UNITED STATES rATEuT orricn.

CABLETSON ELLIS, OF MONTCLAIR, NEW JERSEY, ASSIGNOR TO ELLIS-FOSTER '

"i, COMPANY, A CORPORATION OF NEW JERSEY. '

SOLIDIFIED OIL AND PROCESS OF MAKING SAME.

1,109,119.

Speci?cation of Letters Patent.

Patented Sept. 1, 1914.

Application ?ledliarch 29, 1910. Serial No. 552,177. As an illustration to 14 pounds of,_pinc . To all whom it may concern : Oil and 1 pound of stearic acid commingledwao Be it, known that I, CARLETON ELLIS, a incorporated by heat,'wlien_ thestearic citizen of the United States, residing at and acid has thoroughly dissolved in the pine Montclair, in the county of Essex and State 01], 35 pound caustic soda dissolved in slightly of New Jersey, have invented certain new more than its own weight of water is added and useful Improvements in Solidi?ed Oils and ' the mixture stirred thoroughly, the 60
No Drawing. r

10

and Processes of Making Same, of which the heating being carried up preferably nearly following is a speci?cation. , to the boiling point of the pine oil in order T hisinvention relates to solidi?ed oil com to secure proper incorporation. At tempera positions and to the process of making same tures of for example, 40 or 50 C., a sort and relates particularly to the solidi?ed pine of coagulation occurs and a very unsatis

and similar material and the solid product is carried to say 100 C., the. product is derived from cresylic acid and similar car usually ?rm and somewhat opaque. If how bolic acid material. Ordinary pine oil, for ever the temperature is carridilip to nearly 15 example, is, a liquid insoluble'in water and the boiling point of the me 'Oll, a clear 70 having no power of itself of readily emulsi transparent material may e produced. It fying with water. If however, the pine oil is desirable however in actual practice to use is mixed with soap solutions, emulsions may steam jacketed kettles for manufacturing the 20 be obtained. By the use of concentrated product and for that reason, a temperature soaps, such as oleate of potash, the pine oil of 100 to 135 C. is perhaps more-feast. 75
I 4 _ t v I

oilsmade from long leaf pine oil products factory product results. If the temperature

becomes more or less miscible with water

and certain preparations known as soluble has been incorporated, to chill the product
pine oils which are of this character are
now on the market. _

ble.

It 1s alsodesirable, after the material

25

so as to prevent segregation which often occurs on slow cooling. This is very readily The objeect of the present invention is to done in a jacketed kettle by substituting 80 put pine oil and similar oils into a solid cold water in the jacket for the steam pre form and particularly into a form in which viously used for heating. The product 0b

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 ?ne particles throughout .a large body of water. The

if desired may be cast in . tained however

molds which preferably should be chilled,

and also preferably should be exposed a 85

short time to the air or to a vacuum before

and subsequent addition of caustic soda, to product made in this manner is fairly produce a soap in a concentrated condition. soluble. If a small block of material is In the absence of more than a very small placed under running water, it may dis amount of water, practically that amount solve in'from 20 to 30 minutes. For'some just su?ices to put the caustic soda in purposes, such a high grade of solubility is 40 which solution, and at an elevated temperature, undesirable and to reduce the solubility, I
o the pine' oil dissolves the sodium stearate,

ordinary long leaf pine oil may be solidi?ed of ?rmness which such air or vacuum ex by the incorporation with it of stearic acid posure tends to bring about. The pine oil

shipment, in order to develop a high degree

90

95

and on cooling. solidi?es to a hard solid ma

incorporate with the .pine oil, for certain

purposes, various oils suclt as re?ned

teriali 0n, the other hand if oleic acid is mineral oils or crude petroleum. For ex used with caustic potash, for example, as the ample, in the above formula, if crude petro 45 saponifying agent, a liquid material is de leum is substituted for one-third or'one-halfv 100 This is usually of a dark grown color of the pine oil mentioned, a relatively - riyed'. ' dee- to the use of red oil or commercial slightly soluble material is secured. This is oleic acid, while the stearic acid products of importance as an .insectifugal material
50

' 'su?iciently'hig'h to effect a perfect solution.

areusually white and even transparent if for repellingand destroying mosquitos and the proportion of stearic acid soap is not the like on ponds or'small bodies of water, vtoo great and if the temperature has been inasmuch as large cakes of the material may

105

1,109,119
stearate and the like may be added as de
I -

v be placed in the water and as these slowly

oil spread. over the surface of the wa

dlssolve, the pine oil and crude petroleum soaps such as aluminum palmitate, zinc
sired.

ter, the insectifugal odors of the pine oil In the solidi?cation of creosote, topro driving the mosquitoes from the neighbor a solidcomposition for preparing shee hood and the crude petroleum oil effectually duce and for similar purposes, the formula ' sealing the surface of the water so as to prevent reproduction of the mosquitos. Of may be varied as followszcresylic acid'10
course, various mineral oils may be used in
stead of crude petroleum oil and an oil of

70

pounds, stearic, acigl, 1 ,poufdfcaiustic soda

1- of a poii'lidi This gives a product of mod:

petroleum, is a very useful material for this

purpose. Waxes act in a somewhat similar manner as respects reduction of solubility 15 but are more expensive and are therefore
wax including scale wax and the like are

about .865 speci?c gravity derived from erate solubility which may be rendered more 75 soluble by the incorporation of potassium '
oleate or sulfonated oils. _Similarly with the pine oil, should it be desired to secure
potassium oleate or any similar soap mate
80

an especially soluble product, sulfonatedoil more limited in application. Crude paraffin in its concentrated liquid or solid forms, or

however fairly cheap and may be included rial, may be introduced to advantage, care being taken to not use such proportions as in varying amounts to secure various degrees to cause liquefaction. _ 20 of solubility. For example, in the formula The process may be applied to various 85 above mentioned, the incorporation of 25% of scale wax reduces the solubility of the ma oils- such as oil of cedar, oil of cedar leaf, terial and 50% makes the product very hard oil of camphor, oil of lemongrass and oils and slightly soluble; with the addition of of birch tar, cajeput, mace. nutmeg and the 25 75%, the material becomes practically too like to secure a solid product. In order to insoluble to be of any great value for most produce a\clear product it is desirable to 90 applications. On the other hand, with the heat the oil after incorporation of the soap addition of 50% to 75% mineral oil, very to a temperature above the boiling point of oily solid products may be secured which water, until the water is eliminated, care be 30 have certain very desirable properties. In ing taken to agitate the oil well during this lieu of waxes, naphthalene may be employed process as the boiling is oftentimes violent. 95 to a greater or less extent. For example, in If alcohol is used instead of water as the the above formula comprising pine oil, stearic acid and caustic soda, 5%, 10% and tion may take upward to say 40 or 50% oflnaphthalene may This is especially the case with methyl alco be incorporated. With the lower percent hol which boils at 66 C. In the case of 100 ages, very little crystallization is evident on. certain essential oils which have rather low
the masses oftentimes are somewhat crumbly alcoholic solvent is to be recommended. In case of cresylic acid or other carbolic 1'05 especially after water has acted upon the acid materials, the solidi?cation may be material for a short time. These solidi?ed oils may be given various colors by the use made such that the product may be cut out of, oil soluble dyes. They maybe combined into the shape of tablets for medicinal uses 45 if desired with ?lling or weighting materials and may be made so ?rm as to be capable of . as for example, if it ' is desired to have the. supporting a coating of some other material. 110 cake heavier than water, such substances as The addition of a little more alkali than
40

boiling points and which are injured by subcooling, but with the larger percentages, jection to high temperatures, the use of an crystallization is so much in evidence that

'

50

material. In the case of pine oil as will 115 as sawdust, wood ?our,-s_tarch', sugar and the, appear from the foregoing formula, 25% of tial oils'may be included if it is desired to caustic soda has been used reckoned on the I glve special odors or .special medicinal or amount of stearic acid, while the actual Sa ' requires onl about 20%.- This 65 other properties to the product. Of course, I poni?cation _, uantity of kali is howevennot 120 greases suchras stearin, tallew, etc, degras, additional wool grease, lanolin_,.various_ resins such as obiectionab e andis rather desirable in or: colophony, dammar, sandarae. coral, .Ponti-' der to rapidly complete saponi?cation. The ianak, guayulei__and similar. resins, may be material may however be made substantially incorporated to a greater or less extent in neutral by using the exact equivalent of accordance with the character-of the product alkali. The stearic acid may be replaced by 125 . desired for special applications. Also rub: still stockto advantage in some cases. oducts particularly the crude Ponti-. The present invention therefore involves h d guayule'gums' containing both-the the process of melting or incorporatin the 6.5 rubber and resinous _ material.v Metallic essential oils" to be solidi?ed, with eely
like may be made use of. Also other essen~

talc, infusorial earth, oxid of iron, etc., may. be em loyed, while, if it is desired to have with the fatty acid employed is usually de- ' the caiie lighter than water, such materials sirable in the solidi?cation of cresylic acid

that actually required for the combination

saponi?able soap-forming fatty acids, adding

130

p 8

way the mass is quickly chilled, there-I ' thereto, the requisite amount of alkali, such under possibly preventing the formation of by as caustic soda, carbonate of soda, potash~ or .50

_ 5 the alkali in-solut-ion, combini'n fthis, pref

soap complexes. whatever the alkali maybe, dissolved in molecular ' By pine oil, orpilof pine, as used herein, "j tov maintain preferably just sufficient vwater _I refer-particularly to the'volatile oils de- .

,agitating'to effect perfect_incorporation and

erably hot, withthe oil, prefera ly hot, car cally refer to spirits of turpentine, Russian rying the freely saponi?able fatty acid-and turpentine, and long leaf pine oil.
_ 1. The herein described ?rm solid insec

rived from genus Pinus and more speci?- "

55

' substantial solution of the soap, referably '_ 10 followed by the step of heating t e oil to a
_ temperature su?icient to expel a substantial

v.I claim:

'

tifugal composition comprising an essential

oil' and a modicum of a soap of stearic acid portion or all of the water whereupon the with su?icient additional water l-'insoluble mass preferably is rapidly chilled to insure material to substantially reduce the solubil- _ . proper setting andto overcome segregation. ity of- the solidi?ed product in water, said in ~It will be evident tothose skilled in the composition being prepared at a tempera

2.,The herein de'scribed'?rm, solid insec of different proportions and suited for many tifugal composition comprising an essential '20 di?erent'applications, and I do not wish to oil and a modicum of a sodium soap 'of' limit; myself strictly to the invention; as stearic acid with suficient additional water- herein set forth and wish. to'qapply or vin insoluble material to substantially reduce 70 voke the doctrine of equivalency so far as the solubility of the solidi?ed product in ' same may be herein applicable, all in view water, said composition being prepared" at a 25 of the present State, of the art and'with due temperature above 100 C. whereby it be recognition" of the _ heretofore employed comes clear and trans arent; methods or. making soluble or solidi?ed oils 3. The herein descr bed solid insectlfugaly 75
in various ways, by the use in'some cases of
.50 oils in a manner foreign to the idea of the
soaps either to produce emulsions or miscible v lene anda modicum or? sodium stearate so

that various modi?cations- may be made un , der the present invention to produce bodies

art, from the information herein set forth, ture above 190 0. whereby it becomes clear
and transparent. ~ -

65

composition comprising pine oil, naphtha-'

as to constitutea clear and trans-.51. present invention, but in some cases employ, blended parent mass. i'ng'materials more orless similar in charac: 4. The herein described solid insectifu'gal _ ter to produce bodies having different prop composition comprising'pine oil, naphtha erties or characteristics from those herein ,a modicum o 'sodiumstearate in as described. The products made under my in lene'and corporated with a non-volatile 'oil\_.to sub? vention are characterized by their peculiar. stantially reduce the solubility of the solidi colloidal condition manifestmg itself 1n va7 ?ed product in water; the components of 85 rious ways. Some of the compositions here' said composition being so blended as to con under for example are _readily fusible when stitute a'clear and transparent cake; 40 ?rst formed but become di?icultlyfusible on o-In testimony whereof I have a?ixed my standing. Seemingly the soap, forming as signature 1n presence of two witnesses.

810

it does in the oil itself exerts by nascent ac

tion some peculiar colloiding in?uence on the oil and it is probably because of, this condi- ' i

'

oABLE'rON. nLLis.
,~ . ->

45 tion of nascency that?rmer, sounder prod-. ucts are obtained. ~Especially does this seem a morepotendfactor after reaction is well

Witnesses:

NATHANIEL L. ,Eos'rER,
- JAMES EMon'r.

At