US1423716A - Process of distilling shale - Google Patents

Description

E. ElIIElMES.` PROCESS OFDISTILLIN'G SHALE.

- -APPLICATION FILED JUNE I3, I92I. www@ RENiEWED APRKB, I9 22. Patented July 2f', i922.

2 SHEETS-SHEET 1.

E. LHEDGES. PROCESS' OF DISTLLING SHALE. APPUCATION FILED JUNE I3, 1921. RENEWED APR. 3,1922.

Patented Juy 25, 192;'.

2 SHEETS-SHEET 2.

VIM

EDWARD E. HEDGES,

ERGCESS 0F DXSTILLXNG EHLEA 'Letters Patent. Irlatented it@ ii.

Application filed une, 19521, Serial lilo, $77,233. 'Renewed April S, lf. eiis No. 55@,'?53tl.

To all wko/m, t may conce/mil Be it known that l, lnwAnn l?. Houses, e citizen of the United States, residing at New Yorlgei'n the county of New York and State of Nefv York, have invented certein new-und useful Improve-ments in `l?rocesses'oif Distill! ing Shale, of which the following is a specilication, reference being had therein to the eccompanying drawings.

This invention relates to process ci treat* ing lrerogen shales for the recovery oi the valuable constituents thereof, especially, though not exclusively, the hydrocarbon con tent, hut also as ys secondary desideratuins waiter-soluble pot/ashr` ammonia, which may be converted into ammonium sulphate, fixed gases which rnay be employedior illuminate lng end heating purposesl and perhaps other minor constituents which may be recovered and utilized or converted into. Valuable by products by subsequent processing. t

It is well known that there are a consider-` able number of oil shale deposits in variouse parts of the world and that the diiierentileposits represent different qualitative and quantitative structures. Not all shales' oontain hydrocarbons which can be liberated in the toi-1n of hydrocarbon oils, but the present invention is directed particularly to kerogen `shales which do contain hydrocarbons in great quantities, which, by the proper treatment, may be liberated in the torni oi hydrocarbon oils analogizing crude Well oils, as found in petroleum fields. Many attempts have been inode to release the hydrocarbons from the shale, such attempts having been more or less successful, but the present invention has for an object to provide a 'process which Will liberate substantially, all o'i' the hydrocarbon content inthe forni of oils analogizing' Well oils, together with such' other constituents ot value as may be found the residuun being a spent for manufacturing cements, or forrinany other purposes', but the 'tur-ther use of such spent shale forms no part of the present process. v The present invention resides in introducing the raw shale7 et atmospherictemperature, at one end of a, retort-7 preera-bly'o the rotating tubular type, but not necessarily limited *thereto7 the requirements 'beiolgr a sufficient agitation and cascad" g of the shale? ,the terni cascading"eonilgrehending the raising of the shale or portions thereof and dropping from such raised position to s lower level :ind progression from the end oi' introduction to the end of discharge. The discharge end of the retort is heated to a high temperature so that ythe shale., in progressing from the introduction "nd, at et# niospheric temperature, is graduali-1;' hestedy and passes through areas oi increasing heet. The gradual heating oi the shale progres'- sively liberstes the several constituent parts which are respectively liberated by; the vveri- -ous temperatures 'and the gases so released are passed baclrivardly or toward the intro-v duction end and discharged, so that the gases y as they are released pass through cooler areas instead oi through hotter eas, being et no time subjected to heat greater than that of the area in which they liberated.

t the end opposite the introduction end, the spent shales are disoharged and the end' of the retort will, therefor@ he referred tous -ithe discharge end, it being understood that the d1scharge end is the end which is heated The drawings accompanying this applica! tion are shown merely for the purpose of 85 illustra-ting un apparatus which 'will carry,- out the invention, and are not intendedr in` any way to limitthe invention to the exact apparatus. nsaid drawings: l Figure l is a longitudinal diametricelpsectional View throughl u rotating' retort 'in which the process may be practised;

, Figure 2 is ,a transverse sectiona-iview through the driving end adjusting nischenisni taken on line 2-2 oi Figure l;

Figure 3 isv a transverse seotionel View through the inlet Worin seal,. taken on line 3-3 of Figure l, and

Figure l is a transverse Fi ure. l. i i

like characters o reference indiicate ycorresponding parts throughout the several views.

employed there shown as, a cylinder 1G mounted inv any approved Way to rovide for rotation end adjustment on -theiidlers 11 and journalhearing 12. The idlers '111 are adapted to to the highest temperature. rlhe heet' et lthe `8@ sectional View through theretort, taken on line f-ll ox we hereised and lowered-dor the purpose i AS inusuali-,ed in the drawings', a renin isv los of raising and lowering the cylinder 1U,such raising and lowering means being shown conventionally as the screw 13. The journal aring 12 is also mounted in an upright 14 which is mounted upon a ball-and-socket bearing 15 which permits the angular vadjustment ot' the lower end of the retort whenv in an f a i )roved manner as b means of ro-' viding a gear 21 about the peri 'hery of such retort adjacent the lower en intergeared with a pinion .22 which, in turn, is pro elled by any approved type of motor, as indicated at 23. i

l At the end opposite the outlet 16 a hopper 24 is provided having an inlet nozzle 25 communicating with a central chamber 26, forming a part of the inlet worm seal feed. This seal feed comprises a partition 27 providing a volute passage from `the central chamber 26 to'the openin 28, whereby the rotation of the retort in t e direction indicated by the arrow at Figure 3 will permit the passage by gravity of material from the central chamber 26 through the volute passage to be discharged at 28 into the interior and at the bottom of the retort. A pipe 29 is introduced through the central chamber 26 and communicates with a condenser indi cated conventionally at 30.

At the end o posite the inlet seal feed, a discharge sealp feed is provided substantially identical with the inlet feed, comprisingr a partition 31 having a volute passage 32 which takes up materialat the bottom of the periphery of the retort and, by reasonof the rotation, moves' the said material upwardly to theY centralchamber 33 which communicates with the discharge 'passage 16. The material is, therefore, introduced into and removed from the retort wholly by reason of the rotation of such retortand maintaining at all times a seal against the introduction'ot air or the outlet of gases except through the passages provided for that purpose.

For the purpose of heating the shale in the retort some kind of heating element is provided, preferably such as will provide heat at one end of the retort, referably the lower end and preferably urt er graduated as to temperature. As shown in the drawing a spiral resistance coil interior of the retort and is inI communica` .passage of the gases longitudinally of the 3a extends about tht tion with the rings 35 and 36. Rolling contacts 37 and 38 conduct to these rings and from the rings to the resistance coil Silvrelectromotive Force from the source 38. A second resist-ance coil 39 is provided within 7@ the retort adjacent the coil 34, con'imu'nicat# ing by means of similar rings a() and 41 and. similar rolling contacts 42 and 43 with a vsource of electromotivedorce 44. The two" sourcesf'of electromotive force 38 and 44y, 7 have been differentiated in the drawing toindicate different potentiality, whereby a current of greater voltage and higher amperage is provided to the coillll than that supplied to the coil 39. This 1s merely for the purpose of indicating that the part oi: the retort at which the coil 34 is shown is hotter than that part at which the ooil 39 is shown and varying the heat whether through the use of electric current and resistance ele- .ment, or otherwise, may be employed for the purpose.

ln practising the process in an apparatus of the .kind disclosed in the drawing, it will be obvious that the ra'w shale finely powdered will be introduced in the hopper 24 and 'passing through the chute 25 and inlet seal feed will be deposited in the interior of the rotating retort. The interior of the retort l is heated as indicated, the lower end or that end farther from the inlet feed being heated to the greater temperature. It is obvious that thel introduction of raw shale at atmospheric temperature continuously will maintain `the inlet end ot the retort in a more or less cooled conditionand that the retort will be increasingly heated Atoward the other end. This is maoe possible from the fact that there is a comparatively small amount of displacement and replacement of gases with- 'in the retort, provision being made for the introduction of steam through the pipe 17 and the withdrawal ,of the gases through the pipe 29, other than which there is no retort. It is obvious that the shales, as they move from the inlet or cooler end toward the hotter end of the retort, as they will by reason of the rotation and inclination of the cylinder, will move gradually from the cooler to the hotter areas, the several volatile substances contained in the shale being, of' course, liberated from' the shale at the various temperatures, and it is obvious also that those substances which are liberated at the 'lower temperatures willbe first liberated as the sha-le moves from the coolerto the hotter area and that when liberated in gaseous form they will move always to and through the cooler areas to be discharged through the pipei29 to the condenser.' As the shale rogresses, therefore, from the cooler to the otter end the several substances will progressively be liberated and volatilized, the gases passingbaclrwardly, or at all times through it@ it is desir 'oceee im the better 'i eer'ooris iii he iiitremw om ein-oligo, Mie *i d boiler ters@ iure, or at some super gere-- Lire which is unimporieo Co die preseiri'y iii om? immedieieiy ees ipoo. sof-,h iixed eeroone eed forms ---ierewiiii writer fue ihereting hydrogen Whioh passes berkwzird 1y ifo eooer end 'through ehe progres-- sie-'ey oooier :Leid eoi'emiiy ding wizh the hydroeerbons jz revioueiy libziddimg hydrogen io die oydrmfmbou 'ioleeoies so ber, ehe ,Humber a f "h hydrocarbon moieeides is more over i f 'i bei which would be Eo dry di v lati n, The passing* of i, ed hydro- Cfeiraone beekwerdiy i- 'the-coder areas i events ore-Shing and also prexf'eniie iixiif of soma. gasee which 'migh oiie ome when eid; Y

heated condi'ioii,

ipe iY i ioe obvioiie ab?) ie; i ence iii miope/riviere between eous eoiieit andthe .Qold cement mi. :my

en so hais while ehe i. iiiiorziei imokwardly, they :are ooi? :ie :my lime passed through :in aree eo ooo?, iis to gein condense the within die rerorf; and -disoherged in gaseous mmdiioii 'Sto eondeiisser.

There is a eertain amouii oi: fixed swoon in lie ehaie after he hydroearifim ,uitro-- end the like have been rei J U xe und @he said'sieie Conaiomg; seid fixed mr-idiomv when approaching the die or hotter end oi the reor, is raked o Such temperature that h eem1 des "introduced, ziciing' upon this di carbon a high eeigjjereture, is deeomposed into its elements, he oxygen combining' .riiii oer form carbon monoxide, or carbon "i1 he hydi'oitarboo vapore, wherev er quent-ity of hohe hydrocarbon We, as released by hee from the f here op the nascent hydrogen, or e, ,r oi euch h drogen, so that there rire a Humber o." hydrogen moms in Some y i die fiydromrooii moecules than found in "eis iie hydro@room wip-ors as releaeed by heatfrsii he einde. Aiso the heating of iie de ,giedueli :i i n h ioniperatm'e, in the p eeence or me J percemng o mi @im Se done by dry hear/.fen fm l 5 pmoieaiiy :di of e liydroeeii'bon oiise ww pass over :is from ehe aree or e. out 62: erea being meer@ e @d run through ai condenser to oon- .o Seide poi'ons hereo, 1; n of the hy'droexir'oon f, ionimiipreggriaed water. The ed gages uiei pees over are, of eouree,

loof; coodeuseble and also cont-ain some fior,

Sie Wider, conve eilig he ammonia ino :mb Y

moiium suiphzite.

The hydrocarbon oiis condensed :mai- "fooe ilo the weil oils and are similarly i refined amd friugtioiimed in e subaiy simiier niemeer.

is no range of' torfipemures wihin .ort which is of present vknown to be miei io the smeessfo! carrying; out or' *diie prowess. fppsiientiy e temperaiure 'of n three to four' hundred degrees Fahren i omini-aimed art the iniroduoioii or cooier of the retort. with e temperature er "imei'ng 1.490 Fahreiiheif, at die dis- 535e or heated end of the retorf, will serve h1 purpose- ;uid wiii carry out :iii the pe eereiibeore mentioned in. the manner deeerfoe The einde after being dio-,Charged from die decker e or hotter end of the retoer mi Coojeiie e considerable quantity 01S be the usual and ordinary apparatus emioyed roi* euch piirpoSeS, end the process carried out in seid :apparatus may be the snai and ordinary erocess'as generaily employed Hiere'for. In other Words, the vapors discharged from he cooler end of the re toi-, after so being discharged, may oe reatin the usual end ordinay manner, no

claim being made in 'ibis application to the further processing of the vapors, this invention residing in introducing ehe Shale et the Cooler end of e retort., iuoreaeing the hea/c hroughout its ien-deh, passing the shale succeselveiy from comer zo hotter areas and the iberzited vapors from hotter to cooler areas, and employing Water Vapor in Contact with sufiioiently heated Xed Caibons to form "-rreter ges and liberate the hydrogen for ectupozi and Wiii'i the iydioeerboii vapors, oei oiibefole described.

`What I claim to he new is: 1.,l`he process oi distilling oil bearing shale, consistinj@r in introdiuzintgr raw shale into one end oiI an elongated retort, moving the 'shale ,along the retort under constant agitation, maintaining heat Within said retort @varying from a temperature to drive off the most volatile ingredients at 'the end Vof introducton to a temperature to decompose Water in the presence oi carbon at the op- Josite end, conducting the released gases ackwarolly through progressively cooler areas, introducinzgy steam into Contact with tlie'heated ,ixed carbon residunni at the hotter end, commingling the released hy decomposition with the yreleased volatile gases, and discharging thespent shale residuum from said hotter end.

2. The process of distilling oil bearing' shale, consisting' in introducing the ranshale into onel end ot an elongated retort, suhstan tielly Without air, moving the shale along the lrevtort under constant agitation, maintain -ii heat Within said retort varying trom a temperature to dri-ve it the most volatile ingredients at the end ot inti'o ;luction to a temperature to decompose water in the presence of carbon at the opposite end, Conducting the released 2gases hackwardly 361 through progressively cooler areas, introduoinigr steam into contact with the heated fixed carbon residuum at the hotter end,- cornrninglinr the gases released by decomposition with the released volatile gases', and discharging the spent shale residuum from the hotter end substantially without admission ot air.

3. The process of distillini oil hearingp shale, consisting in introducing the ran'` shale Y40 continuously into one end ol an elongated retort, sulostantiall)v without air, movingr the Shale along the retort under 4constant agita- `tion. maintaimingr heat within said retort varying from a temperature to drive off the i5 mosty volatile ingredients at the end of introduction to a temperature to decompose Water in the presence oi carbon at the opposite end, conducting the released hack- Wardly through progressively cooler arcas.

introducingl steam iutocontact with the heated fixed carbon residuuni at the hotter end, oornmingling the ,eases released hy decomposition with the released volatile gases,

and continually discharging the spent shale residuum from the hotter end substantially Without admission ot air.`

4t.' The process oll distilling oil hearing shale, consisting in introducing raw shale into one end of an elongated retort.. moving the shale along the retort under constant cascading action, maintaining heat Within said retort varyingl troni a temperature to drive otl' the most volatile ingredients at the end ot introduction to a temperature to de compose water in the presence of carbon at the opposite end, tonducting the released gases backivardly through progressively cooler areas and through the cascaded shales introducing steam into contact with the heated fixed carbonresiduum at the hot-ter end, passing the gases released bv decomposition through the progressivel;v cooler areas to unite with the volatile at release, and discharging the spent shale resid uuln from said hotter end. i

5. The process of distilling4 oil hearing shale, consisting in introducing the raw shale into one end of an elongated retort, substantially Without air, moving the shale along the retortv under constant cascading action, maintaining heat "Within said retort rai-,ying trono a temiiernture to drive off the most volatile `in,,redients at the end o: introduction to a temperature to decompose water in the presence ot' carbon at the lopposite end, conducting the released gases back- Wardly through progressively cooler areas and through the cascaded shale, introducing steam into contact with the heated fixed carbon residuuin at the hotter end, passing thil released by decomposition through the progressii'ely cooler areas to unite With the voliatile' gasesat release, and dischargingy the spent shale residuuni from theliotter end substantially Without admi sion of air.

(fi. The process of distilling' oil bearing1 shale` consisting in introducing the raw shale` continuously into one engl of an elongated retort, suhstantiall)v without air, moving the shale alongn the retort-minierconstant cascadingaction, inaintainingli lat withinsaid retort varying troni 'ateii'iperature toy drive ol'i` the most volatile ingredients at the end ol? introduction to a temperature tocdecoinpose water in the presen of ca'roonhat the opposite end, conducting the released gases hacltwardly tlirmigh progressively Cooler areas and through the cascaded shale, introducing steam into Contact with the heated fixed carbon 'a iduum at the hotter" end, passing thil fases released hy decornvriosition through the progressively cooler areas to unite with the volatile gases at release, and contiruially discharging the spent shale rcsiduum troni the hotter end substantially Without admission o' air.

ln testimony ivliereoic l hereunto ailix rnv signature. i

EDWARD n. fserions.

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