US848903A - Art of distilling. - Google Patents

Description

PATENTED APR.- 2, 1907: H. HIRZBL. ART OF DISTILLING.

APPLICATION FILED PEB- 1, 1900- 2 SHEETS-*SHEET 1- No. 848,903. PATENTED APR. 2, 1907.

H. HIRZEL. ART OF DISTILLING.

APPLICATION FILED FEB. 1. 1900.

2 SHEETS-SHEBT 2.

UNITED STATES PATENT OFFICE.

ART OF DISYTILLINGI Specification of Letters Patent.

, Patented A ril 2, 1907.

Application filed February 1, 1900. Serial No. 3,610,

To all'whom it may concern.- Be it known that I, HEINRICH HIRZEL', a citizen of the Republic of Switzerland, residing at Leipzig-Plagwitz, in the Empire of Germany, have invented cer-tain new and useful Improvements in the Art of Distilling; and I do hereby declare the following to be a full, clear, and exact description of the invention, such as will enable others skilled in the art to which it appertains to make and use the same. I

The present invention relates to the art of distilling mineral oils and productssuch, for example, as etroleum, tar, and the like; and the object of fhe same is to carry out this distilling process free from danger and in a continuous manner, the mineral product being treated in column apparatus and being exposed at all points to the action of heated air or indifferent gases or vapors.

In the process and apparatus covered in my. application for Letters Patent of the United States, Serial No. 637,226, filed May 19, 1897, the gases or liquids are caused to pass through a column apparatus, while at the same time dry steam is carried from the bottom to the top of the column and brought into direct contact with the gases or liquids to be treated. Since under this treatment it is unavoidable that water of condensation is formed and caused to mix with the petroleum or tar distillation products or other distillates, by this means the distillates cannot be obtained free from water, so that it is often very difiicult, particularly in the case of petroleum lubricating-oils, heavy tar-oils, &c., to separate these distillates from the water which they contain. Another disturbing factor is the fact that the residual tar products,

which flow out of the column, are always more or less mixed with water in spite of their high temperature, for the reason that fine bubbles or globules of water are forced out of the steam into the thick tar and having once penetrated the same cannot be eliminated. Such Water-containing tar is unsuitable for many uses. The same difficulty takes place in the distillation of petroleum, in which after distilling off the heavier oils a residue containing water is left, such residue not being capable of being further utilized and treated V on account of its percentage of water.

The-present invention, which is designed to remove the above disadvantages, consists in passing heated air into the heating-columns in lieu of steam in those cases where no danger of ignition or explosion exists and in other cases in passing heated indifferent inert gases (that is, gases which have no'chemical combining action on the material being treat ed) through such columns, such heated air or gases acting similarly to thesteam without, however, producing a residue from the distillation containing water. The air or gases simply escape from the distilling apparatus after the distillate has been condensed and collected by the cooler and, if desired, ass to a gasometer or tank, so as to be availa le for repeated use. r

My invention, moreover, consists in such other features as will be hereinafter described, and pointed outin the claims.

In carrying my invention into effect a column apparatus is employed which is distinthinner sheets, because it is not necessary to cover any steam-coils. 'This is a matter of considerable importance and advantage in many cases where it is desired to heat rapidly and to a high temperature. Moreover, since the several column-trays may be made more'shallow more of such trays may 1 be arranged in a column apparatus of the same.

height, hence making the same far more 'effective than the former forms of column apparatus.

In the accompanying drawlngs I have represented a column apparatus embodying the preferred form of carrying out my invention.

In the drawings, Figure 1 represents avertical central section of such column apparatus, and Fig. 2 a horizontal section of the same. Fig. 3 is a diagrammatical View of a petroleum-distilling apparatus, illustrating one application of my invention; and Fig. 4, a similar view of an appartaus embodying my invention as applied to' the distillation" of tar.

In the drawings, a is thefeed-orific'e for the mineral substance to be distilled, and I is the IIO inlet for the heated gases to be used in the distillation, while i is a valve or cock which regulates' the flow of the said heating-gases channels or chambers 6, (shown in section in Fig. 2,) which communicate with the steampipes d, which pipes are controlled by the cut-off valve d, by which the steam may be admitted to or cut off from the heating chambers or channels e. The trays c are each provided with openings or throats c, as illustrated by Figs. 1 and 2, the edges of the trays being flanged upward around said openings, as will be clear from the drawings. Over these openings are placed hoods f in'the nature of baffle-plates, whereby the vapors, gases, or air may pass upward through the respective openings or throats in the trays and be deflected downward into intimate contact with or through the liquid in the corresponding trays. The liquid proceeds from one tray to the other step by step by means of the overflow-pipes g, as shown, and the column residue passes out of the column through the exit-pipe b in the bottom of the same, while the hot air or indifferent gases introduced at Iescape through the opening is steam in the roof or dome of the column, carrying with themthe distillates.

My new process offers peculiar advantages when employing a system of columns heated to different temperatures for the distillation of petroleum,-as shown in Fig.3., Thereby a continuous distillation and one which is entirely free from danger is obtained. The petroleumto be treated under this process is first led into a distilling-column 1, which is not directly heated by flame, but indirectly by ed through suitable coils, whereby the volatile constituents of the same-the benzin, so called-are driven off. Thereafter the petroleum, which has been freed of its most dangerous and explosive constituentthe benzin-is' carried into a distilling-column m of the type shown in Fig. 1, with separate heating-trays, which will permit a heat ing of the oil to a temperature of from 150 to 160 centigrade, while at the sametime a moderate amount of heated air or gases pass through the column from belowthat is to say, an amount of air or gases, suflicient to produce enough air-current in the column to enable the said air orgases to pass from the bottom to the top of the column. The temperature of the said heated air or gas ispreferably about the same temperature as the. column.

I The passage of these gases through this column causesthat fractioh to be distilled ofi, which under ordinary distilling 1; I processes over a free flame or fire Wlll OIllY boil at a much higher temperature, (between 150 and 300 centigrade.) step furnishes illuminating petroleumv or kerosene, while out of the bottom of taining the heavy oils and the paraflins.

This

thecolumn there passes off a residue con- The lamp petroleum or kerosene driven from the column in this manner is distinguished by the fact that it requires much less sulfuric acid for refining than the product hitherto distilled from the alembic, and in some cases it even enables one to dispense with the use of sulfuric acid entirely for this purpose.

The distillate is, moreover, distinguished by its feebler and mild odor, its light color, and

particularly by the fact that it is entirely free i from paraffin, a result which has hitherto been impossible toattain'in the distillation do not distiloff from below 300 to 360 cen-' These distillates contain the lubrij eating-oils and parali'ins, and these products tigrade.

when obtained from my column under my process are distinguished by much greater purity than those obtained heretofore and may-therefore be manufactured intoproducts of a very high grade. Moreover, greater yield of these products is obtained and also a better, completely-undecomposed etroleum residue which is exceedingly well a apted for heating purposes and for the manufacture of oil or naphtha gas. For the distillation of tar I also make use of several column a paratus of the kinddiereinbefore describe as shown in Fig. 4.that is, a column apparatus having heated tray-bottoms through ICC which heated air or gases are carried in the amounts required. The tar for this pur pose is preferably subjected to a preliminary eating or warming--as, for example, by a steam-coil 0, placed in areservoir 1), containin said tar--and is then passed through a distil ing-column g, like that shown in Fig. 1,

which is substantially the same as used for the distillation of crude benzene or benzol.

out of the wash-oil which has been saturated with the same. In this column apparatus q the tar isheated to from 108 to 115 centirade, and from it is obtained as distillates the action usually designated as light oils. in

good condition. The residual tar which drains out of this column and which has been .de-

prived of its light oilsin the, above manner is now forced into a second column a, which is also like that shown in Fig. 1, by means of a grade.

pump s and While in a heated condition. In this second column apparatus the trays are heated to ahigher temperature. Here also the heated air or gasescirculate throughthe column apparatus from the bottom to the top, their heating capacity being such that the tar which circulates from the top to the bottom is heated to from 150 to 160 centi- The fraction distilled from this column contains the so-called middle oils that is to say, those ingredients which in ordinary distillation will notpass ofi at a temperature lower than from 200 to 300 centigrade. This fraction is distilled off in a perfectly pure condition and without any admixture of oils having a high boiling-point, such as anthracene and the like. The se aration of the middle oils from the heavy oils, which, as indicated above, do not distil off at a column temperature of from 150 to 160 centigrade, is surprisingly sharp and well defined. Moreover, no products of decomposition are formed, so that from this distillate the various ingredientssuch as, for example, carbolic acid and the samemay be obtained in a pure condition far more readily than with a corresponding distillate of a distilling alembic heated over a fire or by direct heat. By my invention one is also enabled to obtain the light oils and middle oils together as one fraction if the tar is distilled from a column heated to from 150 to 160 centigrade. After the tar has passed through such a column and the residue, which has been deprived of the light and middle oils, is drained the same contains only the heavy oils, together with pitch. The heavy oils may also be driven off by means of a column having heating-coils of sufficient heating effect in the trays. For this purpose the tar as it passes is heated to from 175 to 180 centi-- grade, steam of about ten atmospheres pressure being employed for heating the columntrays. The distillate from a column heated in this manner will contain such oils and products as would only be distilled off at temperatures between 300 andv 360 centigrade under ordinary forms of distillation over a direct fire or flame. This column distillate is again free from products of decomposition, and therefore much richer in valuable ingredientssuch, for example, as anthracene and the like.

The employment of a combination of individually-heated column-trays and air or in-v difi'erent gases in contact with the substance to be distilled is entirely new in its application to column apparatus for tar distillation.

Under this process every variety of air maybe distilled by the continuous process without the employment of direct fire or flame,

and it enables one to separate different fractions of distillation for a further treatment and to collect the same.

A very important advantage flowing from the application (5f this new invention -to the distillation of tar resides in the fact that from fifteen to twenty per cent. more distillate is obtained from the same than in the ordinary these products are obtained in the best c'ondition possible with less difficulty and expenditure of time and purifying means than hitherto. Where the tar distillation is carried on in connection with coke-furnaces, the gases from the coke-furnaces may be directly employed as the inert gases to be passed upward through the column. This involves considerable economy, and, moreover, these gases are particularly adapted to the distillation of tar.

A further advantage of the new distilling process for mineral oils, such as etroleum, as well as for tar in the same, is t at it may be carried on with perfect safety, there being no danger of combustion or explosion.

It is to be understood that the two examples of distillation of petroleum and tar are recited merely as examples of the application of the new invention and that the same is not by any means confined to these substances; but it may also be employed for the distillation of the most varied kinds of liquids and distillable substancessuch, for example, for the regeneration of the wash-oil from the benzene or benzol plants-which have become unfit for use.

Having thus described my invention, what I claim as new, and desire to secure by Letters'Patent, is' r 1. The process of continuous distillation, which consists in separating the material to be distilled into a plurality of ortions located one above the other, heating the p01 tions to a temperature approaching but below the boiling-point of the product which is to be obtained, and permitting a heated gas to flow upward into contact with the different portions seriat'im.

2. The process of continuous distillation, which consists in separating the material to be distilled into portions located one above ICO the other, heating said portions to a tempera- I a heated gas through the apparatus in the i opposite direction to'remove and to recover benzin; and passing the treated petroleum, through a second and uniformly-heated column-apparatus of a temperature the neighborhood of 150 to 160 centlgradeagainst an opposed current of heated gas to remove and recover kerosene.

4. The process of continuously distilling petroleum and the like which consists in third and uniformlypassing such petroleum through aheated column apparatus and concurrently passing aheated gas in the opposed direction to remove benzin; passing the treated petroleum through a second and uniformlyheated column apparatus of a temperature 1n the neighborhood of to centigrade against an opposed current of heated gas to remove and recover kerosene, and finally passing the treated etroleum through a lieated column apparatus of a temperature in the neighborhood of to centigrade against anopposed current of heated gas to remove and recover lubricating-oils.

5. The process of continuously distilling oily bodies which consists in passing such oily bodies consecutively through a series of 6. The process of continuously distilling oily bodies which consists in preliminarily heating such oily body, and passing the same j consecutively through a series of column apparatus, each uniformly heated, and certam members of the series being respectively of a temperature in the neighborhood of, 108 to 1 15 centigrade, in the nelghborhood' of 150 to 160 centigrade and in the neighborhood of 175 to 180 centigrade and atv the same time bring into contact with the oily body in each such apparatus an opposed current of heated gasto remove and recover the bodies volatile at the temperature prevailing therein.

7. The process of recovering fractions from a composite oily body which consists in heating it in films to a temperature approachin but below its boiling-point, stripping it 0 constituents of high va or tension at such temperature by. means 0 a gas-current, and repeatin the treatment at a series of successively-hig er temperatures.

8. The process of recovering fractions from petroleum which consists in heating films of petroleum to a temperature near but below the boiling-point of such petroleum, and stripping it of constituents having a high vapor tension at such temperature by means ofa gas-current.

9. The process of recovering fractions from petroleum which consists in heating petroleum in films to a temperature near but below the boiling-point of-gasolene; stripping 1 it of gasolene by means of a gas-current; again heating it in films to a temperature near but below the boiling-point of kero sene, stripping it of kerosene by means of agas-current; and again heating it in films to a temperature near but below the boilingpoint of lubricating-oils, and stripping it of such lubricating-oils by means of a gascurrent.

In testimony whereof I afliX my signature in presence of two witnesses.

HEINRICH HIRZEL.

Witnesses OswIN HELBING, RUDOLPH FRIOKE.

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