US1656716A - Process of separating liquids - Google Patents

Description

Patented Jan. 17,

UNITED STATE s T caries.

JULIUS ,ALsBnne, .0? NEW Yonx, N. Y.,',AssIGNon TO B. H LLER & comm, or

CHICAGO, ILLINOIS, A CORPORATION QFILLINOISL .rnoonss or snrnnarme m ms j i 1! Drawing.

gravity may'bereadily separated from one another. 7

Further, said invention has for its object to provide a process of the character specified in which the specific gravity of certain of the liquids in a mixture to be separated is .varied or unbalanced relative to the specific gravity of other of said liquids whereb to permit of the separation thereof.

Further, said invention has for its object to rovide a process of the character specified by means of which certain of the liquids of a mixture dispersed throughout other of said liquids thereof constituting a carrier or vehicle may be readily separated from said carrier or vehicle.

Further, said invention has for its object to rovide a process of the character specitied by meansof which substantially a com; plete separation of certain of the relatively immiscible liquids of substantially the same specific gravity from other thereof may be effected.

Further, said invention has for its object to provide a process of the character specified in which the specific gravity of certain of the liquids of a mixture is increased relative to other of said liquids whereby to permit of the separation thereof.

Further, said invention has for its object to provide a process of the character specified in which the liquid mixture is saturated with a medium soluble in certain of said liqluids whereby to relatively vary or unba ance the specific gravities of said liquids to permit of the separation thereof.

Further,said invention has for its object to provide a process of the character specified by means of which an immiscible liquid or liquids dispersed throughout a liquid medium or vehicle of substantially the same specific gravity are separated from said medium or vehicle by saturating the mixture with a suitable salt or salts soluble in said medium.

Further, said invention has for its object to provide a process-of thecharacter specified by means of which the smoke flavor and aroma bearing constitutents of the conden small pieces and Application filed October 31,1925] Serialii'o. 85,94i'ff sateobtained from the destructive distillation of ve etable matter may be readily separated rom the water and .deleterious elements. of said condensate.

Further, said invention has for its object to provide ap'rocess of the character speci fied in which the specific gravity of the watery and deleterious elements or portions of said condensate is varied relative to that of the smoke flavor and aroma bearing constituents thereof whereby to permit of the separation of the same. 7 v

' Further, said invention has for its object to rovide a process of the character spedlie in which said condensate is saturated with a neutral salt or salts soluble in Wa er whereby to unbalance the specific gravity of the water and deleterious elements relative to that of the smoke flavor and aroma bearpermit of the separation,

ing constitutents to thereof. Other objects will in part be obvious and in partbe hereinafter described.

To the attainment of the aforesaid objects and ends my invention consists in the ess comprising the. successive steps inafter more fully described ed out in the claims.

' As one example, my process is described 1' s5 smoke flavor and aroma bearing constitu ents from the water and deleterious elements of the condensate" obtained from thejdeherein as being employed for separating the structive distillation of vegetable matter.

In producing said condensate I. first take a quantity of suitable vegetable matter such as maple, hickory beech orbirch wood; corn cobs, etc., according to the preference of the particular user. I have found maple "and then pointl wood is very satisfactory, as it yields a smoke flavor and aroma bearing composition better suited for use inconnection with meat and other food products. t I

The wood is next preferably reduced to placed in a suitable closed retort and subjected to heat for a sutlicient length of time to effect the destructive distillation of the wood. In order to obtain the best results the destructive distillation should referably be effected at a slow" rate of combustion, and in the presence of a limited supply of air which may be introduced into the retort in any suitable or convenient manner.

The volatile products coming over are re- Ill - be washed by passing the said gases through e. quantity of the end material or condensate ceived in a condenser where the same are brought into a liquid state, and thereupon the same are conducted to a suitable receiver. The resulting condensate consisting essentially of the smoke flavor and aroma. bearing constituents, and water, methyl alcohol and other deleterious constituents is then separated from the fixed gases such as carbon monoxide and carbon dioxide and other gases which may be present in smaller quantities or traces. The said gases may be discharged into the atmosphere or conducted by suitable meansto a furnace to be used as fuel.

Before the gases are discarded or conducted away for use as fuel, the same should obtained from a previous run in order to extract a certain amount of the smoke flavor and aroma, bearing constituents which pass through the condenser.

The condensate or condensates above specificd including the condensate through which said gases have been passed are then preferably conducted to a suitable storage tank or container in which the mass may be suitably agitated to produce a uniform mixture.

, The destructive distillation of vegetable matter, woodctc. results in a product which on standing separates out into two portions ,viz, a tarry or oily layer, and a watery layer 1 *known as'pyroligneous acld. Thls watery layer also contains tarry and oily matter,

. methyl l ohol, acetic acid, acetone and many other substances/ The oily and tarry substances are desirable for flavoring purposes or to give the end product the true smoke flavor and aroma, and also contribute'to' the strength of the end product.

The methyl alcohol, acetic acid, acetone etc. constitute undesirable elements.

I have observed that the immiscible smoke flavor and aroma bearing constituents in said watery layer, probably because of the stabilizing action of certain of the constituents thereof, tend to form a natural emulsion with the water and deleterious constituents present. Said smoke flavor and aroma bearing constituents disperse throughout the watery layer, although-there is a tendency for the same to separate into a thin layer, sometimes at the top and sometimes at the bottom according to the condensate, the smoke flavor and aroma bearing constituents and the pyroligneous solution or medium in which the same is dispersed having substantially the same specific gravity. I

I have discovered that the smoke flavor and aroma bearing constituents may be readily separated from the deleterious constituents and water by varying the specific gravity of the liquid condensate until said useful or desirable constituents tend to separate into a layer, from the water and deleterious constituents. Preferably the specific gravity of the liquid is changed or varied by adding to the liquid mixture a suitable soluble. neutral salt, such as sodium chloride, sodium nitrate or a combination thereof or the like in quantities sufiicient to cause the separation into a distinct layer at the top of the mixture of substantially all of, or the major portion of the desired smoke flavor and aroma bearing constituents therein. To eflect this separation, I preferably employ sodium chloride whiclris added until no more dissolves, and then sodium nitrate is added in suflicient quantity to completely or substantially saturate the mixture whereby to relatively unbalance the specific gravity of the water and deleterious elements relative to the smoke flavor and .aroma bearing constituents, and create a difi'erence in the specific gravities of the liquids, suflicicnt to permit of the separation of one from another.

After the necessary quantity of salt has been added to the liquid mixture and agitated to producea solution the saxne is allowed to stand until the separation of the said smoke flavor and aroma bearing constituents from the deleterious constituents,

'terious elements of the total condensate, is

then drawn off at the bottom. The separation of the smoke fla\ or and aroma bearing constituents'from the water, salt or salts and deleterious elements may also be effected by centrifugal or other suitable methods. The portion of the mixture remaining consists of the smoke flavor and aroma bearing constituents containing traces of deleterious substances. Said remaining portion is then washed, by adding thereto more water containing the required amount of neutral salt or salts or combination of neutral salts, to provide a liquid of the desired specific gravity. The mixture is allowed to stand until separation into layers is eliected, and the salt solution is then drawn oft. The wash ing may be repeated until substantially all of the deleterious substances are removed from the smoke flavor and aroma bearing constituents. To effect the maximum separation of said smoke flavor and'aroma hearing constituents from the water and deleterious substances it has been found in practice necessary to raise the specific gravity of the liquid condensate to about 1.2444. Said product or smoke composition is finally thoroughly mixed and pumped into a storage tank provided with an agitator. The tank is preferably closed to prevent evaporation and exclude air. y

The salts employed may be separated and recovered by the usual methods. The recovered salts, containing traces of the dc: sirable smoke flavor and aroma bearing constituents, may be then employed in the treatment of other condensates, or may be separately used until said salts become so contaminated as to be unfit for use.

The product or smoke flavor and aroma bearing constituents separated from said condensate by the process above described is a dark brownliquid possessing a strong smoky odor, taste and color, and is substantially free from water and deleterious substances. a

In view'of the. fact that said composition,

possesses an odor and flavor of comparativey greatstrengthonly a small quantity will be required to impart the desired taste, aroma, and color to an article. For some purposes the same may be diluted by adding [thereto an excipient, such as a suitable solvent or vehicle,as, for example, ethyl alcohol,

or water in which the same emulsifies. When the diluted composition is to remain unused for longperiods an additional stabilizer, such as gum arabic, may be added thereto in sufficient quantity tomai-ntain the liquid emulsified for said period. I

It the composition comprising the smoke flavor and aroma bearing constituents separated from the water and deleterious ele- .ments by the process above described is to be employed in, connection with a food product, a sutficient quantity thereof of suitable strength may be applied directly to the exterior surface of the food productor other article to be treated, or the same may be combined directly therewith, or' with one or more of the ingredients of the food product in order to impart to the food product the degree of smoke flavor and aroma desired.

It is to be noted that where an article of food suchas meat is subjected to the customary smoking'operations in order to impart thereto the well known smoky flavor and aroma, and at thesame time to preserve the meat, a comparatively long time is required to accomplish the desired result, the article losin thereby considerable weight by'reasoni o the evaporation of the Water therein, and that even after long ex osure to the action of the smoke the fumes 0 not,

as a rule, penetrate very deep below the surface of the meat. However, when my process. is employed to efiect the separation of the constituents of the condensate obtained from'the destructive distillation of vegetable matter, a product is obtained bythe use of which the desired smoky flavor, aroma and color may be economically and uickly imparted to the meat without causing shrinkage of the meat due to loss of water, and that the smoky flavor, aroma and color will be uniformly distributed throughout the entire mass.- Further, the said composition will also serve to preserve the meat against deterioration.

The term immiscible, as herein used, is intended to include such liquids which are substantially insoluble one in the other, but which may be mixed by dispersion or emulsification and which thereafter will not readily, or at all, again separate.

Having thus described my said invention what I claim and desire to secure by Letters Patent is:

1. The process of separating relatively immiscible liquids of substantially the same specific gravity which consists in taking the condensate obtained from the destructive distillation of vegetable matter and includ ing smoke flavor and aroma bearing constituents and Water and deleterious constituents, relatively varying the specific gravity of said smoke flavor and aroma bearing constituents and the water and deleterious constitu'ents, and mechanically separating said smoke flavor and aroma bearing constituents from the water and the deleterious constituents, substantially as specified.

2. The process of separating relatively immiscible liquidsof substantially the same.

cific gravities of the liquids, and mechanically separating said smoke flavor and aroma bearing constituents from the water and deleterious constituents, substantially as sp,ec1fied.'

3. The process of separating relatively immiscible liquids of substantially the same speclfic gravity which consists in taking the condensate obtained from the destructive distillation of vegetable matter and including smoke flavor and aroma. bearing constituents, water and deleterious constituents, adding a neutral salt soluble in Water to said condensate in a quantity sufficient to substantially increase the specific gravity of the Watery portion of said condensate, and separating the salt solution and deleterious constituents from said smoke flavor and aroma bearing constituents, substantially as specified.

' 4. The process of separating relatively immiscible liquids of substantially the same specific gravity which consists in taking the condensate obtainedfrom the destructive distillation of vegetable matter and including smoke flavor and aroma bearing constituents and water containing deleterious constituents; saturating said condensate with a neutral salt soluble in water, and mechanically separating the smoke flavor and aroma bearing constituents from the Water, salt, and deleterious constituents, substantially as specified.

5. The process of separating relatively immiscible liquids of substantially the same specific gravity which consists in taking the condensate obtained from the destructive distillation of vegetable matter and including smoke flavor and aroma bearing constituents and water containing deleterious.

constituents, saturating said condensate with sodium chloride and sodium nitrate, and mechanically separating the smoke flavor and aroma bearing constituents from the remainder of said condensate, substantially as specified.

6. lhe process of separating relatively immiscible liquids of substantially the same specific gravity which consists in taking the entire condensate obtained from the destructive distillation of vegetable matter and including smoke flavor and aroma bearing constituents dispersed throughout water containing deleterious constituents, adding -to said condensate a. medium serving to vary the specific gravity of the water and the deleterious constituents relative to the specific gravity of said smoke flavor and aroma bearing constituents, separating the smoke flavor andaroma bearing constituents from the water and the deleterious constituents, washing the smoke flavor and aroma bearin constituents thus obtained with a liquid having a specific gravity substantiallyditferent from that of the said smoke flavor and aroma bearing constituents, and again separating said last named liquid from said smoke flavor and aroma bearing constituents, substantially as specified.

7. The process of separating relatively immiscible liquids of substantially the same specific gravity which consists in taking the condensate obtained from the destructive distillation of vegetable matter and comprising smoke flavor and aroma bearing constituents, water and deleterious constituents, adding a neutral salt soluble in water in quanity sufficient to relatively vary the specific gravities of said smoke flavor and aroma bearing constituents and said water and deleterious constituents, mechanically separating said water and deleterious constituents from said smoke flavor and aroma bearing constituents, subjecting said smoke flavor and aroma bearing constituents obtained to the action of a neutral saltsolution, and mechanically separating said smoke flavor and aroma bearing constituents from said salt solution and the contained deleterious substances, substantially as specified.

8. The process of separating relatively immiscible liquids of substantially the same specific gravit which consists in taking substantially al of the condensate obtained from the destructive distillation of vegetable matter in presence of a limited supply of oxygen, saturating said condensate with a neutral salt soluble in water, and mechanically separating the smoke flavor and aroma bearing constituents of said condensate from the deleterious elements and the salt water,

substantially as specified.

Signed at the city of New York, in the county and State of New York, this 27th day of October, one thousand nine hundred and twenty-five.

JULIUS ALSBERG.