USRE7826E - Improvement in the production of deodorized heavy hydrocarbon oils - Google Patents

Description

. ZShggts-Sheet 1- v J. MERRILL y rnonucnon 0F DEODORIZED HEAVY HYDROCARBON ans. 1%. 7,826. Reissud July 31, 1871.

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I 'J'. MERRILL. PRODUTION OFDEODORIZED HEAVY HYDROCARBQN OILS.

No. 7,82 6 Reissued July 31,1877.

- To all whom it may concern UNITED STATES PATENT OFFICE.

JOSHUA MERRILL-OF BOSTON, MASSACHUSETTS.

IMPROVEMENT IN THE PRODUCTION OF D EODORIZED HEAVY HY DROCARBON OILS.

Be itknown that l, JosnnA Mnnnum, ol'

',the city of Boston,in the county of Suffolk and State of Massachusetts, have invented certain new and useful Improvements relating to the Manufacture of Heavy Hydrocarbon Oils, con sisting of, first, an improved heavy hydrocarbon oil; second, a process by which'such oils are produced or manufactured; third, a dc vice or arrangement of devices for superheat ing steam in carryingiivn said process or other process or distillation and 1 do hereby declare that the following is a full and correct description thereof. l

My inventioureldti-s to the heavy hydrocarbon oils which have heretofore been pro duccd by distilling crudc petroleum. or the crude oils obtained from the distillation of bituminous coals, bituminous shales, bituminous schists, asphaltum, and other substances producing hydrocarbon oils by distilhition.

It has been the practice to treat such heavy oils with acids and'alkzdies for the purposeol' removing the disgustingodor peculiar to these oils, which renders them extremely objection able for use in the arts and for lubricating purposes.

Such processes are wellknowinandimprove the character of the odor of the oils; but, nevertheless, the oils so treatedhave a per sistent disagreeable smell, which makes them ofl"ensivo and undesirable for use in close warm rooms, as in woolen-manufactorics.

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 hydrocarbon oils, 1 take the heavy oils which have'been separated from the lighter oils and from 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 tire underneath, and slowly and gradually raise thev temperature until from ten to thirty per cent. of the contents oi 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, oii'cnsive, and disgusting odor; but the oil remaining in the still,i f the and parafliue oils.

opi-ration has been properly conducted, is free from the characteristic ofi'ensive odor ofihylj drocarbon oils, and has no smell encept a slight odor similar to thatof 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. If mixed with twenty per cent ot' sperm-oil, it does not perceptibly change the smell of the sperm-oil.

The process may be conducted in acornmou still, heated by fireheat, as above Incutioued, but will be facilitated, and oil ot'lightcr color produced, by introducing superheated steam into the heated oil within the still, as lwrcinafter more fully described.

When operating by this process upon the pa'rafline heavy oils obtained from petroleum, bituminous coals and sliales, and substances producing parafiine oils, I carry on the distillation until the oil which comes from the condenser has a specific gravity of 36 Baums hydromrter, when, if the process be stopped, the remaining oil in the still is inodorous, or free from empyreumatic odors; but by carrying on the. distillation further, a l raising the temperature until the, oil runs ng from the condenser has a specific gravity of 32 Baum, the remainingoil will be thicker or'more oily, and yet inodorous.

When operating upon heavy oils made fromusphaltum, lcontinue the distillation until the oil running over from the condenser has a specific gravity of from 28 to 25 Baums hydrometer.

The temperature within the still will depend upon the character of the oil acted upon, am upon the mode of working the still. When superheated steam is used the temperature is much lower than when the operation is conducted without it, the steam inaterially assisting in vaporizing the matter that it is desirable to remove. lt isnot practicablc'to specify particularly the specific gravity of the heavy oils used in.

producing my improved oil. These oils are well known to the trade, and distinguished from the lighter burning-oils and naphthas 3 by the term heavyoils', theirspe cific gravity varying greatly between the asphaltum oils 2 14sec Heavy hydrocarbon oils produced from the same substances vary considerably in specific gravity, by reason of the presence of more or less of the lighter oils which are. always to he tound mixed with them, and, therefore, the

percentage of oil that is tobe distilled over in working this process will vary considerably. v

I do 'not assume to know the reason why theabove-described process produces heavy oils free from the characteristic odors othydrocarbon oils, but suppose that these odors arise from matters resulting from decomposition at the temperature at which the heavy oils vaporize and go'over, and that these mat- 'ters, afterthey are condensed "with the heavy oils, will vaporize at a temperature lower than i that required to vaporize and distill river the heavy oils, and, therefore, may be separated from the heavy oilsby distillation in a-closc still at a temperature below that required to distill overthe heavy oil, which, not being vaporized, will remain freclfromthe odorous matters which would result FTOIILGGUOIHPOSI tion at the temperature required to vaporize it and dist-ill it'over.

In carrying on my process to make my improved oil, I use the heavy hydrocarbon oils for sale in theF market, whether they have been treated bj chemicals or. not, the result of the process ip either case being the same. The accompanying drawings represent the distilling apparatus I prefer to use in carry ing out my invention, Figure 1 being a front" 1 elevation of thefjstill and condenser; Fig.2, a

plan view; and'Fig.3 a vertical cross-section of the still and furnace,

Letter 11. represents the still; 1), the tireplace, formed 1n brick-work, upon which the still is placed, the fire being applied ,to the bottom of the still; 0, the grate; d, the ash pit; e, the outlet from the fireplace to the chimney; f, the qnan-hole for access to the iuterior of the still, covered by a suitable manhole plate; g, the gooseneck or pipe leading from-the still to the condenser h; i, the can ing surrounding the still, provided with doors j j 7', covering apertures in front of the arising,

and lids k k 70k,- covering circular apertures in v the top of the'casing, designed to be opened to admit airto the body of the still within the casing, in order toregulate the temperature of the still, or to cool it down ,rapidly .whcn the tire is removed from below. in is a small filling-pipe, shown broken off in the drawing, but which should be connected with a pump or reservoir of oil, and furnished with a shoton cock, to be closed when the still-is tilled.

So far the apparatus is substantially the same as that described in the Letters Patentof the United States granted to me my 30,

1861. I v V I-will now. proceed .to describe an apparatns that I have since invented for superheating steam and applying it to the heated oil within the still, and which may he used with any still heated by a fire.

l place a pertect-lytight coil of steam-pipe, n, within the still, at or near the bottom, and connect one end oi thcccil with a-steamboiler by a pipe, 7:, which passes through the top of the still, and is furnished with a cock, "n to control the admission of steam to the coil. The other end of the coil is connected with an outlet-pipe, p, which passes up through the top of the still. Astop-cock, p, is placed near the open end of the outlet-pipe. A return-pipe, 0', connected with the outlet-pipe 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'esc'ape of -the su perheated steam into the oil. The return-pipe 1 has a stop-cock, r, to control the passage .of

the superheated steam from the outlet-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 hllpe'ifhflhillg coil and pipes is that the steam is superheated in the coil to about the tempera ture 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 outletpipe, lll

order that the operator may, by turning the cool: 12' near the open end of the outlet-pipe,

discharge any water that has got into the coil, and ascertain when the steam has become sufficiently superheated before letting it into the oil within the still through-thereturn-pipe.

It is obvious that this arrangement of pipes for superheating and discharging superheated steam into the oil can be used for any opera tions carried on in stills which require superheated steam of about the temperature of the contents of" the still. I

In carrying on my new manufacture of do odorizing lieavy oils with this apparatus, I place the heavy oil to be deodorized in the still, and heat it by the fire beneath to the required temperature to commence the opera tio'n, the steam heingshnt off from the coil 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 Fehrenhcits thermometer, depending upon the boiling-points of the oils treated,

which vary greatly, I open the steam-cock carefully, and let steam pass into and through the coil, wherein it becomes rapidly super heated to about the temperature of the oil.

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

The superheated steam passes up through the body of the oil and over to the condenser,

carrying along with it the more volatile portions oi the oil, which condense and flow from msao 5 -When cool it is drawn into suitable tanks, and is ready for sale and use.

divested of its and pungent odors, having only a slight em 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 be used, either alone or mixed with other oils.

I prefer to use superheated steam in work- It has been so completely ing the above-described process, because 1 can work at lower temperature than by the the heat alone; but I do 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 the still, or'by any known mode of heating a still which will heat the oil sufficiently to distill over the portions of the oil necessary to be removed; but in that case I am obliged to conduct the process at higher temperatures, and the remaining oil left in the still is darker in color than when superheated steam is used in combination with the fire-heat.

From theabove it will be obvious that a part of my'invention consists in aunew process for producing 'heavy hydrocarbon oils, suitable for lubricating and other purposes,

apd free from the characteristic odors of heavy hydrocarbon oils, from heavy hydrocarbon oils, by distilling from them the volatile matters from which the objectionable odors arise, and, at the same time, preventing new formationsof 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 inthe 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 lighterburning-oils and naphthas liave'not been separated so long as they contain heavy oils, because the naphtha and lighter oils will go over first, leaving 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- I. The above-described heavy hydrocarbon oil, sui table for lubricating and other purposes, free from the characteristic odors of hydrocarbon oils, and having a slight smell like fatty 2. The above-described newmanufacture of (leodorized heavy hydrocarbon oils, suitable for lubricating and other purposes, free from the characteristic odors of hydrocarbon oils, and having a slight smell like fatty oil, from heavy hydrocarbon oils, ,by treating them substantially as herein before described.

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

their stop-cocks, arranged substantially as described,

, JOSHUA MERRILL. Witnesses:

WILLIAM W. SWAN,

H. G. Oursran.

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