US769681A - Process of treating oils. - Google Patents

Description

No. 769,681. PATENTED SEPT. 6, 1904. A. G. CALKINS.

PROCESS OF TREATING OILS.

APPLIOATION FILED SEPT. 2a, 1902.

no MODEL.

WVz'frzeail QM (I C /M 5 $63. W AM ffZ/Wfl UNITED STATES Patented September 6, 1904:.

PATENT FFICE.

ALBERT C. CALKINS, OF LOS ANGELES, CALIFORNIA, ASSlG-NOR OF ONE- HALF TO HENRY E. BRETT, OF LOS ANUELES, CALIFORNIA.

PROCESS OF TREATING OILS- SPECIFICATION forming part of Letters Patent No. 769,681, dated September 6, 1904.

Application filed $eptember 23,1902. Serial No. 124,583. (No specimens.)

To (LZZ who/1t it WMLZ/ concern:

Be it known that LALB ear G. UALKINs, a citizen of the United States, residing at Los Angeles, in the county of Los Angeles and State 5 of California, have invented certain new and useful Improvements in Processes of Treating Oils; and I do hereby declare the following to be a full, clear, and exact description of the invention, such will enable others skilled in the art to which it appertains to make and use the same.

This invention relates to improvements in the process or method of treating and retining of oils and similar fluids, and 1 )art-icularly 5 such oils as contain asphaltum and similar impurities and which it is desired to treat by acid whose oxidizing effect upon the anilin coloringmatter in the oils is beneficial and which acid will also percipitate the asphaltum,

so that the treated oil will be suitable in quali ty and color for lubricating stock; and one of the objects of this invention is to produce a process or method which will avoid the loss of the lighter distillates during the treatment of the oil.

Another object of the invention is to use the agitating medium more than once in a complete circuit and to use the lighter serials in combination with a fluid as an agitating me- 0 dium.

'ith these and other objects in view the invention consists, essentially, in the method or process hereinafter more fully described, and substantially as illustrated in the accompanying drawing, showing one form of apparatus that may be employed in carrying out the process or method.

.In the treatment of oil containing asphaltum it is found that even after distillation a cer- 4 tain amount of asphaltum will remain in the oil, and the treating process must be resorted to to eliminate what remains. Ordinarily the excess of residual acid is neutralized by the use of some alkali, such as caustic soda, and

these successive operations are all performed in a tank havinga conical bottom and suitable connections for drawing 03' the precipitated acid compounds, &C. The mixing of the acid with the oil is performed by means of a blow- 5 ing-engine arranged to deliver air or other agitating medium through a pipe leading down into the tank or receptacle, so that the violently-rising air creates active ebullition in the tank and exposes all of the oil to the action of the acid. In fact, the action of the air practically atomizes the oil and acid and makes as perfect a mixture and exposure to the acid as can be obtained by mechanical means. lVhen this operation is performed in a tank or receptacle open at its top, a large percentage of the lighter fractionsin the oil is necessarily evaporated and driven off with the air, which is being constantly forced up through the oil, and this loss is serious in the treatment of oil containing light distillatcs which are 5 used for their explosive nature in gasolene and vapor engines, as these lighter serials that are so readily evaporated and carried off by the.

. air frequently constitute the most valuable part of the distillate for engine use. 7

By means of this invention the loss of the lighter distillates is avoided by treating the oil in a closed treating tank or receptacle and withdrawing the air or agitating medium forced in by the blowing-engine to again supply such engine, so that there will be a com plete circulation or circuit of the air or agitating medium through the tank.

Referring now to the drawing forming part of this application, there is shown one 30 form of apparatus which may be employed in carrying out the herein-described process or method, although this invention is in no manner limited to use with such apparatus.

Upon the drawing the reference character 5 1 designates a tank or other treatingrecepta cle, preferably provided with a top or cover 2, completely closing the tank, in which there may be formed a manhole 3 to afford access to the interior of the tank or receptacle, which 9 latter may be supported upon any suitable structure by means of brackets 4, and the tank 1 may be provided with a suitable valved outlet 5 for the purpose of withdrawing any asphaltum or tarry compound, and the tank or receptacle is preferably unobstructed interiorly by any cross-plates, partitions, or other barriers. A suitable pipe or connection 6 may be provided, preferably at the top of the tank, through which the oil may be introduced thereinto, and a connection 7 may be provided between the top of the tank and any suitable form of blowing-engine 8 or equivalent device to supply air to the blowing-em gine, and a discharge-pipe 9 is preferably secured in and depends from the top of the tank to nearly the bottom thereof in order to liberate the air or agitating medium at or near the bottom of the tank or receptacle, so that the same can rise therethrough and agitate the contents thereof, as Will be readily understood.

Connected with the exposed end of the discharge-pipe 9 is a suitable pipe 10, communicating with the blowing-engine 8, so that the air or agitating medium is forced by the engine 8 through the pipe or connection 10 into and through the discharge-pipe 9, from which the air or agitating medium is liberated to rise, substantially as hereinbefore explained.

The pipe or connection 7 is preferably provided with a suitable cut-off or valve 11 for the purpose of closing the suction-pipe or connection 7 whenever it is desired to use the same in the manner now in vogue, which may be done by removing the cover of the manhole 3 and turning said cut-off or valve 11 so as to admit air therethrough to the engine 8, whereupon the engine will take air in the ordinary manner, and the air will escape through the manhole after having passed through the contents of thetank or receptacle.

It is found that after an asphalt-base oil has been run or distilled for the asphaltum contained the distillate or the product from which the asphaltum has been eliminated by distillation still contains from ten to twenty per cent. of tarry matter that can only be removed by acid treatment, and the tarry compound which is precipitated out of the distillate by a sulfuric-acid treatment is of a consistency of heavy coal-tar, and as the precipitations of the tar commences the moment the acid comes in contact with the oil it is only necessary for the tank l'to be entirely unobstructed interiorly, as otherwise it would immediately clog and it would be impossible to remove the tar.

1n the use of the construction herein shown and described the precipitated compounds settle into the conical bottom of the tank 1 and are drained off through the large outlet pipe or connection 5, which is desirably provided with a cook or cut-off 12 of any suitable construction. The consistency, thickness, and volume of the tarry material which is removed by the acid treatment is such that in the treatment of heavy asphaltic oils the outletpipe 5 is preferably made of large diameter to facilitate the withdrawal of this material.

By the use of the closed unobstructed tank described and shown herein should the oil being treated be too heavy and viscous to permit air agitation a volatile oil may be added to thin the heavy oil and none of the added volatile oil will be lost. during the agitation.

None of the vapor taken up by the air is removed or condensed by the apparatus herein shown and described, and no fresh air is admitted during the treating operation; but the treatment is effected without any loss of distillates and without the admission of any atmospheric air after the operation has commenced, and in case too much pressure should accumulate in the tank by the rapid generation of sulfurous-acid gas the tank may be vented through the valved pipe or connection 6, which may also be employed for supplying oil to the tank; but oil may also be introduced through the manhole 3, if found desirable in practice.

The operation of this invent-ion in connection with the apparatus illustrated in the accompanying drawing is substantially as follows, to wit: First a suitable amount of oil is introduced within the treating tank or receptacle, and the desired quantity of sulfuric acid is added or supplied, whereupon the sulfuric acid will be broken up or be decomposed when it comes in contact with and attacks the oil containing the carbon compounds in solution. and when the acid decomposes a large percentage of sulfurous-acid gas is generated, but is prevented from escaping into the outer air by reason of the tank or receptacle being closed. This sulfurous-acid gas is withdrawn through the suction-pipe 7 by the action of the blowing-engine 8 and is forced back to the treating tank or receptacle through the connection 10 into and through the dischargepipe 9 and liberated at the bottom of the treating tank or receptacle in such a manner as to cause this gas to rise up through and agitate the contents of the tank, as will bev readily understood.

By means of this process or method of treat ing oil the sulfurous-acid gas is passed and repassed through the oil, whereby a double effect is attained of precipitating the tar and acid compounds thereof, as Well as having the benefit of the bleaching effect of the sulfurousacid gas, which is known to be one of the best, if not the greatest, of bleaching agents, and by means of this invention it is possible to so pass and repass the sulfurous-acid gas through the tank without any material change in the gas, as all condensing agents between the tank and the blower are avoided.

By means of this process or method there is secured a return of the generated sulfurousacid gas in bleaching-and treating the oil for color, and this gas will be generated in the treatment of the oil by the acid for precipitating the tarry matter in the oil, substantially as before described.

From the foregoing it will appear that in the apparatus herein shown and described there is an interiorlyunobstructed treating tank or receptacle to prevent clogging by the precipitated tarry matter, a closed treating tank or receptacle to avoid the loss of any light distillates and to provide means whereby air or an agitating medium may be forced 3 again and again through the oil or material to be treated in a continuous circuit and the j sulfurous-acid-gas fumes be returned through and through the mass of oil without subjecting the user to the loss of the light distillates.

From the foregoing description and the accompanying drawing it will be understood that this method or process of treating oil or other materials consists substantially in sub jecting the oil to the action of acid within a closed interiOrly-unobstructed treating tank or receptacle to produce a precipitation of the tarry matter in the oil, then to produce an upward circulation of air from the bottom to the top of said tank by means of a blower. whose suction-pipe is connected with the top of the tank while its discharge-pipe discharges to the lower portion of the tank, the suction and discharge pipes being free of condensers, so that the oil may be acid-treated and may be subjected to the blowing action for producing ebullition without the loss of the lighter distillates and the sulfurous acid gas generated within the tank may be returned through the same means used in producing the ebullition without any resulting condensation of the gas.

It is not desired to confine this invention to the specific apparatus herein shown and described for carrying out this process or method, as it will be understood that any suitable apparatus may be employed for this purpose without departing from the spirit and scope of this invention.

1 claim- 1. The herein-described process or method of treating oil or other fluids which consists in confining the oil within a closed treating receptacle or tank; subjecting the oil to the action of sulfuric acid to precipitate tarry matters within the oil withdrawing the sulfurousacid gas generated within the tank and return- I ing the same to and through the contents of l the tank to bleach and agitate the oil.

2. The herein-described process or method of treating oil or other fluids which consists in subjecting the oil to the action of an acid while in a closed treating receptacle or tank introducing an agitating medium through. the oil; withdrawing the lighter vapors from above the oil and returning the same together with the agitating medium and evolved gas to and through the oil and acid to facilitate the treatment of the oil.

3. The herein-described process or method of treating oil or other fluids which consists in subjecting the oil to the action of an acid; then introducing an agitating medium through the oil and returning to and through the oil and acid in a continuous circuit the agitating medium and fluids generated by the action of the acid to agitate the acid and oil.

4:. The herein-described process or method of treating oil or other fluids which consists in subjecting the oil to the action of sulfuric acid while in a closed treating receptacle or tank; withdrawing the air and the evolved gas from above the oil and passing and repassing the same continuously up through the oil and acid to agitate the oil and acid and to subject the oil to the bleaching action of the evolved gas.

5. The herein-described process or method of treating oil or other fluids which consists in confining the oil within a closed receptacle; subjecting the oil while in such receptacle to the action of sulfuric acid to precipitate the tarry matters in the oil; withdrawing the air above the oil and liberating the same below the oil to rise therethrough and agitate the same and finally passing and repassing the con1- mingled air and sulfurous-acid gas evolved by the action of the acid on the oil to bleach the oil by the action of said gas.

In testimony whereof l have signed my name to this specification, in the presence of two subscribing witnesses, at Los Angeles, in the county of Les Angcles and State of California, this 12th day of September, 1902.

ALBERT (J. GALKINS.

\Vitnesses:

AMELIA UrUusT, R. E. BRINKER.

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