4251 4255.output

* 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.
the first and second portions of the gate are inclined to each other
at an angle of from 150 to 160 .
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 provided
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
A high quality text as facsimile in your desired language may be available
amongst the following family members:
DE1083985 (B)
DE1083985 (B) less
Translate this text into Tooltip
[78][(1)__Select language]
Translate this text into
The EPO does not accept any responsibility for the accuracy of data
and information originating from other authorities than the EPO; in
particular, the EPO does not guarantee that they are complete,
up-to-date or fit for specific purposes.
COMPLETE SPECIFICATION -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 dipenicillin, 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-chlorohydrocortisone, 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
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

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%
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.
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% - " "
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
0.9 gram Sodium Chloride Gran. U.S.P.
0.4 gram Tween 80
q.s. 100 cc. Water for Injection
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

four degrees centigrade, no change in physical characteristics of the
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
0.2 gram Tween 80
0.18 gram Methylparaben U.S.P.
0.02 gram Propylparaben U.S.P.
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
After storage of the resulting suspension for thirty days at
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
0.4 gram Tween 80
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

suspension is evident
The separated solids are readily re-suspendible and syringeability
through a 27 gauge needle is satisfactory.
EXAMPLE 5.
2.5 grams Sterile Micronized Progesterone
U.S.P.
0.4 gnam Tween 80
q.s. 100 cc. Water for Injection.
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
The separates solids are readily resuspendible.
There is no evidence of caking or cry;stal growth during storage at
the indicated temperatures.
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
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

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.
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.
reconstitution with an aqueous vehicle to provide la satisfactory,
therapeutic suspension is made up in the following formulation:
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.
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.
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)
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.
reconstitution with an aqueous vehicle to provide a satisfactory,
Itherapeutic suspension is made up in the following formulation:
milligram)
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.
Polyvinyl Pyrrolidone 10 milligrams Polyethylene Glycol 4000
U.S.P.
14.25 milligrams Sodium Citrate 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)
coated with 4% lecithin 255,000 units Procaine Penicillin 0(912 (280
milligrams) units per milligram)
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.
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)
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
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
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
-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.
U.S.P.
10 milligrams Po 1 y v i n y 1 Pyrrolidone
U.S.P.
1 milligram Tween 80 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)
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
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.
following: 250 milligrams Erythromycin S'tearate salt
powder
U.S.P.
Ta the resulting mixture is added sucrose, coloring, sodium cItrate
and preservatives.

milligrams of erythromycin stearate.
EXAMPLE 22.
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
milligrams of the erythiomycin ester.
EXAMPLE 23.
A therapeutic ;ereparation for oral use in dry form and suitable for
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.
milligrams of tetracycline.
EXAMPLE 24.
formulation: 210,000 units Procaine Penicillin G (988 (214
malligrairs) units p r n;illigram)--
coated with 1.25% lecithin 150 milligrams Tetracycline Hydrochlor
ide
U.S.P.
The mixture is blended and sterilized. The dry, sterile material is
therapeutic prepared tion containing more than 200,000 units of
penicillin in combination with tetracycline hydrochloride.

EXAMPLE 25.
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.
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.
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
U.S.P.
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
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.

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
The resulting aqueous suspension is stable and is suitable for
parenteral use.
Following the procedure described supra except for the replacement of
9-a-fluorohydrocortisone 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
U.S.P.
0.9 gram Sodium Chloride U.S.P.
0;4 gram Tween 80
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.
9-a-fluorohydrocortisone acetate by 9-a-chlorohydrocortisone acetate
the corresponding therapeutic composition containing 9-a- chlorohydro
cortisone acetate is obtained.
Similarly, by replacing 9-a-fluorohydrocortisone acetate by
9-a-fluorocortisone acetate in the procedure above, the corresponding
therapeutic composition containing 9-a-fluorocortisone acetate is
obtained.
EXAMPLE 29.
formulation: 150 milligrams Tetracycline Hydrochlor

ide
10.0 grams Sterile, micronized 9
a - Fluorohydrocortisone
Acetate
U.S.P.
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 streptomycin,
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-'.-halohydrocortisone 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
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-
.-fluorohydrocortisone 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.
9-e-fluorohydrocortisone 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.
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
A high quality text as facsimile in your desired language may be available
amongst the following family members:
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
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.
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.
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.
* Sitemap
* Accessibility
* Legal notice
* Terms of use
* Last updated: 08.04.2015
* Worldwide Database
* 5.8.23.4; 93p
* GB784661 (A)
Description: GB784661 (A) ? 1957-10-16
Process for the production of austenitic springs for watches, and like
apparatus, and springs obtained by this process

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.
Indox at aoceptance:-Classes 83 ( 2), A 155; and 83 ( 4), V 2
Intemnational Classification:-3 821 'h B 23 p.
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.
* Sitemap
* Accessibility
* Legal notice
* Terms of use
* 5.8.23.4; 93p
* GB784662 (A)
Description: GB784662 (A) ? 1957-10-16
Manufacture of finely dispersed organic or inorganic pigments
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.
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.
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.
* Sitemap
* Accessibility
* Legal notice
* Terms of use
* 5.8.23.4; 93p

4251 4255.output

More Related Content

What's hot

Viewers also liked

Similar to 4251 4255.output

More from j1075017

Recently uploaded

4251 4255.output