolt the
sintered material free from the pallet.
This invention provides a sintering machine having guide rails in
which the inverting of the pallets is effected at a higher level and
with a sharper turn and in, which an increased and more regular
gravitational effect is obtained.
According to the invention, there is provided a sintering machine
having pallet-supporting guide rails at each side of said machine,
said guide rails comprising an upper reach,;a lower reach, and a
connecting reach extending from said upper reach to said lPice 3 x 6 d
l lower reach in a compound curve, comprised by two merging arcuate
parts of different radii having its shorter radius at its upper part
and its longer radius at the part of the merging continuous curve
adjacent the lower reach The arrangement according to the invention
causes the pallets to be inverted at a higher level and with a sharper
turning movement to vertical position and then to continue downwardly
from this higher level on a more gradual slope and with improved
gravitational effects to, the lower reach for return to the loading
end of the machine.
The various features of this invention are illustrated by way of
example in the accompanying drawings in which: Figure 1 is a side
elevation of a,part of a sintering maichine embodying the invention
near the delivery end thereof; Fig 2 is a detail sectional view
showing the manner of mounting the guide rails; Fig 3 is a vertical
section of the sintering machine taken on line 3-3 of Fig 1.
In the embodiment of the invention shown in the accompanying drawings,
a sintering machine is provided with a, number of windboxes of which
the end windbox 10 is located near the discharge end of the machine
These windboxes may be provided' with outlet openings or passages 11
through which air is withdrawn, and with suitable clean-out doors 12.
A succession of pallets 1,3 witch may be of any usual or suitable
construction, pass over the windboxes fitting tightly against the
upper open ends thereof so that air is drawn downwardly through the
pallets to the windboxes.
The pallets are guided in their passage over the windbox '10 by pairs
of rails 14 and 15 at the sides of the windbox, each pair comprising
an upper rail 16 and a lower rail 17 between which pass wheels 118 The
rails 1,6 and 17 may be supported upon a framework indicated at 19.
After passing beyond the wind'box 10 the pallets may be sealed by a
dead plate" positioned 'at 20, Fig 1 After passing beyond the dead
plate the rail's 116 and 17 curve 85603 8.5 downwardly at 21 This part
of the rails is curved in a relatively sharp or large curvature the
radius being correspondingly short For example, in the embodiment
shown in Fig.

1 the centre of curvature of this part of the rails is the point 22
The same curvature extends approximately throughout a quarter turn,
bringing the pallets to a substantially vertical position.
As the rails continue downwardly their curvature is lessened as at 23
and continue at this lesser curvature or greater radius until the
curve joins the lower reach 24 of the rails For example the curvature
of the section 23 may be centered at the point indicated at 25, Fig 1,
thus a connecting reach is provided comprised by two merging arcuate
parts of different radii It will be apparent, therefore, that the
pallets are brought to a vertical position and thereafter begin to
become inverted at the level of the points 22 and 25, whereas if the
curve were constant or with -a constant radius the point at which they
reach a vertical position and begin to become inverted would be midway
between the upper and lower reaches and therefore much lower Moreover,
the sharpness of the upper quarter of the curve serves to bring the
pallet from the horizontal to the vertical position much more quickly
so that the rear or trailing end is quickly throwm forwardly as the
leading edge drops This -rapid swinging throws the looser material on
the top of the pallet forwardly, clear of the rails The pallet then is
in substantially vertical position as it drops into the lower more
gradual curvature of the part 23 and strikes the preceding pallet with
an impact distributed throughout the full areas of the colliding ends
of these pallets, thus avoiding a chipping or cutting of this face
that may occur with an edge to edge impact The emptying of the pallets
is therefore brought to a higher level as the material in the pallets
is jarred loose when a pallet moves from the position indicated at 26
to -that indicated at 27 through the short intervening space and
strikes the next preceding pallet.
Moreover, there is a continual gravitational effect from the higher
level of the points 22 and 25 at which the weight of thz pallets is
exerted downwardly on the return curve.
This gravitational effect is also more regular and effective in
returning the pallets along the lower reach of the guide rails to the
loading end of the machine.
As each pallet breaks from its horizontal position on the upper reach
into the curved portion 21 some of the material will spill.
To prevent such spilling onto the inverted 60 pallet a chute 28 is
provided between the upper and lower reaches and having a widened
hopper 29 to collect the spilled material and delivery it through the
chute to sidewise delivery openings 30 65 The guide rails may be of
any suitable construction As shown in detail in Fig 2 they may
comprise a supporting plate 31 having spaced sidewise extensions 32
and 33 on which the upper and lower rails 16 and 70 L 7 are securely
bolted The sidewise extensions may be braced at intervals by suitable

brackets 34 The rails may be assembled of short lengths arranged and
bolted end to end to form a continuous guide 75 Through the above
invention the return of the pallets to the loading end is made more
effective and the discharge of the sintered material takes place at a
level at which it may be more conveniently collected and handled 80
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* GB785604 (A)
Description: GB785604 (A) ? 1957-10-30
Improvements relating to wall-supporting structures for mines
785 o 604 Date of Application and filing Complete Specification Jan
26, 1954.
No 2310/54.
Application made in Germany on Feb 14, 1953.
9 9 g g / Complete Specification Published Oct 30, 1957.
Index at Accepmance: -Classes 89 ( 1), A( 6: 7); and 89 ( 2), G 3.
International Classification: -FO 6 b.
Improvements relating to Wall-Supporting Structures for Mines We,
GUTEHOFFNUNGSHUTTE 3 TERKRADE AKTIENGESELLSCHAFT, or
Oberhausen-Sterkrade/Rhld, Germany, a German body corporate, 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 wali-supporting structures for mines, and
more particularly to pit-shaft supporting structures, the individual

members of which are connected to one another by means of a connecting
disc and a clamping bolt or other clamping member.
It is well known that the work of extraction in underground workings
has anelfect on the existing excavations in the mine and the
wallsupporting structures which have to be provided within these
excavations Under the pressure exerted by the ground upon the
wallsupporting members, the later gradually depart from their original
positions and are displaced more or less relatively to one another
Such effects of extraction are particularly noticeable in the shafts
and especially in blind shafts, in which the erected structure and the
shaft guide poles are displaced from their correct positions.
For this reason, the guide poles must be reset from time to time in
order that they may be again restored to occupy as far as possible a
vertical position, so as to avoid disturbance of, or danger to, the
haulage operations taking place in the shaft.
It has been proposed to provide slots in the wall-supporting members
for the reception of the clamping bolts, so as to facilitate the
resetting operations Such slots, however, only permit of a very
limited amount of adjustment, so that the connections have to be
remade from time to time, for which purpose it is usually necessary to
bore a number of fresh holes for the fixing bolts and the entire
connection has to be shifted These operations are tedious and involve
an undesirably long interruption of the haulage operations.
The present invention has for its object to avoid these drawbacks and
to enable the connecting points of the wall-supporting members lPrice
3 s 6 d l to be displaced to a sufficient extent, not only in one
direction as by means of a slot, but in all directions in one plane in
order that the work of resetting the structure inside the shaft may be
facilitated and protracted interruption of the shaft haulage
operations may be avoided.
For this purpose, in accordance with the invention, in a mine
wall-supporting structure, more especially a pit shaft supporting
structure, individual members are connected together by means of a
connecting disc and a clamping member, for instance a clamping bolt,
the connecting disc comprising two disc members, one of which is
rotatably guided within the other, and the clamping member is arranged
on the inner disc member eccentrically with respect to the outer disc
member Such a connection, in contradistinction to a slot connection,
permits of adjustment with a range of up to 3600, so that the
adjustment is not limited in any direction.
It is advantageous to mount the inner disc member eccentrically within
the outer disc membr and the clamping member eccentrically with
respect to the inner disc member Adjustment is then possible, not only
by hand but also automatically under the influence of the soil

pressure, without any breakage occurring within the connection By
mounting one disc member rotatably within the other, if the forces
acting on the connection exceed a predetermined maximum value, the
connection is able to yield even without loosening the clamping
member, by relative rotation of the disc member under the action of
the said forces.
The invention is illustrated in the accompanying drawings, in which:
Fig 1 is a vertical section through one example of a connecting disc
made according to the invention; Fig 2 is a section of the line I-I of
Fig 1; Fig 3 is a front view of a mine wallsupporting member provided
with connecting discs according to the invention; Fig 4 is a section
on the line II-II of Fig 3; 785,604 Fig 5 is a front view showing the
manner of using the connecting disc according to the invention for
securing a bunton in position; and Fig 6 is a section of the line
III-III of Fig 5.
Referring to the drawings, within an outer disc member 1 is
eccentrically mounted an inner disc member 6 The disc member 1 is
inserted in a bunton 2 provided as shown in Fig 1 with a supporting
plate 8, prongs 4 or the like provided on the disc 1 being driven into
the bunton 2 so as to hold the disc member 1 more securely in position
The disc members 1, 6 are clamped to the bunton 2 and plate O by means
of a bolt 3 which passes through an eccentric hole in the inner disc
member 6 and is thus arranged eccentrically with respect to the inner
disc member As shown in Fig 1, the bolt 3 is provided with a
tightening nut 5 which, however, may be replaced by a quick securing
device, for instance in the Dorm of a cotter or wedge fastening.
After slackening off the nut 5, and withdrawing the prongs 4 from the
bunton 2, the outer disc member 1 can be rotated around the inner disc
member 6 and, it required, the inner disc member 6 can be rotated
around the bolt 3, for instance into the position shown in dot and
dash lines in Fig 2 The double eccentric adjustment thus provided
permits of accurate adjustment of the outer disc member 1 into any
desired intermediate position within the limits of adjustment provded
by a complete revolution of the respective disc members 1 and 6,
including displacement in only one direction, e.g in the vertical
direction without accompanying displacement in the horizontal
direction, i e sideways If rotation, for instance of the outer disc
member 1 around the inner disc member 6 produces displacement of the
member 1 in both directions, i e vertically and horizontally, any
undesired displacement in the horizontal direction can be compensated
by rotating the inner disc member around the bolt 3.
The inner disc member 6 can also rotate within the outer disc member l
around the bolt 3 under the forces due to working of the ground
resulting from excavation operations.

Figs 3 and 4 illustrate by way of example the connection to one
another of two shaftsupporting frames or rings 9 by means of a strut
10 with the use of connecting discs according to the present invention
The strut is provided at each end with a lug 11 which receives the
outer disc member 1 within which is eccentrically mounted the inner
disc member 6, the member 1 being rotatable in the lug 11, which lugs,
upon angular movement of either disc or both discs will be displaced
with respect to the bolt 3 The clamping bolt may be rigidly connected
to the supporting frame 9, which may together with the member 1 be
provided with a roughening, grooving or the like in order to increase
the adhesion between them Fig 3 shows the clamping bolts 3 at the ends
of the strut 10 offset out of line with one another and clearly
discloses the adjustability of the members mounted in the pit 70
shaft.
In Figs 5 and 6 is shown the use of the connecting disc according to
the invention for connecting a shaft-supporting frame or ring 12 with
a bunton 2, the arrangement being 75 similar to that shown in the
upper part of Fig.
3 The wall of the shaft in Fig 6, as well as in Fig 4, is designated
14.
The connecting discs according to the invention permit of a reduction
as well as of an 80 increase in the distance between two supporting
frames or rings For this purpose it is not absolutely necessary to
slacken off the nut 5, since even if the bolt 3 is tightened up, the
inner disc member 6 can yield through rotation, 5 in the outer disc
member 1 and thereby allow dtlz cennection to adjust itself
Furthermore, it is possible at any time to effect adjustment by hand,
namely after slackening off the nut 5, and to an extent amounting up
to 360 90 A special advantage of this invention is that any lack of
truth in the wall of the holes in the guide poles which have been
bored above ground can be conveniently taken care of while erecting
the poles in the shaft, as well as any 95 lack of truth of the holes
relatively to one another in the transverse direction of the guide
poles There is therefore no difficulty in subsequently adjusting the
guide poles lengthwise of the buntans in the event of any deviation
100 from the vertical.
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* GB785605 (A)
Description: GB785605 (A) ? 1957-10-30
Improvements in or relating to data recording apparatus
Inventor: DANIEL BROIDA 7 C@ Date of Application and filing Complete
Specification: Feb 16, 1954.
No 4512/54.
Complete Specification Published: Oct 30, 1957.
Index at acceptance:-Classes 100 ( 4), C 2 OA; and 106 ( 1), M( 1 X: 5
A).
International Classification:-B 41 j G 06 k.
COMPLETE,SPECIF If CATION Improvements, in or relating to Data
Recording Apparatus We, THE BRITISH TABULATING MACHINE COMPANY
LIMITED, a British Company of 17 Park Lane, London, W 1, 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 apparatus for recording data in such a way
that, in a single operation, a document is produced in a form which
allows of manual or machine processing.
It is well known to record data by means of holes punched in a
statistical card or a tape.
The data is then sensed, by electrical or mechanical means, to control
a counter or a multiplying mechanism, for example Thus such a form of
recording is particularly adapted for machine processing.
On the other hand, it is inconvenient to have to read punched data
visually, when it is required, for example, to manually process the
data by selecting cards by hand from a master file It is usual to feed
such cards, after punching, through an interpreter, which prints the
equivalent of the punched data along the top edge of each card, to
provide visually readable characters.
The present invention resides in a recording member adapted to record
on a document at least one visually readable character and a coded

representation of such character for reading by a machine, the
representation-forming part of said member being constituted by a
plurality of bar-like elements indicating a plurality of predetermined
code localities on the face of said member, and a further barlike
element or elements disposed in one or more of said localities in
accordance with the representadtonal code employed.
The invention also provides recording apparatus which includes a
plurality of recording members each adapted 'to record on a document
one or more visually readable characters and a coded representation of
the or each such character for reading by a miachine, the or each
representation-forming part of each member being constituted by a
plurality of bar-like lPrt 1 elements indicating a plurality of
predetermined code localities on the face of said member, and a
further bar-like element or elemenits disposed in one or more of said
localities in accordance with the representational code employed.
The invention will now be described, by way of example with reference
to the accompanying drawing, in which: Figure 1 is a perspective view
of a type slug; Figure 2 shows in enlarged form, part of a document
which has had data recorded thereon; Figure 3 shows an elevation view
of a type wheel; Figure 4 shows, in enlarged form, part of a document
which has had data recorded thereon by type wheels of the kind shown
in Figure 3; Figure 5 shows, in enlarged form, part of a document
which has had data' recorded thereon in a modified form.
The invention is particularly suitable for recording data, such as a
serial number, on documents of the general category of cheques, money
orders, postal orders etc It is necessary to have the serial number
easily readable for the convenience of the issuing office or the user.
A Mt the same time, the number is desired in a form suitable for
machine processing, to allow documents to be automatically sorted,
and/or listed.
A machine for sorting cheques and similar documents is shown and
described in specificaition No 740 Q 65,6 The serial, number, or other
data is printed on the cheque and is also represented by holes punched
in a selected part of the cheque, in accordance with a code employing
two' out of five elements for each character Although the cheque can
be processed manually and by a machine, the method of recording
involves separate printing and punching operations which increases the
cost of production and introduces the possibility of disagreement
between the data recorded by the two methods.
A type slug 1 (Figure 1), such as that of a typewriter, has formed
thereon, in the usual FM 605 manner, a character 2 In addition, the
slug carries five timing bars 3 which indicate or define five
predetermined code localities In any of these localities, a, code bar
or bars 4 may be disposed to represent the value of the character 2 in

the code employed It is convenient to have each code bar as a
continuation of the timing bar which defines the locality in which the
code bar is disposed, as shown in Figure 1, but they may be separate.
A document 5, with a ten digit number printed on it, using a
typewriter having type slugs similar to that of Figure 1, is shown in
Figure 2 This illustrates one "two element out of five" code which may
be used Since a printed character 2 a, corresponding code marks 4 a
and timing marks 3 cr are all printed simultaneously by one type slug,
there is no possibility of an error in coding and the recording
operation requires the minimum of time.
The code marks 4 a and the timing marks 3 a may be sensed by an
arrangement similar to that shown in the above-mentioned
specification, the optical system being modified to operate on a
decrease in reflected light, instead of an increase in transmitted
light Since five timing marks 3 a are printed, the plate acting as a
slit for the timing photo-cell has one -hole only, which is positioned
to allow sensing of the timing marks As the document 5 is fed through
the sensing position, the recorded digits will be sensed in turn to
operate two counting gas tubes for the timing and code marks In the
case of the perforated cheques, the timing mark allowed the sensing to
be independent of the exact timing of the cheque feed and also
provided a means for eliminating errors in sensing which might be
caused by additional holes or marks The timing marks 3 a serve an
additional purpose in that they ensure correct sensing of the code
marks 4 a even if the characters 2 ai are not evenly spaced, owing ito
uneven wear on tlhe carriage escapemient of the typewriter, for
example.
If the data is being entered into an accumulator, it may be more
convenient to sense all denominations of a number simultaneously.
This would necessitate an arrangement for simultaneously scanning all
the digit positions of the document 5 This disadvantage is overcome by
turning the marks through a rightangle relative to each character and
placing them beside the character, so that the printed result is as
shown on a document 6 (Figure 4).
If this document is fed in a direction at rightangles to the lines of
characters, all the denominatlons of a number may be sensed
simultaneously by an appropriate number of photocells.
By employing a multiple wheel printer, of the kind used in punched
card tabulating machines, all the digits of a number may be printed
simultaneously Each type wheel 7 (Figure 3) carries the characters 0
to 9 and the associated code bars and timing bars.
Alternatively, the wheels may be replaced by type bars, each of which
carries ten type slugs.
In some applications, the wider spacing between characters, required

by the form of printing shown in Figure 4, may be a disadvan 70 tage
To avoid this, the timing and code bars on the type slug or wheel may
be re-arranged relative to the character to provide a printed document
10 (Figure 5) in which the space between characters may be
substantially the 75 same as that for the document 5 Timing marks 3 b
and code marks 4 b are printed below each character 2 b, instead of
beside the character, as in Figure 4 A start mark 8 is printed between
the character 2 b and the first 80 of the timing marks 3 b, and a stop
mark 9 is printed after the last of the timing marks.
The two marks 8 and 9 extend beyond the area occupied by any of the
characters 2 b and they are sensed by an additional photo-cell 85 The
first pulse from this cell is used to make effective the cells which
sense the marks 3 b and 4 b in much the same way as the edge of a
cheque is used to control the sensing in the Specification already
referred to The second 90 pulse from this cell renders the sensing
cells ineffective The third pulse renders them effective again, to
read the second number, and so on, alternate pulses rendering the
cells effective and ineffective This control by the 95 marks 8 and 9
prevents the generation of spurious pulses when the characters 2 b
pass the sensing photo-cells.
The use of two code elements out of five for each character is
convenient for expressing 100 decimal values The same principle may be
extended to alphabetic data or 'to sterling values.
For example, the use of -two code elements out of eight provide
sufficient combinations for coding the letters of the alphabet 105 For
the majority of application, recording of the data by a normal
print-ig process is sufficient When it is desired to provide the
greatest possible protection against subsequent alteration of recorded
data, the code and tim 110 ing bars may be made to project, beyond the
face of the type member, sufficiently far to cause embossing of the
document The embossed marks may then be used to control the sensing
mechanism Alternatively, a special 115 printing ink may be used so
that the marks hiave a property, such as fluorescence or
ferromagnetism, which will effect a suitable sensing mechanism.
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* GB785606 (A)
Description: GB785606 (A) ? 1957-10-30
Improvements in or relating to louvre ventilators
7855606 7 iventoi's':-GWYNFOR JENKINS and STANLE 6 Y ARCHER WINTERTON
DRAKE.
Date of filiny Comr plete Specifcation: Feb 22, 1954.
A 1 ppitcation Dale Feb 23, 1953 No 4937153.
Complete k S Ipecfication Pablished: Oct 30 195 ?.
Index at Acceptance:-Class 137, A(ID 1 F: 202).
International Classification: li.
COMPLETE SPECIFICATION.
Improvements in or relating to Louvre Ventilators.
We, PEARMAN BRIGGS LIMITED, a British Company, of Cainscross, Stroud,
Gloucestershire, 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 louvre ventilators more especially though
not exclusively for vehicles, such for example as the Molly croft or
lantern roof lights of a caravan.
Due to the small height of the vertical panels of the Mollycroft or
lantern roofs of caravans it is a matter of some difficulty to
accommodate suitable ventilators therein since the framing of the
louvre has to be inset from the edge of the panelling at the top and
bottom and, after the width of the framing has been taken into
account, very little vertical height remains for the louvre panel
itself Such louvre panel is usually transparent so that the ventilator
also forms a roof light or window.
According to the invention the foregoing 23 difficulty is overcome by
the provision of a louvre ventilator comprising a shroud in the form
of a frame open at the front and back which snugly fits into the
opening in the panelling or wall to form a thin lining for such
opening, said frame having a narrow inwardly turned flange or lip at
its front edge, and a louvre panel which in its closed position lies

against the inner surface of said inwardly turned flange or lip to
close the opening at the front of the frame and is capable of being
turned about its lower edge, away from the inwardly turned flange or
lip in the direction of the back, to an open position in which it
slopes 4 o upwardly and away from said surface.
The aforesaid shroud is preferably constituted as a pressing or
moulding in light gauge material having an outwardly turned lPrice 3 s
6 d 1 rr 4 c,l flange at its open back which overlies the material of
the panelling and enables the shroud to be secured to the latter If
desired the shroud may also comprise lug portions which form stops
enabling the louvre panel to be retained in its open position and
which locate the louvre panel in such manner as to avoid the necessity
for a hinge.
Preferably the louvre ventilator also comprises an external canopy in
the form of a flanged shallow dish open along its lower end, such
canopy being secured to the outside of the panelling to overlie the
opening in the latter and extend downwardly below the lower edge of
such opening so that, with the louvre panel open, air is enabled to
enter while rain is excluded When the ventilator is also required to
constitute a window the louvre panel is of transparent material, for
example clear acrylic resin sheet, and the shroud may also be of
plastic, for example polyvinyl chloride, sheet moulded to shape If
desired the external canopy may also be moulded from acrylic resin.
By reason of the invention a satisfactory louvre ventilator is
provided which is completely draught-proof regardless of weather
conditions, as air passing therethrough is deflected upwardly by the
louvre panel, and which is moreover effective in the prevention of
condensation, for example in the interior of a vehicle to which the
louvre ventilator is fitted In addition the ventilator is capable of
rapid and economical manufacture and incidentally also reduces
assembly costs inasmuch as the rough machining of the opening in the
panelling is automatically concealed by the aforesaid shroud so that
the usual cleaning or finishing operations reauired on the opening are
eliminated Furthermore the construction 785,606 of the louvre
ventilator is such that the masking of the opening in the panelling
when spray-painting the panel is considerably simplified; moreover the
louvre panel a is completely removable to provide easy access to the
external canopy for cleaning purposes.
The application of the invention to a Mollycroft lantern roof light
and ventilator for a caravan will now be described, by way of example,
with reference to the accompanying drawings, in which: Figures 1 and 2
are respectively rear and frontal perspective views of the shroud ajid
also show the louvre panel in the open position; Figure 3 is an end
elevation of the shroud and external canopy mounted in and on the

panelling; and Figure 4 is a front perspective view of the external
canopy removed.
Referring to Figures 1 to 3 of the drawings, the shroud 10 is
constructed as a pressing in thin sheet meterial of the same shape as
the opening in the vehicle body panelling so that it forms a lining
for such opening.
Usually there are four such openings along each side of the lantern
roof, the openings being customarily of elongated rectangular c)
shape, in which case the shroud is also rectangular in shape as
illustrated It is advantageously constructed as a pressing in light
gauge polyvinyl chloride sheet material, preferably white in colour to
enhance the appearance of the finished window The shroud 10 is open at
the front and back, i e.
at the outside and inside respectively, and the depth of the shroud
from front to back corresponds to the thickness of the vehicle body
panelling 11 adjacent the window opening 12 formed therein, as shown
in Figure 3 The shroud 10 has a narrow inwardly turned flange or lip
13 at its outer or front edge 10 a against the inner surface 4 S of
which the closure or louvre panel 14 lies in the closed position of
the window.
At its inner edge the shroud 10 is formed with a wider outwardly
turned flange or lip which, when the shroud is fitted into ao the
opening 12 in the body panelling 11, lies against the inner surface 1
la of such panelling and may be tacked or otherwise secured thereto to
hold the shroud in position The main or central portion 16 of the
shroud section lying between the flanges or lips 13, 15 slopes
outwardly to enable the shroud to be easily pressed into the window
opening 12.
Cemented or otherwise secured to the inner surface of each vertical
end portion 16 a of the shroud is a lug 17 of the same material, such
lugs being substantially triangular or sector-like in shape and
provided at their inner inclined edges with a laterally turned flange
or lip 18 which flanges or lips face towards each other and form a
stop or rest to locate the louvre panel 14 in its open position The
vertical edges 17 a of the lugs 17 are disposed parallel to the inner
surface of the inwardly turned front flange 7, or lip of the shroud,
and at such short distance therefrom as to leave a vertical channel 19
therebetween, as shown most clearly in Figure 3 In this channel the
louvre panel 14 lies in the closed position of the 75 window The panel
14 is formed by an elongated substantially rectangular sheet of
PERSPEX (Registered Trade Mark) which has a narrow portion cut away
from each vertical side edge 14 a to leave a short trans so versely
projecting tongue 20 at the upper end of each side edge above the
upper edge of the lug 17 This tongue falls into the vertical channel

19 already referred to in order to hold the panel 14 in its closed 55
position The lower edge of the panel 14 at each end thereof rests
freely in the corner or angle formed between the lower ends of the
inwardly turned flanges or lips 18 of the lugs 17 and the inner
surface of the in lij wardly turned flange or lip 13 of the shroud
whereby a free hinge arrangement is provided for the panel At its
centre the latter has a short strip 21 of PERSPEXcemented thereto
edge-on in order to form a handle i by which the panel may be raised
to lift the tongues 20 clear of the vertical channel 19 and enable the
panel to be turned to its open position.
As shown in Figures 3 and 4, the com I i} bined window and ventilator
is completed by an external canopy 22 which is also of elongated
substantially rectangular shape and of slightly larger dimensions than
the shroud This canopy is adapted to be 14 ll secured to the outer
surface of the body panelling 11 over the window opening 12 therein in
order to render the window draught and weather-proof Like the louvre
panel 14 of the window the canopy 110 22 is also of transparent
material, for example acrylic resin sheet, which is pressed to formn a
shallow dished tray open along its lower longer edge 23 and flanged,
as shown at 24, along its remaining three sides The 113 flange 24 is
provided at spaced intervals with countersunk bores 25 to permit
attachment of the canopy to the body panelling, as by means of wood
screws 26 By reason of the somewhat greater vertical dimensions 124 of
the canopy 22, as compared with the shroud, -the open lower end of the
former 23 depends below the bottom of the shroud 10, as will be seen
in Figure 3, and consequently prevents entry of rain or draught 125 It
will be understood that the louvre panel 14 can be lifted from the lus
17 which retain it in position so that the panel is completely
removable for cleaning purposes and, with its removal, cleaning of the
inside 13 o 785,606 of the transparent canopy 22 is also facilitated.
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* 5.8.23.4; 93p
* GB785607 (A)
Description: GB785607 (A) ? 1957-10-30

Manufacture of organic hydroperoxides
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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.
Manufacture of Organic Hydroperoxides
We, THE DISTILLERS COMPANY LIMITE, a British Company of 12, Torphichen
Street,
Edinburgh 3, Scotland, 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 present invention relates to the oxidation of meta-and
para-diisopropylbenzene to give the corresponding dihydroperoxides,
and is supplementary to and a modification of the process described in
our copending British application Nos. 21225/52 and 7433/53,
Serial No. 727,498.
In our copending British application Nos.
21225/52 and 7433/53, Serial No. 727,498 is described a process for
the production of diisopropylbenzene dihydroperoxides which comprises
reacting meta-and/or para-diisopropylbenzene in the liquid phase at
elevated temperatures with molecular oxygen to produce a concentration
of monohydroperoxide of at least about 45% by weight, contacting the
oxidate with a non-acidic aqueous solution to extract the
dihydroperoxide, which may subsequently be recovered from the aqueous
extract, and subjecting the residue of the oxidate to further
oxidation, preferably with the addition of fresh diisopropylbenzene in
suicient amount to keep constant the total volume in the system. The
process may be operated under fully continuous or semi-continuous
conditions.
When an oxidation reaction of this type is continued for a protracted
period the rate of production of dihydroperoxide on the basis of a

constant reaction volume decreases progressively. This appears to be
due to the build up in the oxidate of undesirable by-products which
are not extracted by the non-acidic aqueous solution and which
interfere with the oxidation reaction. The resulting fall in rate may
be very slow but ultimately makes it necessary to stop the oxidation
and to remove in one way or another the interfering products.
It has now been discovered that commercial diisopropylbenzene, which
consists mainly of a mixture of the meta-and para-isomers, contains
varying amounts of 1: 1: 3-trimethylindane, and that the higher the
trimethylindane concentration in the diisopropylbenzene fed to the
oxidation reactor, the more rapid is the progressive decrease in the
oxidation rate of the diisopropylbenzene. This was surprising since
experiments had shown that trimethylindane was oxidised more rapidly
than metaor para-diisopropylbenzene, and that it would not be expected
to accumulate. However, it appears that it is converted to oxygenated
organic compounds which are not extracted by the non-acidic aqueous
solution.
In addition to trimethylindane, commercial diisopropylbenzene contains
small amounts of ortho-diisopropylbenzene, the presence of which is
also undesirable since it is substantially inert in the oxidation
reaction for the production of hydroperoxides. However, attempts to
separate off the trimethylindane and the ortho-diisopropylbenzene by
normal distillation techniques were not successful owing to the
proximity of the boiling points of these compounds (205 and 203.7 C.
respectively) to the boiling points of meta-and
para-diisopropylbenzene (203.2 and 210.4 C. respectively), and even
after fractionation in a highly efficient fractionating column it was
not possible to obtain meta-and para-diisoproylbenzene fractions
completely free from both trimethylindane and
ortho-diisopropylbenzene.
This finding is confirme by Melpolder et al,
J. Amer. Chem. Soc. 70,935,1948, in their study of the isolation and
physical properties of the diisopropylbenzenes. These investigators
found that"a combination of distillation, fractional crystallization,
adsorption, sulphonation, and hydrolysis"was required for complete
separation of pure isomers. However, they were more concerned with the
purity of the isomers separated than with a practical process for
their production, and they did not concern themselves with the
by-products in the diisopropylbenzene fraction which made separation
difficult, nor did they concern themselves with means for avoiding
these by-products, or their effect on a subsequent oxidation process.
It has further been discovered that metaand para-diisopropylbenzenes,
which are produced by the alkylation of benzene or isopropylbenzene
for instance with propylene, may be obtained substantially free from

both trimethylindane and ortho-diisopropylbenzene by carrying out the
alkylation in the presence of specific amounts of aluminium chloride
and within a specified temperature range, and that the rate of
oxidation of meta-and para-diisopropylbenzene prepared in this way can
be maintained at a comparatively high level for long periods.
Accordingly, the present invention comprises the process for the
production of diisopropylbenzene dihydroperoxides by reacting
metaand/or para-diisopropylbenzene in the liquid phase at elevated
temperatures with molecular oxygen to produce a concentration of
monohydroperoxide of at least about 45%, by weight, contacting the
oxidate with a nonacidic aqueous solution to extract the
dihydroperoxide and subjecting the residue of the oxidate to further
oxidation, characterised by the use as feed of diisopropylbenzene
which is substantially free from trimethylindane and
ortho-diisopropylbenzene and which has been produced by the alkylation
of benzene or isopropylbenzene, or by the disproportionation of
ortho-diisopropylbenzene or polyisopropylbenzene in the presence of
aluminium chloride as catalyst under reaction conditions whereby
substantially no trimethylindane or ortho-diisopropylbenzene are
produced.
The meta-or para-diisopropylbenzene starting material for the
oxidation reaction of the present invention is produced by the
catalytic alkylation of benzene, isopropylbenzene, or mixtures of the
two compounds, as such or dissolved in an inert solvent, using as
alkylating agent propylene, n-propanol, isopropanol, or isopropyl
chloride, in the presence of aluminium chloride, under conditions
which are specified hereinafter. The alkylating agent, which is
preferably propylene, is mixed with the benzene or isopropylbenzene in
an amount which is preferably slightly less than the stoichiometric
quantity required for the theoretical reaction. Thus, if benzene alone
is used as starting material the optimum molar ratio of propylene to
benzene has been found to be about 1.98: 1.
Alternatively the meta-and para-diisopropylbenzene starting material
is produced by the catalytic disproportionation of tri-, tetra-or
higher isoproplbenzenes, hereinreferred to collectively as
polyisopropylbenzenes ; or by the disproportionation (i. e.
isomerisation) of ortho-diisopropylbenzene, in the presence of
aluminium chloride under conditions which are specified hereinafter.
The essential feature of the alkylation or disproportionation process
is that isomerisation should take place resulting in the production of
a mixture which is in equilibrium both with respect to the proportions
of benzene and of mono-, di, tri-, and tetra-isopropylbenzenes, and
with respect to the proportions of ortho-, meta-, and
para-diisopropylbenzenes, the proportion of ortho-diisopropylbenzene

being substantially zero, while at the same time avoiding the
production of any appreciable amount of trimethylindane, the formation
of which is apparently irreversible. The critical conditions necessary
to achieve this result are the temperature range and the amount and
type of catalyst used, and these variables are to a great extent
interrelated.
Temperatures for alkylation and disproportionation reactions with
aluminium chloride generally range from room temperature to about 150
C. We have found, however, that it is only in the limited temperature
range of about 40 to 115 C., and preferably from about 60 to 80 C.,
that it is possible to obtain efficient production of meta-and
paradiisopropylbenzene substantially free from trimethylindane and
ortho-diisopropylbenzene.
Furthermore, the desired result will only be obtained within this
temperature range if the reaction time and the amount and type of
catalyst used are suitably adjusted for any particular temperature.
The aluminium chloride catalyst for the alkylation or
disproportionation reaction may be activated, if desired, by treatment
with reagents such as hydrogen chloride or isopropyl chloride. In
general, with activated catalysts, while maintaining the temperature
within the preferred range, the reaction time should be shorter, and
the amount of catalyst lower than with unactivated catalysts,
depending mainly on the degree of activation. In general an amount
between 0.1 and 12 moles per cent of aluminium chloride based on the
benzenoid starting material may be used. It is desirable to use the
lower concentrations of aluminium chloride catalyst ir. the range set
forth with the higher temperatures in the range set forth, and vice
versa. The degree of activation must also be taken into account, the
more highly activated the catalyst, the lower the amount of catalyst
which will be required ; with activated catalysts generally
proportions in the range 0.1-2.0 moles per cent are suitable.
The activation of the catalyst may be carried out by conventional
methods. It is preferred to use a liquid ternary complex alkylation
catalyst, AlC1-HCl-alkaryl hydrocarbon, prepared by sparging a stirred
mixture of e. g. cumene and aluminium chloride with hydrogen chloride.
Alternatively, the complex may be made by agitating a mixture of 1
mole of cumene or polyisopropylbenzene and 1 mole of aluminium
chloride while-mole of isopropyl chloride is gradually added. The
degree of activation is controlled by the proportion of hydrogen
chloride or isopropyl chloride added.
The presence or absence of tri-methylindane and
ortho-diisopropylbenzene may be detected by infra-red absorption
analysis.
It has been noted above that the alkylating agent, which is preferably

propylene, is mixed with the benzene or cumene in an amount which is
preferably slightly less than the stoichiometric quantity required for
the theoretical reaction, this being well known in the art for the
production of the optimum yield of diisopropylbenzene with a minimum
of mono-and poly-isoproylbenzenes. However, alternatively, mono-and
poly-isopropylbenzenes may be produced in larger amounts if their
simultaneous production is required.
Moreover, the mono-and poly-isopropylbenzenes obtained as by-products
may be recycled to the propylation step, or to a disproportionation
step in which they are contacted with aluminium chloride under the
reaction conditions set out above to ensure the non-production of
ortho-diisopropylbenzene and trimethylindane, to produce further
amounts of meta-and para-diisoproylbenzene.
Furthermore, where it is desired to produce either meta-or
para-diisoproylbenzene solely the unwanted constituent of the
equilibrium mixture may be separated off by distillation and recycled
to an isomerisation step, carried out in the presence of aluminium
chloride under the reaction conditions described above to produce an
equilibrium mixture containing a further proportion of the desired
constituent.
Before being oxidised the resulting product is desirably first treated
to remove the catalyst, for instance by treating with dilute aqueous
hydrochloric acid and washing with water.
Alternatively, the catalyst may be removed by hydrolysis with water
followed by filtration, or by washing with an excess of alkali, or by
centrifuging, decanting or filtering.
The mixture of meta-and para-diisopropylbenzene produced as described
above may be used as such in the oxidation reaction according to the
process of the present invention, when a mixture of the corresponding
hydroperoxides will be produced. Alternatively the mixture of isomeric
diisoproylbenzenes may be fractionated to isolate the two isomers and
these fractions may be used in the oxidation. The starting material
for the oxidation advantageously contains a small proportion of
hydroperoxide or other initiator for the reaction. This is
conveniently added as a diisopropylbenzene oxidation product from a
previous oxidation.
In the oxidation reaction the trimethylindane-free diisopropylbenzene
is reacted with molecular oxygen, the dihydroperoxide so produced is
extracted from the oxidate with a non-acid aqueous solution and the
residue of the oxidate is subjected to further oxidation.
The steps of oxidising and extracting may be carried out alternatively
or concurrently. In the former case they may be repeated several times
since the"oxygen efficiency,"that is the ratio of moles of
hydro-peroxide produced to moles of oxygen absorbed, is surprisingly

maintained at a high level for a long time.
If the process is carried out in a concurrent manner the
diisopropylbenzene and oxygen are continuously or intermittently
supplied to the reaction zone, the dihydroperoxide is continuously
extracted from the oxidate and the residue of the oxidate is returned
to the reaction zone.
The molecular oxygen may be in the form of pure oxygen, or of a
gaseous mixture containing oxygen, such as air, and may with advantage
include a proportion of ozone. When using dilute oxygen it is
advantageous to employ super-atmospheric pressure. It is advantageous
to adjust the quantity of oxygen-containing gas in such a way that an
excess of oxygen over that absorbed by the reaction mixture is
introduced therein. The excess may vary within wide limits. It has
been found that it is advantageous to have an excess of at least 10%.
It is preferred to perform the oxidation in the presence of alkaline
substances, such as the oxides or hydroxides of the alkali and
alkaline earth metals, or their salts with weak inorganic or organic
acids, such as the carbonates, bicarbonates, or acetates, or in the
presence of other basic substances such as ammonia in order to prevent
the development of excessive acidity. Excess of alkali should however
be avoided and preferably only so much should be added as will give a
pH value of between about 6 and 10 in an aqueous phase in equilibrium
with the oxidate. Where a concurrent alkali extraction of the
dihydroperoxide is being employed, as is described below, the
resulting raffinat which is recycled to the oxidation reactor, usually
contains small amounts of alkali and this is normally sufficient to
maintain the pH of the reactor contents at between 6 and 10, acidic
by-products being neutralised and continuously removed from the
oxidate during the alkali extraction.
The oxidation reaction may be carried out within a wide range of
temperatures, for instance 50 to 150 C. When the reaction is carried
out in the homogeneous liquid phase suitable temperatures are between
70 and 120 C. and preferably between 80 and 110 C., at normal
pressure. Under heterogeneous conditions, for instance in the presence
of water, temperatures between 80 and 95 C., and preferably about 90
C., have been found to be suitable at normal pressure. The reaction
may be carried out at atmospheric pressure, or at superatmospheric
pressures, with consequent widening of the temperature range, or at
subatmospheric pressure.
The dihydroperoxide is separated from the oxidate by extraction with a
non-acidic aqueous solution, i. e. a solution having a pH value of
above about 7. It has been found that the dihydroperoxide is
relatively soluble in such solutions, whereas the monohydroperoxide
and the diisopropylbenzene starting material are relatively insoluble

and remain in the oxidate.
Extractants which may be used include most non-acidic or basic
inorganic solutions such as, for instance, aqueous solutions of
alkaline or alkaline earth metal hydroxides, carbonates or
bicarbonates, or of the salts of these metals with weak inorganic or
organic acids. The use of aqueous sodium hydroxide is preferred.
The concentration of the alkali solution used as extractant may vary
within wide limits, and the optimum concentration for any particular
alkali may readily be determined by one skilled in the art. Thus for
sodium hydroxide concentrations of up to 15% weight/volume are
suitable and preferably between 1 and 8% weight/volume. Higher
concentrations, for instance up to 25% weight/volume, may be used if
desired, but at these concentrations precipitation of the sodium salts
of the mono-and di-hydroperoxides is liable to occur.
When the oxidation is carried out in the presence of water the oxidate
may be separated from the aqueous phase before being extracted.
The extraction may be carried out by methods known in the art on a
part or the whole of the oxidate, which may be at, or preferably
below, the oxidation temperature.
Advantageously, a counter-current process may be used, for example, in
a column, or a series of vessels, the raffinat from which part or all
of the dihydroperoxide has been removed being recycled to the
oxidizer. In this way more dihydroperoxide and less monohydroperoxide
are extracted per part of extraction solvent.
The dihydroperoxide can also be isolated if the extraction is carried
out with an amount of alkali which is insufficient for the extraction
of the whole of the dihydroperoxide but under these conditions
difficulties in phase separation may be encountered if the aqueous
phase becomes saturated with dihydroperoxide.
Where an intermittent process for the extraction of the oxidate is
being employed this is desirably carried out to such an extent that
the dihydroperoxide content of the oxidate remains below 25%
weight/weight. If the extraction process is a continuous one the
dihydroperoxide content of the oxidate is desirably kept below 10% and
where the starting material is para-diisopropylbenzene preferably
below 5%, to avoid crystallisation of the paradihydroperoxide from the
reaction mixture in the extraction train, due to its low solubility.
Although the extracting solution is selected so that the
monohydroperoxide is substantially insoluble in it, small amounts of
the monohydroperoxide may be taken up by the solution and these may
contaminate the recovered dihydroperoxide. It is, therefore, preferred
to re-extract the aqueous alkaline extract with a solvent for the
mono-hydroperoxide, for instance benzene or, preferably,
diisopropylbenzene.

Similarly, small amounts of alkali may be taken up by the oxidate
during the extraction. As has been noted above this assists in
maintaining the pH of the reactor contents between 6 and 10. If the pH
of the reaction mixture tends to rise above 10, however, the rainate
may be washed with water to remove the excess alkali before being
returned to the oxidation reactor. It may also be necessary to remove
any entrained aqueous alkali phase by mechanical means, for instance
by centrifuging.
In the various methods of carrying out the process of the present
invention, the dihydroperoxide extracted may be replaced by a
corresponding amount of fresh diisopropylbenzene. Furthermore, since
during the oxidation of by-products such as carbinols and ketones may
also be formed, in a continuous process it may be desirable to prevent
too great an accumulation of these by-products in the reactor by
bleeding off part of the reactor contents, and extracting the
by-products therefrom.
However, we have found that by the use of trimethylindane-free
starting materials substantially reduced quantities of
oxidationinhibiting by-products are formed.
The meta-and/or para-diisopropylbenzene dihydroperoxides may be
recovered from the aqueous alkaline extract by methods known in the
art, for instance by careful addition of acids to a pH of about 7 to
10.
The following comparative examples illustrate the production of
diisopropylbenzene free from ortho-diisopropylbenzene and
trimethylindane and the effect of the use of trimethylindane-free
starting materials in the oxidation reaction of the present invention.
In the examples the parts by weight and parts by volume bear the same
relationship to each other as do kilograms to litres.
EXAMPLE 1.
This example illustrates the preparation and oxidation of a
substantially trimethylindanefree sample of diisopropylbenzene, and
the oxidation of a sample of diisopropylbenzene containing about 11 %
of trimethylindane.
(a) Propylene was passed into a vigorously stirred mixture of
isopropylbenzene and powdered anhydrous aluminium chloride maintained
at about 60 C., over a period of 7.5 hours. The total propylene added
amounted to 0.98 moles per mole of isopropylbenzene. The aluminium
chloride was present in an amount of about 7 , by weight based on the
weight of isopropylbenzene. On termination of the reaction the
reaction mixture was allowed to cool and stand, whereon it settled
into two layers. The clear upper oil layer was separated off and
washed to remove traces of catalyst. It was found to contain benzene
and mono-, di-, and tri-isopropylbenzenes. The diisopropyl benzene

fraction amounted to 56% of the total and consisted of 64.5. %
meta-diisopropylbenzene, 35. 5% para-diisopropylbenzene, and less than
0.2% of trimethylindane. The oil was fractionally distilled to obtain
a meta-diisopropylbenzene fraction containing less than 0.1% of
trimethylindane. This fraction was oxidised as follows:
An apparatus for continuous oxidation was used whereby the
meta-diisopropylbenzene could be fed into the system continuously
while practically pure meta-diisopropylbenzene dihydroperoxide was
removed from it as the main reaction product.
It consisted of a reactor in which the metadiisopropylbenzene was
oxidised under stirring at 90 C. with molecular oxygen. This vessel
was equipped with an overflow which allowed about 1,200 parts by
volume of reaction space in the reactor, which under stirring and
gassing conditions usually contained 1100 parts by volume of liquid
reactants. The oxidate overflowed from the reactor to a reservoir from
which it was pumped to a countercurrent extraction column packed with
porcelain rings.
In the column the oxidate flowed upwards through a countercurrent of
4% weight/ volume sodium hydroxide solution, to the top of the column
from where it overflowed and was returned by gravity to the oxidiser.
The oxidate was introduced below and the alkali solution at the top of
the packing, the space above and below the packing serving to allow
the separation of the phases. The efficiency of this column was such
that practically all the dihydroperoxide was removed from the oxidate
in the alkali extract, while the remainder of the product containing
practically all the monohydroperoxide was returned to the reactor.
As dihydroperoxide was removed from the system fresh
nzeta-diisopropylbenzene was fed into the reactor.
In operation 1810 parts by weight of metadiisopropylbenzene containing
less than 0.1'% of trimethylindane were charged into the reactor and
reservoir, and 100 parts by weight of a meta-diisopropylbenzene
oxidation product containing 50 parts by weight of hydroperoxide
calculated as diisopropylbenzene monohydroperoxide were introduced to
the reactor as initiator. The reactor was heated to 90 C. and oxygen
introduced below the stirrer which was designed to give efficient
gas-liquid mixing. There was an induction period of 16 hours after
which oxidation proceeded smoothly. Circulation of the
diisopropylbenzene through the extraction column was started soon
after the beginning of the oxidation (i. e. at 16 hours), and was at a
rate of 700-800 parts by volume/hour. At this rate of circulation it
was unnecessary to add alkali to the reactor to maintain the pH above
6. The monohydroperoxide level reached 46% after 48 hours oxidation,
and for the remainder of the run averaged 55% w/w.
The rate of production of dihydroperoxide rose to a maximum of 23

parts by weight/ hour after 100 hours oxidation, and thereafter
suffered a gradual decrease, being 17.6 parts by weight/hour after 690
hours oxidation.
(b) By way of comparison a commercially available sample of
diisopropylbenzene was fractionated to obtain a
meta-diisopropylbenzene fraction, which contained about 11% of
trimethylindane. This was oxidised in the same apparatus and under the
same conditions as in (a) above. The rate of dihydroperoxide
production rose to 17-18 parts by weight/ hour after 100 hours
oxidation but after a further 187 hours had dropped to 10 to 12 parts
by weight/hour.
EXAMPLE 2.
An aluminium chloride alkylation catalyst complex was prepared by
passing hydrogen chloride through a mixture of aluminium chloride and
twice its weight of cumene. This catalyst was used for the propylation
of benzene using a 2: 1 molecular ratio of propylene: benzene, and 2.5
moles % of aluminium chloride on benzene. The catalyst containing 33
parts by weight of aluminium chloride and 780 parts by weight of
benzene were agitated in a vessel and 847 parts by weight of propylene
were passed in over a period of 8 hours, the vessel contents being
maintained at 60 C. At the conclusion of the reaction the reaction
mixture was washed with dilute hydrochloric acid, water, and dilute
sodium carbonate solution, to remove the catalyst. The alkylate was
distilled and gave a composition as shown in Table 1.
TABLE 1.
Benzene 2. Z ight
Cumene 14.9
Diisopropylbenzene 51. 4
Polyisopropylbenzene 31. 5
The diisopropylbenzene fraction was further fractionated and the
ortho-diisopropylbenzene and trimethylindane content determined by
means of infra-red spectroscopy. The composition of this fraction is
shown in Table 2.
TABLE 2.
o-diisopropylbenzene < 0. lght
m-diisopropylbenzene 64
p-diisopropylbenzene 35.5
trimethylindane 0
The diisopropylbenzene fraction was then ready to be oxidized
according to the process of the present invention as described in
Example 1.
EXAMPLE 3.
An anhydrous aluminium chloride catalyst was used for the propylation
of benzene using a 2: 1 molecular ratio of propylene: benzene, a

contact time of 30 minutes and a temperature of 80 C. The alkylate on
distillation gave a composition as shown in Table 3.
TABLE 3.
Weight %
Benzene 1
Cumene 14
Diisopropylbenzene 57
Triisopropylbenzene 27
Polyisopropylbenzene 1
The diisopropylbenzene fraction on further distillation was found to
contain about 65% by weight of the m-isomer. No o-isomer or
trimethylindane could be detected. The diisopropylbenzene fraction was
then ready for oxidation according to the process of the present
invention as described in Example 1.
By way of comparison with the examples quoted above the following
experiments are set out to show the results obtained when the critical
limits defined in the specification are not adhered to. The alkylation
reactions were carried out similarly to that described in
Example 1, using an unactivated catalyst except that lower and higher
temperatures were used. In Table 4 are shown the compositions of the
diisopropylbenzene fraction obtained in each case.
TABLE 4
<img class="EMIRef" id="026415671-00060001" />
Proportions of Isomers in diisopropylbenzene
Run Temperature
No. % olaho % meta % para % trimethylindane
1 +10 C. 7.5 38 54.5 0
2 +95 C. 0 63. 5 34.5 2
3 120 C. 0 56 35 7
The results shown in Table 4 illustrate that at temperatures below the
critical limits set out the undesirable formation of
ortho-diisopropylbenzene occurs while at temperatures above these
limits trimethylindane is formed.
What we claim is :-
1. The process for the production of diisopropylbenzene
dihydroperoxides by reacting meta-and/or para-diisopropylbenzene in
the liquid phase at elevated temperatures with molecular oxygen to
produce a concentration of mono-hydroperoxide of at least about 45% by
weight, contacting the oxidate with a nonacidic aqueous solution to
extract the dihydroperoxide, and subjecting the residue of the oxidate
to further oxidation, characterised by the use as feed of
diisopropylbenzene which is substantially free from tri-methylindane
and ortho-diisopropylbenzene and which has been produced by the
alkylation of benzene or isopropylbenzene or by the disproportionation

of ortho-diisopropylbenzene or polyisopropylbenzenes, in the presence
of aluminium chloride as catalyst under reaction conditions as
hereinbefore defined.
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