WO1981002023A1

WO1981002023A1 - Aerosol preparation

Info

Publication number: WO1981002023A1
Application number: PCT/US1980/000036
Authority: WO
Inventors: J Albanese
Original assignee: Chemsico Inc; J Albanese
Priority date: 1980-01-17
Filing date: 1980-01-17
Publication date: 1981-07-23
Also published as: BR8009019A; JPS57500069A

Abstract

An aerosol preparation of water base character for providing a continuous film upon dispensing comprising a water phase and a continuous phase wherein the active ingredient may be water soluble or water insoluble, or may be in emulsions, a liquefied or compressed gas propellant, or combinations thereof, an agent for controlling the manner in which the propellant leaves the developed film, and a dispersal agent consisting of cocodiethanolamide.

Description

AEROSOL PREPARATION DESCRIPTION

This invention relates in general to aerosol prepara¬ tions and more particularly such preparations of water base character for providing a continuous unbroken film upon dispensing.

Heretofore, 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 technology are two-fold: 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 con¬ tinuity 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 polydimethyl- siloxanes emulsified in water and in these emulsions the water is on the outside or in the continuous phase. Attempt¬ ing to use such an emulsion as a mold release, for example, would have disappointing results because the silicone would be distributed unevenly upon the applied surface and the compound would not serve to bring about reliable mold re¬ lease. 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 ingredients are altered by the presence of water and/or emulsifiers and their performance is not what would be expected should suc have been applied in pure form or in solvent reduction. The active ingredients as applied are altered in appearanc from the pre***-emulsion state. For instance, active ingredi ents which have been transparent become pasty or creamy ; resultant applications have been disappointing. Exemplary of this would be to prepare a silicone emulsion wherein th silicone would be in the oil or continuous phase and attem 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 presence of the water and/or- emulsifiers severely limit the release effect of the silicone. These compounds simply have not worked. When applied the silicone emulsion ispas.te<-like or creamy in appearance and not characteristic of the transparent quality of polydiraethylsiloxane which would be the preferr appearance, The present accepted incapacity of aerosols to be use with water based coating agents , as for example, latex paints, has been an especial problem of long standing. Wi 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 aromati aliphatics, chlorinateds, fluorinateds and the like, where in, in most instances, the propellant is generally soluble in such solvents and may be considered chemically as part the solvent/active mixture- Thus, in effect, resort has necessarily been made to a single phase system or solution wherein the active ingredient, such as an oil-based paint, is dissolved within a suitable solvent other than water, a particularly, within a wide range of compatible organic solvents. However, the utilization of such solvents or

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Λ>. WI carriers has involved inherent peril factors, as for example, aerosol paint is extremely flammable by reason of the incorporated solvent; and the majority of commercially used and available solvents 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 un¬ economic 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 cased paints, among others.

Therefore, it is an object of the present invention to provide an aerosol preparation which is water based and is productive of an uninterrupted, continuous film; which eliminates all of the various hazards associated with the dispensing of aerosolized ingredients carried in the requisite organic solvents or vehicles; and which obviates the use of an auxiliary solvent for the propellant.

It is another object of the present invention to pro¬ vide a preparation of the character stated which is capable of producing 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 further object of the present invention to pro¬ vide a preparation of the character stated wherein an agent is embodied for controlling the manner in which the pro¬ pellant 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 characte istics of being smooth, even, and unbroken; with molecula continuity of the active ingredient.

It is a further object of the present invention to pr vide a preparation of the character stated which may incor porate as active ingredients liquids as well as flowable powders, without the necessity of predilution.

It is another object of the present invention to pro¬ vide 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 oth non-aqueous solvents, and for improving the effectiveness systems which presently incorporate water as a carrier.

It is a further object of the present invention to pr vide a preparation of the character stated which is capabl of the equally efficacious application of both water solub and water insoluble active ingredients for providing a continuous film and wherein the physical and chemical char teristics of such ingredients are unaltered from the pre- diluted state thereof.

It is a still further object of the present invention to provide a preparation of the character stated which upo dispensing provides a continuous film as distinguished fro the foams and sprays heretofore attained by aerosolization of emulsions; which films are nonproductive of corrosion; which are not fundamentally flammable or toxic so that cir cumscription as to usage is eliminated thereby presenting breadth of application hitherto unknown in the aerosol fie It is another object of the present invention to pro- vide a preparation of the character stated which has a sub stantially indefinite shelf life; merely requiring a degre of agitation prior to each application regardless of the transpired interval between dispensing.

It is a further object of the present invention to pr vide a preparation of the character stated which may be mo economically produced; there being no necessity of complex instrumentation and equipment for formulation as the same may be accomplished in accordance with well-known produc¬ tion techniques; and which may be charged to individual containers and subjected to the preferred propellant with presently, generally utilized 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-producing agents so as to be endowed with a unique neo-universality; 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 invention 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 film formation by oil based paints and the like. The system of the present preparation does embody generally immiscible phases, one of which may be considered a water phase, the other a continuous phase, which phases are normally clearly defined, sharply distinct, and separated. The active ingredient, 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 predetermined 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 unho ogenized 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, uninterrupted by any type of lacunae, pores, or geometric formations so that a coating with desired thick¬ ness and being entirely continuous is developed. As in¬ dicated, the present invention has been proved to be completely successful with water based paints, as well as numerous other film-produciήg agents. Although the constituents of the preparation will be discussed in great detail below, attention is directed to the unique dispersa agent which is critical for the development of aerosol pre parations of this invention. It has been found that a specific cocodiethanolamide from that class of chemicals which has been heretofore recognized as emulsifiers pos¬ sesses certain unexpected and surprising properties when used in a predetermined proportionality in the two phase system of the present invention. This particular cocodiet anolamide is an amber liquid having a congealing point of approximately 6°C. 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 This compound is soluble in alcohols, glycols, ketones, esters, aromatic and aliphatic carbons, and chlorinated solvents, while also being dispersible in water at low con centrations of 1 to 2%. It is also soluble at higher con¬ centrations and with a 10% solution being quite viscous approximating a gel.

It is to be thus understood that the term " cocodieth olamide" as referred to and described herein shall be that form of the compound possessing the above-described physic and chemical characteristics.

It has been discovered that providing cocodiethanolam in an amount approximating 0.5% by weight of the system or preparation will react with the water phase and the contin ous phase when it is not in an emulsion to bring about wha is generally considered an unstable emulsion, that is, where-^*- in the phases tend to separate, but are capable of being brought into relative stability by agitation, and upon spray¬ ing the phases separate and revert to their constituent components whereby the active ingredient does not produce a continuous film but one which is highly irregular and in¬ terrupted, 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 proportion¬ ality, a discontinuous 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. This, the foregoing merely underscores that cocodiethanolamide as used in the aforesaid proportion with the active ingredients of the preparations of this in¬ vention, when such active ingredients are initially in an unemulsified condition, serves in its characteristic func- tion as an emulsifying agent.

However, if the quantity of cocodiethanolamide is in¬ creased beyond 2.5% as within the specific range 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 resem¬ blance 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, t is atypical of traditional technology having, as stated, t immiscibility of the two phases being sharply defined. Wi out any intention of limitation, the preparation herein wi be referred to as a "dispersion" to facilitate exposition. The agitation prior to dispensation merely promotes a mome tary intermixture so that upon discharge the dispersion characteristics control as distinguished from the emulsion characteristics which would be overriding if the cocodieth olamide was below 2.5%. A continuous film is promoted by the dispersion as distinguished from the discontinuous cha acter of the dispensing of an emulsion.

As developed more fully hereinbelow, the preferred effective range of cocodiethanolamide for aerosol preparat of the 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 char- acter and quality of the developed film. Above 10% it has been discovered that the applied coating develops an un¬ desirable 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 recognize that the use of emulsifying agents in emulsions cause a predictive response. It is recognized that there are nu¬ merous factors which contribute to the relative stability or instability of a particular emulsion but generally when the emulsifier is below a predetermined proportionality th associated emulsion will be in an unstable state with the phases separated. As the emulsifier is added, the emulsio 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 erst- while stability so that if a stable emulsion did exist, one would necessarily expect that the further addition of the cocodiethanolamide would be without effect. 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 characteristics 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 investi¬ gatory efforts.

As developed hereinabove the systems of the present in¬ vention are discussed as being in a non-emulsified state, independent of the cocodiethanolamide. However, the fore¬ going clearly comprehends that through the addition of the cocodiethanolamide the various systems transitorily move into an unstable emulsion, then into a stable emulsion as further cocodiethanolamide is added, and then into a dispersion as the requisite energy level is achieved through the incorpora¬ tion of a predetermined amount of cocodiethanolamide. The¬ oretically, a requisite amount of energy is manifestly re¬ quired to achieve the dispersion state attained by the pre¬ determined 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 characteristics to water and oil mixtures when used as described and in a quantity requisite to provide the necessary energy to exceed a stable emulsion state as such is determined in accordance with recognized technology. The extreme importance of this unique property is more fully understood when the cocodiethanol¬ amide is added to existing stable or unstable emulsions.

It has been found that adding 0.5% by weight of coco diethanolamide to a preparation which contains a stable emulsion is adequate to provide the necessary energy to cause such preparation to take on the unique characteristi of the dispersion of the present invention.

With preparations comprising unstable emulsions, the cocodiethanolamide must be added in a quantity sufficient provide the necessary energy to render such emulsions stab and then to progress therebeyond to the unusual and unexpe ed dispersion state developed by the present invention. I is understood that the emulsified conditions of such activ ingredients, that is whether the same are in stable or un- stable 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 cocodiethanolam to attain the dispersion with the resultant preparation having the predetermined-characteristics.

It should be, of course, understood that with unstabl emulsions as herein discussed, generally accepted emulsify agents may be used for rendering such systems stable and w the cocodiethanolamide being thus added thereafter. Conse quently, 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 uniq functions only after the particular emulsion has reached a state of stability.

Illustrative of the foregoing is the utilization of cocodiethanolamide with latex paints which comprehend pain which are stable emulsions as well as those which have var ing degrees of instability. The addition of cocodiethanol amide in an amount of no less than 0.5% to stable emulsion creates the necessary dispersion so that the particular paints are rendered amenable for aerosolization in conjunc¬ tion with the other prerequisites of the invention. Similar¬ ly, 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 un¬ broken coating or film upon the applied surface. The foregoing clearly demonstrates that the specific emulsifiers in latex paint have provided energy that coco¬ diethanolamide would have had to supply to achieve a stable emulsion had such not been present. This energy is added to that of the cocodiethanolamide and with the prescribed addi- tion thereof, as in the order of 0.5% to stable emulsions, incorporating sufficient energy to change the stable emul¬ sions 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 in water so that the oil is now in the continuous phase. Such addition will also change the emulsion to the dispersion for the present invention so that the resultant film presented upon application of the particular preparation will be trans¬ parent and not creamy like an emulsion indicating that phys¬ ical 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 un¬ achieved in this manner, the cocodiethanolamide may be added in an amount up to but not to exceed ιo_% and the increased amount will provide desired characteristics, such as, for instance, the degree of cohesiveness, and the particular

* Emulsions offerred by General Electric Co,, of Waterford, New York as SM2033, SM2035, etc. thickness of the resultant film as may be shown, such amou within the range of 0,5 to 10% by weight of the preparatio being easily experimentally determined.

Active ingredients peculiarly adapted for incorporati in aerosol preparations of the present invention may be wa 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 copoly acetate emulsions, alkyd emulsions and polyurethane emulsi mold release and lubricating agents, as for instance, sili cones, namely the alkyl polysiloxanes and polyorganosiloxa lecithin and other soya or animal fat derivatives; stearat telefluoromers, as Teflon*; also synthetic lubricants, suc as butoxylated and ethoxylated glycols; as well as poly- butene used for transmission belt dressing, etc; and vario common greases, such as lithium stearate, calcium stearate petroleum, aluminum naphthenate, and the like for utiliza¬ tion as lubricant coatings; moreover, mineral seal oil, as both a penetrant and a lubricant, as well as petroleum bas hydrocarbon oils and- synthetic oils are amendable to incor ration in preparations of the present invention. A furthe category of active ingredients would be constituted of the waxes, including animal waxes, such as beeswax and stearic acid; vegetable waxes, such as carnauba, bayberry and cand ilia, 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 in¬ gredients 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 b virtue of the uniqueness of this invention may now be aero ized in water borne systems to provide a continuous film which was heretofore deemed impossible through such aeroso ization. All these compositions are of the type wherein t intended usage or purpose requires an unbroken coating.

* TEFLON is a trademark of E. I. DuPont De Nemours & Co Inc. for tetrafluoroethylene resins.

A. Other active ingredients suitable for preparations of the present invention are water soluble compounds which, for purposes of illustration only, comprehend: methoxy polyethylene glycols useful for lubricants and as ointment bases for cosmetics and pharma¬ ceuticals; water soluble resins, such as hydroxyethyl celluloses and ethylene copolymers useful for coatings, paints, adhesives, caulking compounds, and for textile opera- tions; water soluble herbicides, such as paraquat, diethanolamine sale of 2,4-dichlorophenoxy acetic acid, diethanolamine sale of 2- (2-methyl-4-chloroρhenoxy) propionic acid; and water soluble alkyl glycols and alkyl esters encompassing butoxylated and ethoxylated groups used for lubrication, hydraulic fluids, and for cosmetic and pharma¬ ceutical applications.

Accordingly, the range of treatments is infinite when it is recognized that such preparations can provide lubrica¬ tion, 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 embodies in aerosol prepara¬ tions of the present invention are of generally accepted types, that is liquefied, such as, hydrocarbons or halocarbons as fluorocarbons, and blends of the same, or compressed gases, or combinations of liquefied and compressed gases. The selection of the foregoing is dependent upon desired char- : acteristics relating to evaporation rate, solubility, eco¬ nomics, pressure and safety. The well known fluorocarbon 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 possible enviromental 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 pre¬ parations 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 consider¬ ations 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 conti¬ nuity of the active ingredient, a film controlling agent or so-called "film controller" is utilized. As will be developed herein the use of a "film controller" thus obviat the utilization of organic auxiliary solvents. These film controlling agents are of such character that the active ingredients may be substantially insoluble therein. Additi ally, such film controlling agents possess an initial boili point about 300 F. assuring that the water within the film will evaporate at an earlier stage. Although the precise mode of reaction is not fully understood, it is believed th the molecular structure of such film controlling agents exert a repressive effect upon the propellant so as to in¬ fluence the manner in which the propellant leaves the film. Thus, the inclusion of the novel film controllers in the present preparation in conjunction with the dispersal agent within the range stated in some manner synergistically provides the resultant film with the smooth unbroken char¬ acter, devoid of pores and other geometric formations asso¬ ciated with foams. Among the agents suitable for controlling the propella in the manner above described are mineral oils with boiling points above 300 F. including white oils, such as DRAKEOL*#7, paraffinic oils, and isoparafinic oils; including glycols with initial boiling points above 350°F., such as propylene glycol, ethylene glycol, hexylene glycol, dipropylene glycol, diethylene glycol and triethylene glycol; including glycol ethers with initial boiling points above 350°F,, such as dipropylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monomethyl ether, diethylene glycol monobutly 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 360°F., 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 organic 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 of solubility of the active ingredient may be tolera¬ ted 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 directly, but with the said agent being incorporated subsequent 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,

*DRAKEOL is a trademark of Pennreco, Inc. to identify a series of white mineral oils, colorless, odorless and tasteless hydrocarbon distillates meeting the D.S.P. XV and N.F.X. requirements for "petroleum liquidum".

**HI-SOL is a trademark of Ashland Chemical Company for aromatic petroleum solvents. wherein a typical spray would produce beading on the foilage and consequently poor coverage for the herbicide. The nature of this invention is such that the herbicide ca now be delivered onto the foilage with molecular continuit that is, in a smooth unbroken film making the herbicide much more efficacious. The mechanism that accomplishes th 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 invention to work as expected rather than delivering either foam or an uneven or broken film that would be expected in a situation where the activ ingredient was fully soluble in the water and a film contr ler 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 qui distinct from solution formation.

Aerosol preparations having the properties of the present invention have the following general formula where in liquefied propellants, namely the hydrocarbons and halo¬ carbons are used:

PERCENT BY WEIGHT

ACTIVE INGREDIENT Approx, 1% to 50% PROPELLANT Approx. 5% to 30% DISPERSAL AGENT:

Cocodiethanolamide 2.5% to 10% FILM CONTROLLING AGENT Approx. 1% to 20% WATER Approx. 10% to 91.4% In those preparations wherein compressed gas constitu the 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^! FILM CONTROLLING AGENT Approx, 1% to 20% WATER Approx, 10% to 94,3%

In those preparations wherein the propellant is constituted of a combination of the liquefied 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% DISPERSAL AGENT:

Cocodiethanolamide 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.

The applications of these formulations will become more intelligible as a study is made of specific formulae herein- below. 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 propellant and, similarly, levels above 20% appear to have an adverse effect in controlling the departure of the propellant.

EXAMPLE 1

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 ) 5 %

( 1, 000 cs ) 10% FILM CONTROLLING AGENT White Oil (Drakeol #7) 5%

DISPERSAL AGENT Cocodiethanolamide 3%

PROPELLANT

70% Isobutane 15%

30% Propane WATER 62%

The 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 dispensin but, manifestly, other propellants are equally effective whether the same are liquefied, or compressed gases, or both as is exemplified by the following:

EXAMPLE Ka)

• PERCENT BY WEIGHT

ACTIVE INGREDIENT

Dimethylpolysiloxane (10,000 cs) 5%

II

( 1,000 cs) 10%

FILM CONTROLLING AGENT

White Oil (Drakeol #7) 5%

DISPERSAL AGENT

Cocodiethanolamide 3%

PROPELLANT

Propane (liquefied) 5%

Nitrogen (gaseous) .5% WATER 71.5%

EXAMPLE ; ii

The following exemplifies the constitution of an aerosol preparation in accordance with the present inventi useful as a general or all-purpose lubricant:

PERCENT BY WEIGHT ACTIVE INGREDIENT Silicone grease 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 preparation 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. EXAMPLE III

The formula of this example is merely illustrative of the proportionality of the constituents for bringing about a continuous film as used for a dressing upon belts of various types, such as, conveyors and the like. PERCENT^' BY WEIGHT

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 fore¬ going formula is a compressed gas, nitrous oxide, which thus demonstrates 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 penetrant 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%

This particular formula is of interest in that it demon¬ strates 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% FILM CONTROLLING AGENT

Propylene Glycol 10%

DISPERSAL AGENT Cocodiethanolamide 3.5%

PROPELLANT

Isobutane 20%

WATER 56.5%

*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.

"BU

0M ty- WI

■ A 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 applica¬ tion. 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: PERCENT BY WEIGHT

ACTIVE INGREDIENT

ACRYLOID B66* 10%

FILM CONTROLLING AGENT HI-SOL 15** 10% DISPERSAL- AGENT

Cocodiethanolamide 4%

PROPELLANT

CO2 (gaseous) 5%

WATER ^" 71%

*ACRYLOID is a trademark of Rohm & Haas of Philadelphia, Pennsylvania for acrylic ester resins in organic solvent solution-

**HI-SOL is a trademark of Ashland Chemical Company for aromatic petroleum solvents.

Thus, in this example the active ingredient is actually a solution and in such form is fully effective for aero- solization 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 Mineral Oil 7%

PROPELLANT

Propane 15%

WATER . - 17%

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 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:

O. i ,. wi 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 active ingredient is in a stable emulsion, Also in this particular formula the film controlling agent is added after or with the dispersal agent in view of its lack of compatibility with the particular active ingredient in ^"its emulsion.

In studying the foregoing formulae it will be apprecia- ted 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 keeping with customary techniques.

The formulations herewith submitted serve to demonstrate the broad range of active ingredients that may be incorpora¬ ted 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

*Typιcal 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. **Ξee the first footnote on Page 15.

0ΛPI co ponents 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 under¬ taken under normal ambient conditions and thus obviating the necessity of environmentally controlled conditions. One such procedure is: - the continuous phase is first prepared by intermixing the particular active in¬ gredient in the indicated proportion and the selected film controller or film controlling 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 of the dispersal agent, cocodiethanolamid with intermixing 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 pres.ent technology, with the intermixtu which has been maintained in an agitated state to the poin 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 separated state pending subsequent agitation immediately prior to dispensing, However, in the event the particular active ingredien and the film controlling agent are not compatible, that is, wherein the same upon intermixture would tend to cause a precipitate to form or some other unwanted chemical reacti the film controlling agent is not added until after the water has been provided. By introducing the film controll agent at this particular stage, the formation of a precipi is obviated. Examples VI, VII and VIII hereinabove are, as

_ O. ^v _' 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 formulations the film control- ling agent is added after the water has been incorporated. 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 production, so as to obviate expenditure for complex, costly equipment or the maintenance of close tolerance conditions. 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 disper- sion 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 developed hereinabove, aerosol preparations may be formulated according to the present invention wherein the active ingredient is in an emulsion in its pre-preparation state. Thus, the water-base paints are recognized as being in emulsions, but any of the water insoluble active ingredients herein identified may also, if desired, be pre-emulsified. Recognizedly, in view of the water content of any such pre-emulsions, the water constituent of the preparation of the present invention will be, accordingly, affected, Thus, the following will constitute general 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.

o.Mpi - In those preparations wherein the propellants are liquefied, namely from the group consisting of hydrocarbon and halocarbons, the following is applicable:

PERCENT BY WEIGHT ACTIVE INGREDIENT IN EMULSIONS (Excluding Any Solvent in the Emulsion) Approx. 1% to 93.5- PROPELLANT (Liquefied) Approx. 5% to 30% DISPERSAL AGENT:

Cocodiethanolamide 0.5% to 10% FILM CONTROLLING AGENT Approx. 1% to 20% WATER 0 to Approx. 92.5%

In those preparations wherein compressed gas consti¬ tutes 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% 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 of a combination of the liquefied and compress 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. 89.3%

Claims

CLAIMS 1, An aerosol preparation in the form of a dispersion for providing a continuous, unbroken film comprising an active ingredient, a propellant, a film controlling agent for controlling the manner in which the propellant leaves the film, water, and a dispersal agent consisting of cocodiethanolamide.

2. An aerosol preparation according to claim 1 wherein the active ingredient is from the class consisting of water soluble and water insoluble compounds.

3. An aerosol preparation according to claim 2 wherein said film controlling agent constitutes approximately 1% to 20% by weight of the preparation.

4.

An aerosol, preparation according to claim 2 or claim 3 wherein said film controlling agent is from the class consisting of mineral oils having boiling points of 300°F., glycols having an initial boiling point above 350°F., glycol ethers having initial boiling points above 350°F. and aromatic blends; with initial boiling points above 360°F<

5. An aerosol preparation according to claim 3 wherein the active ingredient and the water jointly constitute more than 50% by weight of the preparation.

6. An aerosol preparation according to claim 5 wherein said propellant is from the class consisting of liquefied hydrocarbons and halocarbons, compressed gases, and combinations thereof.

7. An aerosol preparation according to claim 6 wherein said active ingredient is not in a pre-emulsified state, and said cocodiethanolamide is within the range of 2.5% to 10% by weight of the preparation,

8. An aerosol preparation according to claim 6 wherein said active ingredient is pre-emulsified, and said cocodiethanolamide is within the range of 0.5% to 10% by weight of the preparation.

9, An aerosol preparation according to claim 6 wherein said active ingredient is pre-emulsified in an unstable emulsion, and said cocodiethanolamide is in an amount sufficient to exceed stabilization of said emulsion by at least 0.5% by weight of the preparation.

10, An aerosol preparation according to claim 3 wherein said propellant is from the class consisting of liquefied hydrocarbons and halocarbons, said propellant constituting approximately 5% to 30% by weight of the preparation.

11, An aerosol preparation according to claim 10 wherein said cocodiethanolamide is within the range of 2.5% to 10% by weight of the preparation.

12. An aerosol preparation according to claim 3 wherein said propellant is from the class consisting of compressed gases, said propellant constituting approximately 2% to 5% by weight of the preparation.

13, An aerosol preparation according to claim 3 wherein said propellant is a combination of compressed gases and a liquefied hydrocarbon or halocarbon, said propellant constituting approximately 3.1% to"35% by weight of the preparation wherein the gaseous component does not exceed approximately 5% and said liquefied component does not exceed approximately 30%.

14. An aerosol preparation according to claim 1 wherein the active ingredient comprises the active phase of water- base paints, waxes, greases, polysiloxanes, alkyl poly-^' siloxanes and polyorganosiloxanes, polybutene, petroleum based hydrocarbon oils, and synthetic oils, methoxy polyethylene glycols, water soluble resins, water soluble herbicides and water soluble alkyl glycols and alkyl esters encompassing butoxylated and ethoxylated groups.

OA-. WIP

15. An aerosol preparation according to claim 14 wherein the active ingredient constitutes approximately .1% to 50% by weight of the preparation,

16,

An aerosol preparation according to claim 15 wherein the film controlling agent is from the class consisting of mineral oils having boiling points of 300°F. , glycols having an initial boiling point above 350°F., glycol ethers having initial boiling points above 350°F. and aromatic blends with initial boiling points above 360°F.

17, An aerosol preparation according to claim 16 wherein the film controlling agent constitutes approximately 1% to 20% by weight of the preparation.

18, - An aerosol preparation according to claim 7 wherein the active ingredient comprises waxes, greases, poly- siloxanes, alkyl polysiloxanes and polyorganosiloxanes, polybutene, petroleum based hydrocarbon oils, and synthetic oils, methoxy polyethylene glycols, water soluble resins, water soluble herbicides and water soluble alkyl glycols and alkyl esters encompassing butoxylated and ethoxylated groups,

19.

An aerosol preparation according to claim 8 wherein the active ingredient comprises the active phase of waterbase paints and the following in emulsions: waxes, greases, polysiloxanes, alkyl polysiloxanes and poly- organosiloxanes, polybutene, petroleum based hydrocarbon oils, and synthetic oils.

20. An aerosol preparation according to claim 1 wherein the active ingredient is a water soluble compound from the class consisting of methoxy polyethylene glycols, water soluble resins, water soluble herbicides and water soluble alkyl glycols and alkyl esters encompassing butoxylated and ethoxylated groups.

O PI _ ^RNAT-G_

21, An aerosol preparation according to claim 20 wherein the film controlling agent is from the class consisting of mineral oils having boiling points of 300°F. , glycols havi an initial boiling point above 350°F., glycol ethers havin initial boiling points above 350°F. and aromatic blends wi initial boiling points above 360°F., said film controlling agent constituting 1% to 20% by weight of the preparation.

22. An aerosol preparation according to claim 1 wherein the active ingredient is from the class consisting of wate insoluble compounds comprising the active phase of water-b paints, waxes, greases, polysiloxanes, alkyl polysiloxanes and polyorganosiloxanes, polybutene, petroleum based hydrocarbon oils, and synthetic oils, said active ingredie constituting approximately .1% to 50% by weight of the preparation-

23. An aerosol preparation according to claim 1 wherein the active ingredient is from the class consisting of wate soluble and water insoluble compounds in the form of liqui and flowable powders.

24. An aerosol preparation according to claim 1 wherein the active ingredient is from the class consisting of wate insoluble compounds in emulsions comprising the active pha of water-base paints, waxes, greases, polysiloxanes, alkyl polysiloxanes and polyorganosiloxanes, polybutene, petrole based hydrocarbon oils, and synthetic oils, the film controlling agent is in an amount constituting approximate 1% to 20% by weight of the preparation, the propellant is from the class consisting of liquefied hydrocarbons and halocarbons constituting approximately 5% to 30% by weight of the preparation and the cocodiethanolamide is within the range of 0.5% to 10% by weight of the preparation.

25, An aerosol preparation according to claim 24 wherein the film controlling agent is from the class consisting of mineral oils having boiling points of 300°F. , glycols having an initial boiling point above 350°F., glycol ethers having initial boiling points above 350°F. and aromatic blends with initial boiling points above 360°F., and the water is within the range of 0 to 92,5% by weight of the preparation.

26. An aerosol preparation according to claim 1 wherein the active ingredient is from the class consisting of water insoluble compounds in emulsions comprising the active phase of water-base paints, waxes, greases, polysiloxanes, alkyl polysiloxanes and polyorganosiloxanes, polybutene, petroleum based hydrocarbon oils, and synthetic oils, the film controlling agent is in an amount constituting approximately 1% to 20% by weight of the preparation, the propellant being a compressed gas and constituting approximately 2% to 5% by weight of the preparation and the cocodiethanolamide is within the range of 0.5% to 10% by weight of the preparation.

27. An aerosol preparation according to claim 24 wherein the film controlling agent is from the class consisting of mineral oils having boiling points of 300°F., glycols having an initial boiling point above 350°F., glycol ethers having initial boiling points above 350°F. , and aromatic blends with initial boiling points above 360°F., and the water is within the range of 0 to. 89.5% by weight of the prepara- tion.

28. An aerosol preparation according to claim 1 wherein the active ingredient is from the class consisting of water insoluble compounds in emulsions comprising the active phase of water-base paints, waxes, greases, polysiloxanes, alkyl polysiloxanes and polyorganosiloxanes, polybutene, petroleum based hydrocarbon oils, and synthetic oils, the film controlling agent is in an amount constitut approximately 1% to 20% by weight of the preparation, the propellant constituting a combination of compressed gases and a liquefied hydrocarbon or halocarbon, said propellant constituting approximately 3.1% to 35% by weight of the preparation wherein the gaseous component does not exceed approximately 5% and said liquefied component does not exceed approximately 30%.

-29- An aerosol preparation according to claim 24 wherein the film controlling agent is from the class consisting of mineral oils having boiling points of 300°F., glycols having an initial boiling point above 350°F., glycol ether having initial boiling points above 350°F. and aromatic blends with initial boiling points above 360°F., and the water is within the range of 0 to 89,3% by weight of the preparation.