5691 5695.output

* GB786099 (A)
Description: GB786099 (A) ? 1957-11-13
Improvements in or relating to devices for tightening screw closures in or
around the mouths of bottles or like containers
Description of GB786099 (A)
of 4
1 -f bi v-:_
PATE Nr SPECIFICATION
4 86 A i.
fl Ufr Fin;:e Specification J': u, 4, 1936.
-l I, June v, 195-5 XYO 169385.
1 uzi,-e 9; l Rncotinn Pzublished Xci 1 t 3, 1 P 5 Index at
Acceptance:-Class 125 2,, E 2 t A: D 6).
International Classification:-B 67 b.
COMP Oi LETE SPECIFICATION.
SECIFICATION NO 78 e,099 Iw UN 54 TOPF MONAI: 3-CK By a direction
given under Section 17 ( 1) of thne Patents Act 1949 this appali tion
proceeded In the nane of The Crown Cork Conpan T Lim 7 ited, a British
colpa njy Apexes iorits, Southall, liiddlesex.
THE PATWIT OFFICE, loth January, 1958 LV v3 Ao t fls L,Fvwa Vs A Hyll
O i ut relating to devices for tightening screw closures in or around
the mouths of bottles or like containers, and has for one of its
objects to provide a simple construction lo which will operate
efficiently and can be fitted to existing machines, such as those for
applying crown stoppers to bottles.
Some known devices for tightening screw stoppers in place in bottles
embody an Archimedean screw and nut, one or the other of which is
caused to revolve because of relative longitudinal movement between
the two parts This longitudinal movement enables the bottle to be
operatively engaged by the stopper-tightening means, and the rotary
movement screws the stopper home.
The device according to the present invention, however, does not
employ an Archimedean screw and nut.
Another previous proposal entails that the screw stoppers are fed into

a head which in turn feeds individual stoppers into bottles and screws
them home by a friction device.
A plunger engages the stopper and during the initial part of its
travel towards the bottle screws the stopper gently under very light
pressure (caused by its own weight or a spring) into the bottle The
plunger is axially mounted in relation to a revolving and endwise
movable spindle that is loaded by a weight or spring, and rotates the
plunger lPri e DB 01863/1 ( 6)/3625 150 1/1 It t O X Ib;t IU LM 5,L 1
X 9; UI Ill LLAU 1 a L Usvn V 1.
a weight or spring and apply a heavier load to tighten the stopper to
the required extent.
The screwing operation is automatically discontinued by the clutch
members being taken out of contact with each other by one of the
endwise-moving parts of the device encountering an abutment.
The device according to the present invention embodies some of the
constructional features of the previous proposal just mentioned, but
it permits clutch slip to occur at a selected stage in the
closure-tightening operation so as to prevent damage to the closures
and containers The invention is applicable to screw stoppers which
enter the mouths of the containers, and to screw caps which are
received around the outside of the rims of the mouths of the
containers.
According to the invention there is provided a device for tightening
screw closures in or around the mouths of bottles or like containers,
comprising in combination a spring-loaded plunger whereof one end is
axially and telescopically mounted in relation to a spindle, and the
other end carries closure-engaging means, which springloading and
telescopic mounting enables the closure-engaging means to make
operative engagement with closures on containers of different heights,
rotary driving means connected to said spindle, co-operating clutch
PATENT SPECIFICATION
Date of filing Complete Specification: June 4, 1956.
Application Date: June 3, 1955 No 16038/55.
Complete Specification Published: Nov 13, 1957.
Index at Acceptance:-Class 125 ( 2), E 2 (A: D 6).
International Classsification:-B 67 b.
COMPLETE SPECIFICATION.
Improvements in or relating to Devices for Tightening Screw Closures
in or around the Mouths of Bottles or like Containers.
We, THE CROWN CORK COMPANY LIMITED, a British Company, and NORMAN
BECK, a British Subject, both of Apexes Works, Southall, Middlesex, 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 is for improvements in or relating to devices for
tightening screw closures in or around the mouths of bottles or like
containers, and has for one of its objects to provide a simple
construction which will operate efficiently and can be fitted to
existing machines, such as those for applying crown stoppers to
bottles.
Some known devices for tightening screw stoppers in place in bottles
embody an Archimedean screw and nut, one or the other of which is
caused to revolve because of relative longitudinal movement between
the two parts This longitudinal movement enables the bottle to be
operatively engaged by the stopper-tightening means, and the rotary
movement screws the stopper home.
The device according to the present invention, however, does not
employ an Archimedean screw and nut.
Another previous proposal entails that the screw stoppers are fed into
a head which in turn feeds individual stoppers into bottles and screws
them home by a friction device.
A plunger engages the stopper and during the initial part of its
travel towards the bottle screws the stopper gently under very light
pressure (caused by its own weight or a spring) into the bottle The
plunger is axially mounted in relation to a revolving and endwise
movable spindle that is loaded by a weight or spring and rotates the
plunger lPrice through a friction clutch The spindle may be driven by
a pulley or by a flexible shaft The plunger is independently movable
in an endwise direction and terminates at its lower end in a fitting
that is adapted to bear on the stopper after the latter has been
brought to a position over the mouth of the bottle.
After the aforesaid initial part of the travel of the plunger is
arrested by its contact with the revolving spindle, the plunger and
spindle descend together under the action of a weight or spring and
apply a heavier load to tighten the stopper to the required extent.
The screwing operation is automatically discontinued by the clutch
members being taken out of contact with each other by one of the
endwise-moving parts of the device encountering an abutment.
The device according to the present invention embodies some of the
constructional features of the previous proposal just mentioned, but
it permits clutch slip to occur at a selected stage in the
closure-tightening operation so as to prevent damage to the closures
and containers The invention is applicable to screw stoppers which
enter the mouths of the containers, and to screw caps which are
received around the outside of the rims of the mouths of the
containers.
According to the invention there is provided a device for tightening
screw closures in or around the mouths of bottles or like containers,

comprising in combination a spring-loaded plunger whereof one end is
axially and telescopically mounted in relation to a spindle, and the
other end carries closure-engaging means, which springloading and
telescopic mounting enables the closure-engaging means to make
operative engagement with closures on containers of different heights,
rotary driving means connected to said spindle, co-operating clutch
909 786,099 members appropriated one to the plunger and the other to
the spindle to convey the drive to the plunger, and spring means
urging the clutch members into operative engagement, which combination
is characterised in that the spring means are readily adjustable from
the exterior of the device and are set to exert such a pressure on the
clutch members as will permit clutch slip to occur after a selected
degree of closuretightening has been imparted by the rotation of the
plunger This provision for ready adjustment of the compression of the
clutch spring will be found to be of great importance in the operation
of the device Preferably, the spindle, plunger, clutch, plunger spring
and clutch spring are received in a casing with the plunger protruding
through the lower end thereof which is closed by a screwed bush the
inner end of which bears against an end of the clutch spring thus
permitting the compression of the latter to be adjusted from the
exterior of the device.
In a preferred construction, a driving pulley and the upper of the
clutch members are rigidly mounted on or connected to the spindle,
which is secured against endwise movement, and conveniently the
plunger reaches through and is connected to the lower of the clutch
members by a longitudinal slot -in the plunger and a cross pin on the
clutch member.
The closure-tightening device according to the invention may be
embodied in a single head or a multi-head machine and may be manually
or automatically operated In a multi-head machine in which the
closuretightening devices, embodying pulleys as aforesaid, are moved
through a circular path to and from the closure-tightening station, it
is advantageous so to arrange the devices that a single driving belt
can make contact with all of the pulleys When dealing with closures
having a right-hand screw thread in a multi-head machine, as just
mentioned, in which the devices travel anti-clockwise, when viewed
from above, along their circular path to and from the
closure-tightening station under which the containers are -50 placed,
the belt may be held stationary so as to drive the pulleys as the
devices of which they form part travel along the said path.
For a more complete understanding of the invention, there will now be
described, by way of example only and with reference to the
accompanying drawings, one construction of machine according to the
invention for tightening screw stoppers into the inside of the mouths

of bottles or the like It is to be understood, however, that the
invention is not restricted to the precise constructional details set
forth.
In these drawings:i.5 Figure 1 is a vertical section through one head
of a multi-head machine, parts of the said machine being shown in
chain lines; Figure 2 is a side elevation of a duel purpose multi-head
machine embodying the invention, this Figure being on a 74) scale
smaller than that of Figure 1; and Figure 3 is a plan view of certain
of the parts shown in Figure 2.
Like reference numerals indicate like parts throughout the drawings 5
Referring firstly to Figure 1, in the construction of
closure-tightening head according to the invention therein shown,
there is bolted on to a machine frame 10 an annular mounting flange 11
which lies horizontally so Upstanding from this is a tubular casing 12
having an annular cap 13 at its upper end.
The bore of the flange 11 is screwthreaded and receives a bush 14, the
upper end of which, inside the casing, is cupped 85 at 15 to receive
the lower end of a coiled clutch spring 16, and the lower end of the
bush 14 reaches below the flange 11 This bush has recesses 17 in its
lower exposed face whereby it may be turned by a suitable 90 tool from
the outside to vary the setting of the bush in the flange and
consequently to adjust the compression of the clutch spring 16 The
under face of the flange 11 is recessed to accommodate a locking ring
18 95 which is screwed upon the bush 14 against the flange to prevent
undesired movement of the bush Protruding through the bush 14, and
taking a bearing in the central bore thereof, is a plunger 19 which at
its exposed 104) lower end 20 carries the closure-engaging means This
lower end 20 is enlarged and has a central recess in its under face An
inverted saucer-shaped rubber tightening pad 21 is housed in this
recess and its rim 1 i 5 underlies the rim of the Dlunger end 20.
An annular retainer 22 of L shaped crosssection is screwed upon the
lower end 20 of the plunger to secure the pad 21 in place.
It will be seen that the exposed recess in 110 the pad 21 has a
downwardly and outwardly flaring side wall intended to be indented, at
an appropriate situation along its depth, when it operatively
encounters the closure such as 23, thus taking an efficient grip 115
upon the latter.
The annular cap 13 at the upper end of the tubular casing 12 affords a
bearing in which there is rotatably received a spindle 24 which has a
telescoping connection, 120 hereinafter described, with the upper end
of the plunger 19 The spindle 24 is tubular, open at its lower end
into which the plunger 19 reaches, and closed at its upper end except
for an axial lubricating conduit 25 12-5 Above the closed end, the
spindle terminates in a spigot 26 on which is keyed a pulley 27 with a

Vee groove to receive a belt 28 This pulley 27 is clamped in position
against a shoulder in the upper end of the spindle 24 9,0 16 can be
readily determined for different types of closure and container.
If there is only one tightening head in the machine, the belt drive to
the pulley will be continuous If, however, as is shown in 70 Figures 2
and 3, the machine embodies a plurality of tightening heads moving
through a circular path 41 to and from a closuretightening station, a
single constantly running belt 28 can make contact with the 75 pulleys
27 on all of the tightening heads.
In some circumstances, a stationary belt 28 can be used If the
closures, such as 23, have right-hand screw threads, and if the
tightening heads travel anti-clockwise, when 80 viewed from above, as
shown by the arrow 42, Figure 3, along their circular path to and from
the closure-tightening station, the belt 28 may be held stationary so
as to drive the pulleys 27 as the heads of which they 85 form part
travel along the said path In the path of the tightening heads there
is located a cam device (not shown) which, at the closure-tightening
station, raises the container in opposition to the plunger spring 90
31, thus enabling the tightening head to function until slip, governed
by the clutch spring 16, occurs The containers may, conveniently, be
carried to the tightening heads by a conveyor and a star device which
95 latter moves each container in turn into operative position During
their travel on the conveyor the containers have closures loosely
applied to them by hand.
The tightening head according to the in 100 vention may be embodied in
a machine the only function of which is closure tightening, or, as
shown in Figures 2 and 3, it may be an alternative fitting to replace
a crowning head, viz a head which applies crown cork 105 stoppers to
containers, so that the machine has a dual function The hopper 43
{igure 2) serves to receive crown cork stoppers and may have at its
lower end a chute for delivering these stoppers to the 110 crowning
heads, but in the drawings the chute and crowning heads are absent and
in their place a bracket 44 of L shaped cross-section has been secured
to the lower parts 45 of the hopper 43 115 If the invention is applied
to a dualpurpose multi-head machine as just mentioned, and if a
stationary belt 28 is to be employed, as aforesaid, use may be made of
the parts 45 to anchor the belt 28 That 120 is to say, one end of the
belt 28 is bolted to a part 45 at 46 The belt is then led around an
idle pulley 4-7 to take it clear of the bracket 44, and then led
around the pulleys 27 on the tightening heads back almost to 125 the
anchoring bolt 46 Between this free end of the belt and the anchoring
bolt a coiled spring 48 is connected to stretch the belt.
Tt is to be understood that the invention 130 by a nut 29, and a
lubricant cup 30 is provided which delivers lubricant through the

conduit 25 to the hollow interior of the spindle In this hollow
interior there is housed a coiled plunger spring 31, one end bearing
against the inner face of the closed end of the spindle and the other
end being received in a cup 32 formed in the upper end of the plunger
19 to apply loading to the plunger The lower end of the spindle 24
reaches below the lower face of the cap 13 and has an out-turned
flange 33 which constitutes an upper clutch member An annular ball
thrust bearing 34 is mounted between this flange 33 and the lower face
of the cap 13, and as the driving pulley 27 has only a slight
clearance from the upper face of the cap 13, the spindle 24 is held
against longitudinal movement, though it is free to rotate.
The upper end of the aforesaid clutch spring 16 bears against a thrust
ring 35 which encircles the plunger 19 and carries an annular ball
thrust bearing 36 upon which is mounted an annulus 37 of L shaped
cross-section which constitutes a lower clutch member One Dart of this
annulus 37 constitutes a guide for the plunger 19 in its telescoping
movement The plunger has a longitudinal slot 38 formed through it near
its upper end to receive a cross-pin 39 carried by the annulus 37 so
that the annulus and plunger will rotate together whatever the
longitudinal disposition of the Dlunger g 3 may be within the limits
imposed by the aforesaid slot 38 in it The other Dart of the annulus
has Dinned to it a friction disc 40 which makes contact with the under
face of the upper clutch member 33 under the pres4) sure of the clutch
spring 16.
The closure-tightening head just described may reciprocate vertically,
as a whole, or the bottles or other containers may be received up a
table which is raised or lowered It is intended that the closures (for
example 23) shall be placed in or on the container mouths by hand
before the tightening head operates.
The spring 31 loading the plunger 19 enables various heights of
containers to be o O accommodated and ensures that there shall be
sufficient resistance to the relative longitudinal movement of the
tightening head and the container for the closure to be adequately
gripped by the rubber tightening pad 21 While it is so gripped, the
friction clutch 33, 37, 40 is transmitting drive to the plunger 19, so
the tightening proceeds.
1 However, thee comuression of the clutch spring 16 is so selected and
carefully adjusted that the clutch will slip when the closure has been
adequately tightened.
When this occurs, the plunger 19 will cease to rotate until the
tightening head and the container are moved apart longitudinally.
The compression needed in the clutch spring 786,099 is not restricted
to the precise constructional details set forth.

* Sitemap
* Accessibility
* Legal notice
* Terms of use
* Last updated: 08.04.2015
* Worldwide Database
* 5.8.23.4; 93p
* GB786100 (A)
Description: GB786100 (A) ? 1957-11-13
Improvements in tampons or other absorbent plugs
Translate this text into Tooltip
[75][(1)__Select language]
Translate this text into
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.
COMPLETE SPECIFICATION.
Improvements in Tampons or other Absorbent Plugs.
We, MARK BARENT & SYDNEY WALGATE
JOHNSON, both British Subjects, and both of 4 New Court, Lincoln's
Inn, 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:
Sponge-like or cellular structures made of polyvinyl acetals are
known. They are characterised by being extremely soft when moist and
firm when dry. The structures may be made, for example, as described
in Specification No. 573,966 or in French
Specification No. 769,011, by treating a polyvinyl alcohol, which
usually contains some ester groups, with an aldehyde in the presence
of an acid catalyst while the reaction mixture is foamed, for example

by stirring.
After the reaction has been initiated the mixture is poured into a
mould and allowed to set. The sponge-like or cellular structure
obtained is then washed and dried.
This invention is based on the discovery that a dry sponge-like or
cellular structure of a polyvinyl acetal has properties which render
it extremely suitable for medical use as tampons. that is to say as
absorbent plugs for insertion in body cavities.
According to this invention a tampon is made by compressing a dry
cellular structure of a polyvinyl acetal so that its final volume is
no more than half its volume in the uncompressed state. The product of
the invention is therefore such a structure which when wetted swells
to at least twice its dry volume. A cellular structure of a polyvinyl
acetal is very soft when wet and has a very smooth texture. As a
result there is little chance of the body cavity being abraded by the
tampon either when the tampon is in position or when it is being
withdrawn.
Further, when moist the tampon is so soft that it will not cause
discomfort if its swollen size is larger than the size of the body
cavity.
The preferred polyvinyl acetal is polyvinyl formal but polyvinyl
acetals made from other aldehydes can also be used.
The dry cellular structures are capable of a very high degree of
compression and possess the surprising property that they retain the
shape into which they are compressed, so long as they are not
moistened or heated. We have been able to compress such a structure so
that its final volume is 71 times smaller than its original volume.
In practice there is no need to compress the structure to this extent,
although the higher the degree of compression the greater the volume
of liquid which can be absorbed in relation to the dry size of the
tampon, as the amount of liquid which can be absorbed is a function of
the size of the tampon when wet. The size of the tampon is limited
only by the need for ease of insertion. We prefer to reduce the volume
to no more than one third of the volume in the uncompressed state,
rather than only to half its uncompressed volume, particularly for
catamenial use.
Several important consequences follow from this property of high
compressibility.
First, it is possible to obtain a structure which is capable of
swelling and absorbing a large quantity of liquid. Second, the small
volume of the dry structure makes for easy insertion in the body
cavity. Third, although the tampon is greatly swollen when wet it can
be withdrawn through a small body opening without injury either to the
body or the tampon as it is also very soft when wet. Moreover, tampons

according to this invention are somewhat softer than conventional
cotton tampons when dry.
The compression can be carried out in any convenient manner for
example, by punching the dry structure through a die, in a press or by
rolling between contra-rotating rollers. Compression is assisted by
heating the structure to a temperature up to 100 C.
Advantageously the structure in its uncompressed state is a prism and
in its compressed state is a cylinder, and is compressed both axially
and radially. The prism may be triangular, but is preferably
rectangular, in cross-section. Rectangular and triangular prisms can
easily be cut from a block of the cellular structure, making the
manufacture of the tampons or the like simple, as it is unnecessary to
cast each prism separately.
Further, as the prisms are compressed to cylindrical shape, there is
not the wastage of material which would be involved if cylindrical
shapes were cut out directly.
Moreover, although a cylindrical tampon in this shape tends to regain
its prismatic shape when it swells, the moist material is so soft that
the edges of the prism do not abrade the body cavity. They also
exercise a wiping action, which may be desirable.
The manufacture of tampons in this way is extremely simple. The
polyvinyl acetal can be made in the form of large blocks in a simple
type of mould. The cutting of the block into, for example, rectangular
prisms can be accomplished by a simple operation and the prisms
obtained fed to a device which compresses them to substantially
cylindrical shape.
The tampons need not be of cylindrical shape; they can be of any
convenient shape, for example, they may be conical.
The tampons according to this invention are of particular value for
catamenial use.
In this use a tampon is inserted in its compressed, dry form into the
vagina, absorbs the menstrual discharge, expands in size and becomes
soft. In expanding in size the tampon tends to fill the vaginal canal,
and in this way the channelling, and therefore leakage, which occurs
with cotton tampons is reduced. Thus, the tampon which is initially
hard and sufficiently small to be inserted without difficulty either
with or without an applicator, or with or without a lubricant, can be
easily removed without discomfort or damage to the mucous membrane or
skin.
Preferably a cord is attached to the tampon or the like for ease of
removal from the vagina or body cavity. The cord may merely be looped
through one end of the tampon as the polyvinyl acetal structure is
strong enough, even when wet, not to be torn when the cord is pulled.
The degree of compression should be such that the dry tampon is as

small as possible to facilitate insertion and also so that a number of
tampons can he packed into a small volume for carriage, for example,
in a woman's handbag.
The size of the tampon can vary, but we have found, for example, that
a prism measuring 1" x 1" x 2q" can be compressed to give a
cylindrical tampon 2" in length and 43' in diameter. The compression
ratio, which is a measure of the absorptive capacity, is 2.8:1.
It is important that the tampons, whether for catamenial or other use,
should be sterile.
Sterilisation can be achieved by carrying out the manufacture under
sterile conditions, or as a subsequent step. It is conveniently
carried out by drying a deposit of a sterilising agent onto the dry
structure before it is compressed. A suitable agent is cetyl
trimethylammonium bromide. This can be applied to the dry structure by
immersing it, for example, in a solution containing 1 part of the
agent dissolved in 800 parts of water, squeezing it to remove excess
agent and then drying it.
As an example of the manufacture of a tampon according to this
invention, a mixture of 65 lb. of a 20 dispersion of polyvinyl alcohol
(containing some ester groups) in water, 101- ozs. of of
paraformaldehyde, 2ozs. of a 2Goo solution of saponin and 132 pints of
60% sulphuric acid was stirred together by whisking with a mechanical
stirrer.
The aerated mixture was then poured into rectangular moulds and
maintained therein at a temperature of about 30 C. for 24 hours.
The blocks of polyvinyl formal were removed from the moulds, washed
free from acid and then dried by heating at a temperature of 60 to 70
C. in an oven for 3 days.
A number of prisms measuring 3" > 1" x 1" was then cut from the blocks
and compressed to cylindrical shape, the dimensions of each cylinder
being 24" in length and " in diameter. The tampons obtained thus had a
compression ratio greater than 3:1 and were suitable for absorption of
a menstrual discharge.
A number of prisms measuring I3116"x
1/16"X211 was also cut from the blocks.
Some of these were compressed in a conical die to a conical shape
having a base diameter of -3-" tapering to -1-'', and a hight of 13g".
In this case the compression ratio was approximately 3.5:1.
A further set of these prisms was compressed in the same conical die,
but in this case the compressed tampons were driven right through the
die as cylinders " in diameter and 1" in height. Here the compression
ratio was 7.5:1.
Both these compressed structures were siutable for use as catamenial
tampons.

What we claim is : -
1. A method of making a tampon which comprises compressing a dry
cellular structure of a polyvinyl acetal so that its final volume is
no more than half its volume in the uncompressed state.
2. A method according to Claim l in
* GB786101 (A)
Description: GB786101 (A) ? 1957-11-13
Improvements in or relating to locking devices controlled by shock
Inventor: DOUGLAS LOUIS AS'HTON DRIVER 7 Date of Application and
filing Complete Specification: June 24, 1955.
No 18272/55.
Index at acceptance:-Classes 40 ( 4), J 3 M; and 80 ( 3), Zil.
International Classification:-FO 6 h H 04 m.
i COMPLETE i Si PECIF'Is CATION Improvements in or relating to Locking
Devices Controlled by Shock We, STANDARD TELEPHONES AND CABLES
LIMITED, a British Company, of Connaught House, 63 Aldwych, London, W
1 C 2, England, 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 locking devices controlled by shock.
According to the invention, there is provided equipment for
automatically retaining a removable object in position on a support
during shock which normally permits removal of the object from its
support and Which automatically locks the movable object to its
support during shock.
According to the invention, there is also provided equipment for
automatically retainZO ing a removable object in position' on a
support during shock comprising a retaining component which must be
displaced to' permit removal of the object, and a retaining device

having two members one of which is displaced by the displacement of
the retaining component, the two members of the device being capable
of displacement relative to each other in response to shock so that
displacement of said one member due to displacement of the retaining
component is prevented during shock.
By means of the invention, it is, for example possible to provide a
mounting for a telephone on board a ship which prevents the telephone
being dislodged by the shock caused by a salvo fired from the ship, or
by the expl Bosion of a depth-charge near the ship which does not
impair the use of the telephone at other times.
The invention will now be described with reference to athe
accompanying drawings in which: Fig 1 is a sectional plan view of a
mounting for hand Inicrotelephone embodying 'two 'devices according to
the invention at right angles to each other, one form of
construclPrice 3 s 6 d l Zion being shown above the centre line and an
Altermative form of construction below the centre line.
Figs 2, 3 are elevational views of the two devices in, Fig 1, Fig 4
shows diagrammatically an alternative arrangement of two devices
controlling clip members.
Fig 5 shows diagrammatically a plunger controlled by one device.
Figs 6, 7 show diagrammatically a plunger controlled by two devices at
right angles to each other, The device shown in 'the upper half of
Fig.
1 and in Fig 2 comprises a locking member 1 suspended by two pairs of
helical springs 2; from brackets 3 ' on one arm of two mutually
perpendicular arms of a framework 4.
Screws 5 permit each spring to be adjusted individually The locking
member 1 has a hollow cylindrical bore 6, the diameter of which is
enlarged at one end to form a recess 7 A disc 8, normally housed in
the recess 7 and having a diameter slightly less than that of the bore
'6, is carried on a rod 9 capable of axial movement in holes in the
framework 4.
At one end of the rod 9, a collar 10 'holds a spring 111 in
compression against the framework 4, whereby, the,disc 18 is held in
the recess 7, and the clip 12, which is pivotally mounted at 13 ' on
the framework 4, is forced against a stop 14 'The clip 12 is one of a
pair which engage opposing surfaces of a handmircrotelephone 15 ' and
hold it in position, and both of which clips must 'be displaced, as
shown by dotted lines, to remove the handmicrotelephone.
When the telephone 15 is removed, the clip 121 is displaced against
the action of the spring 11 and the disc '8 travels down the bore '6
The required alignment is obtained by means of the adjusting screws 5
of the springs 2 Suppose, now, that the structure (e g a ship), to
which the framework 4 is attached, is submitted to shock when the

telephone 15 is in the position shown in Fig 1 The struc869101 ture
and the framework 4 move under the influence of the shock The locking
member 1 remains stationary due to its inertia and the accommodating
action of the springs 2 The resulting movement of the locking member 1
relative to the rod 9 places the bore 6 out of alignment with the disc
18 which is consequently held captive in the recess 7 and prevents
displacement of the clip 12.
The telephone 15 however is not rigidly attached to the framework 4
and there may be a tendency to relative movement between the telephone
and the framework under shock, resulting in displacement of the clip
12 and the disc 8 It is therefore essential to ensure that the locking
member 1 traps the disc 8 in the recess 7 before the disc 8 has been
able to enter the bore 6 This can be achieved if the difference in
diameter of the disc 8 and the bore 6 is small and less than the
difference between the thickness of the disc 8 and the depth of the
recess 7.
When the shock has passed the locking member 1 and the rod 9 resume
their original relative positions, so that, the disc 8 is free to move
down the bore 6.
The device so far described will respond to any shock which displaces
the locking member 1 in any direction in the plane in which the
locking member is free to move The device however, will not respond to
a shock perpendicular to this plane A second identical device is
therefore provided so as to be responsive to shock in this direction
The two devices at right angles to each other are together responsive
to shock from any direction The position of the second device is shown
in the lower half of Fig 1 Each device controls one clip 12 of a pair
of clips, both of which must be displaced to permit removal of the
telephone The two devices together, therefore, constitute apparatus
which holds the telephone 15 in position during shock from any
direction.
i An alternative construction of the device is shown in the lower half
of Fig 1 and in Fig.
3 A locking member 1, having, as before, a bore 6 and a recess 7, is
supported within a cylindrical drum 16 by a coiled spring 22.
The coil is tapered towards its middle portion where contact is made
with the locking member 1 A rod 9, carrying as before, a disc 8, is
capable of axial movement in a hole in the framework 4 and in a hole
in Ma plate 17 A compression spring 11 is housed within the bore 16
The plate 17 is secured to the framework 4 by screws 18 with engage
holes tapped in the framework 4 Two flange members 19, provide
end-seatings for the drum 1,6 and have holes 21 which are a loose fit
around the screws 18 The flange member 20 is extended centrally to
provide a sliding surface for the locking member 1 Alignment of the

bore 6 and the disc 8 is obtained by means of the play in the holes 21
When alignment has been secured, the screws 18 are tightened home The
device operates in the same way as the device already described, the
coiled spring 22 acting in place of the pairs of springs 2.
The device can also be used in pairs to pro 70 vide apparatus
responsive to shock in any direction.
Fig 4 shows diagrammatically a pair of clips controlled by tvo devices
at right angles to each other, as already described Each 75 shaded
square represents a device having a rod of which one end is seen,
capable of movement in the direction shown by the arrow.
Arms convey the movement of the clips to the rods As both clips must
be displaced to re 80 lease an object held between them, the object
will be locked in position by shock from any direction.
Fig 5 shows one device in which the rod is extended to form a plunger
which is locked 85 by shock in any direction to which the device is
responsive Fig 6, shows two devices at right angles 'to each other An
extension of the plunger of the first device abuts one arm of a
bell-crank The other arm of the bell-crank 90 abuts the rod of the
second device Consequently the plunger is locked in position by shock
from any direction Fig 7 is an alternative arrangement to Fig 6 in
which the second arm of the bell-crank is connected by 95 a pin to an
extension of the rod of the second device.
* Sitemap
* Accessibility
* Legal notice
* Terms of use
* 5.8.23.4; 93p
* GB786102 (A)
Description: GB786102 (A) ? 1957-11-13
Improvements relating to casting resins
A high quality text as facsimile in your desired language may be available

amongst the following family members:
FR1154015 (A)
FR1154015 (A) less
COMPLETE SPECIFICATION Improvements relating to casting Resins
We, THE BRITISH THOMSON-HOUSTON
COMPANY LIMITED, a British Company having its registered office at
Crown House,
Aldwych, 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 preparation and casting of flexible
resins.
It is desirable and sometimes necessary in casting resins to emplloy a
resin which, when set, is flexible tor semi-fleible. The resin may be
required to have this flexibility both at room temperature and lower
temperatures for instance, down to -65 C. The known flexible resins
are unsuitable because they harden too quliddy on lowering of their
tam- perature or because they are difficult. to handle in the uncured
state.
It is well-known that flexible resins can be produced by the
cross-linking of certain unsaturated polyester resins with a
polymerusable monomer, but even when a filler lis incorp orated with
these resins and an acceptable degree of flexibility obtained at room
rem- perature, the resin hardens rapidly with decrease in temperature,
and if an electrical component is cast in such a resin, the latter
cracks too easily at low temperature. While it may be possible to
reduce the temperature at which cracking occurs by increasing the
thickness of the resin wall around the embedded component, this
increase in the dimensions and weight of the casting represents
serious disadvantages, particularly to equipment which is for use on
aircraft.
Kaown flexible resins may also be made based on the reaction product

of a polyisocyanate and a polyhydric compound but the toxicity of
isocyanates is a serious disadvantage to their use.
Further known flexible materials may be obtained based on epoxy
resins. The preparation of epoxy resins is described lin
Specifications 772,289 and 766,817. These are complex polyether
compounds containing terminal epoxy groups and these resins may be
hardened by amines, dicarboxylic acids or their derivatives. These
normally-rigid epoxy resins are rendered flexible by the addition of a
modifying agent A degree of resilience can be introduced into the
epoxy resin by modification with a polyamide resin but the mixture is
very viscous even when the lowest viscosity epoxy resins ate employed,
and they also possess very short pot life. Acid polyesters can also be
employed as modifying agents for epoxy resins in conjunction with
anhydride hardeners but curing times are long and although a large
measure od flexibility is possible in this way at room temperature,
flexibility disappears as the temperature is lowered and no advantage
is gained at temperatures below -40 C. Epoxy resins may also be
reacted wlith polysuiphides but the offiensive smell of the latter
together with the general poor electrical properties of the final
resin limit its use for many electrical appllica- tions.
Our invention provides an improved casting resin composition which
overcomes these defects.
We have found that if an epoxy resin which is liquid at ordinary
temperatures is mixed with a specific type of organic base namely, an
aromatic diamine in a quantity normal for hardening, this mixture may
then be blended in the liquid state with a liquid polyester resin
containing a polymerisable monomer and a small amount of a peroxy
catalyst. This. can be hardened with the aid of heat to a homogeneous
clear resin having a varying degree of flexibility according to the
formulation of the resin in a manner hereinafter described.
The above order of mixing is not vital and indeed it is more
convenient sometimes to dissolve the aromatic diamine in the polyester
resin and polymerisable monomer mixtare, and to dissolve the organic
peroxy compound in the liquid epoxy resin. The two mixes are then
blended together.
Our improved casting resin composition, which is liquid at room
temperature, thus comprises five components. These five components are
defined below and are advantage ously used in the proportions given.
1. A mixed unsaturated polyester resin, preferably containing an
inhibitor, derived from the esterification of an alpha-beta
unsaturated and a saturated dicarboxylic acid or anhydride with a
polyhydric alcohol, in which the molar ratio of saturated to
unsaturated dicarboxylic residues in the polyester ranges between 50
to 1 and 2 to 1 and preferably between 20 to 1 and 5 to 1. The

preferred saturated dicarboxylic acids or anhydrides belong to the
aliphatic series. Aromatic dibasic acids or anhydrides are slow in
esterification and result in a harder resin. If used, it as preferred
that they should comprise only part of the saturated dicarboxylic acid
comp onent
2. From 10,% to 100% by weight and preferably from 30% to 60% by
weight, based on the above polyester, of a polymerisable monomer,
which is miscible with both the above polyester and the epoxy resin
described below, and which contains the group
CH2=CH-, i.e. a vinyl compound.
3. From 0.01% to 5% by weight and preferably from 0.1% to 11% by
weight, based on the combined weight of the above unsaturated
polyester tlesin 1 and the polymerisable monomer 2, of an organic
peroxy compound.
4. From 10% to 200% by weight and preferably from 25% to 120% by
weight, based on the polyester resin 1, of an epoxy resin which is
liquid at ordinary room temperatures and comprises a complex polyether
composition containing terminal epoxy groups
CH2=CH
V
0
5. From 10% to 80% by weight and usually from 12% to 40% by weight,
based on the epoxy resin 4, of an aromatic diamine, for example a
phenylene diamine, a tolylene diamine, a naphthylene diamine,
benzidine, and a diamino diphenyl methane, particularly 4:41 diamino
diphenyl methane.
The improved casting resin according to our invention has the
following properties:
1. It has a low viscosity.
2. It has a long pot life.
3. It is easy to handle.
4. It cures quickly at moderately elevated
temperatures, e.g. 100 C.
5. The cured resin adheres well to a wide
variety of materials.
6. There is no adverse interaction with
copper.
7. The cared resin has excellent water re
sistance its electrical properties being very
little affected by continued exposure to humid
conditions.
8. When employed in the preferred man
ner with a filler, castings can be made with
out risk of cracking and cast components can

withstand temperatures as low as -65 C.
without crackling.
Any one of the above properties can be
varied or accentuated by small changes in the
formulation within the limits of the invention.
The following information is given as a
general guide to the way in which these varia
tions in properties may be brcught about
1. The viscosity is most easily controlled
by varying the concentration of the polymer
isable monomer, for instance styrene, although
increase in styrene content tends to produce
a harder final product.
2. A faster setting composition may be ob
tanned by increasing the concentration of or
ganic peroxy compound or by using a poly
ester resin component with a higher degree
of unsaturation or both. The latter modifica
tion besides increasing the rate of reaction
also increases mechanical strength and im
proves the electrical properties still further
but decreases flexibility. Both modifications
tend to reduce shelf-life.
3. Increase in epoxy resin concentration
improves mechanical strength but decreases
flexibility.
4. Usually the ratio of aromatic diamine to
epoxy resin is fairly critical wheti good elec
tricel properties are required and there is an
optimum ratio for each combination of resin
and diamine which corresponds to that norm
ally recommended and employed in the simple
and xvell-known aromatic diamine- epoxy
resin compositions. If the aromatic diamine
concentration be lowered below the optimum,
a more flexible product is obtained bnt com
plete polymerisation is difficult and the elec
trical propertie-Thferior. If on the other
hand the aromatic diamine concentration be
increase above the optimum, a more flexible
resin is also produced and the electrical
properties are also inferior, particularly after
a period of heat ageing which would not affect
the normal composition.

As lis usual in most casting resin applications, a a filler is
normally required Fillers such as quartz, silica, mica, and talc are
satisfactory.
The preferred filler is talc.
The invention is of particular value in the
casting of miniature transformers and chokes,
especially those employing cold rolled grain oriented silicon iron.
When a rigid type of resin casting is employed, stresses set up within
the core due to the contraction of the resin on setting may cause
serious changes to take place in The electrical chFaracteristiics of
the core. For instance, it is not uncommon for a miniature transformer
constructed of cold rolled steel laminations to have its magnetisation
current increased tenfold after casting in a rigid epoxy resin. When
such a unit is cast in the flexible resin described in Example 1
hereinafter given, and containing a filler, no significant change
occurs in the magnetising current
Similarly it is common to find thait chokes vary in inductance before
and after casting in rigid resins by a serious amount. Such variations
can be substantially eliminated by this invention.
The following examples are given by way of illustration:
EXAMPLE 1.
An unsaturated polyester resin was prepared from:
Adipic acid - - 445 gms.
Maleic Anhydride - 25 gms.
Propylene glycol - 280 gms.
All the components were heated slowly in an atmosphere of nitrogen to
230 C and held at 230 C. until an acid value of 30-45 mg.
KOH/gm. was obtained. V;acuum was then applied and heating continued
under vacuum to an acid value of below 12 mg. KOH/gm.
The resin was cooled to 90 C. and 0.03 gm.
of quinone added as inhibitor.
150 gms. of the above unsaturated polyester resin were dissolved in 65
gms. of monomeric styrene, and to this solution there was added 36
gins of 4:41 diamino diphenyl methane and complete solution effected
by warming to 70 C. In a separate vessel 120 gms. of an epoxy resin
known as Araldite 33/900 were mixed with 0.5 gm. of tertiary butyl
perbenzoate. (" Araldite" is a registered
Trade Mark). The two components were then mixed in the cold and the
viscosity of the composite resin was 167 No. 4 Ford Cup seconds at 20
C.; it possessed a shelf life of 5t days at normal temperature.
A 1/4" thick disc of this resin was cast by pouring the resin mixture
into a shallow tray and stoving for 4 hours at 1100 C. At the end of
this time the resin had set and was transparent and flexible.
EXAMPLE 2.

150 gms. of a polyester resin in which the molar ratio of saturated to
unsaturated dicarboxylic add residues was 6:1 and which possessed an
acid value lof 12 mg. K.OH/gm.
were dissolved in 65 gms. of styrene followed by 36 gms. of 4:41
diamino diphenyl methane, complete solution being effected by warming
to 70 C. In a separate vessel 120 gins. of an epoxy resin, Araldite
33/900, were mixed with 0.5 gm. t-butyl perbenzoate.
The two components were then mixed in the cold and the viscosity of
the composite resin was 180 No. 4 Ford Cup seconds at 20 C.; it
possessed a shelf life of 5 days under normal ambient conditions.
A sample disc, cast in the mianner described in Example 1, was
flexible but noticeably harder than the resin described in Example 1.
EXAMPLE 3.
200 gms. bf the same polyester resin used in Example 1 were dissolved
in 75 gms. of styrene containing 0.009% quinone as inhibitor followed
by 36 gms. of blenzidline which was helped to dissolve in the solution
by warming to 60 C. In a separate container 0.5 gm. of
t-butyl-perbenzoate was mixed with 120 gms. of the epoxy resin known
as Araldite
F. The two mixes were then blended together in the cold. A sample disc
was cast in a similar manner to that employed in the previous examples
and a flexible transparent resin was again obtained.
EXAMPLE 4.
150 gms of the polyester resin employed in Example 1 were dissolved in
65 gms. of tbutyl catechol inhibited styrene and 22 gms.
of 2:4 tolylene diamine was dissolved in the mixture by warming to 809
C. In a separate container 0.5 gm. t-butyl perbenzoate was dissolved
in 120 gms. of Araldite 33/900. The two components were mixed together
and la cast sample disc was prepared from this composite resin and
hardened by baking for 4 hours at 110 C. A flexible resin was
produced.
EXAMPLE 5.
200 gms. of the unsaturated polyester resin employed in Example 1 were
dissolved in 75 gms. of styrene and 36 gms. of 4:41 diamino diphenyl
methane were dissolved in the mixture by warming it to 70 C. In a
separate container, 0.5 gm. t-butyl perbenzoate was dissolved in 120
gms. of Araldite 33/900.
The two components were mixed together in the cold.
A number of specimens for testing for tensile strength were cast from
this resin and cured for 16 hours at 90 C. These were subsequently
heat-aged at 125 C. In Table 1, there is listed the tensile strength
and elongation at break data obtained at 22 C. after various periods
of heat ageing.
TABLE 1.

Days heat ageing Ultimate Stress Elongation at at 125 C. P.S.I. break
0 1000 80
2 1040 68
6 1115 53
17 1165 39
24 1280 36
EXAMPLIZ 6.
120 gms. of the same polyester resin used in Example 1 were dissolved
in 60 gm. of styrene followed by 36 gm. of 4: 41-diamino diphenyl
methane, complete solution being effected by warming to 70 C. 0.4 gm.
of tbutyl perbenzoate was dissolved in 120 gms.
of Araldite 33/900 and the two components mixed together in the cold.
The viscosity of this mixture was 125 No. 4 Ford Cup seconds at 22 C.
A disc sample, 4" diameter w" thick, was cast in a mould and hardened
by baking overnight at 90 C. The electrical properties of this sample
were then measured.
The power factor, permittivity, and electrical strength lare given
below:
tan # .03 at 20 C.
" .03 " 55 C.
" .05 " 75 C.
" .1 " 90 C.
Permittivity 4.5 at 20 C.
Electric Strength at 90 under oil 29 kV (minute value) which
corresponds to 450 v/miL
EXAMPLE 7.
Three similar miniature transformers were constructed leach with a
core made from cold rolled grain oriented silicon iron laminations and
subsequently cast in three different types of resin, i.e. unmodified
epoxy resin, semi- flexible polyester resin, and the epoxy/polyester
resin described in Example 1. Each was employed with a filler. Mica
was used in the case of the rigid epoxy resin, a silica and talc
mixture for the flexible polyester resin and 70 parts by weight of
talc per 100 parts by weight of the fepoxy/polyester resin. The epoxy
resin was handled during the casting process at 125 C. but the
flexible polyester and the epoxy/polyester composition were both
handled cold.
The same mould was used to cast each transformer; thus the same resin
casting was obtained in all three cases. The dimensions of the
transformer were approximately x " x 1" x 3" high. A vacuum casting
tech- clique was employed in each case and the baking process was that
normally applicable to the resin involved. The polyester/epoxy
composition was baked for 6 hours at 90 C.
Each transformer was then tested to determine its change in magnetic

properties with temperature and the results ara recorded in
Table 2.
TABLE 2.
Temperature ( C.) 18 C. before 18 C. after -40 C. -65 C. +18 C. +110
C.
casting casting
Casting I mag. Core I mag. Core I mag. Core I mag. Core I mag. Core I
mag. Core
Resin loss loss loss loss loss loss
<img class="EMIRef" id="026473762-00050001" />
Epoxy/
Polyester 4.3 0.45 4.5 0.36 15.0 0.62 23.0
0.75 4.8 0.40 4.0 0.35
Flexible/
Polyester 4.4 0.45 4.4 0.35 16.0 0.64 Cracked
at -50 C.
Rigid
Epoxy 4.3 0.40 45.0 1.10 67 1.45 71 1.45 44
1.11 6.1 0.39
In the above table:
I mag. stands for magnetising current and is measured in milliamps.
Core loss is measured in watts.
It will be seen that the magnetising current and core loss are not
adversely affected after casting into either the epoxy/polyester
composition or the flexible polyester, but that after casting into the
rigid epoxy resin the magnetising current increased tenfold and the
core loss was more than doubled. The flexible polyester cracked at -50
C. whereas the epoxy/polyester and the rigid epoxy cast transformers
did not crack at -65 C. Comparison of the magnetising current and core
losses of the latter two resins at -65 C.
shows the superiority of the epoxy/polyester in this application.
EXAMPLE 8.
Three similar choke cores were cast in the same three casting resins
employed in
Example 7. These chokes each possessed a cold rolled grain oriented
silicon iron laminated core. These chokes were of the same physical
size as the transformers and all three were cast in the same mould.
Each casting bad a minimum thickness of 1/8" round the core. These
three chokes were then subjected to tests to measure their inductance
over a wide temperature range, the results of which tests are given in
Table 3.
TABLE 3.
Inductance in millihenries
Epoxy/ Flexible Rigid

Temp. Conditions Polyester Polyester Epoxy
+ 18 C. before casting 16.36 16.30 16.32
+18 C. after casting 16.34 16.56 14.23 -4 C. ,, " 15.44 15.58 13.25
-65 C. " " 15.02 Cracked at -55 C. 12.95
+18 C. " " 16.36 14.38 +110C. ,, ,, 16.34 16.27
It will be observed that the smallest change in inductance before and
after casting is obtained with the epoxy/polyester casting resin and
the total range of inductance for the chokes is lower for the
epoxy/polyester casting than for the rigid epoxy casting over the
temperature range - 65 to + 110 . The flexible polyester resin cast
choke cracked at -55' C.
What we claim is:
1. A method of making a casting resin composition which consists in
preparing a mixture comprising (1) a mixed unsaturated polyester
resin, (2) a polymerizable monomer which is a vinyl compound miscible
with the polyester and with the epoxy resin hereafter specified, (3)
an organic peroxy compound, (4) an epoxy resin which is liquid at
ordinary temperatures, and (5) an aromatic diamine.
2. A method according to claim 1 in which constituents (1), (2) and
(5j are mixed together with enough heating to effect comlete solution,
then constituents (3) and (4) are mixed together without heating, and
finally the two mixtures are blended in the cold to give the casting
composition.
3. A method according to claim 1, in which the polyester resin
contains an inhibitor, e.g.
quinone.
4. A method according to claim 1, in which the polyester resin is
derived from the esterification of an alpha-beta unsaturated and a
saturated dicarboxylic acid-or anhydride with a polyhydric alcohol,
and has a molar ratio of saturated to unsaturated dicarboxylic
residues in the polyester ranging between 20 to 1 and 5 to 1.
5. A method according to claim 1 in which the polymerisable monomer,
e.g. styrene, is present in an amount equal to 10%-100% by weight of
the polyester
6. A method according to claim 1, in which the organic peroxy
compound, e.g. tertiary butyl perbenzoate, is present in an amount
equal to 0.01 %-5-0A of the combined weight of the polyester resin and
the pclymerizable monomer.
7. A method according to claim 1, in which the epoxy resin is present
in an amount equal to 10%-200% by weight of the polyester resin.
8. A method according to claim 1, in which the aromatic diamine is
present in an amount equal to 10 %-80 % by weight of the epoxy resin.
9. A method according to claim 1, in which the aromatic diamine is one
of the following - a phenylene diamine, a tolylene diamine, a

naphthylene diamine, benzidine, or a diamino diphenyl methane.
10. A method according to claim 1, in which a filler is included with
the other constituents of the composition.
11. A casting resin composition which has been made by the method
claimed in any of the preceding claims.
12. A solid flexible resin which has been produced by baking a casting
resin composition made by the method claimed in any of the preceding
claims.
13. A transformer lor a choke having a core consisting essentially of
laminations of coldrolled grain-oriented silicon iron, the assembly
having been immersed in a mould filled with a casting resin
composition made by tbe method claimed in any of the Claims 1 to 10,
and thereafter baked to produce a moulded anticle of solid flexible
resin containing the core.
PROVISIONAL SPECIFICATION Improvements relating to casting Resins
We, THE BRITISH THOMSON - HOUSTON
COMPANY LIMITED, a British Company having its registered office at
Crown House,
Aldwych, London, W.C.2, do hereby declare this invention to be
described in the following statement:
It is desirable and sometimes necessary in casting resins to employ a
resin which, when
* GB786103 (A)
Description: GB786103 (A) ? 1957-11-13
Improvements in or relating to low temperature methods for preparing high
melting point greases
A high quality text as facsimile in your desired language may be available
amongst the following family members:
US2892778 (A)
US2892778 (A) less

7 M arc, Date of Application and filing Complete Specification: June
27, 1955.
No 18533/55.
(to m e Application made in United States of America on Oct 25, 1954;
Index at acceptance:-Classes 2 ( 3), C 2 837 (B 1: K); and 91, F( 1:
2: 3).
International Classification:-CO 7 c Cl Om.
COMPLETE SPECIFICATION
86.103 Improvements in or relating to Low Temperature methods for
preparing High Melting Point Greases We, CALIFORNIA RESEARCH
CORPORATION, a corporation duly organized under the laws of the State
of Delaware, United States of America, and having offices at 200, Bush
Street, San Francisco 4,, California, 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 pertains to a new method of preparing grease
compositions having high melting points; that is, high dropping
points.
High melting point lubricants are now essential for the proper
lubrication of automotive wheel bearings, steel mill equipment, high
speed motors, universal joints, airplane motors, jet engines and
guided missiles In recent years there has been a continuing trend to
manufacture machines having higher speeds and having greater loads on
bearings and gears Because of the greater speeds and increased loads,
such machines function at higher temperatures than heretofore,
requiring the use of higher temperature lubricating compositions for
proper lubrication.
Military and industrial grease specifications describe greases having
dropping points of 400 F as a minimum.
Prior methods of preparing greases have shown that the components of
the greasethickening agents (for example, fatty acids and metal
hydroxides) can be added to the oil, and the resulting composition
heated to high temperatures, forming the metal soap-thickening agent

in situ, after which the composition is cooled to form a grease
structure On the other hand, the metal soap grease thickeners per se
can be incorporated directly in the base oils, and the oil
compositions heated to the high solubilizing temperatures, after which
the composition is cooled to form the grease structure Following the
formation of the grease structure by either of these prior processes,
the greases can be passed through colloid mills lPrice 3 s 6 d l to
modify the physical properties thereof, such as the dropping point.
In the preparation of high temperature greases (i e, greases having
high dropping points) by these prior processes, the greasethickening
agents and the base oils must be heated to temperatures at which the
thickening agents become solubilized in the base oils and, in the case
of high melting greases, thel temperature may be in the range of 6000
F and higher.
When such high temperatures become essential in the formation of
greases, various other problems arise For example, the high
temperatures cause oxidation of the grease base oil, a discoloration
of the greases, and other deleterious results The high temperatures
make it necessary to use special heating equipment to obtain the
greater amounts of energy which are required Also, special oils are
needed for conducting the heat from a central heating system, and
these oils must be changed frequently because of their degradation at
high temperatures Furthermore, it becomes necessary to have special
equipment to cool the compositions from such high temperatures down to
ambient temperatures.
It is a primary object of this invention to prepare grease
compositions by a method which overcomes the objections noted
hereinabove.
According to the invention there is provided a process for preparing a
grease corn position, comprising forming a blend consisting
essentially of a lubricating oil, an organic acid the metal salt of
which is capable of thickening a lubricating oil to form a highmelting
point grease, a basic substance (as hereinafter defined) in an amount
sufficient substantially to neutralize said organic acid, and alcohol
or water as a solvent for said basic substance, heating the blend to a
temperature below that sufficient for substantial saponification of
the organic acid, subjecting the blend to a shearing force supficient
to form a salt by saponification of the organic acid, and essentially
simultaneously stably to disperse the salt in the oil to thicken the
oil to the consistency of a grease.
As used herein, the terms "a basic substance" and "metal base " mean
the oxides and hydroxides of the metals of Groups I, II, HI and IV of
Mendeleef's Periodic Table.
The amount of organic acid which is used is that which, upon

saponification, provides sufficient metal salt to thicken the base oil
to the consistency of a grease Thus, the organic acid may be employed
in an amount of from 5 % to 50 % by weight, based on the blend Because
of the greater efficiency obtained from the grease thickening agent by
the process of this invention, it may be necessary to use only from 7
% to 30 % by weight, based on the blend of such organic acid.
In the preferred process of the present invention, the organic acid is
first dissolved (or dispersed) in the base oil, after which the metal
base and the solvent for the metal base are mixed into the base
oil-acid blend at temperatures ranging from 100 F to 1400 F However,
the temperatures may range from room temperature to no more than about
F The resulting admixture is then heated, with agitation, to a
temperature not more than 2500 F, preferably no higher than 2200 F,
for the primary purpose of forming a uniform blend During this
heating, metal base solvent may incidentally be removed from the
lubricating oil composition The admixture is then cooled to a
temperature below 200 F, preferably below 1750 F.
The mixture is then subjected to a shearing force sufficient to cause
a reaction between the acid and the base substance to form a salt, and
essentially simultaneously to disperse the salt thus formed in the oil
to form a grease structure The shearing forces are sufficient to form
a salt of the acid of the thickening agent and substantially
simultaneously to stably disperse said salt in the oil to form a
stable gel structure and thicken the oil to the consistency of a
grease Generally, shearing forces sufficient for the foregoing purpose
have shearing rates in the range of 500 to 1 x 101 ' reciprocal
seconds; preferably from I x 101 to 1-x 107 reciprocal seconds.
The shearing forces of the process of the present invention can be
obtained by the use of the Manton-Gaulin Homogenizer, the Eppenbach C
Golloid Mill, the Cornell Homogenizer, high-speed gear pumps, and
other equipment which can impart the necessary shear rates to
compositions exemplified hereinabove.
Although-it is preferred that the ingredients are blended together
carefully until a uniform blend is obtained, a homogeneous mixture
prior to the action of the shearing forces is not essential.
By the grease manufacturing process described herein, greases having
dropping points in excess of 5000 F can be prepared by heating the
components of grease compositions to temperatures no greater than
about 2000 F The temperature is below that suffi 70 cient for
substantial saponification of the grease thickening agent acid For
example, a grease having a melting point of about 600 + O F can be
prepared by heating a base oil and salt-forming components to tempera
75 tures no higher than approximately 2000 F.
Such large temperature differentials are of considerable advantage in

saving energy, permitting the use of less expensive equipment, forming
light-colored high-temperature 80 greases, and allowing greases to be
prepared in a much shorter space of time than heretofore possible.
As used herein, -the term "grease thickening agent acid" means an
organic acid from 85 which the metal salt grease-thickening agent is
formed; that is, an organic acid the metal salt of which thickens
lubricating oils to the consistency of a grease.
As used herein, the term "high melting 90 point " refers to greases
having melting points greater than 3000 F.
Grease-thickening agents which form high melting point greases include
the metal salts of terephthalic acid, terephalamic acid, iso 95
phthalamic acid, amic acids, and soap-forming acids capable of forning
high melting point greases.
Other terephthaiainates which form high melting point grease
compositions include 100 those prepared from terephthalamic acids of
the formula:
I.
C OR CO R wherein R represents hydrogen or a hydrocarbon radical and R
1 represents a hydrocarbon radical containing from 10 to 22 carbon
atoms.
Examples of terephthalamic acids and derivatives which can be used in
the process of this invention for the preparation of high melting
point greases include N-decyl terephthalamic acid; N-dodecyl
terephthalamic acid; N-tetradecyl terephthalamic acid; Nhexadecyl
terephthalamic acid; N-octadecyl terephthalamic acid; N-eicosyl
terephthalamic acid; N-docosyl terephtha Lemic acid; methyl, N-decyl
terephthalamate; ethyl N-decyl terephthalamate, propyl N-decyl
terephthalamate; butyl N-decyl terephthalamate; pentyl Ndecyl
terephthalamate; hexyl, N-decyl tere786,103 decyl isophthalamic acid,
N-hexadecyl iso phthalamic acid, N-octadecyl isophthalamic acid,
N-eicosyl isophthalamic acid, N-docosyl isophthalamic acid, monodecyl
terephthalate, monododecyl terephthalate, monotetradecyl
terephthalate, monohexadecyl terephthalate, monooctadecyl
terephthalate, monocicosyl terephthalate, and monodocosyl
terephthalate, Polyamic acids which can be used according to the
process of this invention to form thickening agents for high melting
point greases include those which are formulated as follows:
phthalamate; heptyl N-decyl terephthalamate; octyl,N-decyl
terephthalamate; decyl N-decyl terephthalamate; ethyl N-octyl
terephthalamate; ethyl,N dodecyl terephthalamate; ethyl N-tetradecyl
terephthalamate; ethyl Nhexadecyl terephthalamate; ethyl N-octadecyl
terephthalamate; and ethyl N-eicosyl tere' phthalamate.
Similarly, the following isophthalamic acids, and esters of
terephthalic acid can be used in the process of this invention to form

higb melting point greases: N-decyl isophthalamic acid, N-dodecyl
isophthalamic acid, N-tetraii.
wherein R, R, and R, are hydrocarbon radicals, R, is hydrogen or a
hydrocarbon radical, and z is a positive integer denoting the number
of times the bracketted group recurs in the acid molecule.
The process of this invention is particularly well adapted to the
preparation of high melting point greases such as those which are
obtained by the use of acids set forth hereinabove However, other
acids which can be used in this process include fatty acids, the metal
soaps of which thicken lubricating oils, such as oleic acid, stearic
acid, and hydroxystearic acid.
Grease-thickening salts are formed in the process herein by the
reaction of the above.
noted acids with basic substances, that is, oxides and hydroxides of
the metals of Groups I, H, Im I, and IV of Mendeleef's Periodic Table
Particular metals include aluminium and lead, and the metals of Groups
I and II of Mendeleef's Periodic Table, such as lithiumi, sodium,
potassium, calcium, barium, strontium, magnesium, zinc, and cadmium.
The basic substances are used in amount sufficient to substantially
neutralize the greasethickening agent acid in the formation of
grease-thickening salts.
For the purpose of obtaining uniform distribution of the basic
substances in the 'lubricating oils, the basic substances are
dissolved (or dispersed 5 with the aid of water or alcoholic solvents
such as methyl alcohol and ethyl alcohol Although it is desirable to
use solvents which can be readily distilled from the lubricating oil
composition, a solvent may be used which becomes part of the grease
composition (e g, glycerol).
Lubricating oils which are suitable base oils for grease compositions
prepared according to the process of this invention include a wide
variety of lubricating oils, such as naphthenic base, paraffin base,
and mixed base mineral oils, other hydrocarbon lubricants, e g,
lubricating oils derived from coal products, and synthetic oils, e g,
alkylene polymers (such as polymers of propylene and butylene, and
mixtures thereof), alkylene oxide type 75 polymers, dicarboxylic acid
esters, liquicf esters of acids of phosphorus, alkyl benzenes, and
organic silicon compounds Synthetic oils of the polymerized alkylene
oxide type which may be used include those which may be exempli 80
fied by the alkylene oxide polymers (e g, propylene oxide polymers),
and derivatives, including alkylene oxide polymers prepared by
polymerizing the alkylene oxides, e g, propylene oxide, in the
presence of water or 85 alcohols, e g, ethyl alcohol; esters of
alkylene oxide type polymers, e g, acetylated propylene oxide polymers
prepared by acetylating propylene oxide polymers containing hydroxyl

groups; and polyethers prepared from alkylene 90 glycols, e g,
ethylene glycol.
The polymeric products prepared from the Various alkylene oxides and
alkylene glycols may be polyoxyalkylene diols or polyalkylene glycol
derivatives; that is, the terminal 95 hydroxy group can remain as
such, or one or both of the terminal hydroxy groups can be removed
during the polymerization reaction by esterification or
etherification.
Synthetic oils of the dicarboxylic acid ester 100 type include those
which are prepared by esterifying such dicarboxylic acids as adipic
acid, azelaic acid, suberic acid, sebacic acid, alkenyl succinic acid,
fumaric acid, and maleic acid with alcohols such as butyl alcohol,
hexyl 105 alcohol, 2-ethylhexyl alcohol, and dodecyl alcohol Examples
of dibasic (dicarboxylic) acid ester synthetic oils include dibutyl
adipate, dihexyl adipate, di-2-ethylhexyl sebacate, and di-n-hexyl
fumarate polymer Synthetic 110 oils of the alkyl benzene type include
those which are prepared by alkylating benzene (e.g, dodecyl benzene
and tetradecyl benzene).
Synthetic oils of the type of organic silicon compounds include the
liquid esters of silicon 115 and the polysiloxanes The liquid esters
of silicon include those exemplified by tetraethyl is 0 0 o 0 0 0 -IN
-(CR, C NH NH C R CCNH- NH)z C C -OH 786,103 silicate tetraisopropyl
silicate and tetra(methyl2-butyl) silicate.
The following examples illustrate the preparation of grease
compositions from a mixture of the base oil, the acid from which the
salt grease thickening agent is formed, a basic substance, and a
solvent for the basic substance, according to the present invention.
Example 1 illustrates the preparation of a monoester of a
terephthalamic acid, the soaps of which are used as grease-thickening
agents.
EXAMPLE 1.
Preparation of the Methyl Ester of N" Octadecyl " Terephthalamate.
A mixture of 45 pounds of dimethyl terephthalate and 255 pounds of
benzene was heated to 1300 F until all of the dimethyl tereplithalate
was dissolved, after which a solution of 12 3 pounds of potassium
hydroxide in 58 5 pounds of absolute alcohol was added The heating was
continued at 1300 F for an additional 50 minutes.
It is to be particularly noted that in this reaction only one methyl
group is saponified, and when this saponification has been completed,
the salt precipitates from the benzenealcohol mixture.
gallons of water were added to the above mixture to dissolve the
potassium salt of mo nomethyl terephthalate thus formed The aqueous
layer of the salt was separated, and to this aqueous layer was added 3
5 liters of concentrated sulfuric acid at room temperature to form the

free acid having the formula:
CII 3 02 C-C:ootfl This acid was filtered, washed with water, and
dried in zacuo After purification, the neutralization equivalent of
the acid thus formed was 180, which is equal to the theoretical
neutralization equivalent.
28 pounds of the acid were dispersed in 37 pounds of benzene and
heated to about ' F, after which 20 5 pounds of thionyl chloride were
added over a period of 2 hours at 185 ' F After the complete addition
of thionyl chloride, the mixture was refluxed for 4 hours The excess
thionyl chloride and benzene were then removed by distillation.
The product obtained at this point has the formula-:
C H 302 c {C 3 K Dcoc C A mixture of 25 pounds of this acid chloride,
9.5 pounds of triethylamine and 26 6 pounds of "octadecyl'" amine was
heated at about 160 ' F until the amine had substantially wholly
dispersed, after which the mixture was heated at 180 ' F for 15
minutes.
To the above mixture was added 15 gallons of water at 195 F, after
which the mixture was filtered.
The methyl ester of N-" octadecyl " terephthalamic acid thus prepared
was washed three times with hot water and dried The zaponification
equivalent of the final product was 471 (the average of four
determinations).
The "octadecyl" amine used herein was a commercial preparation of
amines known as "Armeen HT," sold by the Armour Company, and
containing 25 % hexadecylamnine, % octadecylamine, and 5 %
octadecenylamine 85 % of this mixture consists of nprimary amines.
EXAMPLE 2.
Preparation of a Grease Thickened with Barium N-" Octadecyl "
Terephthalamate 75 A mixture of 250 grams of the methyl ester of N-"
Octadecyl " terephthalamate of Example 1, 97 5 grams of a barium
hydroxide monohydrate in 1500 grams of water, and 2152 5 grams of a
California solvent refined 80 paraffin base oil having a viscosity of
480 S.S U at 100 ' F, was blended together by heating to a maximum
temperature of 220 ' F This mixture wjas then passed through a
Manton-Gaulin colloid mill at the rate of 85 3 pounds per minute at a
pressure of 4000 psig The temperature of the mix as it went into the
mill was 130 ' F, and the temperature of the grease coming out of the
mill was ' F The resulting grease composition 90 had a worked
penetration of 335 after 60 strokes in an ASTM worker, and the
dropping point was 4780 F.
EXAMPLE 3.
Preparation of a Grease Thickened with 95 Calcium N-"Octadecyl"
Terephthalamate.
A mixture of 250 grams of the methyl ester of N-" Octadecyl "

terephthdtamate of Example 1, 22 5 grams of calcium hydroxide in 25
grams of water, and 2227 5 grams of 100 a California solvent refined
paraffin base oil having a viscosity of 480 S S U at 100 ' F.
was slowly heated to a temperature of 200 ' F., then cooled to a
temperature of 130 ' F.
At this latter temperature, the -mixture was 105 passed through a
Manton-Gaulin colloid mill at a rate of 3 pounds per minute at a
pressure of 4000 psig The temperature of tha thickened composition as
it came from the colloid mill was 170 ' F 110 EXAMPLE 4.
Preparation of Lithium Hydroxy-Stearate Thickened Grease.
A mixture of 250 grams of 12-hydroxystearic acid, 41 5 grams of
lithium hydroxide 115 monohydrate in 250 grams of water, and 2208 5
grams of a California solvent refined paraffin base oil having a
viscosity of 480 S.S U at 100 ' F was heated to a temperature of 180 '
F with continuous stirring The 120 temperature of the mixture was then
lowered to 125 ' F, after which the mixture was charged to a
Manton-Gaulin colloid mill at My 786,103 The temperature to which the
ingredients of the grease composition are originally heated before
they are subjected to a shearing force is below that sufficient for
substantial saponification of the salt-forming organic acid; that is,
the temperature is such that just prior to the time when the
ingredients of the grease composition are subjected to a shearing
force, the organic acid and the basic substance are present as such,
and not as salts or the organic acid.
Table I hereinbelow presents data showing that a grease structure is
not obtained during the initial heating of the grease components prior
to the milling step These data were obtained by heating a mixture
consisting of methyl,N-" Octadecyl " terephthalamate, an aqueous
slurry of sodium hydroxide and a California solvent refined base oil
having a viscosity of 480 SSU at 1000 F to the temperature noted The
grease-thickening agent was present in an amount of 10 %, by weight.
The worked (PJ 0) and unworked (P 0) penetration values (at 77 F) and
the dropping point were determined (The worked penetration was
obtained after 60 strokes in the ASTM worker).
the rate of 3 pounds per minute at a pressure of 4000 psig The
temperature of the grease composition as it came from the mill was 180
F The grease composition had a worked penetration of 380 after 60
strokes in the ASTM worker, and a dropping point of 3030 F.
In the several examples noted above, it is readily seen that the
temperatures at which the grease compositions were formed were
considerably lower than those which were necessary when a
grease-thickening agent is solubilized in an oil via the usual methods
of heating and dissolution For example, the grease composition of
Example 6 was formed in a very short period of time at a maximum

temperature of 1800 F However, no grease would have resulted therefrom
if, for example, the hydroxy-stearic acid, lithium hydroxide
octahydrate, and oil had been merely heated at 180 F for such a short
period of time without further treatment It would have been necessary
to heat the composition for a number of hours (i e, approximately 10
hours at that temperature) to obtain the same grease structure in the
base oil which was here obtained in a matter of only a few minutes.
786,103 S TABLE I
Temp to which Unnilled Milled ( 1) sample had been Sample heated
before Dropping Dropping Number milling, 'F Point, O F PO P 6 O Point,
'F PO P 60 1 100 100 430 + 430 + 2 125 100 430 + 430 + 500 + 340 3 150
100 430 + 430 + 500 + 189 280 4 175 164 351 430 + 500 + 174 265 220
190 430 + 500 + 6 250 183 430 + 500 + 7 300 206 430 + 500 + 265 8 ( 2)
180 ( 1) The samples were passed through a Manton-Gaulin mill at a
pressure of 4000 psig.
rate of 3 pounds per minute at a ( 2) This sample consisted only of
the base oil and the grease-thickening agent acid, not the salt.
The electron-photomicrograph of Figure 1 of the accompanying drawings
illustrates the appearance of a grease-forming composition after it
had been heated, and before it was passed through a colloid mill The
picture shows that a grease structure had not been obtained This
particular electro-photomicrograph was obtained of a mixture of 330
grams of methyl,N-" Octadecyl" terephthalamate, grams of sodium
hydroxide in 30 grams of water, and 264 Q grams of a California
solvent refined paraffin base oil having a viscosity of 480 SSU at
1000 F which was heated to F for a period of approximately 30 minutes.
The electron-photomicrograph of Figure 2 of the accompanying drawings
illustrates the appearance of the grease structure after the above
mixture had passed through a MantonGaulin colloid mill at the rate of
450 grams per minute The resulting grease had a worked penetration of
296 after 60 strokes in the ASTM worker.
* Sitemap
* Accessibility
* Legal notice
* Terms of use
* 5.8.23.4; 93p

5691 5695.output

Recommended

Recommended

More Related Content

What's hot

What's hot (20)

Viewers also liked

Viewers also liked (15)

Similar to 5691 5695.output

Similar to 5691 5695.output (20)

More from Иван Иванов

More from Иван Иванов (20)

Recently uploaded

Recently uploaded (20)

5691 5695.output