US1343674A - Distillation of petroleum-oils - Google Patents

Distillation of petroleum-oils Download PDF

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US1343674A
US1343674A US133871A US13387116A US1343674A US 1343674 A US1343674 A US 1343674A US 133871 A US133871 A US 133871A US 13387116 A US13387116 A US 13387116A US 1343674 A US1343674 A US 1343674A
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vapors
still
condenser
distillation
valve
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US133871A
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Robert E Humphreys
William M Burton
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Standard Oil Co
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Standard Oil Co
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G9/00Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
    • C10G9/06Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils by pressure distillation
    • C10G9/08Apparatus therefor

Definitions

  • FIG. 2 is anenlar ed horizontal sectional; view thrfough'the aph jflgm by which'i'the Stoker-controller is governed;
  • -F1g. 5 is an enlarged section throu h the needlevalve by'which the vapors of istillation are admitte'd'td the final condenser.
  • the numeral ' designates a furnace structure, and the numeral .11 a mechanical or automatic stoker for" firin thesame.
  • astill 12 to beheated thereby, which still may be of the form illustrated in the patent to Robert Humphreys' (one of the present applican 'No. 1,122,003, or may be of any other convenient-form.
  • a vapor-conduit 13 leads rearwardlyand upwardly, and is surmounted by .an aircondenser in the form of a radiator 14, all
  • the said valve we prefer to needle 27 with an extended ro -connection.
  • Gay-Lussactower 21' whih may be filled with crushed quartz, coke brother inert material forming a permeable bed.
  • a gasoutlet pi e 22 is connected with the top of top and bottom ofthe' tower Intermediate the length of the vapor-"pipe 15 there is inserted a ressure-control valve '70 the Gay: ussac tower and liquid inlet and, outlet p1pes23, 24 are connected with the,
  • the pipe 15 has tapped rovide the thereinto a pressure-conduit 31 which leads tothe lower side of the diaphragm chamber 32 (Fig. 2).
  • a flexible and imperforate diaphragm 33, mounted horizontally within the said chamber has attached to its center a rod 34 carrying a knife-edge 35, which bears against the lower face of a balance beam 36, fulcrumed on a knife-edge 37, as shown in Fig. 2..
  • the free end of the beam 36 carries suitable weights which may be arranged in the usual manner to secure accurateloading of the beam. Midway of its. length thebeam supports a stirrup .38,
  • a condi1it'- 4O connects a port in this casing with the base of a cylinder 41, from which power is derived for operating the valve of the Stoker-en no, as will later appear.
  • The.ad-- mission 0 -fl1iid under pressure to the conduit 40, or the exhaust of fluid therethrough,
  • valve 39 ise'ffected by the movement of thevalve 39, the latter being provided, for instance, -w1th straight andangular passages 42, 43,
  • a piston 46 operates, the piston-rod thereof being connected, as illustrated diagrammatically in Fig. 1, with one end of a rocking-lever li' journaled in suitable supports above the still.
  • One end of the lever 47 is connected, as by the chain 48, ⁇ vith a lever e19 which actuates the throttle-valve ,of .a, steam -engine 50, whichfis belted to drive the necl'ianical stoker "11.
  • a second chain connection 51 which the flow of air for combustion in the V Method of operation.
  • valve 27 maybe closed and the heating continued until a pressure of four atmospheres or upward, depending upon the'specific-character of the charge under treatment, is reached.
  • this desired normal operating pressure has been. reached is the needle-valve 2?.will be. slowly opened to permit the "vapors to'pass to the condenser 16, where they are condensed, the
  • the balance-beam 36 is permitted to fall, thereby admitting fluid under pressure to the cylinder 41 and elevating the piston 4-6 therein.
  • the connections engine 50 is thereby opened, permitting the engine to accelerate andto drive the'stoker 11 at a faster rate, whereby the supply of fuel to the furnaceis increased.
  • the damper 52 will'be opened to supply the increased amount of air required for the higher rate of combustion. This more energetic firing of the furnace 10 will continue until the increased evolution of vapors within the still has raised the pressure therein to the predetermined point, and, upon this pressure being attained the Stoker-en- 'gine will be automatically slowed down and the damper returned to,the normal position. Conversely.
  • any increasein pressure within the .still will operate through the connections described to decreasethe speedv of thestoker and correspondingly restrict the supply of air to the furnace grates.
  • These latter elements are so designed and proportioned as to condense from the outgoing, stream of vapors and to conof a. distillate collected.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Description

R. E. HUMPHBEYS AND W. M. BURTON.
DISTILLATION 0F PETROLEUM OILS.
APPLICATION FILED NOV. 28, I9I6. 1,343,674. Patented June 15, 1920.,
S-SH E] I.
'zaaerz, .212? 376 I L-zz;
R. E. HUMPHREYS AND W. M. BURTON.
DISTILLATION OF PETROLEUM OILS.
APPLICATION FILED NOV. 28, I916.
1,343,674. Patented June 15, 1920.
2 SHEElS-SHEEI 2.
UNITED I STATEiliTE-NT OFFICE.
I 301mm E. HUMPHREYS, or. WRITING, INDIANA, AND WILLIAM mncnron, :or omcae -xnnmom, ass cnons TO 'rnnsreunann on. COMPANY, or CHI; GAGO, ILLINOI S, A conrona'rxon or INDIANA.
DISTILLATION F PETROLEUH-OILS.
Application filed November 28, 1916. Serial No. 133,871.
cerned with a distillation processinwhich relatively hea are treated un er high temperatures and petroleum hydrocarbons pressures for thepurposelof effectin their conversion into relatively light h orocarbo'n s, the object of our invention emg to secure the lar est possible yield of light hydrocarbon o the desired character, at a minimum cost of treatment. The manner in which this object is accomplished by our invention will be fully understood from the following specification, taken in connection with the accompanying drawings, in which-' Figure 1 isa side elevation'of a'still and its connected apparatus arranged for carrying out our invention, the showing being :Iargely diagrammatic; Fig. 2 is anenlar ed horizontal sectional; view thrfough'the aph jflgm by which'i'the Stoker-controller is governed; Fig. 3 is an 'enlar ed section through the stoker control va ve; 4 is an enlarged section through the cylinder of the stoker control mechanism; and -F1g. 5 is an enlarged section throu h the needlevalve by'which the vapors of istillation are admitte'd'td the final condenser.
Referring more particularly to the drawings, the numeral 'designates a furnace structure, and the numeral .11 a mechanical or automatic stoker for" firin thesame. Above the furnace 10 there is mounted astill 12 to beheated thereby, which still may be of the form illustrated in the patent to Robert Humphreys' (one of the present applican 'No. 1,122,003, or may be of any other convenient-form. From the still a vapor-conduit 13 leads rearwardlyand upwardly, and is surmounted by .an aircondenser in the form of a radiator 14, all
of the conduits of which are so arranged as to drain their condensate backwardly.
Specification of Letters Patent.
tate of Indiana,-
-. the said valve we prefer to needle 27 with an extended ro -connection.
Patented June From the top of the radiator 14; a Gag outlet pipe 15- is carried, this pipe fee the final condenser 16, which Wlll ushally be mounted in a water-bath '17,;as' illus trated. The condensate from the condenser 16..drains into a-receivin -drum- 18, from which it may be drawn 0' intermittently through'the gasolene main continuously or 19. The upper end of the receivin sdrum 18 has tapped thereinto a pipe 20 whic leads into the lower portion'of the body of a. 1
Gay-Lussactower 21', whih may be filled with crushed quartz, coke brother inert material forming a permeable bed. A gasoutlet pi e 22is connected with the top of top and bottom ofthe' tower Intermediate the length of the vapor-"pipe 15 there is inserted a ressure-control valve '70 the Gay: ussac tower and liquid inlet and, outlet p1pes23, 24 are connected with the,
respectively. I z
25, which is prefer-ab y of the construetion illustrated in Fig. 5, having an exceedii-igly small valve aperture 26, the size of whlch may be accurately controlledby a needle 27. For the convenient manipulation of 28 through which the valve may be controlled from the ground level as by means .of'the hand-wheel 29, operating through the miter gears 30. I
' Between the radiator 14 and pressurecontrol'valve the pipe 15 has tapped rovide the thereinto a pressure-conduit 31 which leads tothe lower side of the diaphragm chamber 32 (Fig. 2). A flexible and imperforate diaphragm 33, mounted horizontally within the said chamber has attached to its center a rod 34 carrying a knife-edge 35, which bears against the lower face of a balance beam 36, fulcrumed on a knife-edge 37, as shown in Fig. 2.. The free end of the beam 36 carries suitable weights which may be arranged in the usual manner to secure accurateloading of the beam. Midway of its. length thebeam supports a stirrup .38,
which through a suitable link-connection operates a piston-valve 39, vertically reciprocable within a cylindrical casing. A condi1it'- 4O connects a port in this casing with the base of a cylinder 41, from which power is derived for operating the valve of the Stoker-en no, as will later appear. The.ad-- mission 0 -fl1iid under pressure to the conduit 40, or the exhaust of fluid therethrough,
ise'ffected by the movement of thevalve 39, the latter being provided, for instance, -w1th straight andangular passages 42, 43,
respectively, arranged in the manner shown in Fig. 3 and adapted according to the psition of the valve to connect the conduit 40 with a fluid-pressure pipe 4st In with an I furnace 10 is controlled.
-ofjthe nature of exhaust pipe 45.
Within the cylinder 41 a piston 46 operates, the piston-rod thereof being connected, as illustrated diagrammatically in Fig. 1, with one end of a rocking-lever li' journaled in suitable supports above the still. One end of the lever 47 is connected, as by the chain 48, \vith a lever e19 which actuates the throttle-valve ,of .a, steam -engine 50, whichfis belted to drive the necl'ianical stoker "11.
from the lever 1T operatesa damper 52, by.
A second chain connection 51 which the flow of air for combustion in the V Method of operation. In utilihing the apparatus above described :t'or the purpose of converting relatively high" boiling-point petroleum hydrocarbons,
such, for instance, as fuel-oil, gas-oil, or the'like residues, into lighter hydrocarbons gasolene, the procedure is as follows:
' The still 1 2 having been charged with-a quantity ofsuch heavy hydrocarbons, the
furnace 10 is fired, and the automatic or mep 1 chanical stoker 11 is putintooperation to continuously supply tothe furna'cethje normal amount of fuel. During the' initial heating of the charge within the still 12,
that is, up to the time when this charge reachesa temperature of 300 F. orthereaboutytheneedle-valve 27 is preferably kept wide open in order that any small 7 quantitiesbf low-boiling point liquids present'in' the charge,and more especially any, .-waterj which may. have become accidentally admixed therewith, may be freely driven off.
llhen the above-mentioned temperature has been reachedthe valve 27 maybe closed and the heating continued until a pressure of four atmospheres or upward, depending upon the'specific-character of the charge under treatment, is reached. l-Vhen this desired normal operating pressure has been. reached is the needle-valve 2?.will be. slowly opened to permit the "vapors to'pass to the condenser 16, where they are condensed, the
condensed distillate draining into'the receiving-druin 18.
collected in the reservoir 18 is dependent to an extraordinary degree .upon theregu larity with which the distillation process .is' conducted, small variations in the temperature and pressure and rate of evolution I 'of vapors within the still causing wholly disproportionate variations. in the character" We find that thequalityof'the distillate" fact we find it .of the'utmost practicalim- :portance to control the operation of the distillation apparatus with the greatest degree of-accuracy. The desired results are ob tained by the apparatus illustrated through themanual operation of the needle-valve 27 controlling the discharge of vapors from the upper end of the air-condenser, and by the automatic operation. of the Stoker-coninstance, if the pressure within the still drops. below the predetermined operating pressure the balance-beam 36 is permitted to fall, thereby admitting fluid under pressure to the cylinder 41 and elevating the piston 4-6 therein. -Through the connections engine 50 is thereby opened, permitting the engine to accelerate andto drive the'stoker 11 at a faster rate, whereby the supply of fuel to the furnaceis increased. Simultaneously the damper 52will'be opened to supply the increased amount of air required for the higher rate of combustion. This more energetic firing of the furnace 10 will continue until the increased evolution of vapors within the still has raised the pressure therein to the predetermined point, and, upon this pressure being attained the Stoker-en- 'gine will be automatically slowed down and the damper returned to,the normal position. Conversely. any increasein pressure within the .still will operate through the connections described to decreasethe speedv of thestoker and correspondingly restrict the supply of air to the furnace grates. Bythe proper manlpulation of'the needlevalve127, and through the automatic control of the firing of the furnace, we find it possible to accurately regulate the progress of the distillation,conversion, and separationtaking place within the still 12 and the con- 'nectedinclined vapor conduit 13 and radiator 14. These latter elements are so designed and proportioned as to condense from the outgoing, stream of vapors and to conof a. distillate collected. In view .ofthis "illustrated the throttle-valve of the stokers tantly return to the still for further treatment therein those constituents of the mixture of hydrocarbon vapors which is evolved in the still which have not undergone sufiicient decomposition, while permitting all of those constituents which have been slifii I i ciently converted to pass without condensation. Inasmuch as the reflux fractionating condenser, made up of the elements 13 and- 1.5 vapors passing from the still must be con- 14 ,is capable of effecting an accurate and complete "separation "between,..the vapors which have been sufiiciently decomposed and-those which have not been sufliclently decomposed only when ItheIr-ate of flow of the vapor current pastthe condensing. surfaces closely approaches the normal or. predetermined rate of'flow for which the condenser was designed, it will be, understood that in view of this consideration alone the utmost accuracy of regulation ofthe process of distillationis required. This requirement of accuracy or regularity ofaction will be better understood when it is stated that ap proximately seventy-five per cent. of the stantly condensed and returned-to the still b the reflux fractionating condenser, only a out twenty-five per cent. ofsuch vapors passing the' valv e 25. It is therefgre' aparent that if the rate ofdistillation should e so increased as to permit only 2% more vapors to pass through the conduitI3' -andthe tank 18. So also, if the pressure is per mitted. to risefisli htly, the resultant decreased rate. ofevjo ution of vapors (assuming that the firing remains the same) will cause a considerable; proportion of the sufficiently decomposed vapors which should passthronlgh the condenser to becondensed therein.
by which they .are either cracked into incondensable gas or otherwise detrimentally affected. ;For these physical reasons only,
therefore, and without regard to theserious resultsfrom a chemical standpoint which. are entailed by'relatively minute or inconsiderable .variations" in the distillation and conversion process, it is important for the certain proportion of the vapors produced wlthin the still are of such a character that they fail to condense under these conditions,
and such vapors collect in-the space above the liquid in the receiving-drum 18; From this drum they are led through the pipe 20 {into the bottompf the Gay-Lussac tower 21; to pass upwardly through the interstices of the material within the tower. In their upward progress they meet a downwardly I flowing current of a suitable absorbing menv struum. such, for instance, as a finished or refined naphtha, the specific gravity of. which. it is desired to lower. -By reason of' the'intimate contact between the] gas and hose desirable'constituent's, being returned to the still,- suffer fui'therichange the liquid thus afforded a considerable proportion of the gas becomes absorbedin the liquid, enriching the latter and lowering its specific gravity. The ihcondensable gas which has failed of absorption f escapes through the pipe 22 and may. be led to a gasometer 'or directly to affurnace to be used as gaseous fuel; The enriched naphtha is withdrawn from the bottom of the tower through the pipe'24. I
-While we have shown and described in considerable detail onespecific form of apparatus for-carrying out our invention, together with the QXflCfPIOGBdUIGItQbG fol lowed in the use. of this apparatus-'in the treatment of agiven class of raw materials for obtaining a particular product, it is to be understood that the foregoing is by way of'illustration..only and for the purpose of making the nature and objects of the in vention more clear-and that the invention is not to be regarded asliniited to the illustrativeprocess described except in-so far as. such limitations are included within the terms of theaccompanying claims, inwhich it is our intention. to claim all novelty inf herent in our invention as broadly as is permissible in'view of the prior art.
What we claim as new and desire to secure by Letters Patent, is
1. Theprocess ofwdistillin'grelatively heavy petroleum oils to obtain therefromrelatlve'ly light oils which consists in subr i ng a liquid-body of such heavy 011 to distillatiomleading ofl theevolved vaporsElOO through a reflux fractionating condenser int free communication with the still, restricting the outlet from the said-condenser to maintain a pressure of upward of 4 atmospheres in thesame and in the still to which it is connected, causin said condenser to continuously condense rom the mixture of vapors therein substantially all insufficiently decomposed products without condensing any substantial proportion of sufiiciently def composed products, by controlling such rel.
;.stri'cted outlet, and condensing and collect ing the sufliciently decomposed vapors which:
pass the said restricted outlet. 1
2'.' The' process ofdistilling relatively heavy petroleum' oils to obtain therefrom relatively light oils, which consists in .sub-
-'jecting a *li uid body of such heavy oil to distillation, eading ofi the. evolved vapors through a reflux fractionating condenser in.
free communication with the still, restricting the outlet from the sa-idcondenser to maintain a pressure of upward of 4 atmospheres in the same and in the still to which it is connected, causin vapors therein substantially all insufiiciently decomposed products without condensing 1 anysubstantial proportion of s'ufiiciently decomposed products, .by controlling such resaid condenser to continuously condense. rom the mixture of s'tricted outlet, passing-the Vapors escaping 'it is connected; causing said condenser to continuously-condense" from the mixture of ,v'apors therein substantially all insufliciently from the said outlet through a condenser, collecting the condensate, and subjecting the uncondensed vapors to the action of vextensive surfaces of "an absorbing menstruum.
3. The process of distilling relatively heavy petroleum oilsto obtain therefrom relatively light oils whichzconsists'in sub jecting a liquld body of such heavy oil to.
distillation, leading olf'the evolvedvapors through arefluxfiractionating condenser-in free communicationwith the still, restrict ing the outlet from the said condenser to; maintain a pressure of upwardof 4,at'1nos-- pheres in the some and in the which decomposed" products Without condensing 1 any. substantial proportion ofs'u fliciently decomposed products, by control-ling such re: striated outlet, condensing and collecting .the sufficiently decomposed, vapors .Whieh pass the said restricted outlet, and a'utomati-' Cally controlling the heating of the 'still by the vapo'rpressure therein; 1 V
, .ROBERT HU lHPI-IREYS.
WILLIAM MJBURTON.
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