USRE7733E - Improvement in processes and apparatus for the manufacture of deodorized heavy - Google Patents

Description

MAM;

2 Sheets-Sheet 1. J'. MERRILL.

. PROCESS AND APPARATUS FOR THE MANUFACTURE OF IDE OIDORIZED HEAVY HYDROCARBON OILS. No. 7,733.

Reissued June 12, I877.

V/VgTNEss'ssi mvsm'rbm l 2 Sheets-SheetZ'. I. MERRILL. PROCESS AND APPARATUS FORTHE MANUFACTURE OF DEODORIZED HEAVY HYDROCARBON QILS'. No. 7,733; A Reissued June 12, 1877 A ,5; '1 -lIwl|-'.m|

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WITNESSES? I \xluvsm' oaz FIG.3. I

and State of Massachusetts, have invented l to the manufacture of heavy hydrocarbon oils,

other processes of distillation; and I do hereof removing the disgusting odor peculiar to warm rooms, as in woolen manufactories.

UNITED STATES PATENT OFFICE;

JOSHUA' MERRILL, OF BOSTON, MASSACHUSETTS.

IMPROVEMENT IN PROCESSES ANDAPPARATUS FOR THE MANUFACTURE OF DEODORIZED HEAVY HYDROCARBON OILS.

Specification forming part of Letters Patent No, 90,284, dated May 18 1869 reissue No. 1,738, dated June 12, 1877; application filed May 25, 1877.

To all whom it may cancer-a: Be it known that I, JOSHUA MERRILL, of the city of Boston, in the county of Sutl'olk certain new and useful improvements relating consisting of, first, an improved heavy hydrocarbon oil; second, a process by which such oils are produced or manufactured; third, a device or arrangement of devices for superheating steam .in carrying on said process or by declare thatthe tbllowing is stall and correct description thereof.

My invention relates to the heavy hydrocarbon oils which have heretofore been pro duced by distilling crude petroleum or' the crude oils obtained from the distillation of hituminous coals, bituminous shales, bitmninous schists, asphaltum, and other substances producing hydrocaibonoils by distillation.

It has been the practice to treat such heavy oils with acids and alkalies, for the purpose these oils, which renders them extremely objectionablej'or use in the arts and for lubricating purposes. f v I Such processes are well" known, and improve the character of the odor of the oils; but, nevertheless, the oils so treated have a persistent disagreeable smell, which makes them ofi'ensive and undesirable for use in close Attempts have been made to remove the smell by filtration, with but partial success.

To make heavy hydrocarbon oils free from the characteristic unpleasant odors of heavy, hydrocarbonoils, 1 take theheavy oils which have been separated from the lighter oils andfrom mechanical impurities by distillation, and, after chilling and expressing the solid parafline, when such operation is necessary, place them in a still, heated by a fire underneath, and slowly and gradually raise the temperature until from ten to thirty per cent. of the contents of the still are distilled over, when the still is cooled down and the remaining contents removed.

The matters which go over to the condenser have a very foul, offensive, and disgusting odor, but the oil remaining in the still, if the operation has been properly conducted, is free from the characteristic offensive odor of hy'- drocarbon oils, and has no smell except a slight odor similar to that of fatty oils.

It can be mixed, in all proportions, with sperm, lard, fish oils, and vegetable oils, and is so neutral in its character-that it takes the odor of the oil that it is mixed with. it mixedwith twenty per cent. of sperm oil it does not perceptibly change the smell of the sperm-oil.

The process may be conducted in a common still, heated by fire-heat, as above mentioned, but will be facilitated, aml oil of lighter color produced, by introducing superheated steam into the heatedoil within the still, as hereinafter more fully described.

When operating by this process upon the parafline heavy oils obtained from petroleum, bituminous coals and shales, and substances producing pal-atline oils, I carry on the distillation until the oil which comes from thelcondenser has a specific gravity of 36 Baums hydrometer, when, if the process be stopped, the remaining oil in the still is inodorons or 'free from empyreumatic odors; but by carrying on thedistillation further, and raising the temperature until the oil runningd'rom the condenser has a specific gravity of 32 Banm,

the remaining oil will be thicker or more gily,

and. etinodorons. 7 r

1 When operating upon heavy oils made from asphaltum, -I continue the distillation until theoil running over from the-condcnser has .a specific gravity of't'rom' 28' to 25 Baumes hydrometer v lhe temperature within the still will de-: pend upon the character of the oil'acted' upon,

and upon the mode of working the still.

. When superheated steam is used, the tem- Q,

perature is much lower. than when the operation is conducted without it, the steam materially assisting in vaporizing the matters that it is desirable to remove.

It is not practicable to specify particularly the specific gravity of the heavy oils nsed in producing my improved oil. 1 These oils are we'll known to the trade, and distinguished from the lighter burning oils andnaphthas we top of the casing,

the term heavy oils, their specific g'ravity 1 do not assume to know the reason why the above-described process producesheavy oils free from the characteristic odors of hy' drocarbon oils, but suppose that these odors arise from matters resulting from; decomposition atthe temperature at which the heavy oil s vaporize and go over, and that these mat.

ters, after they are condensed with the heavy oils, will vaporize at a temperature lower thanthat required to vaporize and distill over the heavy oils. and, therefore, may be separated from the heavy oils by distillation in a close still at a temperature below that required .to distill over the heavy oil, which, not being vaporized, will remain free from the odorous matters which would result from decomposition at the temperature required to vaporize it and distill it over.

In carrying on my process to make my improved oil I use the heavy hydrocarbon oils for sale in the market, whether they have been treated by chemicals or not, the result of the process in either case being the same.

The accompanying drawings represent the distilling apparatus I prefer to use in carrying out my invention.

Figure 1 is a front elevation of the still and condenser; Fig. 2, a plan "iew; and Fig. 3 a vertical cross-section of the still and furnace. Letter it represents the still b, the fire-place formed in brick-work upon which the still is placed, the tire being applied'tothe bottom of the still; 0, the grate; d, the ash-pit; e, the outlet from the fire-place t0 the chimney; f, the man-hole, for access to the interior of the still, covered by a suitable man-hole plate; g,the goose-neck or pipe leading from the still to the condenserh; i, the casing surrounding the still, provided with doors. j j j covering apertures in front of the casing, and lids k k k 70 covering circular apertures in the designed to be opened to admit air to the body of the still within the casing in order to regulate the temperature of the still or to cool it down rapidly when the fire is removed from below. m is a small filling-pipe, shown broken off in the drawing, but which should be connected with a pump or a reservoir of oil, and furnished with a shutolfcock, to be closed when the still is filled.

So 'far the apparatus is substantially the same as that described in the Letters Patent of the United States granted to me July 30, 1861.

I will now proceed to describe an apparatus that I have since invented for'superheating steam and applying it to the heated oil with- -order that the operator the oil within A stop-cock,p, is placed near the open end i of the outlet-pipe. Areturn-pipe, 1', connected with the outletp'ipe, between the stop-cock and the still,

passes down into the still, terminating in a horizontal discharge pipe, r, perforated, as usual, with small'holes for the escape of the superheated steam into the oil.

The return-pipe 1' has a stop-cock, 'r, to control. the passage of the superheated steam .fromt'he'odtlet-pipe through the return-pipe to'within the still, so that when it is shut no superheated steam passes into the oil.

The advantage of this arrangement of the superheating coil and pipes is that the steam is superheated in the coil to about the temperature of the oil it is to be applied to by the ,heat of the oil itself, and then carried above the top of the still through the outlet-pipe, in may, by turning the cock p near the open end of theoutlet-pipe, discharge any water that has got into the coil, and ascertain when the steam, has become sufliciently superheated before letting it into the-still through the returnpipe. v Itis obvious that this arrangement of pipes for superheatin g and discharging superheated steam into the oil can be used for any operations carried on in stills whichrequire superheatedsteam of about the temperature of the contents of the still.

In carrying on my new odorizing-heavy oils with this apparatus, I place the heavy oil to berdeodorized in the still, and heat it by the fire beneath to the required temperature. to commence the operation, the steam being shut and the outlet-cock being opened to admit of the expulsion of any water from within the,

coil.

When the oil is heated to from about 220 to 300 Fahrenheits thermometer, depending upon the boiling-points of the oils treated, :3? vary greatly, I open the steam-cock fully, and let steam pass into and through the coil, wherein it becomes rapidly superheated to about the temperature of the oil.

Having ascertained that the steam passing through the coil is sufficiently superheated, I close the on let-cock, and then carefully open the cock in the return-pipe, and let a small amount ,of superheated steam pass down into the still, where it escapes, by the small openings through the pipe, into the'body of the hot'oil.

manufacture of de 1 may be.

The superheated steam passes. up through the body of the oil and over to the condenser, carrying along with it the more volatile portions of the oil, which condense and flow from the condenser into a tank provided for their reception,

I continue this operation, keeping the fire dull and moderate under the still, and the temperature slowly rising all the time, until I distill 011' all the volatile matters, which read: ily flow out with the steam, usually distilling of! from twenty to thirty per cent., as the case I now draw out the fire,then shut oh the steam, and leave the oil to cool in the still. When cool itis drawn into suitable tanks, and is ready for sale and use.

Ithas been so completely divested of its fetid and pungent odors, having only a slight smell like a fatty oil, and has become so oily as to be greatly improved and increased in value as a lubricating oil, or for any purposes for which it may beused, either alone or mixed with other oils."

. I'prcfer to use superheated steam in working-theabove-described process, because I can work'at lower temperature than by the tire heat alone; but Ido not wish to confine this "part of my invention to the use of superheated steam in combination with the tire, because I can accomplish the same result by fire-heat alone applied to t he still, or by any known mode of heating a still which will heat the oil sufliciently to distill over the portions of .the oil necessary to bo removed; but in that case I am obliged toconduct the process at ihi'ghertemperatures, and the relnaining oil left in the still is darker in color than when superheated steam is used in combination with the fireheat.

From the above it-will be, obvious that a part of my invention consists in a new process for producing heavy hydrocarbon oils,

suitable for lubricating and'other purposes,

and free from the characteristicodors of heavy hydrocarbon oils, from heavy -byd'rocarbon oils, byfd'istilling from them the volatile matters from which the objectionable odors arise,

and, at the same time, preventing new formations of such matters, by keeping the temperature of the oil in the still below that at which these matters form by decomposition of the oil.

It will also be evident to those skilled in the art that this part of my invention will be used, if the above-mentioned process be worked to produce the deodorized heavy oils above described, from distilled hydrocarbon oils, from which the lighter burning oils and naphthas have not brcn separated so long as they contain heavy oils, because the naphtha and lighter oils will go over first, lcaving the heavy oil in the still to be operated upon; and also because, as before stated, the distilled heavy oils always contain more or less of the'lighter bodies, owing to the breaking up of a portion of the heavy crude oil in the process of distillation.

I claim- 1. The above-described heavy hydrocarbon oil, suitable for lubricating and other purposes, free from the characteristic odors of hydrocarbon oils, and having a slight smell like fatty oil. a

2. The above-described mode of manufac ture of deodori'zed heavy hydrocarbon oils,

which, when finished, are distillates suitable for lubricating and other purposes, free from the characteristic odors of hydrocarbon oils, and having a slight smell like fatty oil,",b y distilling from them the volatile matters from which the objectionable odors arise, and preventing the formation of such matters by keeping the temperature of the oil in the still below that at which these matters form by decompositionof the oil, substantially as described. Y

3. In combination with a still suitable for distilling oils, the superheating-coil, with its steam-pipe, outlet-pipe, and open return-pipe,

and their stop-cocks, arranged substantially as described. l

JOSHUA MERRILL.

Witnesses: v

SAM. W. BATES, WILLIAM W. SWAN.

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