US1863346A - Automatic engler distillation apparatus - Google Patents

Description

Jun 14, 1932- J. E. MOORE ET AL 1,863,345

AUTOMATIC ENGLER DISTILLATION APPARATUS Filed April 4, 1931 3 Sheets-Sheet l rgg l 3 t .15-

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J. E. MOORE ET AL 1,853,346

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June 14, 1932. J MOORE ET AL 1,863,346

AUTOMATIC ENGLER DISTILLATION APPARATUS Filed April 4, 1931 5 Sheets-Sheet 5 llllli' [ll/8W5: P S John EMoora George WC/ZiZLCG/,

Patented June 14, 1932 units!) STATES PATENT oFricE" Joan E. MOORE, or CHICAGO; rumors, AND enonen w. CHENIGEK, or HAMMOND, INDIANA, ASSIGNORS TO srANnAn-n OIL coMrAnY, or CHICAGO, rumors, Acon- 40? once characters,-

-mod1v.cat1on shown in Flgure 3.

IPO'RATION OF INDIANA AUTOMATIC ENG-LEE DISTILLATION APPARATUS Application filed April 4:, 1931. Serial No. 527,710.

This invention relates to distillation apparatus and it pertains more particularly to automatic means for making the standard Engler distillation teston petroleum oils.

The object of our invention is to eliminate the personal equation from the standard distillation testsso that results on any given oil maybe duplicated more exactly. A further object is to provide an equipment which will be substantially foolproof and which will automatically record the desired infor mation so that it may be operated by inexperienced-persons,and so that a large number of tests may be run simultaneously by one operator. A further object is to provide an improved means for recording the results of distillation tests. Other objects will be apparent as the detailed description of our invention proceeds.

In practicing our invention we provide a system of automatic electric controls for regulating the heat input so that the distillation will proceed at a predetermined uniform rate. The results are automatically recorded on a clock driven graph, one curve showing the temperature at any given time and another curve showing the percent distilled off at any given time. Fromthese curves the percent distilled off at any given temperature can be directly read. The temperature indicator is controlled by current through a thermocouple and the percent distilled indicator is controlled by current through a resistance which is varied by a float in the condensate receiver. The invention will be more clearly understood from the following description of a preferred embodiment thereof.

in the accompanying drawings, wherein similar parts are designated by like refer- Figure 1 is a diagrammatic illustration of our improved invention showing the elec trical circuits involved,

Figure 2 is a chart illustrating the recorded results of an Engler distillation.

Figure 8 is a diagrammatic illustration of another embodiment of our invention, and

Figure 4 is a chart illustrating the results of an Engler distillation recorded on the The conventional. distillation flask 10 is.

provided with a side arm 11, and a Water cooled condenser 12 of the usual type, and the apparatus is set up as directed by the A. S. T. M. specifications. The condenser discharges into a condensate receiver 13, which may be a graduate or other cylindrical vessel. The flask is heated by an electrical resistance heater 14, the temperature of which may be varied throughout a wide range by means of pivoted contact arm 15, the heater being connected directly through wires 17, 18, 19 and 20 to the alternating current source 21, which is preferably the standard 110 volt 60 cycle system. The current to this heater and to the entire apparatus may be turned off or on by means of switch 22.

lVires 22 and 23 lead from wires 18 and Q this circuit will depend upon the type of rectifier used. I e

Wire. 25 leads from oneend ofthe transformer secondary to rectifier 26, which is in turn connected by wire 27 to mercury column 28 which is mounted at the side of distillate receiver 13. A similar mercury'column 29 is mounted on the other side of the receiver and a U-shaped resistant unit 30 is adapted to move up and down in these columns in acordance with the amount ofdistillate in receiver 13, the top of the resistance unit being connectedby anelement 31 to float 32. r

The two legs of the resistance unit 30 may be made of any suitable resistance metal, and if additional length is required it may be formed into a helical coil. As the distillate in the receiver increases in volume, the resistance unit will be moved upwardl out of the mercury (we may provide a suitable counter-balancing weight, not shown, whereby the resistance unit will be at substantial equilibrium in all positions so that it may be:

raised or lowered without a large amount of The other end of coil 34 is connected by wire 36 to magnetic coil 37 which is, in turn, connected by wires 38 and 39 to spaced contacts 40 and 41. A pivoted lever 42 is adapted to make contact with points 40.01 4111s will=be hereinafter described, and-this pivoted "lever is connected by wire 43 to the other .endol th .transfq ner seconda y .iln p rgforming h stand rd Eagle distillation test'it is necessary that a certainrate of distillation be maintained. In order to record the percent off with respect vto ,time, we provide a clock driven graph or chart 44 provided with time indicating increments 45, temperature indicating increments 46 and percent 'o'fl' indicating increments 47 (see igu-re T he-temperature is recorded by'a suitable pen 48. This pen is driven by asuitable operating mechanism (not shown) which is connected by wires 49 and 50 to thermocouple 51 in the neck of flask 1O opposite theopeningofside arm '11.

The-clockworks (=notshown) are suitably connected to rotate contact arm 52 around the circular resistance element 53. This resistance element is connected through resista-nce 54 and wire 55 to wire 27 (the positive side of the rectified circuit). The movable contact arm is-connected by wire 56 through magnetic coil 57, wire 58, wire 39, contact points 40 or 41, lever 42 and wire 43 to the negative side of the rectified circuit.

order that the apparatus may be automatically shut oil when the given temperature is reached we provide a series of points 59 adapted to be contacted by arm 60 which moves with the temperature recording pen 48. Points 59 are connected by conductors 61 to points 62 so that each point 62 corresponds to a given temperature. The switch arm 63 may beset on predetermined point 62 so that when the corresponding point 59 is contacted by arm 60, a direct current will flow through wire 64, wire 65, switch operating coil 66, wire 6? and wire 55 to the other side of the rectified circuit.

The operation of our improved apparatus is as follows; A measured amount of oil is poured into flask 10 and the flask is stop pered and closed up in accordance with A T. specifications. Contact arm 52 is set back of resistance 54 and the clock works are started, The exact position of the contact arm need not be determined with 5 great accuracy but we prefer to have the apparatus so regulated that contact arm 52 will be at the point where resistance 54 taps resistance 53 when the first drop of liquid is distilled. We then close the'switch 22 which turns on the heater 14 and raises the liquid in flask 10 to distillation temperature. The temperature of the vapors in the neck of the flask is recorded by pen 48. When the first drop of liquid drips from the end of the con denser it is caught by a cup 68 which is mounted on one end of lever 42. The weight of this drop causes the lever to swing from contact arm 41 to contact arm 40, thus breaking for an instant the rectified current flowingithrough wire 39, wire 38, coil 37, wire 36 and indicator coil 34. The e'fiectzof this interruption is to cause the indicating pen tomake a sharp mark on the graph (see Fig- 11.r i2.)-

In practice, we prefer to hold the lever against contact arm 40 "by a magnetic coil (not shown) connected in the circuit, so that we will not have to rely upon the weight of the first drop of liquid in cup 68 to continuously hold the lever in operative position.

As the distillation .continuesthe condensate gradually buoys up float 32,'which in turn raises resistance :30 .out of the mercury, thereby increasing the resistance of the percent ofl circuit and decreasing :the current flow through operating coil '34. Pen 35 is thus moved upwardly at a rate which corresponds exactly :to the percent distilled off. If desired, we may increase the current flowing with an increase of condensate; this may be done by mounting the receiver :on a floating resistance unit so that each increment of liquidreceived makes the resistance unit sink further into the mercury, thereby decreasing its eflect.

It should :be noted that this circuit is connected in parallel with the circuit which contains resistance 53 so that changes in this resistance do not change the readings of the percent off curve,

If't'he liquid distills at too rapid a rate, the current flowing through coil 57 will be greater than the current flowing through coil 37.- These coils act magnetically to control the position of contact arm 15, and in this event will shift the arm from medium to low anddecrease the temperature of the heater. On the other hand,if the distillation rate is too slow, the current through coil '37 will be greater than the current through coil 57 and in this event the contact arm 15 will be moved from medium to high. It will thus be seen that we have provided. an automatic means for controlling the temperature of the heater'in accordance with the rate of distillation.

As above stated, contact arm 63 may be set at any desired temperature and when the temperature arm 48 reaches this point, arm 60 will close the circuit through switch operating coil 66 to automatically disconnect the whole system fromthe source of power.

The modification shown in Figure 3 is designed to operate on a slightly different principle. In this system the heater is opcrated in such a manner that the distillation proceeds at a predetermined rate, the clockdriven graph is started when the first drop of liquid drips from the condenser and the temperature is plotted against time. This In this system we provide a fixed base 69 supporting a vertical post 70 and a rotatable screw 71 parallel to post 70 and journaled in bearings 72 and 73. A carriage 74 fits over post 70 and screw 71, and it is internally threaded so that it may be driven by screw 71 to reciprocate up and down on the post. Carriage 74 carries contact arms 75 and 76, which are insulated, from each other and which are a fraction of a centimeter apart. Near the top of post we provide a guide 77 for positioning wires 78; this wire is moved up and down by float 32 and it carries a contact point 78A which is adapted to fit between contact arms and 7 6.

Screw 71 is connected by a shaft or chain 79 to the clock works whichldrives the graph 80. The particular means of driving the screw by the clock works is immaterial and it will not be described in detail.

WVire 19 is connected to one side of the heating element by wire 81. Wire 17 is connected to an intermediate point of the heating element by wire 82 and to the other end of the heating element by wire 83. A relay operated switch 84 normally closes the circuit in wire 82 and it is held in operative position by spring 85. Another relay operated switch 86 is adapted to close the circuit in wire 83,

but it is normally held out of operating position by spring 87. The relay which operates switch 84 is connected by wire 88 to battery 89, and thence by a fine wire 90 to wire 7 8, on which is mounted contact point 7 8A. The

, other side of the relay which operates switch 84 is connected by wire 91 to contact arm 7 5.

The relay which operates switch 87 is connected by wire 88A to wire 88, battery 89, wire 90 and contact point 78A. The other side of this relay is connected by wire 92 to contact arm 7 6. Pivoted lever 42 is connected by wire 93 to battery 94 and thence by wire 95 to solenoid 96, which is, in turn, connected by wire 97 to a contact point with which lever 42 is adapted to engage. Solenoid 96 is adapted to pull operating lever 98 to start the clock mechanism.

The operation of this embodiment is as follows: A predetermined amount of oil is placed in the flask and the apparatus is set up in accordance with A. S. T. M. specifications. Operating switch 22 is then closed, and since switch 84 is normally closed, a current will flow from wires 17 and 19 to the heator 14. The resistance elements in the heater between wires 81 and 82 are designed to give a relatively high heat, a heat which would be normally sufficient to effect distillation at the desired rate.

When the first drop of condensate drips 65 from the condenser arm 11 into cup 68 on lever 42, it closes the circuit in wire 93,-battery 94, wire 95, solenoid 96 and wire 97, and the action of the solenoid on starting lever 98, starts the clock. Up to this time the temperature indicator is moved out on a radial line from thecent-er of the graph (note Figure 4) so that the point on the graph at which the temperature curve leaves the zero radial line is the temperature of the first drop. The clock works, acting through mechanism 7 9,rotates screw 75 to lift carriage 74, and the pitch of the screw thread and diameter of the receiver are designed so that the carriage will move upwardy at a rate corres onding to the desired rate of distillation (that is, the desired rate of the elevation of float 32). If the distillation rate is too slow, contact arm 7 6 will. close circuit through contact point 7 8A to actuate relay operated switch 86 and increase the temperature of the heater. This increase in temperature is large enough to cause-increased distillation suflicient to raise float 32 and thereby disengage point 78A from arm 76. On the other hand, if the distillation proceeds too rapidly, point 78A will contact with arm 7 5, and switch 84 will be opened to shut off the heat entirely. It will be seen that the constant opening and closing of switches 84 and 86 will automatically insure distillation at a constant rate, so that the time increments plotted against the temperature and that the 1 temperature is automatically regulated in accordance with the percent distilled. While we have disclosed preferred embodiments of our invention it is understood that we do not limit ourselves to thedetails therein. set forth except as defined by the followingclaims.

We claim: 1. In adistillation system, means for automatically recording the distillation temperature with respect to time, and means for automatically recording percent off with respect to time whereby the percent oil may be directly read for any temperature.

2. In distillation apparatus, means for moving a graph at a uniform rate, means for automatically recording distillation temperatures on said graph, and means for automatically recording percent distilled off on the same graph so that the temperature will be automatically plotted with respect to percent off.

3. In distillation apparatus of the class described, means for automatically recording the distillation temperature with respect to time, means for recording percent oil withrespect to time, and the second named me ans including means to automatically record the time at which the first drop is distilled.

4:. In' distillation apparatus, a distillate receiver, an electrical circuit, a percent off indicator controlled by said circuit, and means controlled by the amount of condensate in said receiver for varying the resistance in said circuit and thereby varying the position of said indicator.

5. In an apparatus of the class described, means for heating a still, two parallel direct current circuits, means for increasing the resistance in one circuit at a constant rate, means for varying the resistance in the other circuit in accordance with the amount of condensate, and means responsive to changes of current flowing in one circuit relative to current flowing in the other circuit for controlling the said heating means.

6. In a distillation apparatus of'the class described, means for moving a chart at a constant rate, electrically operated means for recording on saicl chart the percent distilled. an electrical circuit connected thereto, and means actuated by the first drop of condensate for momentarily opening said circuit whereby a record is made by said indicator means. i

- 7. In combination, a distillation apparatus, an electrical circuit including two contact points, a pivoted lever adapted to alternately contact said points, and means on said lever for receiving a drop of condensate whereby the lever is caused to move from one contact point to the other;

8. In distillation apparatus of the class described, a condensate receiver, a mercury column adjacent said receiver, a resistance unit extending into said mercury column, and means for varying the immersion of the column in accordance with the amount of condensate in the receiver.

9. In a distillation system of the class described, a heater for a distillation flask, electromagnetic means for controlling the temperature of said heater, two coils operatively associated with said temperature control, means for changing the current flowing in one coil at a constant rate and means for is varied in proportion with the amount of,

liquid which has been distilled.

11. In distillation apparatus of the class de-' scribed, means for heating. a flask; electromagnetic means for controlling the temperature of said heater, a source of direct current, means for connectingtwo circuits in parallel across said direct current source, an electromagnetic coil in one circuit, a variable resistan'ce in the same circuit, means for varying said resistance at a uniform rate, an electromagnetic coil in the other circuit, a variable resistance in said other circuit, means for varying said resistance in accordance with the amount of liquid distilled, an indicator coil in said second circuit, means for moving a chart at a uniform rate, means actuated by said indicating coil for indicating on said chart the percent of said liquid distilled, and means for automatically and simultaneously indicating on said chart the distillation temperatures. V i e I I In witness whereof we have afiixed our signatures. a v JOHN E. MOORE.

GEORGE W. CHENICEK,

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