* GB786099 (A)

Description: GB786099 (A) ? 1957-11-13

Improvements in or relating to devices for tightening screw closures in oraround 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.

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* GB786100 (A)

Description: GB786100 (A) ? 1957-11-13

Improvements in tampons or other absorbent plugs

Description of GB786100 (A) Translate this text into Tooltip

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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.

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

Description of GB786101 (A)

PATENT SPECIFICATION Inventor: DOUGLAS LOUIS AS'HTON DRIVER 7 Date of Application and filing Complete Specification: June 24, 1955. No 18272/55. Complete Specification Published: Nov 13, 1957. 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.

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* GB786102 (A)

Description: GB786102 (A) ? 1957-11-13

Improvements relating to casting resins

Description of GB786102 (A)

A high quality text as facsimile in your desired language may be available

amongst the following family members:

FR1154015 (A) FR1154015 (A) less Translate this text into Tooltip

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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.

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 follow- ing - 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 highmelting point greases

Description of GB786103 (A)

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PATENT SPECIFICATION 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; Complete Specification Published: Nov 13, 1957. 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.

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