US2525051A - Distillation method and apparatus - Google Patents

Description

Oct. 10, 1950 K. 1.. sToRRs DISTILLATION METHOD AND APPARATUS 3 Sheets-Sheet 1 Filed July 19, 1946 I'll/8111 01 K/NDRED L. STORRS By W I WWW Oct. 10, 1950 Filed July 19 1946 I K. L. STORRS DISTILLATION METHOD AND APPARATUS 5 Sheets-S eet 3 upon the degree of refining Patent Oct. 10, 19

s. PATENT orrice nrsrnlm'rron'mmnon Ann armaa'rus Kain-eat. Storrs, new, City. Utah Application .luly 19, 194 Serial N0.'684,720 1 1.1mm (Cl. some This. invention reiates'to the separati n or 7 showing the means for collection and withdrawal volatile 'constituents'from distillab1e' material,

such as coal, by heating the same in a retort and conducting the evolved vapors to condensing means. 7

During the progress of the material through the retort, different volatile constituents are progressively and continuously released from the material and vaporized in different temperature ranges or heat zones, and the different vapors thus evolved are separately and continuously conducted from the respective heat zones to separate condensing means. In this way, substantially purev different vaporized constituents or fractions are separately evolved and. collected, so

I that subsequent fractionation of the condensates is made unnecessary or minimized, depending of fractionation desired.

All grades or kinds of any particular type of material do not have the same constituents, nor

are the respective constituents always released within the same temperature ranges. It is thus apparent that, in order to properly treat a particular kind or grade of material according to the method disclosed in my aforesaid pending application, it is necessary to first determine the constituents of that particular material and the particular temperature range in which each constituent is released or evolved, whereby the apparatus used may, be eorrectlyregulated to suit the-manna. W a. The primarygobject; of {the present-invention, therefore-is to provide a practical methodof and j a paratus for treatinganyparticularkind of distiliablematerialto recover the constituentsthereof and to determinej'the particular heat range in which eachlconstituent{9Quch material is reg leased.

a further'obiectis {to pi-otid' sheare and as paratus of the above kind whereby the treating operation may 1 be easily and'quickl'y' carried out in a reliable manner;

a More specific objects and features of'the'invariation will become apparent from the following description when considered in connection the accompanying drawings, in, which:

Figure 1 is a'fragmentary view, partly in side 'j elevation and partly in section, showing a retort in section on line'la-tof Figure 1;

I Figure 8 is afrastuebtarv perspective view 5-1 frame 5 having a top 6 in the form of a slab of refractory material. Mounted on the frame above the slab 6 and by suitable means I is an endless trough 8 containing fluent material 9 and provided with a refractory lining and bottom facing Ill. A further slab ll of refractory material is mounted on the frame above and in spaced relation to the slab 6 and spaced from and within the confines of trough 8, by suitable means it. Mounted on the slab H are electrical heating elements i3 supplied with current by use of an attachment cord it. Mounted within the confines of trough 8 above the slab ii and heating elements I3 is a vertically reciprocable vibrating pan l5 adapted to receive the material to be treated or analyzed. The pan is has a rim l6 which is provided on its outer edge with a depending flange ii that extends into the trough 8 below the level of the fluent material 9. Mounted on the trough 8 by suitable means It is a hood l9 having an outer vertical wall 20 that surrounds the flange ll of pan I5 and depends within the trough a beneath the level of the fluent material 9; Thus, a fluid seal is provided which prevents escape of gases from the retort between the pan l5 and hood i9 and permits the vertical reciproca- '=tion of said pan relative to said hood. The hood l9 has a suitable opening to facilitate introduction of the distillable material into pan l5, which disk 21 is secured on each shaft 26 between the adjacent bearings 25. Mounted for vertical movement-between the retort and the slab 6 is a. transverse horizontal rod 28 whose ends are engaged by the cams 21, and which has upstanding supports 29 rigid therewith and fixed to opposite sides of the pan l5. An adjusting screw ,30 is slidable through each end of the rock shaft 23 and adjustably threaded into the adjacent end of rod 28. Adjustable on each screw 30 above'the shaft 23 is an abutment washer 3|. A helical compression spring 32 is disposed on each screw 30 between the shaft 23 and the adjacent washer 3|,

and these springs act to yleldingly raise the rod 28 and keep it against the cams 21. Journaled in the lower portion of frame 6 is a transverse horizontal shaft 33 having its ends operatively connected by chain gearlngs 34 with the outer ends of cam shafts 26. Mounted within the frame directly above shaft 33 is a motor operatively connected to shaft 33 by gearing 36 and supplied with current by use of an attachment cord 36'. It wil be apparent that motor 35 may drive the cams 21 to intermittently depress the rod 28 and then allow it to be raised by the springs 32. In this way, pan i5 is rapidly vibrated in a vertical direction so as to correspondingly vibrate the material being treated relative to the pan, and to thereby uniformly heat and rapidly distill the material.

Merely vibrating a mass of finely divided material in some fashion to bring about a condition which has frequently been described as ffluidized," is old and well known. However, there is a wide range of difference in the character of the vibrations when it is desired to attain specific results. The system of vibration involved in the method of the invention as accomplished by the mechanism illustrated and described in the present case is particularly effective to accomplish applicant's unique purpose. This purpose is to cause a mass of finely divided material particles to be so thoroughly disseminated that as faras possible each individual particle shall be effectually exposed to the processing conditions.

The vibratory action of the present mechanism is explained as follows:

The cam shaft 26 is mounted in bearings that are axially fixed center to center with reference to a stationary shaft 23. Seated on the shaft 23 are compression springs 32 and resting on the springs is a vibratory system consisting of a transverse rod 28 having fixed upstanding supports 23 upon which latter is fixed a pan l5 that is designed to contain the finely divided material for processing. The rod 28 does not rest directly on the springs but is supported on adjusting screws 30 which are threaded in the rod 28. Screws 30 pass freely through the springs 32 and through the shaft 23. Also, the screws 38 are provided with abutment washers that bear on the top of the springs and react against lock nuts threaded on the screws. Fixed on the cam shafts 26 are cam disks 2'! the mutually reactive stress of which against springs 32 is taken up by the supports 24 which hold the centers of shafts 23 and 26 fixed relatively to each other.

Each complete rotation of the cam disks results in a cycle of motion consisting of two substantially vertical strokes, one down and the other up. The downstroke is exerted mechanically by the cam disks, and the upstroke by the potential energy stored in the springs during the downstroke. The peculiar nature of the strokes, presently described, characterizes an inventive feature. For example, in Figs. 1 and 2, the rotation of cam disks 2! may be regarded as occurring in cycles repeated indefinitely. A cycle may start when the low part of the cam is in contact with rod 28. Rotation of the cam disks until the high part of the disks contact rod 28 defines a downward may carry the rod 28 somewhat lower than the peripheral point of the cams for the reason that the energy stored in the springs for the upstroke cannot be brought into action sufllciently fast to allow the rod 28 to closely follow the periphery of the cams. Thus, there is a small interval of time during which the fast-moving periphery is free of contact with rod 28, but this freedom continues only until the potential energy stored in the springs asserts itself and causes the rod 28 to be returned to contact with each cam periphery and to strike the same with a sharp hammer impact. This impact jolts the bottom of the pan l5 and shoots the particles upwardly into the desired cloudlike dispersion which brings about the rapid and thorough absorption of heat by the material particles.

A small interval of time at the bottom of a downstroke, where the spring tension is free of cam influence, is not dependent on the momentum of the descending load, but occurs in a degree because the slope of the cam periphery away from its high point, as well as the angular velocity of the cam, determines the point where contact is resumed. Thus, the intensity of the impact that sends the material particles into a shower and the nature of that shower can be nicely determined by recognizing the shape of the cam curve, its angular velocity and the tension of the spring as chief contributing factors to the desired end.

The vibrations produced by the apparatus of the invention are characterized by the sharp hammer-like jolts imparted to the processing pan.

After the desired end temperature has been reached and the treatment has been completed, the pan i5 may be tilted so as to cause the residue to flow from the latter by gravity. At the front, the pan l5 has a depending outlet spout 31 that extends through the slab 6 and into a fluid seal receptacle 38 removably supported on the underside of said slab. A gate valve 39 having a suitable opening means 48 controls flow of the material to the spout 31. The means to tilt the pan I5 may consist of an adjusting screw 4i threaded through a bracket 42 fixed to the frame 5, said screw 4i having a universal connection 43 with a stem 44 secured to an ear 45 rigid with the lower front portion of one of the supports 24. By adjusting the screw 4i, the shaft 23 may be rocked so as to move all parts carried thereby and to accordingly tilt the pan l5 forwardly or return it to a horizontal position. Suitable means 46 may be used to indicate the position of the pan I5.

The hood l3 has a plurality of top outlet pipes 41 and 48 for the evolved gases, each leading to and extending downwardly through the stopper 49 of a separate removable sampling condenser receptacle 58. Each of the pipes 41 and 48 may depend into a body of 'water provided in the associated receptacle 50 to the level indicated at 5|. Outlet pipes 52 may extend upwardly through the stoppers 49 from points above the water level and connect to the inlet of the motor driven suction pump 53 whose outlet 54 may lead to desirably located condensers and reservoirs. Interposed in each of the pipes 41 and 48 between the hood I9 and receptacles 58 is a shut-off valve 55.

In practice, a desired quantity of the distillable material is-introduced into the pan l5 through the opening of hood l9 closed by cover 2|. The heating elements I3 may then be energized and motor 35 is laced in operation so as to cause the pan l5 to be rapidly vibrated in a vertical direction. the sate 28 being closed. The heating ele- 'through outlet spout 31.

ments. II supply a predetermined amount of heat which is not varied or regulated. As the pan II is vibrated vertically, the finely divided or fluent material being treated is given a similar vibration so as to repeatedly rise and fall at uniform intervals relative to the bottom heating surface of pan II. In this way, the particles of material being heated have heat transferred from the bottom or heating surface of pan i thereto, in a rapid and uniform manner. As the operation continues, the temperature of the material gradually increases until the end point of a given temperature range is reached. One of the, valves 55 is then opened and the pump 53 is thrown into operation so as to draw the evolved gases from the hood l9 into the associated condenser receptacle 50, some gases being drawn, through the associated pipe .52, inlet pipe 5!, pump 58, and outlet pipe 54 for condensation and. collection. The valve 55 which has been opened is then closed and the other valve 55 is opened, and the active condenser receptacle 50 is withdrawn from its stopper 49 so that the sample condensate therein may be obtained, an unused receptacle 50 being substituted for that which has been removed. When the other valve 55 is opened, the operation is continued so as to obtain, in the second receptacle 50, and in the same manner, a sample of the condensate of the vapor evolved during the next higher heating stage. This cycle of operation is continued through successive higher stages of heat until the end temperature of the entire method or operation is reached.- By careful operation of and attention to the apparatus, it can thus be readily ascertained as to what vapors are evolved during each of the particular temperature ranges so that proper data may be obtained for progressivedistillation of the same material according to the continuous method disclosed in my aforesaid pending application.

, Upon completion of the distillation operation, the

heating elements iii are rendered inoperative and the pan I5 is tilted byactuation of screw 4| so 1 that the residue of the operation may be discharged from pan I! through spout 31 upon opening gate 38 by actuation of the opening means "I thereof. During the distilling process, the fluent seal of the residue collection receptacle 381 prevented escape of gases from the retort By taking samples of the evolved vapors at relatively short intervals or teni ature change, it can be readily ascertained wh the end temperature for each range of temperature should be in continuously distilling the same material according to the method and with the type of apparatus disclosed in my above mentioned co-pending application, thereby enablin'g the operator of the'latter apparatus to properly operate and regulate the same.

From the foregoing description, it will be seen that the present method contemplates withdrawing the volatile constituents as they are evolved from the material during the different and successively higher temperature ranges, the volatile constituent evolved during each temperature range being prevented from mixing with that evolved during the previous or succeeding temperature ranges. In this way, substantially pure fractions are obtained directly from the retort at different periods of time while the temperature of the material is being raised to the desired final end temperature. I

Modifications, and changes in details of contiti'uction of the apparatus. are contemplated.

such as fall within the scope of the invention as claimed.

What I claim is:

1. The method of separating volatile constituents from a discrete distillable material, which comprises the step of vertically vibrating the material in cycles, each cycle consisting of a downstroke and an upstroke, the downstroke being characterized by mechanical actuation exerted against a yielding tension while the upstroke is characterized by being actuated wholly by the energy stored in the yielding tension during th downstroke, the said upstroke further being subject to the deceleration of gravity acting upon the vibrating mass subjecting said material to a predetermined degree of heat so as to raise the temperature of each particle of the material to the, desired end temperature, thereby causing different volatile constituents of the material to be successively evolved during a plurality of increasing temperature ranges; and separately collecting the volatile constituents evolved at predetermined temperature ranges.

2. The method of separating volatile constituents from a discrete distillable material according to claim 1, wherein a sample of each of said volatile constituents is separately condensed as it is collected.

3. An apparatus for separating volatile constituents from a discrete distillable material, comprising a closed retort provided with a vertically reciprocative receptacle for the material, said receptacle having a bottom heating surface; vertically reciprocative means including a support for the vertically reciprocative receptacle; spring means disposed to exert upwardly directed force upon said support; rotatable cam means operative downwardly upon said support in opposition to the spring force; driving means operative to rapidly rotate the cam means so as to vertically vibrate said receptacle; means to heat said bottom surface to a predetermined end temperature; a suction device operative to separately draw from the retort the volatile constituents evolved during each of a plurality of temperature ranges; and means operative to condense and collect each volatile constituent in the order drawn off.

4. The construction defined in claim 3, wherein is included a bottom outlet for said receptacle, valve means for controlling passage of residue from the receptacle to said outlet, and means operative to tilt the receptacle so as to cause flow of the residue to the outlet after opening said valve means.

5. The construction defined in claim 3, wherein the retort includes a stationary hood provided with outlets for the evolved volatile constituents; and a seal between said receptacle and the hood.

6. The construction defined in claim 3, wherein the retort includes a stationary hood provided with .outlets for the evolved volatile constituents; a seal between the receptacle and the hood; a shut-off valve in each outlet; and wherein the sample condensing and collecting means includes a removable receptacle interposed in each outlet beyond the associated shut-off valve.

7. A method of separating volatile constituents from a discrete distillable material comprising the step of vertically vibrating the material in cycles, each cycle including a mechanically actuated downward stroke exerted against an upwardly directed yielding tension and an upward stroke which is substantially free of the mechanical actuation, but is actuated by the en- 7 ergystoredinthe yielding tensionduringthe downward stroke; subjecting said material during vibration to a predetermined uniform degree of heat suflicient for rapidly and uniformly bringing each particle of the material to the desired end temperature which causes the material so vibrated and heated to rapidly release its volatile constituents.

KIIINDRED L. BTORRB.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS Number Name Date 1,352,696 Roberts Sept. 14, 1920 1,438,039 Rodman Oct. 24, 1922 1,552,539 Brouder Sept. 8, 1925 1,983,943 Odell Dec. 11, 1934 OTHER REFERENCES Badger and McCabe, Elements of Chemical Engineering," 2nd Edition, published 1936 by McGraw-Hill Book Co. (Copy in Library of Congress, pages 335 and 336.)

U. 8. Bureau of Mines, Bulletin 249, Methods of Testing Shale Oil," published 1929 by Government Printing Ofllce, Washington, D. 0., pages 1-28. (Copy in Div. 25.)

Images