Note: Descriptions are shown in the official language in which they were submitted.
` `` 1125458
.~ 1
AEROSOL PREPARATION
DESCRIPTION
This invention relates in general to aerosol preparations
and more particularly such preparations of water base character
for providing a continuous unbroken film upon dispensing.
~eretofore, there have been innumerable, consistently
unsuccessful efforts to develop an aerosol emulsion for pro-
viding a continuous, uninterrupted film or coating, whether
for decorative or protective purposes, such as with paints,
various types of finishes, lubricants, etc., wherein water
constitutes the continuous or external phase.
It is recognized that many active ingredients for film
formation may be emulsified, but to date emulsion technology
has not been satisfactory for providing a continuous film in an
efficacious manner. Shortcomings of existing emulsion tech-
nology are two-foldi
a) Those relating to oil in water have failed because
; the hydrophobic active ingredients must of necessity be in the
oil phase and in this type of emulsion water is the continuous
phase. Consequently, there is no molecular continuiuty of the
active ingredient so that the resultant film would be discontinuous
with uneven distribution of the active ingredient. An example
would be the commercial silicone emulsions which are basically
low viscosity polydimethylsiloxanes emulsified in water and
in these emulsions the water is on the outside or in the
continuous phase. Attempting to use such an emulsion as a mold
release, for example, would have disappointing results because
` ` 1125458
.~ ` 2
the silicone would be distributed unevenly upon the applied
surface and the compound would not serve to bring about reliable
mold release.
b) Those resultant from water in oil are due to the
altered nature of the active ingredient. Though the active
ingredients are in the continuous phase by the nature of the
present emulsion technology, these active inyredients are
altered by the presence of water and/or emulsifiers and their
performance is not what would be expected should such have been
applied in pure form or in solvent reduction. The active
; ingredients as applied are altered in appearance from the
pre-emulsion state. For instance, active ingredients which have
been transparent become pasty or creamy; rèsultant applications
have been disappointing. Exemplary of this would be to prepare
a silicone emulsion wherein the silicone would be in the oil
or continuous phase and attempt to use this as a mold release.
Experience has shown that although the distribution of the silicone
may be even and continuous in this type of emulsion, the pre-
~; sence of the water and/or emulsifiers severely limits the
2~0-` release effect of the silicone. These compounds simply have
not worked. When applied the silicone emulsion i9 paste-like
or creamy in appearance and not characteristic of the trans-
parent quality o~ polydimethylsiloxane which would be the pre-
ferred appearance.
The present accepted incapacity of aerosols to be useful
; with water based coating agents, as for example, latex paints,
,- . .
..
llZ5458
has been an especial problem of long standing. With present
technology, aerosols that require a smooth finish or film on
spraying, such as paints, silicone, or the like have utilized
solvents other than water as the vehicle. Typical of such
solvents are hydrocarbons, such as aromatics, aliphatics,
chlorinateds, fluorinateds and the like, wherein, in most
instances, the propellant is generally soluble in such solvents
and may be considered chemically as part of the solvent,active
mixture. Thus, in effect, resort has necessarily been made to
a single phase system or solution wherein the active ingre-
dient, such as an oil-based paint, i5 dissolved within a suit-
able solvent other than water, as particularly, within a wide
range of compatible organic solvents. However, the utilization
of such solvents or carriers has involved inherent peril factors,
lS as for example, aerosol paint is extremely flammable by reason
of the incorporated solvent; and the majority of commercially
used and available soIvents have low threshold limit values
that are intensified by the atomization process of the selected
aerosol. Furthermore, most of these solvents have undesired
ecological consequences in bringing about a further depletion
of fossil fuel resources; as well as being uneconomic in light
of the continual rise in cost therefor~ Additionally, these
solvents consistently cause unpleasant and even obnoxious
odors.
There has, accordingly, been a continuing effort to solve
this problem as such would eliminate immediately the recognized
and reluctantly accepted hazards of using aerosol systems with
respect to oil based paints, among others.
Therefore, it is an object of the present invention to
.
llZS458
~ 4
~.
provide an aerosol preparation which is water based and is pro-
ductive of an uninterrupted, continuous film; which eliminates
all of the various hazards associated with the dispensing of
aerosolized ingredients carried in the requisite organic sol-
vents or vehicles; and which obviates the use of an auxiliarysolvent for the propellant.
It is another object of the present invention to provide
a preparation of the character stated which is capable of pro-
ducing a continuous film from a broad spectrum of film and
coating agents, such as water-base paints, lubricants, sealants,
mold release, protective coatings, waxes, and the like; and
which incorporates an agent for controlling, through the
molecular structure thereof, the manner in which the propellant
leaves the film.
It is a urther object of the present invention to provide
a preparation of the character stated wherein an agent is
embodied for controlling the manner in which the propellant
leaves the film, and with there being a dispersal agent for
synergistically acting with said film controlling agent to
provide a resultant film having leveling characteristics of
being æmooth, even, and unbroken; with molecular continuity of
the active ingredient.
It is a further object of the present invention to pro-
vide a preparation of the character stated which may incor-
poràte as active ingredients liquids as well as flowable powders,without the necessity of predilution.
It is another object of the present invention to provide
a preparation which effects the use of water as a carrier for
hydrophobic chemicals, for chemicals that have previously
been delivered by means of petrochemical or other non-aqueous
solvents, and for improving the effectiveness of systems
which presently incorporate water as a carrier.
llZ5458
`~ It is a further object of the present invention to
provide a preparation of the character stated which is capable
of the equally efficacious application of both water soluble
and water insoluble active ingredients for providing a continuous
film and wherein the physical and chemical characteristics
of such ingredients are unaltered from the prediluted state
thereof.
It is a still further object of the present invention to
provide a preparation of the character stated which upon dis-
pensing provides a continuous film as distinguished from thefoams and sprays heretofore attained by aerosolization of
emulsions; which films are nonproductive of corrosion; which are
not fundamentally flammable or toxic so that circumscription
as to usage is eliminated thereby presenting a breadth of
application hitherto unknown in the aerosol field.
It is another object of the present invention to provide
a preparation of the character stated which has a substantially
; indefinite shelf life; merely requiring a degree of agitation
prior to each application regardless of the transpired interval
between dispensing.
It is a further object of the present invention to provide
a preparation of the character stated which may be most economic-
ally produced; there being no necessity of complex instrumentation
and equipment for formulation as the same may be accomplished
-25 in accordance with well-known production techniques; and which
may be charged to individual containers and suhjected to the~
preferred propellant with presently, generally utillzed equipment.
Another object of the present invention is to provide a
preparation of the type stated which is extremely effective in
use; which has demonstrated a remarkable versatility in being
adapted for accommodating a most extensive range of varied film-
llZ5458~roducing agents so as to be endowed with a unique neo-uni~er-
lity; and which preparation may be most economically produced
and sold; and with the films developed thereby being tenacious,
durable, and proof against rupture, scuffing or the like
through the normal intended usage peculiar to the particular
film.
The present inYention contemplates the development of
an aerosol~preparation which through its unusual character-
istics is both physically and chemically distinct from the
customary aerosol emulsions, as well as from the single phase
solutions heretofore used for ~ilm formation by oil based
paints and the like~ The system of the present preparation does
embody generally immiscible phases, one of which may be con-
sidered a water phase, the other a continuous phase, which phases
are normally clearly defined, sharply distinct, and separated.
The active ingrediènt, for the purposes of this invention, is
primarily in the "oil" or continuous phase, even if it is
water soluble. In addition, the film controller and propellant
are part of the continuous phase. However, there is also, and
most critically, provided within the continuous phase a pre-
determined quantity of what might be referred to as a dispersal
; agent, being soluble in both of said phases but in different
degrees.
The preparation will thus in its normal state be
unhomogenized with the two phases being sharply separated.
When the preparation is to be utilized, immediately
prior thereto the same is agitated and then substantially
instantaneously dispensed, with the discharged material being
a transitory mixture~ As applied, the dispensed matter will
present a continuous film upon the particular surface, unin-
terrupted by any type of lacunae, pores, or geometric formations
so that a coating with desired thickness and being entirely
llZS458
continuous is developed. As indicated, the present invention
has been proved to be completely successful with water based
paints, as well as numerous other film-producing agents.
Although the constituents of the preparation will be discussed
in greater detail below, attention is directed to the unique
dispersal agent which is critical for the development of aerosol
preparations of this invention. It has been found that a
specific cocodiethanolamide from that class of chemicals which
has been heretofore recognized as emulsifiers possesses certain
unexpected and surprising properties when used in a predetermined
proportionality in the two phase system of the present invention.
This particular cocodiethanolamide is an amber liquid having a
congealing point of approximately 6C. and with a specific
gravity at 25%C. of .99. The free or unreacted fatty acid, as
lauric, is 3% - 4% maximum and the pH of a 1% dispersion is
between 8 and 9. This compound is soluble in alcohols, glycols,
ketones, esters, aromatic and aliphatic carbons, and chlorinated
solvents, while also being dispersible in water at low concentra-
tions of 1 to 2%. It is also soluble at higher concentrations
and with a 10% solutlon being quite viscous approximating a gel.
Thus broadly thc lnvontlon contcmplat~s an acrosol pr~-
paratlon in the form of a dispersion for providing a continuous,
unbroken film on a substrate which comprises an active ingredient
selected from the class consisting of water soluble and pre-
emulsified or partially pre-emulsified water insoluble compounds,
a propellant, a film controlling agent for controlling the manner
in whlch the propellant leaves the film, water, and cocodiethanol-
amide in an amount suf~iclent to cause said preparation upon
dispensing to be a dispersion.
-~ 30 It is to be thus understood that the term "cocodiethan-
olamide" as referred to and described herein shall be that form
. ~
~,
,: ` ~' .
" l~ZS45~
of the compound possessing the above-described physical and
chemical characteristics.
It has been discovered that providing cocodiethanolamide
in an amount approximating 0.5% by weight of the system or
S preparation will react with the water phase and the continuous
phase when it is not in an emulsion to bring about what is
generally considered an unstable emulsion, that is, wherein
the phases tend to separate, but are capable of being brought
into relative stability by agitation, and upon spraying the
phases separate and revert to their constituent components whereby
the active ingredient does not produce a con~inuous film but
one which is highly irregular and interrupted, typical of the
results obtained to the present time when water based solvents
are utilized in aerosol form.
If the proportionality of the cocodiethanolamide is
increased as within the range of immediately above 0.5% to
approximately 2,5% by weight, when the active ingredient is
initially in an unemulsified condition, a resulting stable
emulsion is developed and thus the cocodiethanolamide acts in
the expected manner of an emulsifying agent so that upon dispensing
of such a preparation containing such proportionality, a discon-
tinuous broken film may be presented despite the fact that the
emulsion is stable. In its generally normal state such emulsion
gives a visual appearance of a homogenous, pasty character,
consistent with its being considered stable. Thus, the fore-
going merely underscores that cocodiethanolamide as used in
llZ5458
the aforesaid proportion with the active ingredients of
the preparations of this invention, when such active ingredients
are initially in an unemulsified condition, serves in its
characteristic function as an emulsifying agent.
However, if the quantity of cocodiethanolamide is in-
creased beyond 2.5~ as within the specific range of 2.5 to 10%
by weight, the system developed as hereinabove described loses
its stability so that a separation immediately takes place
which, at first glance, would bear a seeming resemblance to
the unstable emulsion incorporating a 0.5% by weight of.
said agent as above described, Despite any visual similarity
between the phase separations of the unstable emulsion and
the preparation incorporating in excess of 2,5% by weight
of cocodiethanolamide, such generally corresponding phases
are quite different both chemically and physically. It is
~suggested that the preparation with the greater quantity
of cocodiethanolamide has become a dispersion, that is atypical
of traditional technology having, as stated, the immiscibility
of the two phases being sharply defined, Without any intention
of limitation, the preparat,ion herein will be referred to as a
; "dispersion" to faailitate exposition, The agitation prior to
dispensation merely promotes a momentary intermi~ture so that
upon discharge the dispersion characteristics control as
distinguished from the emulsion characteristics which would ~e
: . .
.~ - .
llZ5458
overriding if the cocodiethanolamide was below 2.5%. A con-
tinuous film is promoted by the dispersion as distinguished
from the discontinuous character of the dispensing of an emulsion.
As developed more fully hereinbelow, the preferred effec-
tive range of cocodiethanolamide for aerosol preparations ofthe present invention is 2.5 to 3.5% by weight when the active
ingredients are initially in an unemulsified state. However,
research has demonstrated that additional amounts up to 10% by
weight bring about no diminution in the character and quality of
the developed film. Above 10% it has been discovered that the
applied coating develops an undesirable thickness of a generally
lumpy character so that beyond such limit a continuous, unbroken
film is no longer achievable.
This crucial, unexpected action caused by the coco-
diethanolamide is all the more apparent when one recognizes
that the use of emulsifying agents in emulsions cause a predic-
tive response. It is recognized that there are numerous factors
- which contribute to the relative stability or instability o a
particular emulsion but generally when the emulsifier is below
2Q a predetermined proportionality the associated emulsion will be
in an unstable state with the phases separated~ As the emul-
sifier ls added, the emulsion becomes relatively stable, with
the phases intermixing to present a homogeneous appearance;
and~further addition of the emulsifier generally has no effect
upon the stability of the emulsion. But with the present
invention the further addition of cocodiethanolamide beyond
substantially 2.5% by weight of the system brings about a
destruction of the erstwhile stability so that if a stable
emulsion did exist, one would necessarily expect that the
further addition of the cocodiethanolamide would be without effect.
llZS458
As pointed out, this unusual and surprising action of this
particular agent supports the view that the system is no longer
an emulsion with all of the various accepted emulsion character-
istics but becomes a dispersion, with the cocodiethanolamide
manifestly ceasing to act as an emulsifying agent. Therefore,
the crucialness of this agent to preparations formed in
accordance with this disclosure is apparent~ It will be fully
understood that no other compound has been found to possess the
requisite properties despite extensive investigatory efforts.
As developed hereinabove the systems of the present in-
vention are discussed as being in a non-emulsified state, in-
dependent of the cocodiethanolamide. However, the foregoing
clearly comprehends that through the addition of the cocodiethan-
olamide the various systems transitorily move into an unstable
emulsion, then into a stable emulsion as further cocodiethanol-
~ s added
amide~and then into a dispersion as the requisite energy level
is achieved through the incorporation of a predetermined amount
.
- of cocodiethanolamide. Theoretically, a requisite amount of
energy is manifestly required to achieve the dispersion state
. j .
attained by the predetermined amount of cocodiethanolamide.
Understandably, the intermediate or transitory unstable and
stable states of emulsion also require respective critical
energy levels. Accordingly, the present invention teaches
that the specific cocodiethanolamide imparts certain character-
istics to water and oil mixtures when used as described andiA a quantity requisite to provide the necessary energy to
exceed a stable emulsion state as such is determined in accor-
dance with recognized technology. The extreme importance of
this unique property is more fully understood when the coco-
diethanolamide is added to existing stable or unstable emulsions.
llZS4S8
12
It has been found that adding 0.5% by weight ofcocodiethanolamide to a preparation which contains a stable
emulsion is adequate to provide the necessary energy to cause
such preparation to take on the unique characteristics of the
S dispersion of the present invention.
. With preparations comprising unstable emulsions, the
cocodiethanolamide must be added in a quantity sufficient to
provide the necessary energy to render such emulsions stable and
: then to progress therebeyond to the unusual and unexpected dis-
persion state developed by the present invention. It is under-
stood that the emulsified conditions of such active ingredientS,
that is whether the same are in stable or unstable state and
to what degree, may be readily determined by well-known, widely
practiced technology so that as the cocodiethanolamide is
added to unstable emulsions one may determine when the point
:: of stability has been reached and then proceed with further
incorporation of cocodiethanolamide to attain the dispersion
with the resultant preparation having the predetermined
characteristics,
2a It should be~ of course~ understood that with unstable
emulsions as herein discussed, generally accepted emulsifying
agents may be used for rendering such systems stable and with
the cocodiethanolamide being thus added thereafter, Consequently,
:nothing herein is to be interpreted as requiring the use of
cocodiethanolamide for raising the energy level of unstable
emulsions to that of stable emulsions, The primary point is
that cocodiethanolamide provides its unique functions only
after the particular emulsion has reached a state of stability,
- 13
llZS4S8
Illustrative of the foregoing is the utilization of
cocodiethanolamide with latex paints which comprehend paints
which are stable emulsions as well as those which have varying
degrees of instability. The addition of cocodiethanolamide
S in an amount of no less than 0.5~ to stable emulsions creates
the necessary dispersion so that the particular paints are
rendered amenable for aerosolization in conjunction with the
other prerequisites of the invention. Similarly, with paints
which are in unstable emulsions the addition of sufficient
cocodiethanolamide to render same stable plus at least 0.5%
by weight thereabove adapt same to constitute an aerosol
- preparation which thus may be sprayed without foams, film
rupture and the like and create a continuous unbroken coating
or film upon the applied surface.
The foregoing clearly demonstrates that the specific
emulsifiers in latex paint have provided energy that cocodiethan-
` olamide would have had to supply to achieve a stable emulsion
had such not been present. This energy is added to that of the
.
~ cocodiethanolmide and with the prescribed addition thereof, as
`~ 20 in the order of 0.5% to stable emulsions, incorporating sufficient
~; ,
energy to change the stable emulsions into the dispersions suitable
for the present invention.
Another example is provided by silicone emulsions* which
are useful in developing a hard surface polish. Such silicone
emulsions are generally stable so that the mere addition of 0.5%
by weight of cocodiethanolamide will alter the character of the
stable emulsion from oil I~ water so that the oil is now in the
continuous phase. Such addition will also change the emulsion to
the dispersion forthe present invention so that the resultant
;-
film presented upon application of the particular preparation
*; ~mulsions offe~ed hy Gener~l Elec~ c Co~ o~d~New York as SM2a33, ~M2Q35~ etc.
14
~125458
will be transparent and not creamy like an emulsion indicating
that physical and chemical changes have occurred.
However, even though the foregoing has disclosed that
0.5% of the cocodiethanolamide added to a stable emulsion
will endow the preparation with attributes hitherto unachieved
in this manner, the cocodiethanolamide may be added in an
amount up to but not to exceed 10% and the increased amount
will provide desired characteristics, such as, for instance,
the degree of cohesiveness, and the particular thickness of
the resultant fi}m as may be shown, such amounts within the
range of 0,5 to 10% by weight of the preparation being easily
experimentally determined.
- Active ingredients peculiarly adapted for incorporation
in aerosol preparations of the present invention may be water
insoluble and comprehend the active phase of water-base paints
commonly referred to as latex paints, exemplary of which are
acrylic emulsions, vinyl emulsions, vinyl copolymer acetate
emulsions, alkyd emulsions and polyurethane emulsions; mold
release and lubricating agents, as for instance, silicones,
namely the alkyl polysiloxanes and polyorganosiloxanes;
lecithin and other soya or animal fat derivatives; stearates,
telefluoromers, as Teflon*; also synthetic lubricants,
such as butoxylated and ethoxylated glycols; as well as
polybutene used for transmission belt dressing, etc; and
various common greases, such as lithium stearate, calcium stearate,
petroleum, aluminum naphthenate, and the like for utilization
as lubricant coatings; moreover, mineral seal oil, as both a
penetrant and a lubricant, as well as petroleum based hydrocarbon
oils and synthetic oils are amenable to incorporation in prepa-
rations of the present invention. A further category of active
*TEFLON is a trademark of E. I. DuPont De Nemours & Co., Inc~for tetrafluoroe7hylene reslns,
llZ54S8
. 15
- ingredients would be constituted of the waxes, including animal
waxes, such as beeswax and stearic acid; vegetable wa.~es such
as carnauba, bayberry and candelilla, as well as the various
artificial or synthetic waxes as obtained from distillation of
paraffin base petroleum. The foregoing enumerated types and
examples of active ingredients for forming constituents of
aerosol preparations of this invention is not meant to be
exhaustive but merely indicative of the comprehensive range of
compounds which by virtue of the uniqueness of this invention
may now be aerosolized in water borne systems to provide a
continuous film which was heretofore deemed impossible through
such aerosolization. All these compositions are of the type
wherein the intended usage or purpose requires an unbroken coating.
Other active ingredients suitable for preparations of the
present invention are water soluble compounds which, for purposes
of illustration only, comprehend;
me.thoxx ~olye.th~enç ~lycols use~u~ fox
lub.xi~.c~nts a~d a~$ oint~ent ~ases. ~o~ cQs~et~c~ ~nd phaxmaceuticals;
wate~ soluble ~esin~, such as hydroxyeth~l
celluloses a.nd ethxlene copolyme~s useful fox coatin~s~ paints~
: adhesives, caulking compounds~ and ~q~ textile ope~at~ons
wateX sQluble herbIcides~ such as paraquat~
diethanolam~ne salt of 2,4~dichloro~henoxy acetic acid~
diethanolamine salt of 2~(2~methyl~4~chlorophenoxyl propionlc
25 acid; and
wate~ $oluble alkyl ~lycols and alkyl esters
encompassin~ butoxylated and eth~xylated ~aup$ us.ed for
lubrication, hyd~aulic ~luids~ and ~o~ c~smetic and pha~aceutical
applications,
1125458
16
Accordingly, the range of treatments is infinite when
it is recognized that such preparations can provide lubrication,
mold release, adhesives, sealants, water displacement sprays,
wax coatings, polyMeric finishes, such as for floors and like
surfaces; inks and dyes; asphaltic undercoatings, polyurethane
coatings, and paints.
The particular propellants embodied in aerosol preparations
of the present invention are of generally accepted types, that
is liquefied, such as, hydrocarbons or halocarbons, as fluoro-
carbons, and blends of the same, or compressed gases, orcombinations of liquefied and compressed gases. The selection
of the foregoi~g is dependent upon desired characteristics
relating to evaporation rate, solubility, economics, pressure
and safety. The well known 1uorocarbon 12 and fluorocarbon 114
are exemplary of halocarbon propellants equally useful.
Generally the hydrocarbon propellants are liquefied petroleum
gases, such as propane, butane and isobutane, such being more
popular at the present time than the halocarbons due to the
llZ5458
17
possible environmental effects thereof.
Also, compressed gas propellants, such as carbon dioxide,
nitrogen, nitrous oxide~.and dimethyl ether may be used with.the
same facility as with other aerosol preparations but with
attention, of course, directed to such considerations as
stability and pressure requirements for selection determination.
It is to be understood that the choice of propellant
in the present invention is indicated by the same considerations
as in the aerosol preparations generally and, thus, the precise
propellant does not form a part of the present invention.
In order to control the manner in which the propellant
leaves the film so.that a foam is not created and with the
resultant film having the desired leveling characteristics of
being relatively smooth and even, with molecular continuity
of the active ingredient, a film controlling agent or so-called
"film controller" is utilized. As will be developed herein the
, .j
;~ use of a "film controller" thus obviates the utilization of
. organic auxiliary soluents. These film controlling agents are
of such character that the active ingredients may be substantially
insoluble.therein. Additionally, such film controlling agents
possess an initial boiling point above 300F. assuring that the
.water within the film will evaporate at an earlier stage.
. Although the precise mode of reaction is not fuIly understood,
.it is believed that.the molecular structure of such film con-
25 trolling agents exert a repressive effect upon the propellant
so as to influence the manner in which the propellant leaves
the film. Thus, the inclusion of the nGvel film controllers
in the present preparation in conjunction with the dispersal
agent within the range stated in some manner synergistically
.~
18 1 1 Z 5 4S 8
`?rovides the r~sul~ant film with the smooth unbroken character,
~evoid of pores and other geometric formations associated
with foams.
Among the agents suitable for controlling the propellant
in the manner above described are mlneral oils with boiling
points above 3000F. including white oils, such as DRAKEOL*#7,
paraffinic oils, and isoparaffinic oils;
including glycols with initial boiling
points above 350F.,such as propylene glycol, ethylene glycol,
hexylene glycol, dipropylene glycol, diethylene glycol and
triethylene glycol;
including glycol ethers with initial
boiling points above 350F~, such as dipropylene glycol
monomethyl ether, diethylene glycol monoethyl ether, diethylene
glycol monomethyl ether, diethylene glycol monobutyl ether and
tripropylene glycol monoethyl ether; and
including aromatic blends or composition
solvents containing a high content of aromatic hydrocarbons
with initial boiling points above 360F., such as HI-SOL 15**.
Such so-called film controllers need not possess solvency for
the propellant and thus obviate utilization of the heretofore
widespread use of organi~ auxiliary solvents for propellants,
If the active ingredient is hydrophobic, it need not be fully
soluble in either the propellant or the film controller. It
is understood that an inadvertent low degree o solubility of
the active ingredient may be tolerated but such is not preferred
unless the active ingredient is water soluble, Thus, if
during production it was discovered that the active ingredient
and the film controlling agent were incompatible, that is,
productive of a precipitate~ the same would not be intermixed
*DRAKEOL is a trademark of Pennreco, Inc~ to identify a series
of white mineral oils, colorless, odorless and ta~teless hydro-
carbon distillates meeting the U.S.P. XV and N,F~ X requirements
for "petroleum liquidum",
**HI-SOL is a trademark of Ashland Chemical Company for aromatic
petroleum solvents.
~lZ54S8
19
directly, but with the said agent being incorporated sub-
sequent to the inclusion of the water.
These film controllers also allow for another unique
property of this invention, that is, the ability to aerosolize
active ingredients which are soluble in water but in the past
have been more efficaciously delivered in solvent systems.
An example of this would be water soluble herbicides, wherein
a typical spray would produce beading on the foilage and con-
sequently poor coverage fcr the herbicide. The nature of this
invention is such that the heribicide can now be delivered
onto the foilage with molecular contlnuity, that is, in a
smooth, unbroken film making the herbicide much more efficacious.
The mechanism that accomplishes this is not fully understood
but it is necessary for the active ingredients to be soluble
in the film controllers or the propellants to allow the in-
vention to work as expected rather than delivering either foam
or an uneven or broken film that would be expected in a situation
where the active ingredient was fully soluble in the water
~ and a film controller was not present.
Thus, in the present invention the solubility of the
propellant in the film controlling agent is a matter of
indifference since herein the manner of departure of the
propellant from the film is dependent upon a mechanism quite
distinct from solution formation.
Aerosol preparations having the properties of the present
invention have the following general formula wherein liquefied
propellants, namely the hydrocarbons and halocarbons are used:
llZS4S8
PERCENT BY WEIGHT
ACTIVE INGREDIENT Approx. .1% to 50%
PROPELLANT Approx. 5% to 30%
DISPERSAL AGENT:
5 Cocodiethanolamide 2.5~ to 10%
FILM CONTROLLING AGENT Approx. 1% to 20%
WATER Approx. 10% to 91.4%
In those preparations wherein compressed gas constitutesthe propellant, the general formulation will be as follows:
PERCENT BY WEIGHT
ACTIVE INGREDIENT Approx. .1% to Approx. 50%
PROPELLANT Approx. 2% to 5%
DISPERSAL AGENT:
Cocodiethanolamide 2,5% to 10%
15 FILM CONTROLLING AGENT Approx. 1% to 20%
WATER Approx. 10% to 94.3%
In those preparations wherein the propellant is con-
stituted of a combination of the liguefied and compressed
gases, the general formula will be as follows:
PERCENT BY WEIGHT
ACTIVE INGREDIENT Approx. .1% to 50%
PROPELLANT
Liquefied Approx. 2% to 30%
Gaseous Approx. .1% to 5%
25 DISPERSAL AGENT:
CQcodiethanolamide 2.5% to 10%
FILM CONTROLLING AGENT Approx. 1% to 20%
`WATER Approx. 10% to 94.3%
In the three formulae set forth hereinabove, the active
ingredient is not pre-emulsified so that, accordingly, the
cocodiethanolamide will be within the range of 2.5~ to 10%
by weight of the preparation so as to provide the necessary
energy for creating a dispersion.
llZS4S8
21
The applications of these formulations will become more intelli-
gible as a study is made of specific formulae hereinbelow.
However, it will be observed that the range of cocodiethanolamide
is quite defined, all as fully discussed hereinabove; and that with
the proportionality of the propellant and the film controlling
agents therefor all within the stated ranges, Film controlling
agents within an amount less than 1% by weight have not
demonstrated the capacity to act efficaciously with the pro-
pellant and, similarly, levels above 2n% appear to have an
adverse effect in controlling the departure of the
propellant
EXAMPLE I
An aerosol preparation for providing a continuous high
gloss, hard surface coating may be formulated as follows:
PERCENT BY WEIGHT
ACTIVE INGREDIENT
Dimethylpolysiloxane (10,000 cs) S~
~ ( 1,000 cs)10%
: FILM CONTROLLING AGENT
White Oil (Drakeol #7l . 5%
DISPERSAL AGENT
Cocodiethanolamide 3%
PR~PELLANT
7a % Isobutane I5
3~% Propane
~ATER 62%
Thè active ingredient, understandably, comprehends high and
low viscosity forms of the dimethylpolysiloxane in accordance
with accepted practice for conducing to the flowability of
such active ingredient. The isobutane-propane mixture provides
a suitable pressure for dispensing but, manifestly, other
llZ5458
22
propellants are equally effective whether the same are
liquefied, or compressed gases, or both as is exemplified ~y
the following:
EXAMPLE I(a)
PERCENT BY WEIGHT
ACTIVE INGREDIENT
~imethylpolysiloxane (10,000 cs) 5%
" ( 1,000 cs) 10
FILM CONTROLLING AGENT
White Oil ~Drakeol #7) 5
DISPERSAL AGENT
Cocodiethanolamide 3%
PROPELLANT
Propane (liquefied) 5%
Nitrogen tgaseous) .5%
WATER 71.5%
EXAMPLE II
The following exemplifies the constitution of an aerosol
preparation in accordance with the present invention useful
as a general or all-purpose lubricant:
~ PERCENT BY WEIGHT
- ACTIVE INGREDIENT
Silicone grease 3.2%
FILM CONTROLLING AGENT
White Oil 2.5%
DISPERSAL AGENT
Cocodiethanolamide 3%
PROPELLANT
Isobutane 20%
WATER 71.3~
The foregoing formula relates to a silicone lubricant prep-
aration wherein the active ingredient, although constituting,
seemingly, a small percentage of the formula, attains with the
water present a continuous film for assuring appropriate, even
coverage of the devices or elements to be lubricated,
llZS4S~3
EXAMPLE III
The formula of this example is merely illustrative of
the proportionality of the constituents ~or bringing about a
continuous film as used for a dressing upon belts of various
types, such as, conveyors and the like.
PERCENT BY ~EIGHT
ACTIVE INGREDIENT
Polybutene 10%
FILM CONTROLLING AGENT
High Boiling Isoparaffinic Oil 10
DISPERSAL AGENT
Cocodiethanolamide 2.5%
PROPELLANT
Nitrous Oxide (gaseous~ 4%
WATER - 73.5%
It will be observed that the propellant in the foregoing
formula is a compressed gas, nitrous oxide, which thus demon-
strates the capability of propellants of all recognized types
as being suitable with the present invention.
EXAMPLE IV
This example sets forth a formula for a graphite pene-
trant which may be aerosolized and provide a film having the
desired leveling characteristics:
PERCENT BY WEIGHT
ACTIVE INGREDIENT
OILDAG* . 1%
FILM CONTROLLING AGENT
Mineral Seal Oil 5%
DISPERSAL AGENT
Cocodiethanolamide 2.5
PROPELLANT
Propane 10%
WATER 81.5%
*OILDAG is a trademark of Acheson Colloids Co. of Port Huron,
Michigan to identify a concentrated colloidal dispersion of
pure electric-furnace graphite in petroleum oil.
~125~58
24
This particular formula is of interest in that it demonstrates
an`active ingredient which is in colloidal dispersion form.
EXAMPLE V
The formula of this particular example demonstrates
the usefulness of the present invention for providing an aerosol
preparation wherein the active ingredient is a flowable powder:
PERCENT BY WEIGHT
-
ACTIVE INGREDIENT
Benzocaine (ethyl-para-aminobenzoate) 10
10 FILM CONTROLLING AGENT
Propylene Glycol 10%
DISPERSAL AGENT
Cocodiethanolamide 3.5%
PROPELLANT
15 ;Isobutane 20
WATER 56.5~
From this particular example the versatility of the present
invention becomes all the more apparent when its applicability
to flowable powders is observed. Thus, the utilization in the
medical field for topical dressings is of recognized
importance, much less the potential for industrial usages
of material, such as talc, silica, etc. Therefore, the prospect
of providing continuous unbroken films of such materials
presents a wide range of application.
EXAMPLE VI
The following formula is revelatory of the usefulness
of the present invention to provide a hard surface protector
wherein, admittedly, a continuous unbroken film is of extreme
criticality:
,
l~Z5458
- PERCENT BY WEIGHT
ACTIVE INGREDIENT
ACRY:LOID B66* 10%
FILM CONTROLLING AGENT
HI-SOL 15** 10
DISPERSAL AGENT
Cocodiethanolamide
PROPELLANT
C2 ~(gaseous) 5%
10 WATER . 71%
Thus, in this example the active ingredient is actually a
solution and in such form is fully effective for aerosolizatio
to present a smooth, even film wherein such ingredient attains
molecular continuity.
EXAMPLE VII
The following formula is merely illustrative of the
aerosolization of latex paints in accordance with the present
invention:
PERCENT_BY WEIGHT
ACTIVE INGREDIENT
Latex Paint 60%
DISPERSAL AGENT
Cocodiethanolamide . 1
FILM CONTROLLING AGENT
White ~Flneral Oil 7
PROPELLANT
Propane 15%
WATER 13%
In the foregoing example, it is to be observed that
the dispersal agent is in the approximate amount of 1~ which
is quite adequate in view of the fact that the latex paint
is . a stable emulsion so that a lesser amount of the
*ACRYLOID is a trademar~ of Rohm & Hass of Philadelphia,
Pennsylvania for acrylic ester resins in organic solvent
solution.
**HI-SOL is a trademark of Ashland Chemical Company for aromatic
petroleum solvents~
26
5458
dispersal agent is needed to provide the energy for effecting
. ~the requisite dispersion than in those systems wherein the
active ingredient is not in an emulsion. The particular
amount of the dispersal agent being greater than 0.5~ is
in the stated proportionality to provide a certain desired
cohesiveness and thickness to the resultant film.
EXAMPLE VIII
This following formula is fundamentally along the
lines of the preceding example in demonstrating the applicability
of the present invention for use with active ingredients which
are in an emulsion:
PERCENT BY WEIGHT
ACTIVE INGREDIENT
Silicone Emulsion* 69.5%
DISPERSAL AGENT
CocodiethanolaMide . 0.5%
FILM CONTROLLING AGENT
DRAKEOL #7** 10%
PROPELLANT
Isobutane 20%
The foregoing does not require the addition of water in view
of the inclusion of the same within the emulsion of the active
ingredient, The dispersal agent is included in the minimal
amount to bring about a dispersion in view of the fact that the
*Typical silicone emulsions are the preparations of General
Electric Co. identified as SM2033 and SM2035 which are silicones
of different viscosities; which latter may be in a 50:50
relationship in this formulation.
**See the first footnote on Page 18.
llZ5458
27
active ingredient is in a stable emulsion. Also in this par-
ticular formula the film controlling agent is added after or with
the d:ispersal agent in view of its lack of compatibility
with the particular active ingredient in its emulsion.
In studying the foregoing formulae it will be appreciated
that there has been no indication of the inclusion of customary
- preservatives and anti-corrosion agents; the use of which would
be pursuant to the usual considerations and in ~eepin~ with
customary techniques,
The formulations herewith submitted serve to demonstrate
the broad range of active ingredients that may be incorporated
in preparations of this invention for continuous film formation.
It is understood that all of the various propellants and film
~ controllers set forth in the foregoing as examples are equally
effective as are the corresponding components set forth in the
specific examples which latter establish the effectiveness of
the present invention for myriad purposes.
The production of aerosol preparations conforming to the
present invention may be effected in most facile manners, with
all involved steps being generally undertaken under normal
ambient conditions and thus obviatin~ the necessity of environ-
mentally controlled conditions,
One such procedure is: - the continuous phase is first pre-
pared by intermixing the particular active ingredient in the` in~
dicated proportion and the selected film controller or film con-
trolling agent when the same are compatible; that is, wherein upon
intermixture a precipitate or other undesired chemical reaction does
not result, There is then added to the mixture the requisite amount
llZ5458
28
of the dispersal agent, cocodiethanolamide, with intermi~ing
being continued. As thus prepared the active ingredient phase
is subjected to agitation during which the prescribed quantity
of water is blended in and agitation is maintained to effect an
intermixture of the phases, The ultimate dispensing container
is then filled, in accordance with present technology, with
the intermixture which h~s been maintained in an agitated
state to the point of filling~ Thus, the propellant is the
last constituent to be introduced. Substantially instantaneously
upon discontinuance of the agitation, the water phase and the
active ingredient phase will separate and remain in such
spearated state pending subsequent agitation immediately prior
to dispensing.
However, in the e~ent the particular active ingredient
and the film controlling agent are not compatible, that is,
wherein the same upon intermixture would tend to cause a pre-
cipitate to form ox some other unwanted chemical reaction, the
film controlling agent is not added until after the water has
been provided, By iAtroducing the film controlling agent at this
particular stage, the formation of a precipitate is obviated.
Examples VI, VII, and VIII hereinabove are, as stated, demonstrative
of formulations wherein a precipitate would form upon the inter-
mixture of the active ingredient and the film controlling agent so
that in developing the aerosol preparations of said forumlations
- the film controlling agent is added after the water has been in-
corporated. The procedure for developing any of the myriad
formulations embodying the present invention is accomplished in
an economical manner, being fully suitable for high volume pro~
duction, so as to obviate expenditure for complex, costly equip-
ment or the maintenance o~ close tolerance conditions~
` ~lZ5458
29
Immediately prior to a proposed usage, the container for
the particular preparation is manually agitated by the user which
brings about a transitory mixture of the two phases being, in
essence, a quick or temporary dispersion in which state the
discharge occurs. Upon discontinuing discharging the phases
promptly separate into the normal, basically two phase condition
and remain in such state pending subsequent discharge. Thus,
the shelf life of aerosol preparations as developed herein is
extensive since the cyclic mixing and separation as developed
through use and through non-use has no deleterious effect upon
the ingredients and the phases so that regardless of the passage
of time the continuous film produced by this invention is
assured.
As deyeloped hereinabo~e~ aerosol preparations may be
formulated accordin~ to the present invention wherein the
actiye ingredient is in an emulsion in its pre.preparation
' state~ Thus, the water~b,a,se paints are reco~nized as being in
emulsLons,but any of the water ins~lu~le active ingredients herein
identified may also, if desi~ed, be pre~emulsified~ Recognizedly,
in view'of the water content of any such pre~emulsions, the
water constituent of the preparation of the p~esent invention
will be~ accordingly~ affected.
Thus, the following will canstitute yeneral formulae
' depending upon the nature of the propellant used for those active
ingredients which have been pre-emulsified; all as should be
apparent from the above disclosure~
llZ54S8
In those preparations wherein the propellants are
liquefied, namely from the group consisting of hydrocarbons
and halocarbons, the following is applicable:
PERCENT BY WEI5HT
S ACTIVE INGREDIENT IN EMULSIONS
(Excluding Any Solvent in
the Emulsion) Approx. 1% to 93.5%
PROPELLANT (Liquefied~ Approx. 5% to 30%
DISPERSAL AGENT:
10 Cocodiethanolamide 0.5~ to 10%
FILM CONTROLLING AGENT Approx. 1% to 20%
WATER 0 to Approx. 92.5
In those preparations wherein compressed gas constitutes
the propellant, the general formulation will be as follows:
PERCENT BY WEIGHT
ACTIVE INGREDIENT IN EMULSIONS
(Excluding Any Solvent in
the Emulsion) Approx. 1~ to 94.5%
PROPELLANT (Gaseous) Approx. 2% to 5%
20 DISPERSAL AGENT:
Cocodiethanolamide 0.5% to 10%
FILM CONTROLLING AGENT Approx. 1% to 20%
WATER 0 to Approx. 89.5%
In those preparations wherein the propellant is constituted
o~ a combination of the l~quefied and compressed gases, the
general formula will be as follows:
PERCENT BY WEIGHT
ACTIVE INGREDIENT IN EMULSIONS
~Excluding Any Solvent in
the Emulsion) Approx. 1% to 94~3%
PROPELLANT
~Liquefied Approx. 2~ to 30%
Gaseous Approx. ,1~ to 5%
DISPERSAL AGENT:
Cocodiethanolamide 0.5% to 10%
FILM CONTROLLING AGENT Approx. 1~ to 20%
WATER 0 to Approx. 89.33
