* GB784658 (A)

Description: GB784658 (A) ? 1957-10-16

Improvements in or relating to storage devices for cylindrical objects

Description of GB784658 (A)

COMPLETE SPECIFICATION Improvements in or relating to Storage Devices for Cylindrical Objects We, R. H. CORBETT & COMPANY LTMrTED, a British company, of Hydrum Works, Burgess Hill, Sussex, do hereby declare the invention, for which we pra9 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 devices for storing cylindrical objects and provides a device which is particularly suitable for the storage of barrels and drums such as forty-gallon steel drums of oil. The object of the invention is to provide a storage device for cylindrical objects in which the objects can be introduced at one end and removed as and when required from the other end. A further object d the invention is to provide a storage device that includes a gate which normally retains the cylindrical objects in the device, but which can be opened to permit the removal of one, or in certain circumstances, a number of the cylindrical objects and which will in this open position continue to act as a stop for the remaining objects. The invention consists in a storage device for cylindrical objects including an inclined rack at the lower end of which is arranged a gate having first and second angularly dis posed portions and pivoted to the rack in the vicinity of the angle between said portions, said first portion including an upstanding stop member ~ and said second portion being arranged so that it acts as a positive stop member so long as an object is resting on the first portion. The angle of inclination of the rack is such that when a cvlindrical object is introduced at the higher end of the rack it rolls towards the lower end.

In the case of forty-gallon steel barrels of oil it has been found that a gradient of between 1 in 20 and 1 in 30 is required to make the barrels roll towards the lower end without the application of any external force. The need for such a steep gradient arises partly as a result of friction between adjacent barrels and partly because some barrels are not perfectly cylindrical. As a result of this steep inclination of the rack at least some of the barrels acquire considerable momentum by the time they reach the lower end of the rack and an ordinary stop would have to extend almost to the centre line of the barrels in order to prevent them rolling off the end of the rails with sufficient certainty. Consequently when the racks are arranged in tiers a considerable space would have to be allowed between adjacent tiers to permit a barrel being lifted over the stop. If to reduce the necessary clearance between adjacent tiers the stop were replaced by an ordinary movable gate some additional means would have to be provided to prevent more than the required number of barrels from rolling off the end of the raclr when the gate is opened. It will therefore be seen that a storage device in accordance with the invention is particularly suitable for use in connection with the storage of steel barrels of oil, since it operates to allow any desired number of barrels to be released at a time arid may also be designed, as will hereinafter be explained, in such a way that very little additional clearance between the adjacent tiers is required. In order that the invention may be fully understood, an example of a storage device for use with forty-gallon drums will now be described with reference to the accompanying drawings in which: Figure 1 is a plan view of a device in accordance with the invention; Figure 2 is a vertical section on the line 11-11 shown in Figure 1 and shows the gate n the normal position, and Figure 3 is a vertical section showing the gate in the "open" position, with a drum passing therethrough. A rack is formed by two guide rails 1 which are arranged to have a gradient of between 1 in 2G and 1 in 30 and by a suitable supporting framework part of which is shown at 10. A pin 2 passes through holes in the two guide rails 1 and serves as a pivot for a gate. The gate has two parallel shallow V-shaped side members, one arm 4 of the V being longer than the other arm 3 in each case and inclined thereto at an angle of 150 to 160 . The two shorter arms 3 are connected by a positive stop member in the form of a bar 5 which has a circular cross-section- and which is welded to the upper edges of their free ends. The free ends of the longer arms 4 are connected by an upstanding stop member in the form of an angle-ptece 6 which is mounted on corner pieces 7 and which projects above the arms 4 and the

end of the rails 1. The gate has additional strengthening crosspieces 8 and 9, which extend respectively between the arms 3 midway along their lengtll, and between the arms 4 in the neighbourhood of the pin 2. The longer arms 4 are arranged towards the lower end of the rails 1 and sine this part of the gate is made heavier than the remainder, the gate normally occupies the position shown in Figure 2 with the longer arms 4 of the side members parallel to the rails 1 and the shorter arms 3 making an angle of 20 to 30 therewith. When a drum is introduced into the upper end of the empty rack it rolls down the rails 1 and acquires a considerable momentum. The weight and dimensions of the gate are so arranged relative to the length arid gradient of the rails 1 and the size and weight of the drum, that when the drum strikes the bar 5, it moves the gate into the position shown in Figure 3. Friction between the guide ribs of the drum and the bar 5 decelerates the drum which then rolls slowly onwards along the rails 1 until it passes above the Divot nin 2. The gate then moves back into its normal position (Figure 2) and the drum strikes the angle-piece 6 which brings it to rest. As a result of the aforementioned deceleration, the speed of the drum when it strikes the anglepiece 6 is very much less than when it strikes the bar 5. Consequently the height of the angle-piece 6 can be considerab!v less thin the radius- of the drums. Thus when the storage device is designed, as in the present example, for forty-gallon drums having a radius of about 12 inches, the angle-piece 6 may be about 3 inches high. When a second drum rolls down the rails 1 it is brought to rest against the bar 5, since the gate is so dimensioned that the momentum of said second drum is insufficient to cause the gate to turn about its pivot when the first drum is resting against the angle-Piece 6. The gate is also dimensioned in such a way that when the first drum is removed from the storage device, the pressure of the second drum against the bar 5 is alone insufficient to cause the gate to turn about its pivot pin 2. In order to allow the second and any succeeding drums to pass over the gate, mechanically or manually operated means (not shown) is provided to move the gate out of its normal position. For example a hook may be used to pull down the bar 5 or a rope or lever may be attached to the gate in a suitable position. Alternatively, if a fork lift truck is used to remove drums from the end of the rack, one of the folks may be used to move the gate out of its normal posi, on. If a truck having long forks is used, it is possible to remove more than one drum at each pass.

It will be seen that whatever means is used to lift the drums off the end of the rack! the drums need only be raised to the extent of the height of the angle-piece 6 before they can be removed. What we claim is: 1. A storage device for cylindrical objects including an inclined rack at the lower end of which is arranged a gate having first and second angularly disposed portions and pivoted to the rack in the vicinity of the angle between said portions said first portion including an upstanding stop member and said second portion being arranged so that it acts as a positive stop member so long as an object is resting on the first portion. 2. A storage device according to Claim 1 in wrick the inclined rack includes guide rails and a supporting framework. 3. A storage device according to Claim 2 in which the guide rails have a gradient of betiveen 1 in 20 and 1 in 30. 4. A storage device according to any of the preceding claims in which the first portion of the gate is heavier than the second portion of the gate. 5. A storage device according to any of the preceding claims in which the first and second portions of the gate are inclined to each other at an angle of from 150 to 160 . 6. A storage device according to any of the preceding claims in which the upstanding stop member is in the form of an angle-piece. 7. A storage device according to claim 6 in which the height of the angle-piece is about 3 inches. 8. A storage device according to anv of the preceding claims in which an object stopped by the second portion rests against a bar pro- vided on that portion. 9. A storage device according to Claim 8 in which the bar has a circular cross-section. 10. A storage device according to Claim 8 or Claim 9 in which the bar is welded to the upper edges of the free ends of the side members of the second portion. 11. A storage device according to any of the pi.ecedn claims in which mecbanicallv or m3nu?11-y- operated moans is provided to move the gate OUL", of its normal position. 12. A storage device according to any of the

* GB784659 (A)

Description: GB784659 (A) ? 1957-10-16

Therapeutic compositions and aqueous suspensions thereof

Description of GB784659 (A)

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COMPLETE SPECIFICATION -Therapeutic Compositionst and Aqueous Suspensions thereof We, THE UPJOHN COMPANY, a corporation organized and existing under the laws of the State of Michigan, United States of America, of 301 Henrietta Street, Kalamazoo, State of Michigan, United Stales of America, do hereby declare rhe 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 fluid aqueous suspensions of solid insoluble organic medicinal agents. Aqueous suspensions of solid insoluble organic medicinal agents present many problems such as crystal growth, poor suspendibility, sedimentation, caking, agglomeration, difficultly of iesuspendibility after storage, color formation, change in viscosity, poor drainage from the walls of Ithe container, sterilization, and the like. It is therefore importent that these factors which affect the usefulness lof these suspensions should be controlled. It is an object of the present invention to obviate one or more of these problems and to provide a new and improved vehicle for suspending solid insoluble organic medicinal agents. Another object is

to provide aqueous suspensions which are not only non-caking but easily syringeable and therefore suitable for parenteral use. Still another object of the invention is to provide such suspensions which drain cleanly from la container, will not clog the needle of a ilypadermic syringe and are easily resuspended by gentle shaking when settling does occur. A further object of the invention is to provide dry therapeutic compositions containing a solid insoluble organic medicinal agent which will readily form highly satisfactory suspensions on the addition of an aqueous vehicle. Other objects land features of the invention will be apparent to those skilled in the art to which this invention pertains. The invention provides compositions containing a solid, insoluble organic medicinal agent, of specific gravity less than about two dispersed in an aqueous polyalkylene glycol vehicle. The compositions may include soluble active ingredients in addiction to suspended active ingredients. The compositions are available in the form of aqueous suspensions or as dry mixtures to which an aqueous vehicle is added prior to use. Suspensions containing, in accordance with the invention, a solid, insoluble organic medicinal agent and a polyalkylene glycol are unusually stable as they re-suspend easily even after extended periods of time and do not cake or clump. The polyalkylene glycols of the invention are of pharmaceutical grade, nonmtoxic, inert, and capable of being sterilized without change in composition. Polyalkylene glycols include polyethylene glycols and polypropylene glycols and mixtures thereof. On the addition of an aqueous vehicle to a dry composition containing the selected solid insoluble organic medicinal agent and polyalkylene glycol, followed by mixing, a stable suspension is readily obtained. The preferred polyalkylene glycols are the polyethylene glycols of molecular weight between about 200 and about 6000 more especially a molecular weight greater than 4000 and the preferred concentrations range between about 0.1 and about 62 percent by weight of the final product. The optimum concentration of polyalkylene glycol depends upon the molecular weight of the polymer and also upon the solid insoluble medicinal agent used. For example, when a polyethylene glycol ob molecular weight between about 4000 and about 6000 is used in the preparation of an aqueous suspension containing an insoluble penicillin compound, the preferred concentration of polyethylene glycol is between about 0.25 and about 4 percent by weight When the solid insoluble organic medicinal agent is a steroid such as hydrocortisone acetate or cortisone acetate, the optimum range is between about itwo and about twelve percent by weight. When polyethylene glycols of lower molecular weight, i.e., between

about 200 and about 600 are utilized, at least about twenty to about thirty percent by weight thereof is required. A polyalkylene glycol also considered to be within the purview of this invention is an ethylene oxide-propylene glycol condensation product in which the alkylene units consist of ethylene and propylene units, said propylene units being in non-terminal positions and connected to each other in a straight chain. This group of compounds is represented by the following formula: HO(C2H408)a(C3HoO3b(G2H40)eH wherein a, b and c are positive integers which can be varied over a considerable range. Thus, the molecular weight of either ithe lz ropAzabic base (propylene oxide portion) or JiydropAc element (ethylene oxide portion) can be varied in small increments over a wide range. It is desirable to use a product having a bare, i.e., polypropylene glycol unit, molecular weight between about 1500 and about 1800 with between about eighty and about ninety percent ethylene oxide in the condensation product This product can also be designated by reference to the structural formula wherein b is between about 25 and about 32 and a + c is between about 136 and about 368. A typical product is " Pluronic F 68" (Wyandotsre Chemical Corp.) wherein "F" designates the product in fake form. The product is also available in liquid or paste form. The term "solid, insoluble organic medicanal agent" as used throughout the specification and claims refers to materials which possess a specific gravity of less than about two and are also slightly soluble in water, i.e., at least 100 parts or more of solvent are needed to dissolve one part of the medicinal (Haclilt's "Chemical Dictionary "). However, materials of greater water solubility are also to be considered within the designation of a solid insoluble organic medicinal agent provided that the medicinal, in the amount used in the aqueous polyalkylene vehicle, is substantially undissolved therein. Such materials include antibiotics such as erythromycin, and insoluble derivatives including esters thereof, chloramphenicol, tetracycline, oxytetracycline, chlortetracycline, and in soluble derivatives including salts thereof, penicillin salts of substituted alkylene diamines such as N,Nl- dibenzylethylene diamine di - penicillin, N,N1 - di - ( - methylbenzyl) - ethylene diamine di- penicillin, N,Nl - difurfuryl- ethylenediamine di penicillin, N.N1 - his- (3 ,5,5-trimethylhexyl)ethylene - diamine penicillin, aluminium penicillin sulfonamides, procaine penicillins G, O; K, 2-chloroprocaine penicillins, steroids such as progesterone, testosterone propionate, estradiol monobenzoate, cortisone, hydrocortisone, insoluble esters of cortisone and hydrocortisone such as the aces tate, hydrated acetate, propionate, cyclopentylpropionate, diethyl acetate, trimethyl acetate, benzoate, naphthoate, laurate,

palmitate, phenylacetate, phenylpropionate, benzene sulfonate, toluene sulfonate; halo steroids, and more specifically, halo cortisones such as 9.X-chlorocortisone, 9- > -chlorocortisone, 9-,- fluorocortisone and esters thereof, and halo hydrocortisones such as 9-7-chlorohydrocorti- sone, 9-l-fluorohydrocortisone; and esters thereof; -sulfonamides such as sulfamerazine, sulfadiazine, sulfamethazine; and other therapeutic materials such as barbiturates, e.g., phenobarbital, barbital, 2-monobromisovalerylcarbamide (Bromural) Registered Trade Mark, bromodiethylacetylurea (Carbromal), salicylamide, and acetophenetidin. The particle size of the solid, insoluble organic medicinal can be varied over a large range depending upon the medicinal and the mode or method of administration of the therapeutic preparation. For example, for ophthalmic use, substantially all of the particles should be less than about twenty microns and preferably less than ten microns in size. For parenteral use; the particle size can be as large as about eighty microns although it is preferred that a majority of all of the particles should be less than about fifty microns in size. Where the suspension contains a high concentration of the medicinal agent, as for example in procaine penicillin suspensions, substantially all of the particles should be less than about eighty microns in size and preferably should contain a mixture of fine and coarse particles. Fine particles are in the order of two to about ten microns in size and the ccarset particles are betwe n about forty and about sixty microns in size. The ratio of fine to coarse particles can vary in ratios between about 1:1 and between about 1: 4. For oral and general topical use, however, the particle size of the solid insoluble organic medicinal agent is limited only by the specific gravity of the liquid and solid materials and the viscosity of the liquid with the added requirement that the preparation should be fluid in nature, i.e., readily pourable from a container at room temperature and readily resuspendible at room temperature as contrasted with ointments, and water soluble creams, which are not fluid or pourable or readily resuspendible at room temperature. The viscosity of the therapeutic suspensions varies depending upon their mode of administration. For example, for parenteral administration, the viscosity of the suspensions range from as low as about one up to about 150 centipoises at 25 degrees centigrade and in the case of a preparation of low solids content, i.e., between about five to about 25 mgs/ cc. of suspension, it is preferred that the viscosity should be less than about five centipoises and in the case of preparations of high solids content, i.e., more than about 300 mgs./ cc. of suspension, it is preferred that the viscosity should range between about twenty and about 150 centipoises. For general

topical administration, including ophthalmic, oral, nasal, and aural preparations, the viscosity of the therapeutic suspension may range up to about 2000 centipoises or even higher, the only limitation being that the suspension is fluid, pourable and can be re-suspended at room temperature. The viscosity of ophthalmic preparations should preferably be less than about five centipoises. While preparations containing a medicament and a polyethylene glycol are available in the form of ointments, these semi-solid compositions are free from such problems as settling, re-suspendibility, caking and agglomeration of the medicament. Preparations of this nature are limited to local applications on the skin and are not to be used for other modes of administration, i.e., oral, parenteral, aural, ophthalmic or nasal, advantageously available to the fluid suspensions of the invention. Similarly, the fluid suspensions of the invention are distinguisbable from solutions of soluble medicametts wherein the aforementioned problems of suspendibility, re-suspendibility, caking and agglomeration are not encountered. In some instances, the addition of a surface active agent to an aqueous suspension containing a solid insoluble medicinal agent and a polyalkylene glycol improves the quality of the suspension, i.e., suspendibiliy, inhibition of crystal growth and general stability. The non-ionic surface active agents such as the polyoxy- alkylene ethers of partial higher fatty lacid esters of polyhydroxy alcohols (Tweens 20 and 80) Registered Trade Mark, are preferred because of greater compatibility and overall acceptance for medicinal preparations. Other surface active agents such as arylalkyl polyether alcohols including derivatives thereof such as Triton A 20, Triton 770 Registered Trade Mark, fatty acid esters of polyethylene glycol such as Emulsol 0,; dial esters of a sulfosuccinic acid such as the Aerosols, and like non-toxic surface active agents can also be used especially in extemporaneous preparations. These agents can be present in the suspension in amounts varying between about 0.05 and about 1.0 peroent by weight Mixtures of a solid insoluble medicinal agent together with a soluble medicinal agent are also within the purview of the invention. Such mixtures include, for example, a procaine penicillin and sodium or potassium penicillin, N,N1-dib enzylethylene diamine dipenicillin and sodium or potassium penicillin, neomycin sulfate and cortisone, neomycin sulfate and hydrocortisone, neomycin sulfate and insoluble esters of cortisone and hydrocortisone such as the acetate, hydrated acetate, propionate, cyclopentylpropionate, diethyl acetate, trimethyl acetate. benzoate, naphthoate, laurate, palmitate, phenylacetate,

phenylpropionate, benzene sulfate, toluenesulfon- ate, neomycin sulfate and a halo steroid, and more specifically, neomycin sulfate and a halo cortisone such as 9 - a - chlorocortisone, 9-afluorocortisone, and esters thereof, neomycin sulfate and a halohydrocortisone such as 9-achlorohydro-cortisone, 9-a-fluorohydrocorti 5flne, and esters iereof, a procain penicillin and a streptomycin or dihydrostreptomycin salt. A typical composition of the invention may contain, in addition to the solid insoluble organic medicinal agent and polyalkylene glycol, a surface active agent, a lubricant (where ophthalmic use is contemplated), a preservative to inhibit bacterial or fun gal action and Ithereby insure a sterile product, a buffer and an isotonic agent to adjust the osmotic pressure so that it is approximately equivalent to about 0.9 percent saline. Conventional preservatives, buffers, zsotonic agents and lubricants are used. Satisfactory lubricants are glycerol, sorbitol and propylene glycol. Suitable preservatives include " Mefthio- late" Registered Trade Mark (sodium ethylmercurithiosalicylate), chiorobutanol, "Quatresin" (myristyl y-picolinium chloride), benzyl alcohol, sodium benzoate and methylparabl m. For ophthalmic use, "Merthiolate," chiorobutanol and "Quatresin" are preferred. Suitable buffers or stabilizers are sodium or potassium citrate and various mixed phosphate buffers. Where a suspension containing procaine, penicillin, cortisone acetate, hydrocorti sone, hydrocortisone acetate, is prepared, it is desirable to use Sodium citrate as a buffer. The stabilizer content may also be varied within the skill of the ant. Thus sodium or potassium citrate may range in amounts from about 0.5 to about five percent by weight while sodium phosphate, monobasic or dibasic, may be used in amounts varying between about 0.05 and about two percent. For a suspension of procaine penicillin, it is desirable to use sufficient buffer to keep the suspension close to but below a pH of about seven, that is, at a pH between about five and about seven. It should be noted that the pH may change upon storage depending upon the temperature. For example, if the initial pH is between about 6.3 and 6.5, it will probably go down to about 5.5 to 5.8 upon storage at room temperature for any considerable length of time. For oral suspensions, suggested additives are coloring, sweetening and flavoring agents. A range for sucrose may be from five to sixty percent by weigh;t and for saccharin or Sucaryl (sodium N-cyclo hexyl sulfamate), from 0.5 to four percent by weight It is advantageous to include in these compositions hydrophilic materials which are either synthetic in nature such as carboxymethylhydroxymethylcellulose, hydroxyethyl cellulose, dextran,

methylcellulose, polyvinylpyrrolidone, water-soluble salts of carboxy methylcellulose, or natural occurring hydrophilics such as gelatin, alginates, tragacanth, pectin, acacia, and soluble starches. In some instances, improvement in the suspensions of the invention is obtained by coating the insoluble material to be suspended with a phospholipid such as lecithin or cephalin. Where lecilthin is added to the suspension, a concentration between about 0.1 and about 3 percent is used while fas a coating on a procaine penicillin, for example, the amount can vary between about 0.5 percent and about 6 percent by weight It is preferred to include lecithin in aqueous polyalkylene glycol, and more specifically, aqueous polyethylene glycol suspensions containing procaine penicillin. It is apparent from the foregoing that there are many variables involved in the preparation of the desired aqueous suspensions of the invention. Numerous experiments have been conducted in an attempt to adjust the variables in the preparation of the most desirable products. While the basic combination of a solid, insoluble organic medicinal agent, and a polyalkylene glycol is the most important fundamental factor in the invention3 other factors feature additional improvements in the suspension. In the following tables, aqueous suspensions containing solid, insoluble organic medicinals are prepared wherein the effects are noted of variations in the concentration and components of the vehicle. Where solids are used, concentration is expressed in percent weight by volume of the aqueous suspension and in the case of liquid components, the concentration is expressed in percent volume by volume. In each case, water is added to provide a final volume of 100 percent. TABLE I Progesterone Active Compound Polyethylene Tween Sodium Benzyl Methyl- Propyl- Glycol Form Conc. 80 Chloride Alcohol Paraben Paraben 4000 1. Micronized 2.5% 0.4% 0.9% - 0.18% 0.02% 12% 2. ,, " " ,, 1.5% - - 12% 3. " 3, " " - 0. 18% 0.02% 6% 4. ,, " 33 " 3, ,, 3% 5. " 33 3, 3, ,, 3% These compositions were prepared by asep tically mixing the sterilized powdered medi cinal agent with the sterilized vehicle. The resulting suspensions were readily re suspended after storage for sixty days at

forty degrees centigrade, 25 degrees centi grade, and four degrees centigrade and when re-suspended, withdrawal of uniform doses was possible. The supernatant liquid was clear and free of solids on standing. No crystal growth had occurred. The solids did not cake on standing. The vehicles for all the preparations were readily clarified and sterilized by filtration. Little difference in viscosity could be detected between the three percent and twelve percent polyethylene glycol vehicles. While optimum results were obtained when a wetting agent such as Tween 80 was used, satisfactory results were likewise obtained in the absence of a surface active agent. TABLE II *Estrogenic Crystallizate Active Compound Polyethylene Sodium Tween Methyl- Propyl Form Conc. Glycol 4000 Chloride 80 Paraben Paraben Micronized 0.2% 3% 0.9% 0.4% 0.18% 0.02% * Naturally occurring equine estrogens consisting primarily of estrone, equiline and equilenin with possible traces of estradiol. The aqueous suspension was prepared by aseptically mixing the powdered medicinal agent with the sterilized vehicle. The solids exhibited uniform settling properties on standing. Resuspension of the separated solids could be accomplished very readily and when re-suspended, withdrawal of uniform doses was possible. No caking occurred after storage for sixty days at forty degrees centigrade, 25 degrees centigrade, and four degrees centigrade. The vehicle could be clarified and sterilized by filtration. TABLE III Testosterone Active Compound Polyethylene Sodium Tween Methyl- Propyl Glycol Glycol 4000 Chloride 80 Paraben Paraben Form Conc. Micronized 2.5% 3% 0.9% 0.4% 0.18% 0.02% The aqueous suspension was prepared by mixing the powdered medicinal agent with the vehicle. The solid material settled slowly and uniformly, and was very easily re-suspended after storage for thirty days at forty degrees centigrade, 25 degrees centigrade and four degrees centigrade. Uniform doses could be readily withdrawn. - Separation of solids on storage left a clear supernatant liquid. No caking occurred on standing. The vehicle could be readily clarified and sterilized by filtration, TABLE IV *Cyclogesterin

Active Compound Polyethylene Sodium Tween Methyl- Propyl Form Conc. Glycol 4000 Chloride 80 Paraben Paraben Micronized (Progesterone) 2.5% 3% 0.9% 0.4% 0.18% 0.02% (Estrogenic Crystallizate) 0.25% * An aqueous suspension of a mixture of powdered progesterone and powdered estrogenic crystallizate. The aqueous suspension was prepared by mixing the powdered medicinal agent with the vehicle. The solids showed gradual and uniform settling on standing. Resuspension of the separated solids could be accomplished very readily and when re-suspended, with drawal of uniform doses was possible. No caking occurred after storage for sixty days at forty degrees centigrade, 25 degrees centigrade, and four degrees centigrade. The vehicle could be readily clarified and sterilized by filtration. TABLE V Hydrocortisone Active Compound Polyethylene Sodium Tween Methyl- Propyl- Form Conc. Glycol 4000 Chloride 80 Paraben Paraben 1 Micronized 5.0% 12.0% 0.9% 0.4% 0.18% 0.02% 2 ,, ,, 3.0% " 0.4% ,, 3 " ,, 3.0% " 0.3% " ",, 4 ,, 3.0% " 0.2% " " The aqueous suspensions were prepared by mixing the powdered medicinal agent with the vehicle. These suspensions were very stable and highly satisfactory. The solid materials were readily dispersible to form highly satisfactory uniform suspensions. TABLE VI Hydrocortisone Active Compound Polyethylene Sodium Tween Benzyl Form Conc. Glycol 4000 Chloride 80 Alcohol Dextran 1 Micronized 5.0% 12.0% 0.9% 0.4% 1.5% 2 " 5.0% 3.0% 3 " 10.0% 3.0% 4 ,, 5.0% 2.0% 5 ,, 10.0% 2.0% 6 " 5.0% 1.0% " " " 3.0% 7 ,, 10.0% 1.0% " " " 3.0% Th aqueous suspensions were prepared by mixing the powdered medicinal agent with the vehicle. These compositions were satisfactory with regard to clarity of the supernatant liquid, re-suspendibility, and syringeability. In Preparations No. 3 and No. 5, suspem. sions of five and ten percent hydrocortisone were equally satisfactory in these vehicles. The addition of a suspending agent such as dextran (Preparations 6 and 7) increased the viscosity of the vehicle. This additive did not affect the usefulness of the polyalkylene glycol in the vehicle. TABLE VII Hydrocortisone Acetate Active Compound

Polyethylene Sodium Tween Methyl- Propyl Form Conc. Glycol 4000 Chloride 80 Paraben Paraben 1 Micronized 5.0% 12.0% 0.9% 0.4% 0.18% 0.02% 2 " " 3.0% " 0.4% 3 ,, 3.0% " 0.3% 4 ,, ,, 3.0% " 0.2% The aqueous suspensions were prepared by mixing the powdered medicinal agent with the vehicle. These suspensions were highly satisfactory and easily re-suspended after storage tor one month at forty degrees centigrade, 25 degrees centigrade and four degrees centigrade. TABLE VIII Hydrocortisone Acetate Active Compound Polyethylene Sodium Tween Benzyl Dex- KH2 Na2 Form Conc. Glycol 4000 Chloride 80 Alcohol tran PO4* HPO** 1 Micronized 5.0% 12.0% 0.9% 0.4% 1.5% - - 2 " " 3.0% " " " - - 3 ,, ,, 2.0% ,, ,, n - - 4 ,, " 1.0% ,, ,, 3.0% - - 5 ,, ,, 3.0% ,, " " - 0.6% 1.2% * Potassium Phosphate Monobasic. ** Exsiccated Sodium Phosphate U.S.P. The aqueous suspensions were prepared by mixing the powdered medicinal agent with the vehicle. Preparations 1, 2, 3 and 4 were maintained for two months at forty degrees centigrade, 25 degrees centigrade and four degrees centigrade. Preparation 5 was maintained for one month at forty degrees centigrade and four degrees centigrade. Miter the indicated periods of time, these aqueous suspensions were highly satisfactory with regard to clarity of the supernatant liquid, resuspendibility, syringeability and freedom from caking or agglomeration. TABLE IX Cortisone Acetate Active Compound Polyethylene Sodium Tween Benzyl Methyl- Propyl Particle Type Conc. Glycol 4000 Chloride 80 Alcohol paraben paraben 1 Micro-Cryst. 2.5% 3.0% 0.9% 0.4% 1.5% - 2 Micro-Cryst. 5.0% 3.0% ,, 1.5% - 3 Micro-Cryst " " " " - 0.18% 0.02% 4 Micro-Cryst. " " " " 0.3% 5 Micro-Cryst. " " " " 0.2% - " " The aqueous suspensions were prepared by mixing the powdered medicinal agent with the vehicle. Suspensions 1 and 2 exhibited satisfactory resuspendibility and drainage after storage for one month at forty degrees centigrade, 25 degreets centigrade, and four degrees centigrade. After maintaining Preparations 3, 4 and 5 at forty degrees centigrade, 25 degrees centigrade and four degrees centigrade, for two weeks, the samples were satisfactory in appearance, resuspended well, and fluidity and drainage were good.

The micro-crystalline cortisone acetate was prepared by precipitation from methylcello solve and dried by azeotropic distillation with Skellysolve B. The following examples are illustrative of the compositions and process of the present invention but are not to be construed as limiting. EXAMPLE 1. 2.5 grams Sterile Micronized Testosterone U.S.P. 12.0 grams Polyethylene Glycol 4000 0.9 grams Sodium Chloride Gran. U.S.P. 0.4 gram Tween 80. 1.5 grams Benzyl Alcohol N.F. q.s. 100 cc. Water for Injection. The polyethylene glycol, sodium chloride, Tween 80 and benzyl alcohol are dissolved in the water. The resulting solution is then sterilized by filtration. The previously sterilized micronized testosterone is then mixed aseptically with the sterile vehicle and the mixture is then homogenized until a uniform consistency is obtained. Alter storage of the resulting suspension for sixty days at temperatures of forty degrees centigrade, 25 degrees centigrade and four degrees centigrade, no change in physical characteristics, of the suspension is evident. The solids separate leaving a clear supernatant liquid. The separated solids do not cake and resuspend readily with a minimum amount of agitation. There is no apparent change in the viscosity of the suspension. This suspension is suitable for intramuscular use. EXAMPLE 2. 0.2 gram Sterile Micronized Estrogenic Crystallizate 3.0 grams Polyethylene Glycol 4000 0.9 gram Sodium Chloride Gran. U.S.P. 0.4 gram Tween 80 1.5 grams Benzyl Alcohol N.F. q.s. 100 cc. Water for Injection The polyethylene glycol, sodium chloride, Tween 80 and benzyl alcohol are dissolved in water and the resulting solution is then sterilized by passing through a sterilizing filter. The previously sterilized micronized estrogenic crystailizate is then mixed aseptically with the sterile vehicle and the mixture is then homogenized until a uniform consistency is obtained. After storage of the resulting suspension for sixty days at

temperatures of forty degrees centigrade, 25 degrees centigrade and four degrees centigrade, no change in physical characteristics of the suspension is evident. The separated solids do not cake and resuspend very readily with a minimum amount of agitation. There is no apparent change in the viscosity of the suspension. This suspension is suitable for parenteral use. EXAMPLE 3. 5.0 grams Sterile Micronized Hydrocor tisone Acetate 3.0 grams Polyethylene Glycol 4000 0.9 gram Sodium Chloride Gran. U.S.P. 0.2 gram Tween 80 0.18 gram Methylparaben U.S.P. 0.02 gram Propylparaben U.S.P. q.s. 100 cc. Water for Injection The polyethylene glycol, sodium chloride, Tween 80, methylparaben and propylparaben lare dissolved in water and the resulting solution is then sterilized by filtration. The previously sterilized micronized hydrocortisone acetate is then mixed aseptically with the sterile vehicle and the mixture is then homogenized until a uniform consistency is obtained. After storage of the resulting suspension for thirty days at temperatures of forty degrees centigrade, 25 degrees centigrade and four degrees centigrade, no change in physical characteristics of the suspension is evident. The separated solids are readily re-suspendible and syringeability through a 27 gauge needle is satisfactory. This suspension is suitable for parenteral use EXAMPLE 4. 10.0 grams Sterile Micronized Hydrocorti sone 3.0 grams Polyethylene Glycol 4000 0.9 gram Sodium Chloride Gran. U.S.P. 0.4 gram Tween 80 1.5 grams Benzyl Alcohol N.F. q.s. 100 cc. Water for Injection The polyethylene glycol, sodium chloride, Tween 80 and benzyl alcohol are dissolved in water and the resulting solution is then sterilized by filtration. The previously sterilized micronized hydrocortisone is then mixed aseptically with the sterile vehicle and the mixture is then homogenised until a uniform consistency is obtained. After storage of the resulting suspension for thirty days at

temperatures of forty degrees centigrade, 25 degrees centigrade and four degrees centigrade, no change in physical characteristics of the suspension is evident The separated solids are readily re-suspendible and syringeability through a 27 gauge needle is satisfactory. This suspension is suitable for parenteral use. EXAMPLE 5. 2.5 grams Sterile Micronized Progesterone U.S.P. 6.0 grams Polyethylene Glycol 4000 0.9 gram Sodium Chloride Gran. U.S.P. 0.4 gnam Tween 80 1.5 grams Benzyl Alcohol N.F. q.s. 100 cc. Water for Injection. The polyethylene glycol, sodium chloride, Tween 80 and benzyl alcohol are dissolved in water and the resulting solution is then sterilized by filtration. The previously sterilized and micronized progesterone is then mixed aseptically with the sterile vehicle and the mixture is then homogenized until a uniform consistency is obtained After storage of the resulting suspension for ninety days lat temperatures of forty degrees centigrade, 25 degrees centigrade and four degrees centigrade, no change in physical characteristics of the suspension is evident. The separates solids are readily resuspendible. There is no evidence of caking or cry;stal growth during storage at the indicated temperatures. This suspension is suitable for parenteral use. EXAMPLE 6. A stable aqueous therapeutic suspension prepared by the procedure described above and which is suitable for intra-articular injection comprises the following ingredients: 0.05 gram Sterile Powdered Hydrocorti- sone Acetate 0.6 gram Neomycin Sulfate 3 grams Polyethylene Glycol 4000 0.9 gram Sodium Chloride 0.2 gram Tween 80 0.18 gram Methylparaben 0.02 gram Prepylparaben q.s 100 cc. Water for injection The suspension is characterized by good syringeability (27 gauge needle), good drainage and is easily resuspended. EXAMPLE 7.

A stable, aqueous therapeutic suspension prepared by the procedure described above and which is suitable for intra-muscular use comprises the following ingredients: 5 grams Sterile Powdered EIydrcoorti- sone Acetate 1 gram Thiamine hydrochloride 0.2 gram Riboflavin 0.5 gram Pyridoxine hydrochloride 0.25 gram Calcium pantothenate 10 grams Nicotinamide 15 gratis Polyffiylene Glycol 200 0.4 gram Tween 80 0.5 gram Phenol q.s. 100 cc. Water for Injection The suspension is prepared by dissolving the riboflavin and nicotinamide in water, mixing the solution with the soluble materials, filter sterilizing the resulting solution and aseptically adding thereto the hydrocortisone acetate. EXAMPLE 8. A therapeutic preparation in the form of a sterile dry powder suitable for reconstitution with a sterile aqueous vehicle is prepared by mixing and sterilizing the following ingredients and adding the resulting composition to a sterile twenty cc. vial: 10 milligrams Estradiol cyclopentyipropion- ate 250 milligrams Tesosterene 500 milligrams Pluronic F 68 2 milligrams Quatresin To the contents of this vial is added ten cc. of Sterile Water for Injection prior to use. The resulting suspension is highly satisfactory and is suitable for intra-muscular injection. EXAMPLE 9. A sterile ophthalmic suspension containing the following ingredients is prepared by the procedure described above: 1.5 grams Sterile Micronized Cortisone Acetate Ilydrate 1.0 gram 2 - IIydroxy-3-dimethylamino propyl p-(propylamino) benzo ate hydrochloride (Cornecaine) 0.6 gram Neomycin Sulfate 0.45 gram Sodium Citrate U.S.P. 15 grams Polyethylene Glycol 1500 0.02 gram Ouatresin 0.1 gram PVP q.s. 100 cc. Water for Injection

Polyvinyl pyrrolidone is sold by The General Aniline and Film Co. under the Registered trade-marl "Plasdone" and is characterized by a viscosity coefficient, i.e., K value, of 26 to 36 and a molecular weight of about 40,000. The suspension is stable, readily resuspendible and does not cake. EXAMPLE 10. A vehicle is prepared by combining the following ingredients: 30 milligrams Polyethylene Glycol 4000 U.S.P. 9 milligrams Sodium Chloride 4 milligrams Tween 80 U.S.P. 1.8 milligrams Methylparaben U.S.P. 0.2 milligrams Propylparaben U.S.P. q.s. 1 cc. Water for Injection The vehicle is sterilized by autoclaving at 120 degrees centigrade for thirty minutes. To a mixture of the following sterile ingredients 157,500 units Sterile Procaine Penicillin (164 milligrams) G (960 units per milli gram) -- milled (40 to 60 microns) - 4% lecithin coated (4% of lecithin by weight of procaine peni c' 157,500 units Sterile Procaine Penicillin (159.5 milligrams) G (988 units per milligram) - micronized (2 to 10 microns) 4P/o lecithin coated. is added sufficient quantity of vehicle (preparation supra) to provide a total volume of one cc. of suspensiba. The resulting suspension is mixed well and then packaged. The stable therapeutic preparation is suitable for intramuscular injection. EXAMPLE 11. A therapeutic composition in dry form suitable for later reconstitution~with an aqueous vehicle to provide a satisfactory, therapeutic suspension is made up in the following formulation: 225,000 units Procaine Penicillin G (960 (234 milligrams) units per milligram) milled t40 to 60 microns) 4% lecithin coated. 75,000 units Procaine Penicillin G (75 milligrams) (1000 units per milligram) -micronized (2 to 10 microns). 30 milligrams Polyethylene Glycol 6000

The mixture is blended and sterilized. The dry sterile material is added to a vial and wilen Sterile Water for Injection is added to provide a total volume of one cc. of suspension, there is obtained a stable therapeutic suspension containing 300,000 units of penicillin. EXAMPLE 12. A therapeutic composition in dry form suitable for later reconstitution with an aqueous vehicle to provide la satisfactory, therapeutic suspension is made up in the following formulation: 225,000 units Procaine Penicillin G (960 (234 milligrams) units per milligram) milled (40 to 60 microns) .% lecithin coated 75,00() units Procaine Penicillin G (1000 (75 milligrams) units per milligram) micronized (2 to 10 microns) 100,000 units Sodium Penicillin G (1625 units per milligram) - micronized (2 to 10 microns) The mixture is blended with 5 milligrams Sodium Citrate U.S.P. 30 milligrams Polyethylene Glycol 4000 U.S.P. and then sterilized. The dry sterile material is added to a vial and when Sterile Water for Injection is added to provide a volume of 2 cc., there is obtained a therapeutic preparation containing 200,000 units of penicillin per cc. EXAMPLE 13. A vehicle containing the following ingredients: 30 milligrams Polyethylene Glycol 4000 U.S.P. 9 milligrams Sodium Chloride 4 milligrams Tween 80 U.S.P. 1.8 milligrams Methylparaben U.S.P. 0.2 milligram Propylparaben U.S.P. q.s. 1 cc. Water for Injection is prepared and then sterilized by autoclaving at 120 degrees centigrade for thirty minutes. To a mixture of the following sterile ingredients 105,000 units Procaine Penicillin G (988 (106 milligrams) units per milligram) milled (40 to 60 microns) coated with 1.25% lecithin 105,000 units Procaine Penicillin G (988 (106 milligrams) units per milligram) micronized (2 to 10 mic

rons)-coated with 1.25% lecithin 0.3126 gram Dihydrostreptomycin Sul fate is aseptically added sufficient quantity of vehicle (prepared above) to provide a total volume of one cc. of a stable therapeutic suspension containing more than 200,000 units of penicillin in combination with dihydrostreptomycin sulfate. EXAMPLE 14. A therapeutic composition in dry form suitable for later reconstitution with an aqueous vehicle to provide a satisfactory, Itherapeutic suspension is made up in the following formulation: 210,000 units Procaine Penicillin G (988 (214 milligrams) units per milligram) milled (40 to 60 microns) coated with 1.25 lecithin 0.3126 gram Dihydrostreptomycin Sul fate 30 milligrams Polyethylene Glycol 4000 U.S.P. The mixture is blended and sterilized. The dry sterile material is added to a vial and when Sterile Water for Injection is added to provide a total volume of one cc. of suspension, there is obtained a stable, therapeutic preparation containing more than 200,000 units of penicillin in combination with dihydrostrep tomycin sulfate. EXAMPLE 15. A vehicle containing the following ingredients: 10 milligrams Polyvinyl Pyrrolidone 10 milligrams Polyethylene Glycol 4000 U.S.P. 14.25 milligrams Sodium Citrate U.S.P. 2.63 milligrams Methylparaben U.S.P. q.s. 1 cc. Water for Injection is prepared and then sterilized by filtration. To a mixture of the following sterile ingredients: 255,000 units Procaine Penicillin O (888 (275 milligrams) units per milligram) milled (40 to 60 microns) coated with 4% lecithin 255,000 units Procaine Penicillin 0(912 (280 milligrams) units per milligram) micronized (2 to 10 mic rons) coated with 1.25% lecithin is asepltically added sufficient quantity of vehicle (prepared above) to provide total volume of one cc. of a stable, therapeutic suspension containing more than 500,000 units of penicillin. EXAMPLE 16. A therapeutic composition in dry form suitable for later reconstitution with an aqueous vehicle to provide a highly satisfactory therapeutic suspension is made up in the following

formulation: 157,000 units Procaine Penicillin G (988 (107 milligrams) units per milligram) milled (40 to 60 microns) coated with 1.25 % lecithin 55,000 units Sodium Penicillin G (1625 (33.9 milligrams) units per milligram) 0.1563 gram Dihydrostreptomycin Sul fate 0.1563 gram Streptomycin Sulfate The mixture is blended with 2.5 milligrams Sodium Citrate U.S.P. 30 milligrams Polyethylene Glycol 4000 U.S.P; and then sterilized. The dry sterile materials are added to Q vial and when Sterile Water for Injection is added to provide a total volume of one cc. of suspension, ere is obtained a therapeutic suspension containing more than 200,000 units of penicillin in combinationwithstreptomycin sulfate and dihydrostreptomycin sulfate. EXAMPLE 17. A vehicle containing the following ingradients: 10 milligrams Polyethylene Glycol 4000 U.S.P. 2.63 milligrams Methylparaben U.S.P. 10 milligrams Polyvinyl Pyrrolidone 14.25 milligrams Sodium Citrate U.S.P. q.s. 1 oc. Water for Injection is prepared and then filter sterilized. To a mixture of the following sterile ingredients: 52,500 units Procaine Penicillin G milled (40 to 60 microns) -1.25% lecithin coated 157,500 units Procaine Penicillin G mic ronized (2 to 10 microns) 1.25 % lecithin coated 0.3126 gram Dihydrostreptomycin Sul fate is aseptically added sufficient quantity of vehicle (prepared above) to provide a total volume of one cc. of a stable, therapeutic suspension containing more than 200,000 units of penicillin in combination with dihydrostreptomycin sulfate. EXAMPLE 18. A vehicle containing the following ingredients: 10 milligrams Polyethylene Glycol 4000 U.S.P. 10 milligrams Po 1 y v i n y 1 Pyrrolidone U.S.P. 1 milligram Tween 80 U.S.P. 13.66 milligrams Sodium Citrate U.S.P. 2.5 milligrams Methylparaben U.S.P. 0.17 milligram Propylparaben U.S.P. q.s. 1 cc. Water for Injection is prepared and then filter sterilized.

To a mixture of the following sterile ingredients: 255,000 units Procaine Penicillin G (960 (266 milligrams) units per milligram) milled (40 to 60 microns) 255,000 units Procaine Penicillin G (988 (258.5 milligrams) units per milligram) micronized (2 to 10 mic rons)-coated with 1.25% lecithin is aseptically added a sufficient quantity of the above vehicle to provide a total volume of one cc. of a stable, thenapeutic suspension containing more than 500,000 units of penicillin. EXAMPLE 19. A therapeutic~preparation for oral use and in dry form suitable for later reconstitution with an aqueous vehicle is made up by mixing the following: 250 milligrams Oxytetracycline Amphoteric free base powder 150 milligrams Polyethylene Glycol 4000 U.S.P. To the resulting mixture is added sucrose, coloring, sodium citrate and preservatives. Prior to use, water is added to a total volume of five cc. making a highly satisfactory aqueous suspension providing a dose of 250 milligrams of oxytetracyciine. EXAMPLE 20. A therapeutic preparation for oral use in dry form and suitable for later reconstitution with an aqueous vehicle is made up by mixing the following: 150 milligram's Calcium Chlortetracycline powder 150 milligrams Polyethylene Glycol 4000 U.S.P. To the resulting mixture is added sucrose, coloring, sodium citrate and preservatives such as methylparaben and propylparaben. Prior to use, water is added to a volume of five cc. making a highly satisfactory aqueous suspension providing a dose of 150 milligrams of calcium chlortetracycline. EXAMPLE 21. A therapeutic preparation for oral use in dry form and suitable for later reconstitution with an aqueous vehicle is made up by mixing the following: 250 milligrams Erythromycin S'tearate salt powder 30 milligrams Polyethylene Glycol 4000 U.S.P. Ta the resulting mixture is added sucrose, coloring, sodium cItrate and preservatives. Prior to use, water is added to a total volume of five cc. making a highly satisfactory aqueous suspension providing a dose of 250

milligrams of erythromycin stearate. EXAMPLE 22. A therapeutic preparation for oral use in dry form and suitable for later reconstitution with an aqueous vehicle is made up by mixing the following ingredients: 25 milligrams Sodium Carboxymethyl- cellulose (low viscosity) 250 milligrams Cocoa 5 milligrams Soluble Saccharin 250 milligrams Erythromycin Ethyl Car- bonate powder 300 milligrams Polyethylene Glycol 4000 U.S.P. 3.5 grams Sucrose 5 milligrams BenzoicAcid .5 milligram Methylparaben 0.0005 cc. Flavor Prior to use, water is added to a total volume of five cc. making a highly satisfactory aqueous suspension providing a dose of 250 milligrams of the erythiomycin ester. EXAMPLE 23. A therapeutic ;ereparation for oral use in dry form and suitable for later reconstitution with an aqueous vehicle is made up by mixing the following ingredients: 100 milligrams TetracycIine, Crystalline free base 300 milligrams Polyethylene Glycol 4000 U.S.P. To the resulting mixture is added sucrose, coloring, sodium citrate, and preservatives. Prior to use, water is added to a total volume of five cc. making a highly satisfactory aqueous suspension providing a dose of 100 milligrams of tetracycline. EXAMPLE 24. A therapeutic composition in dry form suitable for later reconstitution with an aqueous vehicle to provide a highly satisfactory therapeutic suspension is made up in the following formulation: 210,000 units Procaine Penicillin G (988 (214 malligrairs) units p r n;illigram)-- milled (40 to 60 microns) coated with 1.25% lecithin 150 milligrams Tetracycline Hydrochlor ide 30 milligrams Polyethylene Glycol 4000 U.S.P. The mixture is blended and sterilized. The dry, sterile material is added to a vial and when Sterile Water for Injection is added to provide a total volume of one cc. of suspension, there is obtained a therapeutic prepared tion containing more than 200,000 units of penicillin in combination with tetracycline hydrochloride.

EXAMPLE 25. A therapeutic composition in dry form suitable for later reconstitution with an aqueous vehicle to provide a highly satisfactory suspension is made up in the following formulation: 210,000 units Procaine Penicillin G (988 (21A milligrams) units per milligram) milled (40 to 60 microns) coated with 1.25 lecithin 150 milligrams Tetracycline Hydrochlor ide 0.3126 gram Dihydrostrepton ycin Sul fate 30 milligrams Polyethylene Glycol 4000 U.S.P. The mixture is blended and sterilized. The dry, sterile material is added to a vial and when Sterile Water for Injection is added to provide a total volume of one cc. of suspen sion, there is obtained a therapeutic preparation containing more than 200.000 units of penicillin in combination with tetracycline vdrochloride and dihydro streptomycin sulfate. EXAMPLE 26. A therapeutic composition in dry form suitable for later reconstitution with an aqueous vehicle to provide a highly satisfactory therapeutic suspension is made up in the following formulation: 210,000 units Procaine Penicillin G (988 (214 milligrams) units per milligram) milled (40 to 60 microns) coated with 1.25% lecithin 110,000 units Sodium Penicillin G (1625 (67.8 milligrams) units per milligram) 150 milligrams Tetracycline Hydrochlor ide 30 milligrams Polyethylene Glycol 4000 U.S.P. The mixture is blended and sterilized. The dry, sterile material is added to a vial and when Sterile Water for Injection is added to provide a total volume of one cc. of suspension, there is obtained a therapeutic pr paratipn containing more than 300,000 units of penicillin in combination with tetracycline hydrochloride. EXAMPLE 27. 5.0 grams Sterile, micronized 9-a-Fluoro J"drooortisone 3.0 Igrams Polyethylene Glycol 4000 U.S.P. 0.9 gram Sodium Chloride U.S.P. 0.2 gram Tween 80 0.18 gram Methylparaben U.S.P. 0.02 gram Propylparaben U.S.P. q.s. 100 cc. Water for Injection The polyethylene glycol, sodium chloride,

Tween 80, methylparaben and propylparaben are dissolved in the water and the resulting clear vehicle is then sterilized by filtration. The previously sterilized land micronized 9-afluorohydrocortisone is then mixed with the sterile vehicle and the mixture is then homogenized until a uniform consistency is obtained. The resulting aqueous suspension is stable and is suitable for parenteral use. Following the procedure described supra except for the replacement of 9-a-fluorohydro- cortisone by 9-a-chlorohydrocortisone, the corresponding therapeutic composition containing 9-1-chlorohydroconisone is obtained. Similarly, on replacing 9-a-fiuorohydrocorti- sone in the procedure described supra by 9-a- fluorocortisone, the corresponding therapeutic composition containing 9-1-fluorocortisone is obtained. EXAMPLE 28. 10.0 grams Sterile, micronized 9-a-Fluoro- hydrocortisone Acetate 3.0 grams Polyethylene Glycol 4000 U.S.P. 0.9 gram Sodium Chloride U.S.P. 0;4 gram Tween 80 1.5 grams Benzyl Alcohol N.F. q.s. 100 cc. Water for Injection The polyethylene glycol, sodium chloride, Tween 80 and benzyl alcohol are dissolved in water and the resulting clear vehicle is then sterilized by filtration. The previously sterilized and micronized 9-a-fluorohydro cortisone acetate is then mixed with the sterile vehicle and the mixture is then homogenized until a uniform consistency is obtained. The resulting stable aqueous suspension is suitable for parenteral use. Following the procedure described supra except for the replacement of 9-a-fluorohydro- cortisone acetate by 9-a-chlorohydrocortisone acetate the corresponding therapeutic composition containing 9-a- chlorohydro cortisone acetate is obtained. Similarly, by replacing 9-a-fluorohydro- cortisone acetate by 9-a-fluorocortisone acetate in the procedure above, the corresponding therapeutic composition containing 9-a-fluoro- cortisone acetate is obtained. EXAMPLE 29. A therapeutic composition in dry form suitable for later reconstitution with an aqueous vehicle to provide a highly satisfactory therapeutic suspension is made up in the following formulation: 150 milligrams Tetracycline Hydrochlor

ide 10.0 grams Sterile, micronized 9 a - Fluorohydrocortisone Acetate 3.0 grams Polyethylene Glycol 4000 U.S.P. The mixture is blended and sterilized. The dry, sterile material is added to a vial and when Sterile Water for Injection is added to provide a total volume of one oc. of suspension, there is obtained a therapeutic preparation containing tetracycline hydrochloride in combination wit utility. When these preparations are idispersed in the aqueous polyalkylene glycol vehicles of the invention the resulting therapeutic suspensions are further characterized by excellent stability. Typical combinations include tetracycle and fumagillin; tetracycline and erythromycin including salts and esters of erythromycin; tetracyeline, erythromycin and strepto- mycin, tetracycline, neomycin and a polymixin, e.g., polymixin B; tetracycline, bacitracin and neomycin; tletracycline, cortisone or hydrocortisone (including esters thereof), neomycin and a polymixin; tetracycline, a 9-'.-halo- hydrocortisone or 9 - a- halohydrocortisone e.g., 9-i-flu oro.cortison or 9-fluomhydro co r- tisone (including esters thereof), neomycin and a polymixin; tetracycline, hydrocortisone including a halohydrocortisone (plus esters there of) and an anti-fungal agent such as an alkyl phydroxyb enzoate, Quatresin, sodium caprylate, calcium propionate or zinc caprylate. EXAMPLE 30. 0.05 gram 9 - a - Fluorohydrocortisone Acetate 0.6 gram Neomycin Sulfate 3 grams Polyethylene Glycol 4000 U.S.P. 0.9 gram Sodium Chloride 0.2 gram Tween 80 0.18 gram Methylparaben 0.02 gram Propylparahen q.s. 100 cc. Water for Injection The polyethylene glycol, sodium chloride, Tween 80, methylparaben and propylparaben anl neomycin sulfate are dissolved in water and the resulting cIear vehicle is then sterilized by filtration. The previously sterilized and micronized 9- .-fluorohydro- cortisone is then mixed with the sterile vehicle and the mixture lis then homogenized until a uniform consistency is obtained. * The resulting aqueous suspension is stable and is suitable for parenteral use. Following the procedure described supra except for the replacement of 9-e-fluorohydro- cortisone acetate by 9-7.-chlorohydrocortisone acetate, the corresponding therapeutic composition containing - 9-i-chlorohydrocortisone acetate is Obtained.

Similarly, by replacing 9-fluorohydrocorti sone acetate by 9-i-fluorocortisone acetate in the procedure above, the corresponding therapeutic composition containing 9--fluorocorti- .sone acetate is obtained. EXAMPLE 31. A vehicle containing the following ingredients: 120 milligrams Polyethylene Glycol 400 5 milligrams Sodium Citrate 0.9 milligram Methylp)araben 0.1 milligram Propylparaben q.s. 1 cc. ~ Water for Injection is prepared and then sterilized by autoclaving at 120 degrees centigrade for thirty minutes. To 600,000 units of Sterile N,N1-dibenzylethylenediamine dipenicillin G powder is aseptically added a sufficient quantilty of the above vehicle to provide a total volume of one cc. of a stable, therapeutic suspension. EXAMPLE 32. A therapeutic preparation for oral use and suitable for later reconstitution with water is made up by combining the following ingredients: 0.167 gram Sulfadiazine powder 0.167 gram Sulfiamerazine powder 0.167 gram Sulfamethazine powder, 0.45 gram Polyethylene Glycol 4000 To the resulting mixture is added suitable flavoring, coloring agents and preservatives. Sufficient water is then added so that each five cc. of the stable aqueous suspension provides a dose of .5 gram of the combined therapeutic materials. What we claim is: - 1. A process for the preparation of a fluid, physically stable aqueous suspension of a solid, insoluble, organic medicinal agent of specific gravity less than about two which comprises dispersing said medicinal agent in an aqueous polyalkylene glycol vehicle. 2. A process which comprises mixing a solid, insoluble organic medicinal agent with a polyalkylene glycol of molecular weight greater than about 4000, both of the aforesaid substances being present in a dry mixture, and then dispersing the mixture in an aqueous vehicle to obtain a fluid, physically stable therapeutic suspension. 3. A process as claimed in claim 1 or 2 in which the polyalkylene glycol used is a polyethylene glycol. 4. A process as claimed in any preceding claim wherein the insoluble organic medicinal agent used is an insoluble antibiotic material. 5. A process as claimed in claim 4 wherein the insoluble antibiotic material used is an insoluble penicillin. 6. A process as claimed in claim 5 wherein the insoluble penicillin

used is a procaine penicillin. 7. A process as claimed in claim 6 wherein the procaine penicillin used is lecithin coated procaine penicillin G and the aqueous vehicle includes polyvinyl pyrrolidone. 8. A process as claimed in lany of claims 1 to 3 wherein the insoluble organic medicinal agent used is an insoluble steroid. 9. A process as claimed in claim 8 wherein the insoluble steroid used is cortisone, hydrocortisone or insoluble esters thereof 10. A process as claimed in claim 9 wherein cortisone acetate or hydrocortisone acetate is used:

* GB784660 (A)

Description: GB784660 (A) ? 1957-10-16

Electrolytic cell for producing aluminium of high purity

Description of GB784660 (A)

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CH338970 (A) DE1000156 (B) FR1132770 (A) US2859160 (A) CH372168 (A) DE1092668 (B) CH338970 (A) DE1000156 (B) FR1132770 (A) US2859160 (A) CH372168 (A) DE1092668 (B) less Translate this text into Tooltip

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SPECIFICATION i} PATENT SPECIFICATION 784,660 Date of Application and filing Complete Specification: Oct 10,

1955. Application made in Germany on Nov 5, 1954. Complete Specification Published: Oct 16, 1957. PATENTS ACT, 1949 SPECIFICATION NO 784,660 Reference has been directed, in pursuance of Section 8, to Speclficatlon No 786,379. THE PATENT OFFICE, i.th,;'ay, g 1955 No 28849155. of the Patents Act, 1949, DB 04625/1 ( 3)/3612 150 5/58 R performed, to be particularly described in and by the following statement:- This invention relates to an electrolytic cell for producing aluminium of high purity. Aluminium is produced industrially by fusion electrolysis in which a melt at approximately 1000 C of alumina in cryolite is decomposed by electric direct current. At the cathode, which is formed by the bathshaped furnace basin lined with carbon, aluminium is deposited in liquid form and forms a layer on the bottom of the basin beneath the melt in the basin The metal produced is removed from the furnace at intervals of 24 to 48 hours; a constant amount of metal is however left in the furnace for various reasons The anode consists of carbon blocks which dip into the melt from above Said anode is continuously consumed and must be correspondingly added to, because oxygen separates out at the anode and reacts with the carbon of the anode The reaction products, viz, carbon dioxide and carbon monoxide, escape from the electrolysis furnace The alumina contained in the melt must also be made up from time to time, since it is also used up in the electrolysis process. Referred to one part by weight of aluminium produced at least 1 89 parts by weight of alumina and 0 33 parts by weight of anode carbon are theoretically consumed in the electrolysis In practice, these consumption figures are larger in consequence of losses through dusting volatilisation, current yield, secondary reactions, and so on In the case of the anodes, the consumption can vary in practice for example between 0 37 and 0 57 lPrice 3/63 the substances used For the -purpose of increasing the purity of the aluminium produced, the raw materials themselves 55 for example for producing the alumina and the anodes are purified by using chemical and physical processes, in order to obtain highly pure materials for the electrolysis In the necessary working of the melt 60 in electrolysis furnaces, iron tools are used, such as bars and hooks, which are extremely thick at the end coming into contact with the melt or with the metal, in order to prevent them from assuming high temperatures dur 65 ing the time they are in use, which is deliberately kept short, but remain below the melting point of the melt and thus retain a protective coating of solidified melt When use is made of the known materials of maximum 70 degree of purity

these and other measures lead to a metal of the purity of 99 7 % aluminium The impurities consist of iron, silicon and small quantities of a number of other metals 75 A further increase in the purity of the aluminium necessitates the application of special technical processes, for example electrolytic refining Although this process does lead to a high degree of purity, for ex 80 ample 99 99 %, nevertheless it greatly increases the costs of production On the other hand, in spite of its high price, aluminium of the highest degree of purity has, by virtue of its special technological properties, opened 85 up new fields of application which were closed to the purest aluminium hitherto obtained by simple electrolysis An increase in the purity of this metal without using the special refining processes even if only by 0 1 90 PATENT SPECIFICATION Date of Application and filing Complete Specification: Oct 10, 1955. 784,660 No 28849155. J IX / Application made in Germany on Nov 5, 1954. Complete Specification Published: Oct 16, 1957. Index at acceptance:-Classes 39 ( 3), H( 2 82:3 E 1); and 41, A 1 F. International Classification:-C 22 d, H 05 b. COMPLETE SPECIFICATION Electrolytic Cell for Producing Aluminium of High Purity We, VEREINIGTE ALUMINIUM-WERKE AKTIENGESELLSCHAFT, a body corporate organised under the Laws of Germany, of Am Nordbahnhof, Bonn-on-the-Rhine, Germany, 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 an electrolytic cell for producing aluminium of high purity. Aluminium is produced industrially by fusion electrolysis in which a melt at approximately 10000 C of alumina in cryolite is decomposed by electric direct current. At the cathode, which is formed by the bathshaped furnace basin lined with carbon, aluminium is deposited in liquid form and forms a layer on the bottom of the basin beneath the melt in the basin The metal produced is removed from the furnace at intervals of 24 to 48 hours; a constant amount of metal is however left in the furnace for various reasons The anode consists of carbon blocks which dip into the melt from above Said anode is continuously consumed and must be correspondingly added to, because oxygen separates out at the anode and reacts with the carbon of the anode The reaction products, viz, carbon dioxide and carbon monoxide, escape from the electrolysis furnace The alumina contained in the melt must also be made up from time to time, since it is also used up in the electrolysis process.

Referred to one part by weight of aluminium produced, at least 1 89 parts by weight of alumina and 0 33 parts by weight of anode carbon are theoretically consumed in the electrolysis In practice, these consumption figures are larger in consequence of losses through dusting, volatilisation, current yield, secondary reactions, and so on In the case of the anodes, the consumption can vary in practice for example between 0 37 and 0 57 lPrice 316 l parts by weight of anode carbon There are also lower losses in cryolite, some 0 05 parts by weight. In the electrolysis practically all the impurities of the consumed substances pass 50 into the aluminium produced Aluminium electrolysis therefore requires high purity of the substances used For the purpose of increasing the purity of the aluminium produced, the raw materials themselves 55 for example for producing the alumina and the anodes are purified by using chemical and physical processes, in order to obtain highly pure materials for the electrolysis In the necessary working of the melt 60 in electrolysis furnaces, iron tools are used, such as bars and hooks, which are extremely thick at the end coming into contact with the melt or with the metal, in order to prevent them from assuming high temperatures dur 65 ing the time they are in use, which is deliberately kept short, but remain below the melting point of the melt and thus retain a protective coating of solidified melt When use is made of the known materials of maximum 70 degree of purity these and other measures lead to a metal of the purity of 99 7 % aluminium The impurities consist of iron, silicon and small quantities of a number of other metals 75 A further increase in the purity of the aluminium necessitates the application of special technical processes, for example electrolytic refining Although this process does lead to a high degree of purity, for ex 80 ample 99 99 %, nevertheless it greatly increases the costs of production On the other hand, in spite of its high price, aluminium of the highest degree of purity has, by virtue of its special technological properties, opened 85 up new fields of application which were closed to the purest aluminium hitherto obtained by simple electrolysis An increase in the purity of this metal without using the special refining processes, even if only by 0 1 9 a 784,660 to 0 2 %, would be a technical advance, since in such case important and extensive fields of application can also be opened up to the metal. This desired higher purity of aluminium obtained by electrolysis can for example be achieved by further improving the purity of the materials used, alumina, anodes and cryolite but this method is not feasible since a further increase in the purity of these materials would be possible only by using expensive processes and apparatus, which would render the method uneconomic.

The present invention aims at achieving an increase in the purity of the aluminium produced, in the following manner:The gases, carbon dioxide and carbon monoxide produced at the anode and escaping from the electrolytic cell contain small varying amounts of iron and silicon but also traces of titanium, chromium, vanadium and other metals or compounds thereof in the gaseous or solid state (smoke) The greater part of these substances remains through decomposition or deposition in the electrolysis furnace. The invention is based on the idea of promoting the production and conveyance of the said gases or smokes and effecting their removal and also the removal of their decomposition products from the furnace zone, by imparting a maximum speed of flow to the furnace gases in the furnace until they escape from the furnace, by reducing the extent of their path in the furnace, and by keeping the gases under excess pressure until they escape from the furnace. These conditions are fulfilled by structural measures in the design of the furnace, by disposing individual anode members composing the entire anode at small distances from one another in the furnace and giving them a small width of 200 to a maximum of 700 millimetres At the same time length of such anode members should be greater than 1400 millimetres The current load of these individual anode members should not exceed 10000 amperes, but should be about 5000 to 8000 amperes In the intermediate -50 spaces which are for this purpose not larger than 150 millimetres, preferably about 50 to millimetres wide, there are formed passages of small cross-section, because at about millimetres above the level of the melt a solidification crust forms, which closes off the passage to the top These passages are gas-tight At the head sides of the anodes these passages are constantly kept open by piercing the melt crust by means of crowbars or the like, in order to allow the gases to emerge into the atmosphere. By these measures the reaction gases arising at the underside of the anode, including the afore-mentioned substances contained therein, are conducted into the passages formed between the anodes, over relatively very short paths which correspond at the maximum to half the width of the anodes but which are substantially shorter in the middle In the said passages the gases flow 70 at a high speed and under pressure to the gas outlet points, which are disposed on the head sides of the anodes and which are kept open in the solidification crust covering the entire surface of the melt The substances 75 contained in the reaction gases are protected by this arrangement from decomposition and from deposition inside the furnace and in particular, also by the fact that the gases are always under excess pressure and are driven 80 out at that pressure instead of being drawn off, thereby avoiding mixing with the air of the atmosphere.

These passages, which are situated between the anodes defining their side walls 85 and the bottom surface of which passag-es is formed by the surface of the liquid melt. constantly maintain their upper closure even on the slow downward movement of the anodes corresponding to their consumption, 90 since thev are constantly covered, without assistance, with an upwardly closing solidified layer of melt, which is constantly driven upward by the current of gas This closing layer is also maintained in spite of the move 95 ment of the anode since it constantly becomes automatically renewed. With the afore-described arrangement of the anodes at a small distance of about 40 millimetres from one another, there is a dan 100 ger that the parts of the anodes projecting out of the melt crust will be very intensely attacked by the oxygen of the atmosphere and burnt The heat accumulates in the narrow intermediate spaces between the anodes 105 The intermediate spaces produce a kind of chimney draught through which air is constantly supplied to the critical points, so that the anodes become burnt hollow at their sides to such extent that intolerable losses 110 of anode substance result, apart from the cross-sectional reductions suffered by the anodes and which so change the electrical conditions of the furnace that successful operation is impossible Air burning should 115 therefore be prevented when the electrolysis furnace is to be operated in the aforedescribed manner in accordance with the invention. Known measures, such as for example 120 coating the endangered anode surfaces with phosphoric acid or phosphates, with borax or other boron compounds, or pouring on alumina, cannot prevent air burning, but at best can only limit it Complete prevention 125 of air burning in the intermediate spaces between the anodes is achieved in accordance with a subsidiary feature of the invention by a packing which is introduced into the aforesaid intermediate spaces For the purpose of 130 784,660 producing this packing the intermediate spaces between the anodes at the head sides are temporarily closed by shuttering and a pulverulent substance is tamped firmly into the intermediate space from above After the tamping down, the shuttering can again be removed-and the packing remains firmly in place and completely prevents air burning. Pulveralent substances which in any case have to be continuously added to the melt, such as cryolite, alumina, soda and other substances, individually or in the form of mixtures, are advantageously used as packing substance. In order to enable the invention to be more readily understood, reference is made to the accompanying drawing which illustrates diagrammatically and by way if example, one embodiment of electrolytic cell in accordance therewith.

In said drawing, the reference numeral 1 denotes the cathode, 2 deposited aluminium, 3 the melt, 4 the narrow individual anodes with small intermediate spaces, 5 the crust of solidified melt, 6 the packing between the anodes and 7 the passages which are formed and in which the gases arising on the underside of the anodes as a result of the electrolytic process are collected and led off to the outside The arrow 8 indicates the short path of the gases to the passages. Parts of the electrolytic furnace which are not essential to the invention, such as the current supply cables, the suspension of the anodes, and so on, have been omitted from the drawing The drawing should also 'be regarded as a diagram in that the number of anode strips is in actual fact larger than shown, depending on the size of the furnace.

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* GB784661 (A)

Description: GB784661 (A) ? 1957-10-16

Process for the production of austenitic springs for watches, and likeapparatus, and springs obtained by this process

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PATENT SPECIFICATION Date of Application and filing Complete Specification: Oct 18, 1955. 784,661 No 29687/55. Application made in Switzerland on Oct 18, 1954. Complete Specification Published: Oct 16, 1957. Indox at aoceptance:-Classes 83 ( 2), A 155; and 83 ( 4), V 2 Intemnational Classification:-3 821 'h B 23 p. COMPLETE SPECIFICATION Process for the Production of Austenitic Springs for Watches, and Like Apparatus, and Springs Obtained by this Process We, INSTITUT DR ING REINHARD STRAUMANN A G, a Swiss Corporation of Waldenburg, Basle-Campagne, Switzerland, 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:- In applicants' British Patent No 735,510 there is described a process for the production of alloys in strip form suitable for conversion into watch springs and the like, which comprises homogenising at high temperature and quenching wire made from an alloy, which exhibits a cubic face-centred or a cubic body-centred crystal lattice, drawing, preferably in the cold state, the quenched wire to a diameter such that a reduction in cross-section of between 60 and 85 ,' is obtained and then, after such decrease in crosssection, rolling the wire to produce a flat strip and a total decrease in cross-section of substantially 90 %l", based on the original cross-section, the direction of highest moduIus of elasticity in the flat strip becoming oriented substantially parallel to the direc tion of rolling, the final strip being preferably heat-treated at a temperature of between ' and 600 C for not more than 24 hours. In this way a modulus of elasticity of at least 21.00 kg/mm 2 can be obtained The spring strips produced from a cubic face-centred material according to the method described in the said Patent No 733,510 show a definite predominance of direction 111, i e, orientation of direction 111 of the texture parallel to the direction of rolling, whereby maximum values of the modulus of elasticity and of tensile strength are obtained But such strips showing predominance of the direction 111 parallel to the direction of rolling have so far only been achieved by working from wire to the strip, whilst it has up to now not been possible to produce, starting from broad bands having a rectangular cross-section, lPrice 3/61 rolled spring strips which show a predominance of direction 111 of the texture parallel to the direction of rolling and parallel to the rolling plane Austenitic spring strips hitherto produced by cutting out the spring strips 50 from broad strips in the longitudinal direction, i e, the direction of rolling of

such broad strips-further show inferior elastic properties to strips rolled from wire. It has been observed by X-ray examina 55 tions of textures that, when subjecting a metal band or strip of rectangular cross-section which has previously been homogenised and which consists of an austenitic or cubic face-centred material to a rolling operation, 60 a strong predominance of direction 111 transversely to the direction of rolling, i e, at an angle of 900 to the direction of rolling can be achieved, whilst in the spring strips produced from wire in accordance with the 65 above mentioned patent the direction 111 is situated in the direction of rolling. The main object of the present invention is therefore a process for the production of austenitic springs for watches, and the like 70 apparatus, wherein a band of austenitic cubic face-centred metallic material having a rectangular cross-section, is homogenised and subsequently rolled to a broad band until a degree of deformation of at least 80 %' is 75 reached and a definite predominance of direction 11 in the direction transverse to the direction of rolling has been achieved, the spring strips are cut out from the rolled metal strip in a direction transverse to the direc 8 G tion of rolling, so that the direction 111 lies along their longitudinal axis, and the spring strips are subjected to a heat-treatment at temperatures ranging from 2000 to 600 C 85 The choice of a material with rectangular cross-section can naturally also be based on bar or rod shaped material, which has been given a rectangular cross-section by crushing or pressing in any suitable way 90 ( 784,661 In this way, austenitic springs of superior quality for watches and like spring driven or controlled apparatus are obtained This process is especially suitable for the production of main springs, brake springs, etc for watches It is-due to the present invention -possible to roll strips, from which springs for watches may be cut, to a width of approximately 50 cm Spring strips for watch springs, which were cut transversely to the direction of rolling from such a broad austenitic band, showed a definite predominance of direction 111 in the direction of their length, i e, transversely to the original direction of rolling Tests have as expected,shown that the modulus of elasticity of so-obtained spring strips in a longitudinal direction is just as high as that of the spring strips produced from a metal wire according to British Patent No 733,510. It has also been observed that every austenitic alloy is suitable for the process according to the invention-for example, austenitic non-rusting steels, 18/8 chromium-nickel steels for instance, which do not change from an austenitic structure to a ferritic structure during cold rolling, or age-hardenable austenitic alloys based on Cr-Co-Fe or

Ni-Fe-Cr with the known additions The invention should therefore not be limited in any way to certain austenitic alloys, as any austenitic alloy can be used with the same success for the purpose of the invention. It is essential that the composition of the alloy is chosen in such a way and the heat treatment, i e the homiogenisation is carried out in such a way that the formation of texture is not rendered difficult or even impossible by a change in structure or by segregation which may occur in the course of the 40 production of the broad rolled strip.

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* GB784662 (A)

Description: GB784662 (A) ? 1957-10-16

Manufacture of finely dispersed organic or inorganic pigments

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4 & 11 l PATENT SPECIFICATION iveniors: HANS RAAB and REINHOLD HORNLE 784 Mp 62 I i Date of Application and filing Complete Specification Aug 18, 1955. No 23858/55.

Complete Specification Published Oct 16,1957. Index at Accetance: Classes 2 ( 4), G; and 95, A 14. Inter SPECI FICATIO NO 784, 662 The Inventors of this Invention In the sense of being the actual devisers thereof within lthe nmsean Iz, of eclon 16 of the Patents Act, 1949, are eal S Paeab, F'riedrich Bayer-Strasse i, Leverkuser;_Bayenqerk, Germany, and Reinhold Rornle, C'erstenkar p 12, Koln-Stan 0,velm, Germany, both of Gennan nationality. E Wi THE PATENT OFFICE, :st 'ovember, 95-7 ing tur _ The process according to the invention is characterised by kneading the organic or inorganic pigments with a polyglycol ether in an amount of at least 10 per cent, preferably to 90 per cent by weight based on the amount of the pigment, if desired with the addition of water or other suitable diluting agent The proportions in the mixture are such that the mixture has initially a viscosity of at least 2000 centipoises, preferably 1,000,000 centipoises and more The higher viscosity, for example 1,000,000 centipoises and more, is preferably chosen in order to accelerate the process of comminuting. The polyglycol ethers to be employed are disclosed for example in German Patent Specifications N 1 os 605,973; 667,744; 694,178; 679,710; Austrian Patent Specification 160,871; German Patent Specifications Nos. 824,949; 806,671; and British Patent Specification No 690,355. Suitable kneading devices are the known mixing and kneading machines used for the intimate mixing of viscous pastes such as, for example, the well known Werner & Pfleiderer kneaders or mixing and kneading devices as described in German Patent Specification No. 813,154, or a continuous kneading apparatus such as the Buss-Ko-kneader (cf Ullmanns Encyklopacdia der technischen Chemie, 3rd edition, volume 1, page 727). The process is effected preferably by using lPrice U Ml 00066/14)/3593 100 1 Q/a 7 ror au puts G E finely divided pigments is desirable, for 60 example, for dyeing in the spinning process of polyacrylonitrile, viscose and copper rayon, for colouring lacquers and synthetic resins, in pigment printing, for colouring paper pulp, and for the manufacture of wallpaper colours 65 The following examples illustrate the invention the parts being by weight:EXAMPLE 1 parts of the monoazo dyestuff obtained from diazotized 2,5-dichloro-aniline and 21,31 70 hydroxynaphthoylamino-benzene are treated in a suitable kneading device (Werner & Pfleiderer dispersion kneader) with 100 parts of the condensation product from hydroxydiphenyl, benzyl chloride and ethylene oxide 75 as described in Example 1 of German Patent Specification No 824,949 The viscosity of the paste lies above 106 centipoises After 30 minutes there is added sufficient water so that

the paste is capable of flowing The dyestuff 80 paste shows a uniformly fine division having a particle diameter of 0 3 to 1 micron. EXAMPLE 2 parts of the monoazo dyestuff obtained from diazotized 4-chloro-2-toluidine and 1 85 phenyl-3-methyl-5-pyrazolone are treated with parts of the dispersing agent used in Example I and 30 parts of water in a kneading Vr.) 't at rl PATENT SPECIFICATION liwentors: HANS RAAB and REINHOLD HORNLE 784,662 Date of Application and filing Complete Specification Aug 18, 1955. No 23858/55. Complete Specification Published Oct 16,1957. Index at Acceptance: -Classes 2 ( 4), G; and 95, A 14. International Classification: -C 09 b, d COMPLETE SPECIFICATION Manufacture of Finely Dispersed Organic or Inorganic Pigments We, FARBENFABRIKEN BAYER ARTIENGESELLSCHAFT, a Body Corporate organised under the Laws of Germany, of Leverkusen, Germany, 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 concerns the manufacture of finely dispersed pastes of organic or inorganic pigments It provides a new process having the advantage of readily producing the desired fine dispersion. The process according to the invention is characterised by kneading the organic or inorganic pigments with a polyglycol ether in an amount of at least 10 per cent, preferably to 90 per cent by weight based on the amount of the pigment, if desired with the addition of water or other suitable diluting agent The proportions in the mixture are such that the mixture has initially a viscosity of at least 2000 centipoises, preferably 1,000,000 centipoises and more The higher .5 viscosity, for example 1,000,000 centipoises and more, is preferably chosen in order to accelerate the process of comminuting. The polyglycol ethers to be employed are disclosed for example in German Patent Specifications Nos 605,973; 667,744; 694,178; 679,710; Austrian Patent Specification 160,871; German Patent Specifications Nos. 824,949; 806,671; and British Patent Specification No 690,355. Suitable kneading devices are the known mixing and kneading machines used for the intimate mixing of viscous pastes such as, for example, the well known Werner & Pfleiderer kneaders or mixing and kneading devices as described in German Patent Specification No. 813,154, or a continuous kneading apparatus such as the Buss-Ko-kneader (cf Ullmanns Encyklopxdia der technischen Chemie, 3rd edition, volume 1, page 727). The process is effected preferably by using the pigments to be kneaded in the form of a powder, but moist pastes of the pigments can also be

treated. The new process enables a very rapid production of the fine dispersion of the pigments required for various purposes The process is thus favourably distinguished from the processes hitherto used for this purpose. The finely dispersed pigment pastes which are obtained can easily be homogeneously dispersed by stirring them into aqueous or nonaqueous media in a simple manner This property of the pigments renders them suitable for all purposes where the application of finely divided pigments is desirable, for example, for dyeing in the spinning process of polyacrylonitrile, viscose and copper rayon, for colouring lacquers and synthetic resins, in pigment printing, for colouring paper pulp, and for the manufacture of wallpaper colours. The following examples illustrate the invention the parts being by weight:EXAMPLE 1 parts of the monoazo dyestuff obtained from diazotized 2,5-dichloro-aniline and 21,3 'hydroxynaphthoylamino-benzene are treated in a suitable kneading device (Werner & Pfleiderer dispersion kneader) with 100 parts of the condensation product from hydroxydiphenyl, benzyl chloride and ethylene oxide as described in Example 1 of German Patent Specification No 824,949 The viscosity of the paste lies above 106 centipoises After 30 minutes there is added sufficient water so that the paste is capable of flowing The dyestuff paste shows a uniformly fine division having a particle diameter of 0 3 to 1 micron. EXAMPLE 2 parts of the monoazo dyestuff obtained from diazotized 4-chloro-2-toluidine and 1phenyl-3-methyl-5-pyrazolone are treated with parts of the dispersing agent used in Example 1 and 30 parts of water in a kneading lPrice W,' /tt' Y t 1 I 1 k_ 1, 784,662 device described in German Patent Specification No 813,154, at a viscosity above 10 " centipoises After 20 minutes water is slowly added thereto until the kneaded paste has acquired a fluid state enabling it to be further treated The dyestuff then shows a particle diameter of 0 2-2 microns. EXAMPLE 3 parts of the diazo dyestuff obtained from diazotized o-amido-diphenyl and 3,3 'from diazoatized o-amido-diphenyl and 3,31dimethyl-4,4 '-diaceto-acetylamino-diphenyl are treated with 140 parts of iso-octylphenyl polyglycol ether according to Example 1 of Austrian Patent Specification No 160,87-1, in a kneading device described in German Patent Specification No 813,154, at a viscosity of above 106 centipoises Without further addition of water the particle size of the dyestuff dispersion thus obtained lies around 0 5 micron. EXAMPLE 4 parts of copper phthalocyanine are treated with 90 parts of the dispersing agent used in Example 1 in a kneading device described in German Patent Specification No.

813,154, at a viscosity of above 106 centipoises for 60 minutes The dyestuff then shows a fine even dispersion having a particle size of 0 5-1 5 microns. EXAMPLE 5 parts of the monoazo dyestuff obtained from diazotized 2,5-dichloro-aniline and 21,3 'hydroxynaphthoylamino-benzene are treated with 50 parts of the dispersing agent used in Example 1, and 100 parts of water, in a kneading device described in German Patent Specification No 813,154, at a viscosity of 2700-400 centipoises for 45 minutes. The dyestuff dispersion obtained consists of dyestuff particles having a diameter of 0 3-1 micron When instead of the above mixture, parts of the dispersing agent and 50 parts of water are used, the viscosity of the kneading paste increases to 80000 to 120,000 centipoises The fineness of the dispersion correspends to the aforementioned particle size. The dispersing agent may be added in its pure state or dissolved in the corresponding amount of water. EXAMPLE 6 parts of red iron oxide are treated with parts of the dispersing agent used in Example 1, for 45 minutes in a kneading device described in German Patent Specification No 813,154, at a viscosity of above 106 centipoises The dyestuff then shows a fineness of dispersion having a particle size of 02-2 microns, apart from a few agglomerates having a particle size of up to 10 microns.

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