US2280046A - Oil production - Google Patents

Description

Patented Apr. 14, 1942 UNITEDsT-ATES PATENT OFFICE U ;ff 4s assignor by mesne assignments, to Food Manufacturing Corporation, Chicago, 111., a corporation of New York Serial No. 282,078

b some (or. zoo-412.2)

n The present invention relatesto the extr an tr ssio o o r duct from oi 9 m M materials, and particularly iromseeds eontai ing oil. a a n heh ua me hqd of x ra t on or, ex i es? sion, and particularly where pressure isused, there s u ua o e ressed fr m t es v r materials, the large yield that is desired, Fu her br in r er o incr as the 19 a h x t d or x ed ma er a remnan t tm n s nd s l ent r c sses materna ss ng e en r lly til zed, al o wh h t nd t mak a r du t o in r o uality c m pared with the material that is expressed by the first r b i t p ess n For example, if obtaining oil] from variqus oil C tain n m ter als. as In: in ae .a seed, co n ge ms, on-seeds; ast r beans; sore b an un ow se d peanut n SQ, 292th, i s kimwri t th fi s ressure. an genera y a li ht pres ure; produqes a l bsten il ualit o o l th n is n qdute wheb thetaining materials are given harder pres than is produced after the first pressure.

It is known, for example, that the fi st pressure of sesame, seed produees a subst l' q ty of thanth sec nd, W p s in of the seeds. also. when a to tinu us re such as he exn ler leased or] pressin p t or ins a ce; ti k own. at

t at is der ed Item the. u per, portions bigth p sr s er muc tter that th lnq with s d e m t e ow r or ion t r th E1198- nu a e expo ed to the higher ressu e and. the higher d grees i heat o thi llqwet 'qr nbi the expeller press, I, f

oil

prov d qua ty bas d mn t is .1.Nhfy l '1 a it is also among v objec s o s ve tion to express or xtract oils which ,7 p e r as n m y a p ed, pr du 'ea swa t a n an p at on on y a d not by way o t a y mp ov d quali of expressed or attest d limitation, since various changes therein may be made by those skilled in the art without departing from the scope and spirit ofth'e present in-- vention. f v i It has been found that these improved expressed and extracted products may be produced by an expansion or explosion process, together with various other procedures as for instance steaming, freezing, and so forth.

Depending upon the type of material that is used, various procedures should be employed in orderto produce the res'ults required. For instance, high sugar materials require care so as not to caramelize the sugar present, or high fibrous materials require more violent expansion so as to break or tear the fibers, if this is de sired, or high moisture containing materials should be dried to the required moisture content so as to permit the formation of a sufficiently hards'tructure for the expansion procedure.

For the preferred results in theembodiment of this invention, the materials to be expanded or exploded shouldbe of a moisture content below t and preferably below 15% or 20%,

turecontent as noted herein, before proceeding with the expansion procedure.

Desirably the drying temperatures may vary for example from F. to 212 F., or more or less, depending upon whether vacuum is used, the degree of dryness that is required, or the general characteristics of the material that is being dried. However, for most purposes the preferred temperatures for dehydration run, for example, between F; and F., and the length of time for dehydration necessarily depends upon the amount of dehydration required, the temperature, and other conditions.

Any of the commercial procedures for dehydration may be used for the materials to be expanded or exploded, or, if desired, they may be stored away under proper conditions in a warm or dry room, so as to dry normally,

, The materials which are of the reduced moisture content are then subjected to atreatment at relatively elevated temperatures and pressures.

For best results the pressure shouldusually be above 20 or 25 pounds per square inch, and generally should be above 40 or 50 pounds per square inch, and in some cases it may run as high as 350, 450 pounds, or more, per square inch.

Generally the temperature should be above 200 F. to 250 F., and preferably within a range of about 300 F. to 800 F. The general range is usually between 400 F. and 600 F.

This explosion treatment is carried on for :a, j

time period and at a pressure and temperature yto; contact a considerably larger surface than depending upon a number of factors, as for in" stance, the moisture present in the material, the degree of expansion desired, the type of equipment used, whether dry heat or steam or superheated steam is used for the expansion chamber,

the time, the temperature, and pressure conditions themselves, and other factors.

The required time for explosion may be" 20 minutes or longer, or it may be under minutes and even less than several minutes or less than one minute.

If the product requires a littleadditional moisture for an enhanced explosion operation, this additional moisture may be added to the product or to the expanding chamber, as for example, in the form of water or other aqueous materials or in the form of steam or superheated steam.

In order to prevent or retard any burning, and particularly when the temperatures and pressures are at substantially higher degrees, the expansion or explosion treatment is generally carried out in a steam atmosphere. This steam may be developed by various methods as for instance, from the moisture within the product that is being processed, or by the injection of steam, etc., into the pressure chamber. Drier atmospheres may be used as required, but care should be taken with reference to any burning, or scorching, or caramelizing of sugar, etc., which would have a tendency to affect the quality of the material to be extracted or expressed therefrom.

a After this treatment at elevated temperatures and pressures, the material that is being treated is suddenly and instantaneously released to atmospheric pressure and temperature, or to substantially lower temperatures and pressures, as for instance byopening the particular vessel in which these foods have been treated whether such vessel be in the form of an autoclave, a pressure 'gun, or some other similar suitable apparatus.

.- After the material has been treated in accord with the process described herein, it is found that the structure thereof hasv been changed, or at least it has been modified so as to enable the enhanced extraction and expression procedures of this invention.

For instance, in the case of materials such as oil seeds, it is found that these oil seeds, as for instance sesame seeds, now show a relatively good amount of oil on the surface thereof, after the explosion procedure. This loose oil will also be found throughout its structure, due to the destruction, or breaking, or loosening of the oil cells which are contained therein.

The materials resulting from this procedure may now be utilized in the extraction and expression procedures such as are normally used, as for instance, pressure, solvent extraction, and so forth. Upon'the utilization of these expression or extraction processes, it will be found that the amount of oil, that is extracted or expressed, is now present in a larger yield than heretofore, or

that it is of a substantially better grade or quality than heretofore possible for the same degree of heretofore possible, and thereby so as to provide a higher solvent yield with a better quality of the extracted material.

, In the expansion or explosion treatment, although the materials may be ejected from the pressure chamber or gun into atmospheric conditions, it is also possible in order to control the expansion, porosity, cell or structure rupturing, etc., to eject these materials into atmospheres having higher or lower pressures than atmospheric, or into various degrees of vacuum, and also into various atmospheres which may contain carbon dioxide, nitrogen, ozone, or even quantities of oil or aqueous vapors, or they may be ejected into hot water or oil, or into various solvent vapors, or into the liquid solvents such as alcohol, ether, and so forth.

Prior to the dehydration or explosion procedures of this invention, wherever this is required, it is generally advantageous to cut the materials that are utilized into smaller pieces, if they are not already in small pieces. This enables the dehydration and explosion to take place more uniformly and more quickly throughout the pieces.

Although this procedure of explosion, disruption, or expansion may be carried out in one step, it may also be carried out in a plurality of steps in which case the same, or different temperatures and pressures and time periods may be utilized. For example, the material may be subjected to one or two or threev explosion or expansion treatments at the same, or at lower, or higher temperatures or pressures, and for'varied periods of time. a

In many cases, for instance, a multiple expansion procedure at a lower temperature and/or pressure has advantages over a single explosion at a higher temperature and/or pressure in that the material being treated is not given the same degree of violent treatment, or the high pressures or temperatures which would be necessary for the single explosion, whereas the results desired are accomplished at substantially lower pressures and temperatures or with less violent conditions, so as to produce the disruption of the structure, or of the oil cells or other cells.

However, of course, the multiple expansion or explosion may be at high temperatures and pressures and under violent ejection conditions, where this is required. For example, it may be used in some cases where there is a hard shell, surface, structure, which it is desiredto more completely disrupt.

It is desirable at times to place a coating on or within the pieces of the materials being treated, so as to permit the formation of harder walls and thereby so as to result in a greater and more efficient explosion of the product. Starch, resins, gums, and similar materials may be used to provide such a coating, for instance, by preparing aqueous mixtures of them, then coating the product, and then drying thereon.

molten sugar, or into fatty or other vapors, so as to aid in keeping thecells and structures of the material in as soft"acondition as possible, or so as to protect them against discoloration, oroxidation, etc., until the expression orextraction procedure is completed. Also, immediately upon ejection, the materials may be dipped into or coated with a plastic or molten hardened fat, or similar material so as toretard discoloration and other deterioration. V

Aside :from the expansion and explosion procedures herein disclosed, various accessory procedures may be used in order to enhance the extraction or expression procedure. For instance, there maybe used in conjunction with the explosion procedure, various operationssuch as soaking or boiling the material in oil, fat, or aqueous materials, or there may be used freezing, cookin steaming, and so forth, or various combinations of. these or other operations. These procedures may take place at various points, as for instance preliminary to,after, or as an accessory to the explosion operation so as tc further enhance the extraction or expression procedures herein disclosed. t

These procedures, also should be utilized in accord with the product being treated. For instance, freezingmay be utilized as will be described herein. Or, oil seeds may be cooked or steamed in aqueous materials. Or, the materials containing the cil soluble extractives may be boiled in liquid oil qr molten fat. Also, other procedures may be used as required.

able to carry out the freezing treatment in such a way. that there will not be the formation of small fine ice crystals with the consequent lack ofrupture of the cells andstructure, but rather, there should be the formation of relatively large ice crystals sufficient to puncture, break, rupture, or disrupt the cell structure or the fiber, structure or the body structure, substantially throughout the body of the particular material that is being treated. i i

The freezing usually takes place at ordinary atmospheric pressure but it may take place under conditions of pressure or vacuum.

While the steaming process may be utilized in conjunction with products that have a relatively high moisture content, nevertheless, materials As a possible embodiment of this invention,

the material which is to be pressed, or from which the oil is extracted, may be cooked, or steamed, and the resultant product may then be dehydrated to a. sufilciently low moisture content so as to enable the proper expansion or explosion O e ation l l V In orderto retain as much as possible of the flavors, essences, ar1 d qualities of the material, ar u p o e ures ma be se a fo ta okinls o s e ming nd r v cuu o under pressure, etc., or in the presence of inert gases.

Another embodiment of this invention that may be used in order to enhance the extraction or expression qualities as herein described, is to subject these materials to a freezingoperation, and particularly to a. slow freezing operation, which shall have the effect of rupturing the cell structure or softening the fiber and cell structure of the material.

In s bjecting these materials to a freezing operation, the amount ,ef moisture, and the tem peratures thatare required in order to produce the best results may vary depending upon the degree of softeningand rupturing of the cell structure that is required, or upon the nature of the materials that are being treated, or upon other conditions.

However, it has been found that very good results are obtained usually when the moisture content varies, for example, between 30% and 95%,

.but particularly when the moisture content is over 30% to 40%. "Likewise it has been found desirable in many cases, in order to obtain the best results, to permit the freezing to take place slowly at temperatures ranging between 0 F. and 32. F. although inmany cases preferred temperatures rundown to minus 20 F. and minus 40 F. Varying temperatures, further, may be used for varying lengths of timei In general it should be said thatit is desirquired Without these with low moisture contents, may advantageously he steamed. This steaming has a tendency to soften or enhance the quality of the material so as to improve the yield or case of the extractions or expressions therefrom.

One of the results of the cooking, steaming or'freezing processes as herein described, is that the bound oil or similarly closely'held oil materials are released or loosened. These bound elements are usually tightly bound in with the cell structure and are not usually easily removed by the usual extraction or expression procedures. However, by the cooking or steaming or freezing procedures as herein described, with the consequent explosionor expansion treatment, these tightly held materials are released in a much more substantial way so as thereby to enhance the yield, or other quality of the extracted or expressed oil.

Of course, following the cooking or steaming or freezing procedures, these materials must be dried or dehydrated to the required moisture content so as to enable satisfactory expansion or explosion.v

By the use of the cooking or freezing or steami may not be necessary to explode the material in the same violent way, as normally would be reaccessory procedures. Therefore, in many cases, the same high degree of temperature or pressure may be avoided, so as to produce a superior quality of the extracted or expressed material. i

Another accessory treatment that maybe used in carrying out this invention, is a roasting procedure. This roast may take place after, or in many cases, before the explosion procedure. This thereby results in enhanced extraction or expression results. This roast may take place either as a dry roast,.or as an oil roast, or in conjunction ;with the other procedures herein disclosed.

Although explosion, as described herein, is utilized mainly in conjunction with materials which have been dehydrated to, or which are of a low moisture content as, for instance, below 30% to 35% and generally below 20%, nevertheless this explosion may take place with materials, while they contain a relativelyhigh moisture content.

This type of explosion, when the products do not contain a low moisture content, has a tendency to tear orloosen the structure of the material, but does not produce the same general cell disruption as is produced when the material is in a low moisture content condition.

In the extraction or expression of the oil, in

accord with this invention, oilsolvents are many times'used. For example, the solvent material and the exploded material to be treated so as to obtain extractives, etc., therefrom, may be heated together, or the exploded material allowed to soak in the solvent, or the exploded material may be boiled or soaked in an oil medium, or in carbon bisulphide, or in alcohol, or in other solvents.

Also, if desired, the solvent medium and the exploded material to be treated, may be ground together, or the material to be treated may be ground prior to admixture with the solvent. Thereupon anyof the usual pressing procedures, or other extracting or expression methods may be used in order to produce the desired extracted or expressed materials.

For example, exploded oil seeds may be mixed, ground with, or otherwise mixed with a liquid oil and then this combination subjected to the usual pressure or other expression'methods. The liquid oil and the oilseeds may further be heated together so as to enhance the results. Also, if desired, combinations of the whole or ground oil seeds may be dry-heated or steamed, or they may be treated with hot water or cold water or they may be boiled in water so as to enhance the effecting of this invention.

After the explosion treatment, if the exploded products are steamed or are boiled in oil or in water, as required, there is produced entirely new and unexpected results in the expression procedures that follow. This is particularly the case when the product that has been exploded is of a quality, after it has been exploded, that it holds its oil, for instance within the relatively absorbent structure that has been developed by the explosion procedure.

Therefore, under these conditions, the cooking or steaming of these products in water, or the softening or boiling or heating of them in oil, particularly, in many cases, when the products to be expressed are in a broken, pulverized, or ground condition, is very advantageous. For example, the oilseeds or similar products may be steamed, or cooked in water, in which case the oil is in a measure washed out of the material an rises to the surface of the water.

The explosion procedure as described herein is particularly efiective when solvents, as, for instance carbon bisulphide, or alcohol, or other solvents or extracting materials are used. The advantage here is that because of the relatively porous or absorbent condition of the product, after it has been exploded, the entrance of these extraction or solvent materials into the structure of the material is considerably enhanced, and also a larger surface area is exposed to these extracting materials. Thereby, a considerably larger yield or a better grade of extracted material may be obtained, or various economies in cost may result. Where solvents are used, the material that is being processed is then pressed, or otherwise treated in the usual way.

In the carrying out of this invention, the best results are generally obtained with low starch materials, as for instance materials containing under 30% to 40% of starch in their original condition. Particularly where, in the explosion procedure, or elsewhere in these embodiments, the starch that is contained in these materials is gelatinized and swelled so as to cause a relatively collapsible mass or disintegratable mass when heated with water, is'there generally difliculty in the expression or extraction procedures that follow the explosion.

Also, because of the lower degrees of heat and pressure, or because of elimination or'modifica tion of other procedures which tend to reduce the quality of the product being treated, not only is the quality of the oil extracted-under this invention improved, but likewise, the quality of the meal or residue that remains is improved." For instance, the oil cake that remains after sesame seed, for instance, has been treated in accord with this invention is substantially superior to sesame seed which has been treated inthe normal method with considerably more heat and other drastic procedures. Therefore, the meal that remains can bring a considerably higher price from the standpoint of its use for cattlefood, or for other purposes. r

' Example I As an embodiment, of this invention, sesame seed is placed into a closed chamber and the pressure therein is raised to 60 pounds per square inch and the temperature is raised to 450 F. At the end of about 20 seconds, or at the end of about 10 or 15 seconds with an increased pressure, the chamber is instantaneously opened so as to eject the sesame seeds. These seeds are then pressed at about 3000 to 4000 pounds per square inch pressure in the regular hydraulic oil press, or in an expeller press. The resultant presscake may be ground, or treated with hot water, and further pressed, if desired, or solvent extraction processes may be used.

If desired, the exploded sesameseed may first be ground and then treated with hot water, or boiled therewith.

The excess oil may then be skimmed off the top of the water, and the remaining sesame seeds then given one or more pressings as required.

Further, if desired, the exploded sesame seeds may be given a dry roast and then pressed, with or without, previous. grinding. If ground, the ground material maybe given a heat treatment prior topressing with a warm or hot oil. Or, the exploded sesame seeds may be given a short boil in liquid oil, which may be followed, if desired, by a water boil, and then pressing, with or without previous grinding. I

Prior to explosion, the oil seeds may be boiled in water, or then slow frozen, for. instanca'so as to soften them, and then they may be dehy drated to the required moisture content. An oil boiling or oil soaking, or a steaming may also be used prior to the explosion treatment.

This invention also is of particular importance in expressing oils or fats or other extractives from materials which contain low oil contents. By the use of the expansion or explosion treatments as disclosed herein, the structure of these materials are disrupted and considerable additional interior and exterior surface areas exposed, so as to permit more ready accessibility to the extractives therein. Consequently, there results a greater yield and better quality of oil therefrom.

Also an embodiment of this invention relates to the explosion of oil containing seeds so as to have them retain substantially their unity, and then while having them retain this unity, to remove the excess oil therefrom by solvents, by dry heating the seeds, or by water washing, etc. These seeds with a portion of their oil removed may then be used in confections and for other edible purposes where it is desired to use a seed that retains substantially its unity, but with a portion of its oil .removed.

2,280,046 f This 'has heretofore been impossible because, i impreviousmethods;thefpressing and grinding of the seeds to remove the oil therefrom, obviously or various new qualitiesand types of seeds -may i be de'veloped by first removing atleast a portion of the oil'trom the seeds, as herein described, :and then subjecting the seeds from which the oil has beenremovd to another explosion, and then removing a further portion of the oil. This procedure of exploding and removing the oil may be continued two, three or more times so as to re- I move increased amounts of oil therefrom, or so as to produce entirely new types of seeds.

In the carrying out of this invention, the presence of starch or protein material within the product beingtreated, may result in various difficulties either in the explosion procedure or in the extraction procedure. Therefore, where required, the starch or protein contained within these materials may be removed by various methods as, for instance, by washing it out with water, salt water, alcohol, or other solvents or various washing materials as required. Also,

where required, various enzymes may be used toconvert the protein or starch material within the product being treated, into sugars, water soluble peptones, amino acids, as for instance by the use of diastatic' enzymes proteolytic enzymes, etc. These sugars, or peptones, etc., may then be more easily washed'out if this is required.

Aside from oil seeds, various other oil containing materials may be treated so as to have their oils or other extractives removed therefrom. These oils may, for example, be obtained from wild plants, from cultivated plants grown for the purpose, or from wastes or by-products of various industries.

Examples of oils that may be removed or extracted are, for instance, oil of turpentine, sassafras oil, oil of intergreen, oil of witch hazel, oil

of eucalyptus, oil of peppermint, hop oil, oil of spearmint, oil of dill, oil of Wormwood, and so forth. Where desired, alcohol may be used as the solvent for the exploded leaves or branches of the witch hazel containing material, for instance, or the oil may be removed by steam distillation, or other procedures as herein disclosed may be utilized.

Also other oils that may be produced more ef- JaroundQI iO? F. to 150IF'31until themoisture icon- .1. tent reduced to about -"8% to 12% 'Ih'ese; cod

livers are then subjected to a ;pressure fq50 z-pounds per square inch at a temperature of -about r400? -:F.'qin .a superheated steam :atmospher rora ;period 'of '15 seconds. ,Thereupon Lthe pressure kettle is instantaneously topeneduso as to release the cod liver pieces. .Theylmay :then the boiled in water under pressure and the oil is removed therefrom;

Or, if-desired,they mayfirst be ground prior rto boiling .in water.

Or, further, they. may ifirst 1 betagi'vena roast, or heated in oil, .or jotherprowcedures, as di'sclosedherein 'may be used,as,.for

fectively under this invention are, for instance,

those produced from cull citrus fruits of which possibly lemon and orange oils are the most important. Likewise; apricot and bitter almond kernels, or peach and prune kernels, etc., may be subjected to a. single explosion, or a multiple explosion procedure so as to substantially disrupt the structure of the material and thereby so as to facilitate the extraction of the various oils and materials therefrom.

Also, other oil containing materials that may be processed in accord with this invention are for example, nuts, olives, or also, cod livers and various other fish livers, etc.

Example II t For example, fresh cod livers may be cutinto insta'nce, :prior to dehydration they may be slow frozen, or boiled in 1 water, w etc., so as lito :further enhance themexpression .wprocedures 101? this ini f v 5 vention. r

Generally, it is desired to use non-leguminous seeds and materials in carrying out this invention because, although leguminous materials may be treated as described herein, nevertheless there is considerable difficulty in obtaining the adequate yield of oil therefrom due to their increased and very absorbent nature when exploded. This results in their holding the oil therein unusually tightly.

In addition to various nuts, seeds, etc., that may be utilized as herein described for the extraction of oil therefrom, also various spice materials as for instance whole cloves, nutmeg, cinnamon, etc., may be exploded and the flavoring oils more completely and more easily removed therefrom.

Also, aside from the extraction and expression processes noted herein, various other extraction processes may be used as for instance, steam distillation, dry distillation, or other methods and procedures that are preferred, or that are described herein. Still further, various other procedures that may be used in order to produce more effective results in specific cases, aside from extraction with volatile solvents, is the extraction with warm liquid fats or oils, or extraction with cold solid fats.

Particularly is the procedure of extraction with fats or fatty oils of importance, due to the ability of these fatty materials to more readily absorb odors, and also in view of their ability to quickly absorb oil soluble materials, and also so as to enable retention of volatile or fixed fatty elements.

As an example of the absorption of various volatile odors or flavors or fatty elements, the exploded materials may be treated with or dipped lnto warm liquid fats or oils, or cold solid fats, under vacuum or under pressure, as may be desired, or with Or without heat. The relatively porous or expanded nature of the exploded materials, or the disrupted condition of the odor containing or flavor containing cells of the products of this invention, will then more efiectively permit the absorption of the required element by the fats oroils, which, not only provides the extractive element, but, likewise, which retains these flavors, odors, and elements, in a substantially enhanced manner.

What I claim is:

1. The method of extracting an oil from an oil containing material, said method comprising providing the oil containing material with sufficient water within its structure so as to enable ice crystals to form upon freezing, subjecting the resultant material to a slow freezing onditio Sm ller 1116685 and timed at a temperature 0f '15 so as to form relatively large ice crystals therein and thereby so as to disrupt the oil cells therein,

dehydrating the material so as to produce ta firmer structure, subjecting the material to steam at an increased temperature and pressure, suddenly and instantaneously releasing to a lower temperature and pressure so as to disrupt the structure thereof, and then removing the oil therefrom.

2. The method of extracting oil from oil seeds,

said method comprising subjecting the oil seeds 10 to steam at an elevated temperature ranging from 300 F. to 800 F. and to a pressure ranging from 40 to 450 pounds per square inch, followed by instantaneously releasing said temperature and pressure to a lower temperature and pressure, and then extracting the oil therefrom, the moisture content of said oil seeds being under 20%, and the vegetable oil produced from said oil seeds being of substantially enhanced stability against oxidative deterioration.

3. The method of expressing oil from oil seeds,

, said method comprising subjecting the oil seeds to steam at an elevated temperature ranging from 300 F. to 800 F. and to a pressure ranging from 40 to 450 pounds per square inch, followed by instantaneously releasing said temperature and pressure to a lower temperature and pressure, and then expressing the oil therefrom, the moisture content of said oil seeds being under 20%, and the vegetable oil produced from said oil seeds being of substantially enhanced stability against oxidative deterioration.

ALBERT MUSHER.