US2132441A - Extraction of petroleum from solid materials - Google Patents

Description

Oct. 11, 1938. H ROSEN-[HAL 'l 2,13%441.

EXTRACTION OF PETROLEUM FROM SOLID MATERIALS Filed Aug. 4, 1934 l 4 ToPPlG UNIT Patented Oct. 11,

My invention relates to and .methods of extraction utilizing as solvent lo 'particularly those QS at atmospheric pressur is particularly related which EXTRACTION OF kPAT1.=;1\1'1 OFFICE PETROLEUM FROM SOLID MATERIALS Henry Rosenthal, New York, N. Y.

are normally es and tem peratures. the extraction gaseous It of petroleum oil from oil shale in a continuous manner and in a process from the extract as a part of 1,0 `rlng, and where the solvent is recov portion of the petroleum reningy p My invention provides means ,o

petroleum oil from oil shale in a simple 1,5 source oi petroleum,

must be refined and of separate products before the shale be used commercially.

is to subject the petroleum oil to high `t oil are vaporized ter fractionation 20 tures whereby portions and the vapors are recovered af Thus, the usual of the where solvent is removed the petroleum reered as a rocess.

f recovering and inexpensive manner. Where oil shale is used as a the liquid lfractionated into a product obtained number oil canmethod emperaas gasoline, kerosene, gas oil and similar products. The temperatures to which the cr be either below the point terial is subjected may take place prior to the rials into commercial cuts.

the refining operation,

containing hydrocarbon 30 propane, butane, pentane, an

rials of other series which lmay into a liquid under pressure in the usual method being drocarbons from the n 35 are associated, by mean troleum oil. These compo removed from the oil men heat and are recovered gases with 0 This material is a form .45 obtained, in.

" compound.

bilizng is a line lform of cut, the propane cut, or the cut, I use as shale oil 55 elated, r-or I may use` which they have which is a hydrocar tained underA superatmospheric from the rock with` ude ma- 25 or above the point at which pyrolytic reactions separation of the mate- YAs a by-product of there is produced a gas compounds such as d analogous matebe condensed a number of ways;

to rst absorb these hyxed gas wi th which they s of a high boiling peunds are then usually struum by means of separately from the fixed been associated.

of natural gasoline and is usually further fractionated to remove small ell as of a fraction in minating compound. fraction is also is the predominating product of this stastabilized natural gasobon liquid when mainpressure, but

ospheric pressure. These stabilized thatv is, thebutane natural solvent for removing the which it the unstabilized is assonatural fB, by which of the extractor 2. From the hopper, the crushed the sealed inlet compartment yApplication August 4, 1934, Serial No. '738,405

8 Claims. (Cl. 19E-14) a novel processpior of oilfrom oil shale boiling hydrocarbons,

recovery of the solvent from the shale may be eiiected. This separation of the solvent from `the spent shale is accomplished by converting the solvent into the vapor state. By my present 1 invention, these vapors are recovered along with lcondensable vapors produced in the petroleum refinery, in the vapor recovery section of the refinery. v

The objects of my invention,

1. To provide novel apparatus for and methods of separating a solvent from the extract in the process of extracting oil from shale.

2l. To provide novel means for recovering the solvent vapors removed from the spent shale 25 after extraction.

3. To utilize the lighter fractions of petroleum rening as an extraction medium in the removal of shale oil and to circulate these fractins substantially continuously between the ex- 30 tractor and the petroleum renery. Other ob` jects of my invention are apparent from these specifications.

My invention may best be described by reference to the accompanying drawing which is a 35 part of this specification. In this drawing Figure l is a diagrammatic layout of one embodiment of my invention.

Figure 2 is an elevation of a preferred form of extractor for use in connection with my in- 4o vention.

Referring to Figure tank l, and is delivered to extractor the valve 3.

The oil shale is delivered to the4 Crusher 4, 45 where it is reduced to proper size, which I prefer'v shall be such that the crushed material will fall through a one inch screen and will on a half inch the oil shale passes to the screenl properly graded and delivered to the conveyor it is transferred to the feed hopper 1 thus, are: 20

1, solvent is contained in 2, through oil shale is delivered through rotary valve 8 to 9 of the extractor,55

' discharged from rotary from which it passes through rotary valve I to the extraction cylinder II.

The operations within the extraction cylinder can best be explained by referring to Figure 2. The oil shaleV entering the cylinder from rotary valve I0 is passed into the rotating cylindrical compartment, I2a, by means ofthe deector vane rotating cylindrical compartment meets a strong'solution about to be discharged from the extraction cylinder il. The rotation of the compartment I 2a carries the shale forward and upward and discharges it into rotating compartment i221, where the solution strength is somewhat weaker than that in compartment I2a. In a similar manner the shale is carried reaches compartment 12d, into solvent is delivered through the valve 3. The shale, leaving compartment I2dv and delivered to the compartment I2e by defiector vane I3e, is substantially free from shale oil, butA will be wet with solvent besides carrying amounts of solvent by absorption and similar means. therotary cylinder I2e the spent shale is drained of its solvent and is passed by means of deflecto-r vane I3f to the compartment I 4. The spent shale with its absorbed solvent is passed4 from the compartment I4 to the conveyor I5. The conveyor I5 is provided withY a heating jacket I6, into which suitable heating medium is admitted through the valve I1, and discharged through While in the conveyor I5 the spent shale is heated to the rotary valve I9, which discharges the spent shale into the sealedV outlet compartment where it is subjected to a vacuum applied through pipe 2l. This vacuum acts to eliminate the sol- The solvent entering through the valve 3 into I the rotary compartment I2d, passes in contact with the shale about to be discharged from the extraction cylinder. It is then delivered consecutively to rotating cylinders I2C, I2b, and I 2a in counterow to the movement of the shale, and is then discharged from the extraction cylinder by outlet pipe 23.

Again referring to Figure 1, the spent shale is valve 22, to conveyor 24, whichV delivers it to any convenient location.

The solution discharged from the extractor through `the gure, only sufficient detail being shown to fully explain my invention.

The solution passing through valve enters the pump 29 which delivers it to the cracking still 30 where it is subjected to conditions favorable to cause pyrolytic reaction. After passing through the cracking still, the solution is delivered to the reaction chamber 3l and the dephlegmator 32, where a portion is condensed and is recirculated through the cracking still 30 by the pump 34. The vapors from the dephlegmator 32 pass into the rectification portion of the cracking unit as represented by the rectangle 33. This rectangle here represents the various fractionating columns, condensers, storage tanks paratus making up the balance of the cracking unit, including the separator in which the gases 'exhauster 55 including propane, butane etc. are separated from the liquid components. These gases with their condensable vapors are shown as leaving the cracking unit through the valve 35.

The solution passing through Valve 26 is delivered to the tube-still 36 by the pump 31. In the tube-still 36 the solution is heated and delivered to the fractionating column 38 from which as shown a number of side cuts are removed. As shown, a gasoline cut is removed from the top of the column, passed through the condenser 39 and delivered to the separator 40, the gasoline being withdrawn from the bottom of the separator through valve 4I and the vapors and non-condensable gases including propane and butane are Withdrawn from the separator through valve 42.

The vapors and ing unit through gases removed from the crackthe valve and/or removed 4from the topping unit through the valve 42, are

delivered totheA vapor recovery unit 43. This may be of any well known type and therefore only sufficient detail is shown to explain the op eration in connection with this invention. The rectangle 44 represents the usual-absorption unit with the necessary absorbers, compressors, stills, tanks, condensers, etc.V The liquid product comprising propane, butane and pentane is Withdrawn from the absorption unit through the pipe 45 to the stabilizer or column 46. The fixed gases', dissolved in the liquid which is delivered through pipe 45, are removed through pipe 41. The stabilized gasoline is removed from the bottom of the column and delivered to the tank 48. Propane vapors may be removed through valve 49 or butane vapors through valve 50, and delivered to the condenser 5I, in which they are liquefied and fromrwhich the liquid is delivered to tank 52. The propane or butane may be delivered to the solvent storage tank I by opening valve 53, or the natural gasoline may be delivered to tank I by opening valve 54.

The exhauster 55 is connected on its suction side to the sealed inlet compartment 9 and removes therefrom solvent vapors Which enter the compartment 9 through the rotary valve I0 and the air which enters the compartment 9 through the rotary valve 8. I prefer that exhauster 55 be so adjusted that the pressure maintained withinY the sealed inlet compartment 9 be slightly above the pressure of the atmosphere. The compresses the gases and vapors recovery unit 43.

Exhauster 51 is connected on its suction side with the sealed'outlet compartment 20. I prefer exhauster 51 be so adjusted that it maintains Within the outlet compartment a pressure of less than half a' normal atmosphere. gases and vapors removed by exhauster 51 from the sealed outlet compartment 20 are compressed comprises dissolving'shale-oil in a hydrocarbonn;

' oil shale while said hydrocarbon liquid that is gaseous at normal temperatures and pressure by contacting the oil-shale with said hydrocarbon delivered and applied to said is in the liquid phase, maintaining said hydrocarbon in the liquid phase while in contact with said oil-shale; withdrawing the solution; subjecting the solution,while said solution still containssubstantial amounts of the solvent, to the action of heat at such temperature that pyrolytic reactions take place; then separating the solution into fractions, including one fraction of the character of the solvent used; and returning a portion of said fraction to the dissolving step.

2. The method of extracting oil-shale which comprises, dissolving shale-oil in natural gasoline by contacting the cil-shale with natural gasoline delivered and applied to said oil shale while maintained in liquid phase, maintaining said natural gasoline in the liquidphase while in contact with said oil-shale; withdrawing the solution, then subjecting the solution, while it still contains a substantial amount of said solvent, to the action of heat at such temperature that pyrolytic reactions take place; then separating the solution into fractions including one fraction analogous to said natural gasoline; and returning a portion of said latter" fraction to the dissolving step.

3. The method of extracting oil-shale which comprises dissolving Vshale-oil by contacting said oil-shale with butane delivered and applied to said oil shale while maintained in the liquid phase, maintaining said butane in the liquid phase while in contact with said oil-shale; withdrawing the solution; then subjecting the solution, while it still contains a substantial amount of butane, to the action of heat at such temperature that pyrolytic reactions take place; then separating the solution into fractions, including one fraction of "butane; and returning a portion of said butane fraction to the dissolving step.

4. The method of extracting oil-shale which comprises dissolving shale-oil by contacting said oil-shale with propane delivered and applied to said oil shale while maintained in the liquid phase, maintaining said propane in the liquid phase while in contact with said oil-shale; withdrawing the solution; then subjecting the solution, while it still contains a substantial amount of said propane, to the action of heat at such temperature that pyrolytic reactions take place; then separating the solution into fractions including one fraction of propane; and returning a portion of said propane fraction to the dissolving step.

5. The mtehod of extracting petroleum bearing solid material which comprises dissolving a portion of the petroleum in a hydrocarbon liquid that is gaseous at normal temperatures and pressure by contacting the petroleum bearing solid material with said hydrocarbon delivered and applied to said petroleum bearing solid material while said hydrocarbon is in the liquid phase, maintaining said hydrocarbon in the liquid phase while in contact with said petroleum bearing solid material; withdrawing the solution; subjecting the solution, while said solution still contains substantial amounts of the solvent, to the action of heat at such temperature that pyrolytic reactions takey place; then separating the solution into fractions, including one fraction of the character of the solvent used; and returning a portion of said fraction to the dissolving step.

6. The method of extracting petroleum bearing solid material which comprises, dissolvinga portion of the petroleum in natural gasoline by contacting the petroleum bearing solid material with "natural gasoline delivered and applied to said petroleum bearing solid material while maintained in the liquid phase, maintaining said-natural gasoline in the liquid phase, while in contact with said petroleum bearing solid material; withdrawing the solution, then subjecting the solution, while it still contains a substantial amount of said solvent, to the action of heat at such temperature that pyrolytic reactions take place; then separating the solution into' fractions including one fraction analogous to said natural gasoline; tion of said latter fraction to the dissolving step.

'7. The method of extracting petroleum bearing solid material which comprises dissolving a portion of the petroleum by contacting said petroleum bearing solid material with butane delivered and applied to said petroleum bearing solid material while maintained in the liquid phase, maintaining said butane in the liquid phase while in contact with said petroleum bearing 'solid material; withdrawing the solution; then subjecting the solution, while it still contains a substantial amount of butane, to the action of heat at s-uch temperature that pyrolytic reactions take place; then separating the solution into fractions, including one fraction of butane; and returning a portion of said butane fraction to the dissolving step.

8. The method of extracting petroleum bearing solid material which comprises dissolving a portion of the petroleum by contacting said petroleum bearing solid material with propane delivered and applied to said petroleum bearing solid material While maintained in the liquid phase, maintaining said propane in the liquid phase while in contact with said petroleum bearing solid material; withdrawing the solution; then subjecting the solution, While it still contains a substantial amount of said propane, to the action of heat at such temperature that pyrolytic reactions take place; then separating the solution into fractions including one fraction of propane; and returning a portion of said propane fraction to the dissolving step.

HENRY ROSENTHAL.

and returning a por-y

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