(No Model.) F. S. CLARK, PROCESS OF OBTAINING CREOSOTE, &c. No. 388,529, Patented Aug. 28, 1888.

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N. Peters, photo-ithographer, Washington, D.C.

UNITED STATES PATENT OFFICE.

FRANKLIN S. CLARK, OF CHARLESTON, SOUTEI CAROLINA. PROCESS OF OBTAINING CREosoTE, &c. SPECIFICATION forming part of Tetters Patent No. 388,529, dated August 28, 1888. Application filed April 27, 1887. Serial No. 236,289. (No model.) To all, whom, it may concern: acid-such as sulphuric acid-that will accom Beit known that I, FRANKLIN S. CLARK, of plish the liberation of the phenols or creosote, Charleston, in the county of Charleston and which latter floats on the surface as an oil. State of South Carolina, have invented certain When sulphuric acid is employed to set free 5 new and useful Improvements in the Process the creosote, a loss is incurred, as the sulphuric 55 for the Manufacture of Creosote and Acetate acid combines with the caustic soda previously of Soda; and I do hereby declare the following used to purify the turpentine or other oil, and to be a full, clear, and exact description of the they together form sulphate of soda, which is invention, such as will enable others skilled of small commercial value. IO in the art to which it appertains to make and The pyroligneous acid, which is one of the use the same. substances to be considered, is converted into a My invention relates to an improvement in marketable product by treating it with lime the process for the economical production of or carbonate of soda, the result being a pro Creosote from pyroligneous compounds that are duction of acetate of lime or acetate of soda found in the residuum obtained in the distilla by the chemical action of the lime or soda on 65 15 tion of turpentine and lubricating-oil from the pyroligneous acid. This entails an ex resinous Wood or other substances. penditure for lime or carbonate of soda. I Myinvention consists in the economical pro employ a combination process that is based on duction of creosote and acetate of soda from rudimentary principles, which may, be stated the residuums separated in the process of re as follows: First, crude or distilled pyroligne fining turpentine or heavier tarry oils used for ous acid will precipitate creosote (phenols). lubricating purposes from the crude products fron caustic-soda solution or any caustic-alkali of the distillation of vegetable, arboreal, or solution; second, that the above-named pre mineral substances. cipitation also produces acetate of soda by the My improvement also consists in the em union of the acetic acid (of the pyroligneous 75 25 ployment of certain mechanism and manipu acid) with the waste caustic soda or any other lation of the same. caustic-soda liquid free from creosote. The annexed drawing exhibits a side eleva My improved process, which will now be tion of the apparatus preferably used, which described, affords the following - named ad will be hereinafter specifically described. vantages, viz: first, dispensing with the use 8o In the manufacture of merchantable pro of sulphuric acid for purposes of precipita ducts from the organic constituents of resinous tion; second, utilization of the caustic soda by Woods or other proper material four impor its conversion into a valuable acetic-acid salt tant substances are to be considered-viz., or acetate of soda; third, reduction of the turpentine, lubricating-oil, creosote, and pyro amount of lime necessary to make acetate of 85 35 ligneous acid. lime; fourth, obviating the cost of sulphuric In the process of purification of turpentine acid, the danger of handling it, and affording and the heavier lubricating-oil or resinous independence in regard to varying prices of woods the employment of caustic soda is nec sulphuric acid and lime; also, the consolida essary to remove impurities known as “phe tion of two processes into one-viz., the pro- 9o . nols’’ or “creosote. The use of caustic soda duction of creosote and acetate of Soda-ef enhances the cost of the purifying operation fecting a saving by such a union of a reduc if some economic means for the utilization of tion of the space for a plant, less labor to the waste caustic-soda liquors is not employed. return for product, a decrease in cost of in Heretofore no such method has successfully surance, and merchantable product of higher 95 45 been introduced. It is true that the waste grade than is afforded by ordinary processes. liquor of caustic soda resulting from the purifi My improved process and apparatus for car cation of turpentine or the heavier lubricat rying it into effect will now be described. ing-oil has been treated to obtain creosote by F is a wooden or metal receiving-tank, into 5o neutralizing the caustic soda with a mineral which the waste caustic soda or other alkaline Ioo

388,529 liquor resulting from the refining of distillates can also be seen by fapping at one of the test to produce turpentine or heavier oils is run. cocks I some of the acetate of soda and allow B is a wooden vat or tank, located, prefera ing it to run in a fine stream. If all the creo bly, in the same horizontal plane with the sote has been removed, the liquor will be tank F. Proper-sized pipes CG are attached nearly transparent. The pyroligneous acid is to the bottoms of the tanks B F, the pipes be added during constant agitation, which is pref ing bent to curve and extend downwardly into erably effected by the air-currents, as stated, a tank, D, which I term an “agitator.’ The to make a more perfect reaction. After the pipes C G are provided with globe-valves C addition of the necessary amount of acid the O G' to control the escape of fluid from the liquor is allowed to settle, the oil (creosote) 75 tanks to which these pipes are attached. going to the bottom and the acetate of soda The agitator D is preferably made of forming the upper liquid. By opening the wrought-iron, and has a conical bottom, D', lower valve, K, the creosote-oil will pass out to which a vertically-descending pipe, D', is into any suitable receptacle, while the acetate secured near the center of this bottom, a of soda will not appear at the valve until all proper aperture being made at this point to the creosote is out. The valve is then closed. afford an exit passage for the contents of the The creosote thus obtained is a brown to black agitator. A valve, K, is located in the pipe colored oil of a specific gravity 1.080. It con D' to close it, and thus retain liquor in the tains about forty-five percent.of real wood-creo agitator D. The pipes CG are extended near Sote, with water, light tar-oil, (turpentine,) and the inner surface of the agitator D toward heavy tar-oil, Clubricating-oil.) The process the center of its conical bottom on opposite may be used for coal-tar, creosote, or phenols. sides of the orifice made therein. derived from other material. It may be At points R. R., near the upper edge of the worked up for creosote in a pure state, in agitator D, the air-induction pipes H. Hare in which operation the crude oil (creosote) is 90 troduced into it, and are extended down distilled in a tar-still, and the light and heavy wardly to conform nearly to the shape of the oils separated by a fractional distillation and interior Surface and conical bottom of this worked for turpentine and lubricating-oil. agitator. The air-pipes C G are provided The fraction passing off in the middle of the 3O with the valves H'H', these pipes being made distillation and having a specific gravity of 95 to communicate with an air-pump that is lo 1.045 to 1.050 is kept apart and worked fur cated at some convenient point to furnish air ther for creosote by any of the creosote pro jets to the agitator D through the attached cesses. The liquid remaining in the iron tank pipes just mentioned. D after the separation of the creosote is a OO In operation the caustic soda or other al weak solution of acetate of soda, and must be kaline liquid, whether waste or otherwise, boiled down to a specific gravity of 1.230 for that contains creosote residuum from the puri crystallization. This boiling may be done in fication of turpentine or the heavier lubricat a separate vessel or the iron tank in which ing-oil, is run into the reservoir or tank F, the the precipitation was effected, in which case crude or preferably distilled pyroligneous the tank must be made with a steam jacket. acid being stored in the opposite tank, B. A During the evaporation any tar which col sufficient quantity of the waste caustic-soda lects upon the surface must be skimmed off, liquor or other alkaline liquor to constitute a and when the solution is at the required test “charge is allowed to enter the agitator it is run out into a small crystallizing-pan. IO 45 chamber D. After the introduction of the From this point any of the ordinary processes alkaline liquor is effected and valve G closed for making acetate of soda are followed. a limited quantity of the pyroligneous acid is It is obvious that by this process not only decanted from the storage-tank B into the is the acetate of soda produced, but the creo agitator D. The valve C is now shut and the sote contained in the Waste alkaline solution valves H.H.” opened to permit forcible air-jets to as well as creosote from the pyroligneous-acid I I5 enter near the center of the bottom of the solution are deposited, and this without the agitator-chamber and thoroughly mix its con use of sulphuric acid, as previously employed. tents. The forcible commingling of the When I refer in this specification to the use charge of caustic-soda liquor and pyrolig of 'soda’ or 'soda solution,’ it is to be un neous acid in the agitator that has just been derstood that a potash solution operates in described should be continued for ten or fif identically the same way, and my specification teen minutes, when a complete neutralization and claim are intended to refer to both. of the caustic soda will be effected by chemical Having fully described my improved pro affinity, the creosote being precipitated by cess for the utilization of Waste caustic-alka the action of the pyroligneous acid, and ace line liquor and the production of creosote of I 25 tate of soda result from this separation. The commerce and acetate of soda from pyrolig solution may be made slightly acid, if desired, neous acid as treated by my process, what I the effect of adding a slight excess being to claim as new, and desire to secure by Letters precipitate all the creosote, and thus give a Patent, is- - better acetate of soda. The point of acidity The process herein described, which consists may be determined by litmus paper; but it in mingling caustic-soda, solution containing

388,525 3 creosote or analogous phenoloid bodies with In testimony whereof I have signed this pyroligneous acid, thereby occasioning a re-specification in the presence of two subscrib action between the mingled bodies, and de-ing witnesses. positing creosote, and forming acetate of soda, FRANKLIN S. CLARK. 5 by the union of the soda solution and the Witnesses: w acetic acid of the pyroligneous-acid solution, JoHN C. MALLONEE, substantially as described. GEORGE. S. BROWN.