US2274509A - Wax dispersion and method of preparing same - Google Patents
Wax dispersion and method of preparing same Download PDFInfo
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- US2274509A US2274509A US268783A US26878339A US2274509A US 2274509 A US2274509 A US 2274509A US 268783 A US268783 A US 268783A US 26878339 A US26878339 A US 26878339A US 2274509 A US2274509 A US 2274509A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/06—Other polishing compositions
- C09G1/08—Other polishing compositions based on wax
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- This invention relates to water dispersions of wax for use as a protective and lustre giving agent on various surfaces. such as wood or linoleum floors or lacquered surfaces such as automobile bodies and is. a continuation in part of my application Serial No. 42,462, filed September 27, 1935.
- Wax dispersions for floorv use are well known
- Still further objects of the invention are to provide an agent for emulsifying the wax content of the coating which forms only a small quantity of soap that is compatible with the finished product; and whichmay be allowed to remain therein without injuring. itsclarity or water resisting properties; to provide in a coating of this kind a dispersion of casein which, when the coating is semis insoluble in water; to provide volatile agents for bringing about a solution of casein in water and subsequently precipitating it in a-iinely di vided insoluble: state respectively so that the casein can be dispersed throughout the wax consatisfactory substitution tor the standard pests waxes.
- One of the main objects of the invention is to produce a was dispersion which within a comparatively short timeafter application will be permanently and. absolutely waterproof; so that water spilled on a floor will not spot it and the wax finish on an automobile will. moths spotted or streaked by rain.
- Another object is to provide a, wax dispersion which will dry with a finish sumciently bright and transparent so that it produce upon an tomobile body, merely upon drying and without any rubbing whatever, an eflect at least equal to that obtained from the rubbed paste waxes tor merly used.
- Another object is to provide a wax"; dispersion which will age rapidly, so that the izz tel-val between time of application and exposure to water need be at the most a matter oisay' three hours. 7
- Another object is to provide a was dispersion which has the correct surface tension so that when it is applied to a clean surface it will lie smoothly, without leaving any irregularities;
- the preparation ol 2. was: dispersion for use upon floors is a much less exacting task than preparation oi 2, dispersion for as a coumble for lacquered finishes. of these finishes and the necessity of having per feet transparency of the was in order alter the color melee the problem considerably more difilcult, since the grain and irregularities of the floor and the loci: of perfection of he as compared with the lacquered surface mash. irregularities in'the wax coating. For use on wood floors a slight lack of transparency an a slight color in the was: may even be desirable that there is no difilculty with lap marks where I i the applicator passes twice over the same spot;
- Another'obiect is to provide an improved applicator and a method of applying the dispersion
- the waxes and fatty acids employed are not, in the form in which they can be bought commercially, definite chemical compounds. On the contrary. they are The evenness oi texture mixtures of various waxes or of fatty acids, varying in proportions and in purity according to the source from which they are'obtained and even difi'ering when bought from the same source of supply at different times. While the practice of the invention requires a nice balance between the several ingredients it is not a balance which can be expressed in terms of fixed proportions. Different commercial brands of oleic acid, for one example, may differ as to the amount needed in the compound by thirty or forty per cent.
- the commercial oleic acids vary widely in their specifications, and it will be understood that it is necessary to vary the alkaline reagents in accordance with the properties of the oleic acid.
- the saponification value is the closest measure of the alkali content necessary, the higher the saponification value the ance.
- the present-invention in some of its f aspects relates to anovel conception of the properbalance between the ingredients, many of which have been used previously-for similar purposes, by which results not heretofore possible have been attained. Asthe description proceeds, this balance will be indicated by numerous tests, most of them based upon the action of the film deposited from the dispersion, and the manner in which the different ingredients affect this balance will be pointed out.
- the basis of the dispersion is carnauba wax which is customarily used for polishes but which has been generally mixed with a softer wax such as parafiln. lFor both floor use and for use on lacquered surfaces, the hard film produced by carnauba wax alone is very desirable, and the present invention permits its use in this form.
- carnauba wax instead of the carnauha wax, other synthetic or natural hard waxes may be used, with the differences in result to be expected from their nature. With the waxes at present available, c'arnauba wax will be found in general to be the most satisfactory. If a non-slipping wax is desired for floors, some of the carnauba wax may be replaced by candelilla wax but some v of the luster will be sacrificed.
- the -soap forming alkali is divided between a fixed alkali and a volatile alkali.
- the fixed alkali may be composed of triethanolamine alone, but a somewhat harder and smoother film seems to be developed if triethanoiamine is used in combination with an inorganic alkali such as caustic potash.
- Triethanolamine is an extremely effective dispersion agent, and it is preferable to retain some of this material in order to' get a smooth, tough and readily obtainable emulsion.
- caustic potash By the substitution of caustic potash for a portion of the fixed alkali requirements, the irreversibility of the dispersion seems to be increased and the rapidity with which-the film becomes waterproof made greater.
- the triethanolamine seems to act also as a plasticizer,
- a volatile alkali such as ammonia is of importance in giving the desired waterproofing effect upon aging. If the soap-making alkali was altogether composed of triethanolamine, for example, thetotal alkali content would remain constant after the original water of suspension had evaporated, and the coating on the floor would show a tendency to reversibility, spotting badly when water was spilled on it. By making apart of the alkali volatile, this part will evaporate when the coating dried, and the tendency to tend to be milky, due to the incomplete dispersion of the wax in the water, and it will be flocculated on freezing so that it will be practically I proved the spreading qualities of the dispersion. 20
- these alkalis can. both be made'proper constituents of the final wax dispersiori. If formaldehyde is used as the hardening agent, somewhat more care seems to be necessary in the preparation of the'booster solution in order to prevent complete coagulation of the casein into insoluble lumps.
- shellac cut with borax may be: used, I prefer to use an ammonia cut shellac pre-- pared in accordance with the following procedure,
- this water is added 1,475 oz. 26 ammonia and 5 4 ammonia oz. wax free orange shellac.
- the mixture is stirreduntil the shellac is dissolved.
- An additional 3 oz. of shellac is then added and after it has dissolved 18 oz. of boiling water is introduced (In this and subsequent cases,
- shellac solution which should be stored in aglass container until used.
- I also preferably employ what may for convenience be referred to as a waterproofing booster,
- this booster 65 comprises an insoluble substance carried like the wax in' dispersed form and assisting the wax in film formation. I have foundthat the insoluble casein products, such as are obtained by treating an alkaline solution of casein with a precipitating i0.
- these acids can therefore be reduced in the formanner 2% oz. of the booster solution is added, previously mixed with 5% oz. of hot water.
- the total alkalinity of the dispersion is very important. If the alkalinity is too great, the waterproofing qualities of the film will be impaired, and when the product is used on a floor 1 it cannot be applied well over an underlyin coating of wax, digging into this underlying coating and rolling or balling it up. If the alkalinity is too low the dispersion will look milky due to the wax not being held properly in suspension, the wax will settle out irreversibly when the dispersion is frozen, and trouble will be met in applying the dispersion over a previously applied 'wax coating due to a tendency tocollect in drops. The best test of proper alkalinity that I have found is a slightly pink color with phenolphthaieiri.
- a strongly pink or reddish color with this indicator shows that the alkalinity is too great under ordinary conditions.
- the booster solution is arsed, as isrpreferable, the added waterproofing qualities and increased smoothness of application permits a slightly greater range of alkalinity than would otherwise be possible, and gives added protection against injury by freezing during transportation for the commercial grade used in the master formula, the amount of oleic acid can be reduced to 0.65 oz., the other materials being unchanged.
- Another variation consists in replacing the 0.65 oz. of triethanolamine in the master formula with a mixture of 0.13 oz. of caustic potash and 0.31 oz. of triethanolamine.
- the greater alkaline strength of the caustic potash permits a considerable reduction in the total alkali content, and" gives a somewhat smoother film, although it may be desirable to bring the ammonia up to 75 drops.
- some triethanolamine or an equivalent organic soap-forming base is desirable in order to obtain the maximum waterproofing efIect, and that as in the example given, the triethanolamine should be by preference at 'least equal to the caustic potash by weight for the best results.
- caustic soda may be used instead of the caustic potash, but" I believe the combination. ofcaustic. potash and triethanolamine gives the most rapid waterproofing, the highest luster and the-smoothest film.
- the master formula can be converted into an excellent waterproof floor wax, drying with a high luster,
- the titre of the oil may be chosen as desired, or stearic acid may be added to the oleic acid where extra body is desired in the finish. If desired, the entire fatty acid content or a part thereof tages as a floor wax, being waterproof and having if the commercial oleic aid used in that case is reduced to oz. and oz. of oleic acid having a titre of 10 is added; and if the final addition of water is omitted to give a slightly heavier dispersion. The other ingredients in this case remainthe same.
- Another formula having especial utility for use on wood floors isz' l Carnauba wax (only slightly refined) Oleic acid (titre about 7 C.
- the borax, shellac solution, and waterproof booster are what may be called special purpose materials, and may be varied in accordance with the emphasis which is to be placed on their several functions. do, however, vary the proportions of the remaining materials necessary to keep the dispersion in proper balance.
- the shellac and booster solutions are alkaline in reaction, and
- the manner in which the dispersed wax is applied to the surface to be treated is ofcontitre but have a highfree fatty acid content and The amounts of mula givenabove.
- oleic acid of substantially U. S. P. standard issubstituted siderable importance in obtaining the best results. Wood floors should be thoroughly cleaned,
- Morpholine is the trade name of a product which has been; in some instances, called oxazine in the chemical literature. This compound hasthe following formula:
- a wax dispersion base is first formedv preferably by heating together,6.66 .oz. of car-' nauba wax and 40 grams of oleic acid (red oil), the oleic acid, as heretofore set forth, having a lowtitre. These ingredients are melted together in a double boiler and stirred for about 4 min- -utes after which 37 grams of Morpholine are added. After stirring the resulting batch for several minutes, 30oz. of water at from 175 F. to 220 F. is slowly stirred into the melted wax and oleic acid.
- the stock shellac solution may be made in accordance with the formula heretofore set forth but for sprayable compounds it is preferred to produce the same by adding 1.75 oz. of triethanolamine to 24 oz. of. water while the latter is maintained at substantially 200 F.
- crements of 3 oz. each and 40 oz. of water is thereafter added in increments of 8 oz. each duringconstant stirring and while maintaining the batch at substantially 200 F.
- the casein compound of the protective coating may be prepared by introducing 2.068 oz. of casetion of the formaldehyde solution, the batch is again covered and allowed to stand for 22 hours at the end of which time a heavy viscous jell is formed.
- the resulting iell is then thinned by the addition of 6 oz. of water in increments of 1 oz. each which are added only as fast as the water can be absorbed and stirred in. After thorough stirring the thinned jell isallowed to stand for 1 hour and should have a-.viscosity reading of 150 to 200 seconds at 80 F. as tested by a No. 4 Ford cup.
- wax dispersion in which the shellac solution has been in corporated and theabove described casein compound may be incorporated together in any suitable manner.
- 3 oz. of the wax base dispersion containing shellac may be diluted with 12 oz. of 'water at substantially 95 F. by placing the wax dispersion in a container and slowly pouring and stirring the water 'thereinto.
- An aqueous wax dispersion for use in applying a film of wax to automobile finishes and the like comprising carnauba wax, a dispersing soap formed of oleic acid having a titre of less than 8 C., a fixed alkali'sufllcient in amount to substantially completely saponify the oleic acid, and ammonia in sumcient quantity to give to the completed dispersion a slightly alkaline reaction when tested'with phenolphthalein, a waterproofing booster comprising a dispersed insoluble casein compound, borax in sufilcient quantity to cause the dispersion to lie. down shellac.
- An aqueous wax dispersion for use in applying a film .01 wax to automobile finishes and the like comprising carnauba wax, adispersing soap formed of oleic acid having a titre of less than 8 0., a fixed alkali composed at least in part of triethanolamine and sufiicient in amount to substantially completely saponify the oleic acid, and ammonia in sufiicientquantity to give to the completed dispersion a slightly alkaline reaction when tested with phenolp'hthalein, a waterprgoofing booster comprising casein treated with an alkali and zinc sulphate, borax in sumcient quantity to cause the dispersion to lie down smoothly, and a small quantityof ammonia cut shellac,
- An aqueous wax dispersion for use inapply- 'ing a film ofrwax to wood floors comprising a hard wax, a dispersing soap formed of oleic acid having a suflicient stearic acid content to give the oleic acid a titre of 10 C. or higher, a flxed alkali in sufllcient amount to substantially completely saponify the. oleic acid, and ammonia in sufiicient quantity to give to the completed dispersion a slightly alkaline reaction when tested with phenolphthalein, and a waterproofing booster comprising casein treated with an alkali andzinc sulphate.
- An aqueous wax dispersion suitable for use on automobile finishes comprising in substantially the following proportions 'carnauba wax 6% oz., oleic acid (substantially U. .S. P. standard) 0.68 oz., caustic potash 013 oz, ammonia (26) 100 drops, borax 0,13'oz., triethanolamine 0.31 oz., shellac solution 5% 02., aqueous dispersmoothly, and a small quantity of ammonia cut sion 01 an insoluble casein compound oz. and
- carnaubawax by treating the latter with an emulsifying agent comprising a soap formed by the reaction of Morpholine and oleic acid, introducing a triethanolamine cut shellac solution into said emulsion, dispersing in the resulting mixture finely divided particles of insoluble casein derived by precipitation from a Morpholine solution of casein with a precipitating agent comprising formaldehyde, and diluting the resulting product with water to'a sprayable consistency.
- an emulsifying agent comprising a soap formed by the reaction of Morpholine and oleic acid
- introducing a triethanolamine cut shellac solution into said emulsion, dispersing in the resulting mixture finely divided particles of insoluble casein derived by precipitation from a Morpholine solution of casein with a precipitating agent comprising formaldehyde, and diluting the resulting product with water to'a sprayable consistency.
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Description
Patented Feb. 24, 1942 UNITED STATES PATENT OFFICE 2,214,509 wax msransrou arm mrrnon 0F memo same Henry 0. Thompson. Highland Pal-1;, ma.
No mam. Application April is, 1939 Serial Nassau:
This invention relates to water dispersions of wax for use asa protective and lustre giving agent on various surfaces. such as wood or linoleum floors or lacquered surfaces such as automobile bodies and is. a continuation in part of my application Serial No. 42,462, filed September 27, 1935.
Wax dispersions for floorv use are well known,
but have hitherto been subject to numerous objections aswillbepointed out below. As far as I am aware, no previous wax dispersions have been satisfactory for use on automobiles in place of the usual paste waxes. They-would not stand up under the weather conditions imposed on them in this use, spotting badly under the first rain I Commercially, wax dispersions have been nonexistent for automobile use. For use on linoleum floors certain of the prior dispersions have been generally satisfactory, except that they were not completely waterproof and were permanently injured by freezing during transportationybut no priordispersions of which I am aware have had the capability of being used on a wood floor in 8 Claims. (CI.- 106-10),
-sion of wax of this character which is of sprayable consistency; to provide a protective coating of thiskind which air cures to a hard film that is insoluble in water; and to provide aprotective coating which when cured comprises a thin even deposit which permits the luster of the under finish to show therethrough'without altering the color of the under finish.
Still further objects of the invention are to provide an agent for emulsifying the wax content of the coating which forms only a small quantity of soap that is compatible with the finished product; and whichmay be allowed to remain therein without injuring. itsclarity or water resisting properties; to provide in a coating of this kind a dispersion of casein which, when the coating is semis insoluble in water; to provide volatile agents for bringing about a solution of casein in water and subsequently precipitating it in a-iinely di vided insoluble: state respectively so that the casein can be dispersed throughout the wax consatisfactory substitution tor the standard pests waxes. One of the main objects of the invention is to produce a was dispersion which within a comparatively short timeafter application will be permanently and. absolutely waterproof; so that water spilled on a floor will not spot it and the wax finish on an automobile will. moths spotted or streaked by rain.
Another ohiect oi the ing, so that if it is frozen by transportation during" winter it will regain its original properties when thawed out.
Another object is to provide a, wax dispersion which will dry with a finish sumciently bright and transparent so that it produce upon an tomobile body, merely upon drying and without any rubbing whatever, an eflect at least equal to that obtained from the rubbed paste waxes tor merly used. another object is to provide a wax"; dispersion which will age rapidly, so that the izz tel-val between time of application and exposure to water need be at the most a matter oisay' three hours. 7
' Another object is to provide a was dispersion which has the correct surface tension so that when it is applied to a clean surface it will lie smoothly, without leaving any irregularities; and
which for this reason can be applied so rapidly invention is to provide a wax dispersion which will not be injured by freez tent of the coating and the agents maybe dis posed or? by voiatillzatiou during the final curing of the coating; and "to provide a volatile agent for facilitating the dispersion of the was com ponent of the coating in water which will also serve to render the casein soluble in water in order to avoid the addition of difierent agents for these purposes.
Additional ohiectswill appeasirom the following description-anal claims.
The preparation ol 2. was: dispersion for use upon floors is a much less exacting task than preparation oi 2, dispersion for as a coatiile for lacquered finishes. of these finishes and the necessity of having per feet transparency of the was in order alter the color melee the problem considerably more difilcult, since the grain and irregularities of the floor and the loci: of perfection of he as compared with the lacquered surface mash. irregularities in'the wax coating. For use on wood floors a slight lack of transparency an a slight color in the was: may even be desirable that there is no difilculty with lap marks where I i the applicator passes twice over the same spot;
Another'obiect is to provide an improved applicator and a method of applying the dispersion,
particularly upon lacquered surfaces like that or an automobile body,
Further objects of the 'vention are to provide a protective coating comprising a water disper order to darken any light places in the iioor and to produces coating having more apparent For these reasons the invention will first he scribed in its preferred and refined form suitable for use as an automobile wax, and the changes which may be made for floor use will then be indicated. It should be understood, however, that the preferred form of the invention is applicable unchanged as a floor wax, although. in many cases it is preferable for this use to decrease the water content in order to increase the thickness of the deposited'wax coating.
One other prefatory remark is necessary concerning the ingredientsused. The waxes and fatty acids employed are not, in the form in which they can be bought commercially, definite chemical compounds. On the contrary. they are The evenness oi texture mixtures of various waxes or of fatty acids, varying in proportions and in purity according to the source from which they are'obtained and even difi'ering when bought from the same source of supply at different times. While the practice of the invention requires a nice balance between the several ingredients it is not a balance which can be expressed in terms of fixed proportions. Different commercial brands of oleic acid, for one example, may differ as to the amount needed in the compound by thirty or forty per cent. The proportions of the ingredients given, therefore, must be takenas illustrative only; and reference must be made to the general principles indicated below for a guide to the determination of the exact quantity needed for the particular commercial materials used. Furthermore, as the composition of any one ingredient varies commercially, it may require changes in the other ingredients in order to preserve the proper balsirable to employ a volatile alkali such as ammonia. as this will evaporate during the aging period and if the proper proportions have been used, as will be pointed out below, will render the dispersion irreversible once it has been set. As has been pointed out above, the commercial oleic acids vary widely in their specifications, and it will be understood that it is necessary to vary the alkaline reagents in accordance with the properties of the oleic acid. The saponification value is the closest measure of the alkali content necessary, the higher the saponification value the ance. The present-invention in some of its f aspects relates to anovel conception of the properbalance between the ingredients, many of which have been used previously-for similar purposes, by which results not heretofore possible have been attained. Asthe description proceeds, this balance will be indicated by numerous tests, most of them based upon the action of the film deposited from the dispersion, and the manner in which the different ingredients affect this balance will be pointed out.
The basis of the dispersion is carnauba wax which is customarily used for polishes but which has been generally mixed with a softer wax such as parafiln. lFor both floor use and for use on lacquered surfaces, the hard film produced by carnauba wax alone is very desirable, and the present invention permits its use in this form.
If the product'is to be used on a linoleum fioor or on lacquered surfaces, transparency and comparative neutrality as to colorv are important in order not to mask or alter the clear color of the surface towhich the wax is applied; and wax of a good grade should be used. If, on the other hand, the product is to be used on a wood floor, a wax of higher color and less transparency is sometimes more desirable in order to make a 'better showing on the floor and to color up worn spots. I have found, moreover, that some of the cheaper and therefore more highly colored camauba waxes apparently contain some fatty acids and therefore affect the proportions of the fatty acids and alkalis used in the remainder of the formula; and that certain impurities which they contain may cause trouble from fermentation. It is generally desired, therefore, to use what is generally referred to as a pure refined carnauba wax. Instead of the carnauha wax, other synthetic or natural hard waxes may be used, with the differences in result to be expected from their nature. with the waxes at present available, c'arnauba wax will be found in general to be the most satisfactory. If a non-slipping wax is desired for floors, some of the carnauba wax may be replaced by candelilla wax but some v of the luster will be sacrificed.
less the oleic acid which has to be used to produce the necessary emulsifying soap. The change in the amount of oleic acid required is not strictly proportional to the saponification value, butthe requisite amounts can readily be determined by the application of the tests given below.
The -soap forming alkali, as stated above, is divided between a fixed alkali and a volatile alkali. The fixed alkali may be composed of triethanolamine alone, but a somewhat harder and smoother film seems to be developed if triethanoiamine is used in combination with an inorganic alkali such as caustic potash. Triethanolamine is an extremely effective dispersion agent, and it is preferable to retain some of this material in order to' get a smooth, tough and readily obtainable emulsion. By the substitution of caustic potash for a portion of the fixed alkali requirements, the irreversibility of the dispersion seems to be increased and the rapidity with which-the film becomes waterproof made greater. The triethanolamine seems to act also as a plasticizer,
, making the resulting coating much less brittle and giving it less tendency to peel ofl than if the entire alkali content were ofamaterial such as caustic potash. If too much triethanolamine in proportion to the oleic acid is used, the dispersion will not spread evenly and the waterproof qualities of the film will be impaired. If too little is used the luster will be diminished and also there will be too little alkalinity to cause the dispersion to spread over a previously waxed floor.
Proper spreading may be due to a slight cutting viously.
The useof a volatile alkali such as ammonia is of importance in giving the desired waterproofing effect upon aging. If the soap-making alkali was altogether composed of triethanolamine, for example, thetotal alkali content would remain constant after the original water of suspension had evaporated, and the coating on the floor would show a tendency to reversibility, spotting badly when water was spilled on it. By making apart of the alkali volatile, this part will evaporate when the coating dried, and the tendency to tend to be milky, due to the incomplete dispersion of the wax in the water, and it will be flocculated on freezing so that it will be practically I proved the spreading qualities of the dispersion. 20
.tinuing the churning, 1 oz. of 26 ammonia is added slowly in athin stream, 0.8 oz. of zinc sulphate dissolved in 2 oz. of boiling water, and finally cations such as on an automobile.
I assume alkali to bring the dispersion substantially to neutrality and adding enough volatile alkalito carry the dispersion over into an alkaline reaction' when tested with plieneipliuialein. Prefer- I ably the reaction with this indicator shouldprothe use of this agent the hardening and preduce a slight pink color, and not a definite red;
although with the waterproof booster hereinafter described, the range of permissible alkalinity on both the high and low sideis somewhat greater.
In addition to the fatty acid and the basic mathe wax, I preferably use other materials having specific effects in the film depositing action of the dispersion. I have found, for example, that the addition of a small quantity of boraxrim- Without the borax there is a tendency to show theequivalent of brush .hrarks, or for the de posited film to be otherwise irregular in'thickness. The use of borax counteracts this tendteriafusedfor obtaining a dispersing soap, for
cipitating of the casein from alkaline solution can be carried on under such complete control that the precipitated casein compound will be retained in dispersed form in the solution. By using caustic potash andammonia as the alkaline reagents, it will be unnecessary to remove them before adding the precipitated casein compound to the wax dispersion since, as elsewhere pointed out,
these alkalis can. both be made'proper constituents of the final wax dispersiori. If formaldehyde is used as the hardening agent, somewhat more care seems to be necessary in the preparation of the'booster solution in order to prevent complete coagulation of the casein into insoluble lumps.
One way in whichsuch a booster solution may be madewill now be given. To one quart of cold I water is added 5 oz. of casein. To this mixture,
while being churned, is added 0.5 oz. caustic potash dissolved in 2 oz. of hot water; While con- 0.25 oz. of steam distilled yellow pine 011. These ency, and produces a dispersion whichismore easily distributed into even form and therefore I produces a flatter and harder film.
Asan assistance in obtaining a high luster, and to some extent in securing a waterproof film, I
prefer to use a small amount of shellac in aqueous dispersion. While, shellac cut with borax may be: used, I prefer to use an ammonia cut shellac pre-- pared in accordance with the following procedure,
since ammonia cut shellac appears to give a smoother and more waterproof final film. In
this water is added 1,475 oz. 26 ammonia and 5 4 ammonia oz. wax free orange shellac. The mixture is stirreduntil the shellac is dissolved. An additional 3 oz. of shellac is then added and after it has dissolved 18 oz. of boiling water is introduced (In this and subsequent cases,
in a thin stream while the mixture is being 40 stirred. To this mixture 4 oz. additional of similar flake shellac is added and stirred until all the shellac is dissolved. Finally 22 oz. of boiling water is added gradually whilethe mixture is being stirred. The procedure outlined will produce what will be referred to hereinafter as shellac solution, which should be stored in aglass container until used.
I also preferably employ what may for convenience be referred to as a waterproofing booster,
which has in practice given the product exceptional waterproofing properties particularly useful where the wax is. to be applied in exposed lo- For wood floor work, these requirements are not so severe so,
and the booster may be omitted, but I prefer to use it in all cases since it seems not only to give remarkable waterproofing properties but to improve the film formation of the dispersion in many ways. In its preferred form, this booster 65 comprises an insoluble substance carried like the wax in' dispersed form and assisting the wax in film formation. I have foundthat the insoluble casein products, such as are obtained by treating an alkaline solution of casein with a precipitating i0.
as the precipitating and waterproofing material.
materials should be addedslowly while churning at a slow speed, and when the mass reaches the consistency of thick pudding 10 oz. of cold water are added. The resulting produce will be referred to hereinafter as the boostersolution.
If instead of zinc sulphate, formaldehyde is used as a hardening agent the same general procedure is followed except that it is desirable to add the pine oil before the formaldehyde instead of at the end in order to slow down the rapidity of the hardening reaction. The proportions are as follows:
Cold water quarts 1 Casem ounces ,5 Caustic potash do 0.5
Pine oi i do 0.25 Formaldehyde (40% solution in 2 oz. water drops 75 Cold water ounces 12 I will now describe the manner ofmaking one form. of dispersion suitable for floors. It is preferred to make the floor compound with a higher solid content in order to give additionalbody-to the coat even at the expense of the great smoothness which is given by'the degree of dilution in the automobile wax formula. It is preferred pound, intended for floors.
-To make the floor wax dispersion in its preferred form 6% oz. of #srefined camau wax is melted in a steam jacketed kettle and oz. of oleic acid added in a thin stream while stirring. The oleic acid which was used in this example had an iodine value of 92/94, a saponification value'of 492/ 196, a titre of 5/8 C., an acid value of 192/196 and a free fatty acid content of 96/98%. The mixture of oleic acid and wax is stirred for two minutes and 0.6.5 oz. of triethanolamine is then added. To this mixture is added in a thin stream and during churning 0.13 oz; powdered borax. dissolved in 3 oz. of hot water and 75 drops of 26 ammonia (equivalent to about.0.l5 oz.). Boiling water to the-total amount of 26 oz. is then' added slowly. The shellac solution referred to above isthen added slowly while the mixture is being churned, 5% oz. of the shellac solutionbeing diluted with 5% oz. of water before being added. "In a similar a high saponification value. v
these acids can therefore be reduced in the formanner 2% oz. of the booster solution is added, previously mixed with 5% oz. of hot water.
The total alkalinity of the dispersion is very important. If the alkalinity is too great, the waterproofing qualities of the film will be impaired, and when the product is used on a floor 1 it cannot be applied well over an underlyin coating of wax, digging into this underlying coating and rolling or balling it up. If the alkalinity is too low the dispersion will look milky due to the wax not being held properly in suspension, the wax will settle out irreversibly when the dispersion is frozen, and trouble will be met in applying the dispersion over a previously applied 'wax coating due to a tendency tocollect in drops. The best test of proper alkalinity that I have found is a slightly pink color with phenolphthaieiri. A strongly pink or reddish color with this indicator shows that the alkalinity is too great under ordinary conditions. When the booster solution is arsed, as isrpreferable, the added waterproofing qualities and increased smoothness of application permits a slightly greater range of alkalinity than would otherwise be possible, and gives added protection against injury by freezing during transportation for the commercial grade used in the master formula, the amount of oleic acid can be reduced to 0.65 oz., the other materials being unchanged. Another variation consists in replacing the 0.65 oz. of triethanolamine in the master formula with a mixture of 0.13 oz. of caustic potash and 0.31 oz. of triethanolamine. The greater alkaline strength of the caustic potash permits a considerable reduction in the total alkali content, and" gives a somewhat smoother film, although it may be desirable to bring the ammonia up to 75 drops. I believe, however, that some triethanolamine or an equivalent organic soap-forming base is desirable in order to obtain the maximum waterproofing efIect, and that as in the example given, the triethanolamine should be by preference at 'least equal to the caustic potash by weight for the best results. If desired, caustic soda may be used instead of the caustic potash, but" I believe the combination. ofcaustic. potash and triethanolamine gives the most rapid waterproofing, the highest luster and the-smoothest film. The master formula can be converted into an excellent waterproof floor wax, drying with a high luster,
In the master formula given above, changes may be made in accordance with the-nature of the raw materials'used and the'properties of the dispersion which itis desired to emphasize. {A
few of these changes will be indicated here, further changes being readily made bythose skilled to use oleic acid having a low titre, since a thin hard film is desired and the stearic acid in substantial quantities has a tendency to thicken the film and apparently to dull slightly the luster on drying. For. use on wood floors, however, the additional body given by the stearic acid affords a much better appearance, as long as the stearic acid content is not carried to such a degree that the hardness or luster of the film is sacrificed. On automobile work, I have used successfully an oleic acid with a titre as low as 4", and on floors an oleic acid with a titre of 10 or higher ,produces excellent results. For different uses the titre of the oil may be chosen as desired, or stearic acid may be added to the oleic acid where extra body is desired in the finish. If desired, the entire fatty acid content or a part thereof tages as a floor wax, being waterproof and having if the commercial oleic aid used in that case is reduced to oz. and oz. of oleic acid having a titre of 10 is added; and if the final addition of water is omitted to give a slightly heavier dispersion. The other ingredients in this case remainthe same. Another formula having especial utility for use on wood floors isz' l Carnauba wax (only slightly refined) Oleic acid (titre about 7 C. and saponification value about 196) ounces 0.70 Stearic acid (triple pressed) do 0.08 Triethanolamine do 0.65 26 ammonia drops "75 Borax, in 3% oz. water ounces 0.20 Water do 26 Shellac solutionin 5 /4 oz. water do 5 /8 Booster solution in 5% oz. water do- 2% The final addition of water is here omitted.
If the ammonia content is varied it will be in most cases necessary to vary the other alkaline materials so that the total alkalinity remains substantially constant. The borax, shellac solution, and waterproof booster are what may be called special purpose materials, and may be varied in accordance with the emphasis which is to be placed on their several functions. do, however, vary the proportions of the remaining materials necessary to keep the dispersion in proper balance. In particular, the shellac and booster solutions are alkaline in reaction, and
a heavy body with some now-slipping properties.
thus, will directly aflect the amount of other al kali which it is necessary to have in the dispersion. Where a suillcient amount of the booster solution is added, it is possible to omit the am- I monia entirely and still have a, substantially waterproof film. This is apparently due to the protection given to the wax film by the insoluble casein compound. I prefer, however, to use the ammonia, as a. product which ages to a definitely waterproof condition is thereby produced.
The manner in which the dispersed wax is applied to the surface to be treated is ofcontitre but have a highfree fatty acid content and The amounts of mula givenabove. As an example, if oleic acid of substantially U. S. P. standard issubstituted siderable importance in obtaining the best results. Wood floors should be thoroughly cleaned,
preferably with one of the non-explosive petroleum distillates used for dry cleaning. It will not be necessary to remove underlying coatings of wax, even when this is of the paste type, as when properly prepared the dispersed war will lie They l 1 fying agent for dispersing the wax which likewise includes substantially no reagents that remain in the finished film after curing and which have a detrimental effect thereon.
. I have'iound that sufficiently large proportions of casein can be introduced into the wax dispersion when Morpholine is used as the'alkaline reagent by which the emulsifying soap is formed from oleic. acid and as the reagent. for producing a solution of the casein in water prior to its precipitation.
Morpholine is the trade name of a product which has been; in some instances, called oxazine in the chemical literature. This compound hasthe following formula:
i on. CH: Ha. H:
The following procedure has-been found to produce commercially successful sprayable coat- While the specific proportions .of the ingredients involved may ing material of this character.
be varied somewhat, it is particularly desirable to include a large insoluble casein content with- ,out introducing into the product excessive quantitles of the reagents used to facilitate the dispersion of wax and incorporation of insoluble casein therein which have harmful effects upon the air cured film. v
In manufacturing the sprayable coating composition a wax dispersion base is first formedv preferably by heating together,6.66 .oz. of car-' nauba wax and 40 grams of oleic acid (red oil), the oleic acid, as heretofore set forth, having a lowtitre. These ingredients are melted together in a double boiler and stirred for about 4 min- -utes after which 37 grams of Morpholine are added. After stirring the resulting batch for several minutes, 30oz. of water at from 175 F. to 220 F. is slowly stirred into the melted wax and oleic acid. Since the addition of water to the melted wax and oil produces an amber colored jell, precaution should-be taken to add the water slowly enough to avoid clouding of the dell. The contents of the kettle are removed from the boiler and allowed to cool to substantially 150 'F. to 185 F. at which. time the emulsion takes on a dark' coloration.
To the above wax dispersion is-added cutshellac solution preferably formed in a manner hereinafter set forth and referred to as a stock shellac solution. To 12 oz. of this stock shellac solution is added 9 oz. of water which is heated to substantially 175 F. This diluted stool: solution is then slowly pouredwhile stirring into the previously formed wax dispersion. Then 18 oz.
- of waterat substantially 130 F. are added.
The stock shellac solutionmay be made in accordance with the formula heretofore set forth but for sprayable compounds it is preferred to produce the same by adding 1.75 oz. of triethanolamine to 24 oz. of. water while the latter is maintained at substantially 200 F.
crements of 3 oz. each and 40 oz. of water is thereafter added in increments of 8 oz. each duringconstant stirring and while maintaining the batch at substantially 200 F. v
The casein compound of the protective coating may be prepared by introducing 2.068 oz. of casetion of the formaldehyde solution, the batch is again covered and allowed to stand for 22 hours at the end of which time a heavy viscous jell is formed. The resulting iell is then thinned by the addition of 6 oz. of water in increments of 1 oz. each which are added only as fast as the water can be absorbed and stirred in. After thorough stirring the thinned jell isallowed to stand for 1 hour and should have a-.viscosity reading of 150 to 200 seconds at 80 F. as tested by a No. 4 Ford cup. The foregoing wax dispersion in which the shellac solution has been in corporated and theabove described casein compound may be incorporated together in any suitable manner. 'Asone example, 3 oz. of the wax base dispersion containing shellac may be diluted with 12 oz. of 'water at substantially 95 F. by placing the wax dispersion in a container and slowly pouring and stirring the water 'thereinto.
' The above proportions of diluted .wax base are slowly poured into oz. of the casein compound above described during constant stirring. The resulting product is of sprayable consistency and may be applied in-the form of a thin film by any suitable spray device and allowed to air cure. During air curing the volatile ingredients includingany excess Morpholine introduced during solution of casein is eliminated by vaporization leaving a clear luster revealing protective coating on the surface on which it was applied. The casein content not only increases the wetting properties of the coating and facilitates the spraying thereof but also hardens the final film. The shellac alsoserves to harden the film and improve the gloss thereof and tends to stabilize the emulsion.
Although but several specific embodiments of the invention are shown, it is to be understood that various changes in the materials employed and in the sequence of steps, as well as in the temperatures .and periods of heating, may be 12 oz. of flake wax free shellac is then introduced in-inininto 8 oz. of water at room temperature dur- 7 invention.
made without departing from the spirit of the I claim:
1. An aqueous wax dispersion for use in apply- 4 ing a film of waxv to automobile finishes and the like, comprising carnauba wax, a dispersing soap formed of oleic acid having a titre'of less than 8 C. a fixed alkali sufficient in amount to-sub-' stantially completely saponify the oleic acid, and ammonia in sufficient quantity to give to the completed dispersion a slightly alkaline reaction when tested with phenolphthalein, and a waterproofing booster comprising a dispersed insoluble casein compound.
2. An aqueous wax dispersion for use in applyinga film of wax to automobile finishes and the like, comprising carnauba wax, a dispersing soap formed of oleic acid having a titre of less than 8 C., a fixed alkali'sufllcient in amount to substantially completely saponify the oleic acid, and ammonia in sumcient quantity to give to the completed dispersion a slightly alkaline reaction when tested'with phenolphthalein, a waterproofing booster comprising a dispersed insoluble casein compound, borax in sufilcient quantity to cause the dispersion to lie. down shellac.
3. An aqueous wax dispersion for use in applying a film .01 wax to automobile finishes and the like, comprising carnauba wax, adispersing soap formed of oleic acid having a titre of less than 8 0., a fixed alkali composed at least in part of triethanolamine and sufiicient in amount to substantially completely saponify the oleic acid, and ammonia in sufiicientquantity to give to the completed dispersion a slightly alkaline reaction when tested with phenolp'hthalein, a waterprgoofing booster comprising casein treated with an alkali and zinc sulphate, borax in sumcient quantity to cause the dispersion to lie down smoothly, and a small quantityof ammonia cut shellac,
a. An aqueous wax dispersion for use inapply- 'ing a film ofrwax to wood floors comprising a hard wax,a dispersing soap formed of oleic acid having a suflicient stearic acid content to give the oleic acid a titre of 10 C. or higher, a flxed alkali in sufllcient amount to substantially completely saponify the. oleic acid, and ammonia in sufiicient quantity to give to the completed dispersion a slightly alkaline reaction when tested with phenolphthalein, and a waterproofing booster comprising casein treated with an alkali andzinc sulphate.
5. An aqueous wax dispersion suitable for use on automobile finishes comprising in substantially the following proportions 'carnauba wax 6% oz., oleic acid (substantially U. .S. P. standard) 0.68 oz., caustic potash 013 oz, ammonia (26) 100 drops, borax 0,13'oz., triethanolamine 0.31 oz., shellac solution 5% 02., aqueous dispersmoothly, and a small quantity of ammonia cut sion 01 an insoluble casein compound oz. and
desired consistency.
7. The method of making an aqueous dispersion of wax comprising melting together came-aha wax and a soap-forming acid, adding an alkali consisting of an organic base selected from the group of organic bases consisting of triethanoh amine and Morpholine, diluting with water, adding an aqueous dispersion of an alkali out shellac,
addingan aqueous dispersion of an insoluble casein compoundand diluting with water to the desired consistency.
8. 'The method of making a sprayable coating material which comprises emulsifying in water,
carnaubawax by treating the latter with an emulsifying agent comprising a soap formed by the reaction of Morpholine and oleic acid, introducing a triethanolamine cut shellac solution into said emulsion, dispersing in the resulting mixture finely divided particles of insoluble casein derived by precipitation from a Morpholine solution of casein with a precipitating agent comprising formaldehyde, and diluting the resulting product with water to'a sprayable consistency.
, HENRY c. Thom-son.
Priority Applications (1)
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US268783A US2274509A (en) | 1939-04-19 | 1939-04-19 | Wax dispersion and method of preparing same |
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US268783A US2274509A (en) | 1939-04-19 | 1939-04-19 | Wax dispersion and method of preparing same |
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US2274509A true US2274509A (en) | 1942-02-24 |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2423137A (en) * | 1944-08-24 | 1947-07-01 | Glenn P Beach | Cleaning and preserving composition |
US2859123A (en) * | 1953-04-17 | 1958-11-04 | Simoniz Co | Wax and shellac polishing composition |
US2928752A (en) * | 1956-09-15 | 1960-03-15 | Dehydag Gmbh | Paraffin emulsions for protection of masonry surfaces during setting |
US2964487A (en) * | 1958-01-27 | 1960-12-13 | Allied Chem | Wax emulsion polish |
-
1939
- 1939-04-19 US US268783A patent/US2274509A/en not_active Expired - Lifetime
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2423137A (en) * | 1944-08-24 | 1947-07-01 | Glenn P Beach | Cleaning and preserving composition |
US2859123A (en) * | 1953-04-17 | 1958-11-04 | Simoniz Co | Wax and shellac polishing composition |
US2928752A (en) * | 1956-09-15 | 1960-03-15 | Dehydag Gmbh | Paraffin emulsions for protection of masonry surfaces during setting |
US2964487A (en) * | 1958-01-27 | 1960-12-13 | Allied Chem | Wax emulsion polish |
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