US1109119A - Solidified oil and process of making same. - Google Patents

Description

o the pine riyed'.

' deeto the and similar material and the is mixed with soap solutions,

put pine oil and similar oils into a UNITED STATES rATEuT orricn.

CABLET ON ELLIS, OF MONTCLAIR, NEW JERSEY, ASSIGNOR TO ELLIS-FOSTER COMPANY, A CORPORATION OF NEW JERSEY.

SOLIDIFIED OIL AND PROCESS OF MAKING SAME.

1,109,119. No Drawing.

Speciflcation of Letters Patent. Application flledliarch 29, 1910. Serial No. 552,177.

Patented Sept. 1, 1914.

To all whom it may concern Be it known that I, CARLETON ELLIS, a citizen of the United States, residing at Montclair, in the county of Essex and State of New Jersey, have invented certain new and useful Improvements in Solidified Oils and Processes of Making Same, of which the following is a specification.

T hisinvention relates to solidified oil compositions and to the process of making same and relates particularly to the solidified pine oilsmade from long leaf pine oil products solid product derived from cresylic acid and similar carbolic acid material. Ordinary pine oil, for example, is, a liquid insoluble'in water and having no power of itself of readily emulsifying with water. If however, the pine oil emulsions may be obtained. By the use of concentrated soaps, such as oleate of potash, the pine oil becomes more or less miscible with water and certain preparations known as soluble pine oils which are of this character are now on the market.

The objeect of the present invention is to solid form and particularly into a form in which they are only slightly soluble in water, but which by the action of water, become slowly soluble or miscible thus becoming capable of distributing themselves in fine particles throughout .a large body of water. The ordinary long leaf pine oil may be solidified by the incorporation with it of stearic acid and subsequent addition of caustic soda, to produce a soap in a concentrated condition. In the absence of more than a very small amount of water, practically that amount which just sufiices to put the caustic soda in solution, and at an elevated temperature, oil dissolves the sodium stearate, and on cooling. solidifies to a hard solid materiali 0n the other hand if oleic acid is used with caustic potash, for example, as the saponifying agent, a liquid material is de- This is usually of a dark grown color use of red oil or commercial oleic acid, while the stearic acid products areusually white and even transparent if the proportion of stearic acid soap is not too great and if the temperature has been tained however if As an illustration to 14 pounds of, pinc Oil and 1 pound of stearic acid commingled ao and incorporated by heat,'wlien thestearic acid has thoroughly dissolved in the pine 01], 35 pound caustic soda dissolved in slightly more than its own weight of water is added and the mixture stirred thoroughly, the heating being carried up preferably nearly to the boiling point of the pine oil in order to secure proper incorporation. At temperatures of for example, 40 or 50 C., a sort of coagulation occurs and a very unsatisfactory product results. If the temperature is carried to say 100 C., the. product is usually firm and somewhat opaque. If however the temperature is carridilip to nearly the boiling point of the transparent material may e produced. It is desirable however in actual practice to use steam jacketed kettles for manufacturing the product and for that reason, a temperature of 100 to 135 C. is perhaps more-feast. ble. It 1s alsodesirable, after the material has been incorporated, to chill the product so as to prevent segregation which often occurs on slow cooling. This is very readily done in a jacketed kettle by substituting cold water in the jacket for the steam previously used for heating. The product 0bdesired may be cast in molds which preferably should be chilled, and also preferably should be exposed a short time to the air or to a vacuum before shipment, in order to develop a high degree of firmness which such air or vacuum exposure tends to bring about. The pine oil product made in this manner is fairly soluble. If a small block of material is placed under running water, it may dissolve in'from 20 to 30 minutes. For'some purposes, such a high grade of solubility is undesirable and to reduce the solubility, I incorporate with the pine oil, for certain purposes, various oils suclt as refined mineral oils or crude petroleum. For example, in the above formula, if crude petroleum is substituted for one-third or'one-halfv inasmuch as large cakes of the material may I 4 t v I me 'Oll, a clear v be placed in the water and as these slowly I glve special odors or u ber dlssolve, the pine oil and crude petroleum oil spread. over the surface of the water, the insectifugal odors of the pine oil driving the mosquitoes from the neighborhood and the crude petroleum oil effectually sealing the surface of the water so as to prevent reproduction of the mosquitos. Of course, various mineral oils may be used instead of crude petroleum oil and an oil of about .865 specific gravity derived from petroleum, is a very useful material for this purpose. Waxes act in a somewhat similar manner as respects reduction of solubility but are more expensive and are therefore more limited in application. Crude paraffin wax including scale wax and the like are however fairly cheap and may be included in varying amounts to secure various degrees of solubility. For example, in the formula above mentioned, the incorporation of 25% of scale wax reduces the solubility of the material and 50% makes the product very hard and slightly soluble; with the addition of 75%, the material becomes practically too insoluble to be of any great value for most applications. On the other hand, with the addition of 50% to 75% mineral oil, very oily solid products may be secured which have certain very desirable properties. In lieu of waxes, naphthalene may be employed to a greater or less extent. For example, in the above formula comprising pine oil, stearic acid and caustic soda, 5%, 10% and upward to say 40 or 50% of naphthalene may be incorporated. With the lower percentages, very little crystallization is evident on. cooling, but with the larger percentages, crystallization is so much in evidence that the masses oftentimes are somewhat crumbly especially after water has acted upon the material for a short time. These solidified oils may be given various colors by the use of oil soluble dyes. They maybe combined if desired with filling or weighting materials as for example, if

cake heavier than water, such substances as talc, infusorial earth, oxid of iron, etc., may. be em loyed, while, if it is desired to have the caiie lighter than water, such materials as sawdust, wood flour,-s tarch', sugar and the,

like may be made use of. Also other essential oils'may be included if it is desired to .special medicinal or product. Of course, w, t degra wool grease, lanolin ,.various resins such as colophony, dammar, ianak, guayule and similar. resins, may be incorporated to a greater or less extent in accordance with the character-of the product desired for special applications.

other properties to the h d guayule'gums' containing both-the and resinous material. Metallic and for similar it is desired to have the.

I additional dar e. coral, .P nti-' Also rub: oducts particularly the crude Pontisoaps such as aluminum palmitate, zinc stearate and the like may be added as desired. I

In the solidification of creosote, toproduce a solidcomposition for preparing shee purposes, the formula may be varied as followszcresylic acid'10 pounds, stearic acigl, 1 poufdfca ustic soda 1- of a poii'lidi This gives a product of mod: erate solubility which may be rendered more soluble by the incorporation of potassium oleate or sulfonated oils. Similarly with the pine oil, should it be desired to secure an especially soluble product, sulfonatedoil in its concentrated liquid or solid forms, or potassium oleate or any similar soap material, may be introduced to advantage, care being taken to not use such proportions as to cause liquefaction.

The process may be applied to various oilssuch as oil of cedar, oil of cedar leaf, oil of camphor, oil of lemongrass and oils of birch tar, cajeput, mace. nutmeg and the like to secure a solid product. In order to produce a clear product it is desirable to heat the oil after incorporation of the soap to a temperature above the boiling point of water, until the water is eliminated, care being taken to agitate the oil well during this process as the boiling is oftentimes violent. If alcohol is used instead of water as the tion may take This is especially the case with methyl alcohol which boils at 66 C. In the case of certain essential oils which have rather low boiling points and which jection to high temperatures, the use of an alcoholic solvent is to be recommended.

In case of cresylic acid or other carbolic acid materials, the solidification may be made such that the product may be cut out into the shape of tablets for medicinal uses are injured by suband may be made so firm as to be capable of supporting a coating of some other material. The addition of a little more alkali than that actually required for the combination with the fatty acid employed is usually desirable in the solidification of cresylic acid material. In the case of pine oil as will appear from the foregoing formula, 25% of caustic soda has been used reckoned on the amount of stearic acid, while the actual Saponification requires onl about 20%.- This uantity of kali is howevennot obiectionab e andis rather desirable in or: der to rapidly complete saponification. The material may however be made substantially neutral by using the exact equivalent of alkali. The stearic acid may be replaced by still stockto advantage in some cases.

The present invention therefore involves the process of melting or incorporatin the essential oils" to be solidified, with eely saponifiable soap-forming fatty acids, adding as caustic soda, carbonate of soda, potashor whatever the alkali maybe, preferably just sufficient water the alkali in-solut-ion, combini'n fthis, preferably hot, withthe oil, prefera ly hot, carrying the freely s aponifiable fatty acid-and agitating'to effect perfect incorporation and substantial solution of the soap, referably followed by the step of heating t e oil to a temperature suflicient to expel a substantial portion or all of the water whereupon the mass preferably is rapidly chilled to insure proper setting andto overcome segregation. in -It will b evident tothose skilled in the art, from the information herein set forth, that various modificationsmay be made under the present invention to produce bodies of different proportions and suited for many '20 difierent'applications, and I do not wish to limit; myself strictly to the invention; as herein set forth and wish. to'qapply or invoke the doctrine same may be herein applicable, all in view of the present State, of the art and'with due recognition" of the heretofore employed methods or. making soluble or solidified oils in various ways, by the use in'some cases of dissolved in soaps either to produce emulsions or miscible v 50 oils in a manner foreign to the idea of the present invention, but in some cases employ i'ng'materials more orless similar in charac: ter to produce bodies having different properties or characteristics from those herein as described. The products made under my invention are characterized by their peculiar.

colloidal condition manifestmg itself 1n va rious ways. Some of the compositions here'- under for example are readily fusible when 40 first formed but become difiicultlyfusible on standing. Seemingly the soap, forming as it does in the oil itself exerts by nascent action some peculiar colloiding influence on the oil and it is probably because of this condition of nascency thatfirmer, sounder prod- -Especially does this seem ucts are obtained. a morepotendfactor after reaction is well tov maintain of equivalency so far as under way the mass is quickly chilled, therey molecular soap complexes.

' By pine oil, orpilof pine,

possibly preventing the formation of as used herein, "j I referparticularly to the'volatile oils derived from genus Pinus and more specifically refer to spirits of turpentine, Russian turpentine, and long leaf pine oil.

v.I claim:-

' I 1. The herein described firm solid insectifugal composition comprising an essential oil' and a modicum of a soap of stearic acid with sufiicient additional water -'insoluble material to substantially reduce the solubility ofthe solidified product in water, said composition being prepared at a temperature above 190 0. whereby it becomes clear and transparent.

2.,The herein de'scribed'firm, solid insectifugal composition comprising an essential oil and a modicum of a sodium soap 'of' stearic acid with suficient additional waterinsoluble material the solubility of the solidified product in water, said composition being prepared" at a temperature above 100 C. whereby it be comes clear and trans arent;

3. The herein descr bed solid insectlfugal composition comprising pine oil, naphtha-' lene anda modicum or sodium stearate so to substantially reduceblended as to constitutea clear and trans-.51

parent mass.

4. The herein composition comprising'pine oil, naphthalene'and ,a modicum o 'sodiumstearate incorporated with a non-volatile 'oil .to sub stantially reduce the solubility of the solidified product in water; the components of said composition being so blended as to constitute a'clear and transparent cake;

-In testimony whereof I have aflixed my signature 1n presence of two witnesses.

a oABLE'rON. nLLis.

Witnesses:

NATHANIEL L. Eos'rER, J AMES EMon'r.

described solid insectifu gal-