US1310977A - Process of treating vegetable oils - Google Patents

Description

C. 1.- BARTON.

PROCESS -0F TREATING vEGETABLr-I olLs.

V APPLICATION FILED SEPT.22, 1917.

1 ,3 1 O, 977 Patented July 22, 1919.

@UNITED STATES PATENT OFFICE.

CARLETON JOSEPH BARTON, 0F CHICAGO, ILLINOIS.

PROCESS' OF TREATING VEGETABLE OILS.

Specification of Letters Patent.

VPatented July 22, 1919.

Application led September 22, 1917. Serial No. 192,743.

of this kind in which neither acids vnor alkalis are used to provide a process of separating corn oil into the'three parts: (A)

the non-emulsified oil, jthe emulsified oil, and (C) that constituent part of the original oil which, as a result of the emulsifying, appears as wax; to provide a process Iby which the three portions which are chemically and physically different may be each returned to the appearance of the original oil; to provide a process of separating out an edible stable oil without any unnatural acid or alkali taste; to provide a process which returns the emulsifiable oil to original appearance; andto provide a process which returns the waX portion to original appearance.

An illustrative embodiment of this invention is shown in the accompanying drawing, in which:

Figure 1 is a diagrammatic outline -of the complete process.

Fig. 2 is a diagrammatic view of the centrifuge used for one of the steps of the improved process.

Heretofore in the treating of maize or corn oil, the crude oil was heated to approximately 115 degrees Fahrenheit, and caustic soda was added to neutralize the so termed free fatty acids and precipitate the foots. Two products were obtained by this process, the most important being the neutral oil used for culinary purposes; the other product was the foots, and contained neutral oil, glycerin and soap. The non-emulsified product was then filtered through fullers earth, ,and then cleaned by live steam. This filtered product, while edible, possesses an objection, in that the product has a slight flavor which would not be present if no alkali was used in`the process.

The foots, being the precipitated portion containing glycerin, soap and neutral 011,

is usually utilized in the soap making industry as a basis for cheap soaps.

With the improved process herein set forth, a much larger proportion of nonemulsified edible oil isobtained, and it is free from any objectionable flavor.

The process comprises the agitation of crude maize oil with water or live steam,

lheating tov atemperature sufficiently high to cause a partial separation ofthe non-emulsified oil from the emulsified portion and the Water. The best temperature `forthispurposev has been found to be approximately 7 0 centigrade. By this step of the process', non-emulsified oil to the extent of approximately 65.7 per cent. of the original volume may b e separated, preferably allowing the oil to stand forz approximately twenty hours, but this separation may be accom'- plished by mechanical means in less time.

The remaining part of the original mixture, or approximately 34.3 per cent. of the original volume, still contains considerable non-emulsified oil. 'In order to extract this non-emulsified oil the emulsion is reheatedv with Water or steam to a temperature sufliciently high to permit the separation by mechanical means of the non-emulsied oil from Athe emulsified oil and water. In practice approximately 100 degrees centigrade has been found to produce the best results.

When this emulsion has been reheated, it is then, while still hot, run through a specially constructed centrifuge, such as shown in diagrammatic outline in Fig. 2 of the drawings. The centrifuge comprises a receiving bowl 1, a feed p i e 2, a separating bowl 3 of the usual deslgn. .It has been found, however, in 'practice that when it was attempted to pass the hot emulsion through a centrifuge. the machine became clogged with the thick emulsion and would not operate,'and it has therefore. been impossible heretofore -to secure any additional separation of the oils. been overcome by placing a pipe 4 in the receiving bowl 1, so. that the lower end thereof leads into the feed pipe 2 at the bottom of the bowl. Boiling hot water is passed through this pipe 4 immediately preceding the passing of the emulsion from the bowl 1 into the feed pipe 2, and the addition of this hot water is continued during the .entire centrifuging process, the quantity of water supplied being of substantially equal volume to the amount of emulsion.

This difficulty has- The boiling water that passes into the separating bowl 3 is thrown immediately outward to the sides thereof and forms a layer between the separating bowl and the emulsion. This separating layer of hot water prevents any clogging of the separating bowl and as a result an additional nonemulsified oil to the extent of approximately 5 to 10 per cent. of the original volume is separated and drawn olf from the emulsion.

The balance of the emulsion is then placed in a suitable receptacle and boiled with'a dehydrating or any other agent that will break down the emulsion, such as common salt. This emulsion with the breaking agent therein is then boiled for some time until nearly all of the separated water is boiled off, and allowed to stand, whereupon it separates into three layers, the top layer being the converted emulsion (an oil), the center layer being a layer of the unbroken or un- !converted emulsion, and the lower layer being the solution of the water and breaking agent. The clear top layer may then be decanted and this `decanted oil is clear like the original product, maize oil, but of a slightly darker color and a butter-like taste. This oil which has a butter-like taste I have named B-oil. The corn wax is a valuable product of which use is made in the industrial arts.

The corn wax is not soluble in alcohol, but when boiled with the alcohol is dehydrated and ioats on it. After separating, the last trace of alcohol is removed from the C-oil by heating to 130o centigrade. It then has an appearance like the original corn oil.

An alternate process accomplishing the same resultis that of slowly and gently heating the wax-like emulsion after 1t has been spread into a thin surface, as in a film or drum evaporator. Proper temperatures are maintained to insure success;

The complete process comprises the separation of maize oil into three separate and distinct oils as regards chemical compounds and physical characteristics.

Each of the oils has its use in the arts:

Oil A: The non-emulsiied portion.

Oil B: The converted emulsified portion from which the wax-like portion has been removed.

Oil C: The wax-like portion converted into its original physical condition.

The invention may be more specifically illustrated by the following example: Place ten pounds of corn oil in a iuid tight receptacle and add-five pounds of boiling Vhot water. Then maintain the temperature at about the boiling point for twenty-five minutes by introducing a vigorous supply of live steam which serves also to agitate the material. A lower temperature and other stirring means may be employed. As a re- 'and say three pounds of hot water.

sult of this treatment about 34.3 per cent. of the oil becomes emulsified whereby about 3.43 pounds of emulsion is produced. Separation may be effected by gravity or more quickly by a centrifuge. This emulsion is then treated by mixing with about an equal weight of boiling hot water. The material is then run through a special centrifuge, such as shown in Fig. 2, whereby a second emulsion and a non-emulsified oil are obtained, the latter being about 15 per cent. of the original volume of corn oil or about one and one-half pounds.

The next step is to take a quantity of the second emulsion, say three pounds, and add 5 per cent. of salt, c'. e., about .15 pound, This is kept boiling hot Vor nearly so Vfor about twenty minutes whereupon it is permitted to cool. As said material cools, it separates by gravity into three layers. The upper layer consists of clear B oil somewhat darker than the original corn oil. The middle layer consists of corn wax, and the lower layer consists of salt brine. The proportions respectively are about 2 pounds o-f B oil, 1 pound of wax and the remainder being brine and impurities.

A quantity of corn wax, say l pound, is then dissolved in about an equal weight of alcohol. The free alcohol is then` distilled off leaving about 1 pound of clear C oil.

Although certain definite temperatures, percentages, and time intervals have been stated herein, it is to be understood that these may be deviated from and satisfactory results still obtained, and that details vof the process may be altered or omitted without departing from the spirit of this invention as defined in the following claims.

I claim:

1. The process of treating corn oil, which comprises the heating of said oil with steam or water to aK temperature sufficiently high to produce 1an emulsion, removing by means of decantation such part of the non-emulsi-A ed oil from the Warm emulsified oil and water as may be separated by a brief interval of standing, reheating` with additional water the emulsion so obtained to a temperature sufliciently high to permit the 'balance of the non-emulsified oil to 'be separated, while hot, with a centrifuge, and plassing such emulsion through a centrifuge and thereby effecting such separation. l

2. The process of treating corn oil, 4which comprises the heating of said oil with steam or water to a temperature sutfcientlyrhigh to produce an emulsion, removing by means of decantation such part of the non-emulsifled oil from the warm emulsified oil and water as may be separated 'bya brief interval of standing, reheating with water the emulsion so obtained to a temperature suficiently high'to permit the balance of the non-emulsified oil to be separated, while hot,

with a centrifuge, and passing such emulslon, whileshot, through a centrlfuge with a substantially equal volume of hot water, and

, so effecting such separation.

3. The processes of treating maize or corn oil, which comprise the agitation of said -oil with steam. or water at a temperature suliciently high to produce van emulsion and to'cause part `of the warm non- .,emulsied oil to separate by gravity', upon standing, from the emulsiied oil and .water, the removal of such part by decantation,

vreheating with the water the emulsion so l. high to cause a breaking of part of the emulsion into an oil and the separation by gravity of-this from the' unconverted Waxlike portion of the emulsion and the water taining the breaking agent.

4. The processes of treating maize or corn I oil, which comprise the heating Aof said oil with steam or water followed by standing to a ltemperature s'uiiciently high to. produce an emulsion and thereby causing part of the warm. non-emulsifed oil to separate by gravity, upon standing, from the emulsied oil and water, reheatin'g with the Water. the emulsion s`o obtained to a temperature vsl'lfiiciently high to permit the balance of the non-emulsiied oil to be separated, while hot; with acentrifuge, passing such emulsion with a vsubstantially equal volume of hot water through acentrifuge to cause such separation, theaddition of 'a breaking agent to the emulsion last obtained, and the heating of said emulsion and thereby causing a separation of the converted emulsion, the waxlike unconverted emulsion and the wa-f ter Isolution of the breaking agent.

5. The process of treating maize or corn oil, which comprisesthe. agitation ofsaid oil, with steam or Water, and thereby producing an emulsion, heating to a temperature suii'ciently high to cause part of. the non-emulsied oil to separate .by gravity, upon standing, from the emulsied oil and water, lrehearing with water the emulsion so obtained, to a temperature suiiiciently high to permit the balance ofthe non-emulsified oil to-be separated, while hot, with a'centri- 4fuge, passing such emulsion through a centrifuge and thereby causing such separation, adding a breaking agent that will break down the colloidal state of the emulsion last obtained, heating said emulsion to a .tem-

perature suiiciently high to cause a separation of the converted emulsion and the unconverted portion and the water solution of the breaking agent, and subsequently coollng the converted emulsion and thereby causing a further precipita-tion of the uncoverted part of the emulsion. i

6. The processl of treating maize or corn oil, which comprises the agitationk of said oil with steam or water to form Ian emulsion, heatingof said emulsion to a temperature of substantially 7 0 degrees centigrade so 'as to cause part of the non-emulsiied oil to sepalrate by gravity, upon standing, `from the emulsifed oil and water, separating thenonemulsiiied oil from the emulsiied oil and water, 'reheating with water the emusion so obtained, to a temperature suiiiciently high to permit the balance of the non-emulsiiied oil to be Separated, while hot, with a' centrifuge, passing such emulsion through a centrifuge to cause such separation, adding a breaking agent that will 'breakdown the colloidal state of the emulsion last obtained,

heating said emulsion t'o a temperature sufficiently high to cause a separation of the converted emulsion, the unconverted emulsion, andthe water solution'of the breaking agent, and subsequently cooling said con-v verted emulsion to cause a further precipita- -tion of the unconvercd part of theemu-lsion.

7. The process of treating maize or corn oil, which comprises the a 'tation of said oil, with steam or Water, to crm an emulsion, the heating of said emulsion to a temperature suiiciently high to cause part of thenonemulsifed oil to separate by gravit upon standing, from the emulsified oil an water,

separating the non-emulsiied oil from the emulsied oil and water, reheating with water the emulsion so obtained, to a vternperature'of substantially 100' degrees centigrade so as to permit the balance of the non-- cmulsied oil to be 4separated while hot, with a centrifuge, passing such emulsion-through a centrifuge to cause such separation, adding a breaking agent that will break down the 'colloidal state of the emulsion last obtained, heating said emulsion to a temperature sufciently high to' cause a separation of the converted portionz the unconverted portion,

and a Water solutlon of the breaking agent, and subsequently cc oling said converted portion to cause a further precipitation of the unconverted portion.

8. The process of oil, which comprises the agitation of said oil, with steam or water, to a temperature sufficiently high to produce an-emulsion and to cause partof the non-emulsiiied'oil to separate by gravity, upon cooling, from the emulsifed oil and water, separat1ng the nonemulsifled voil from` the emul'sied oil and water, reheatingvwith water the emulsion so obtained to a temperature suiiciently high to permit the balance ofthe non-emulsiied oil to be separated, whi1ehot, with a centreating maizeor corn trifuge, passing such emulsion through a centrifuge to cause such separation, adding N aCl to the emulsion last obtained, heating said emulsion to a temperature suliciently high to cause a separation of Wax, and subsequently chilling said emulsion to cause a precipitation of the wax.

9. The process of treating maize or corn oil, which comprises the heating of said oil, with steam or Water, to a temperature sufficiently high to produce an emulsion and to cause part of the non-emulsified oil to separate by gravity, upon cooling, from the emulsified oil and water, separating the non emulsified oil from the emulsiied oil and Water, reheating With Water the emulsion so obtained, to a temperature sulliciently high to permit the balance of the non-emulsied oil to be separated, while hot, With a centrifuge, passing such emulsion through a centrifuge to cause such separation, adding an electrolyte that will break down the colloidal state of the emulsion last obtained, heating said emulsion to a temperature of substantially 100 degrees centrigrade, so as to cause a separation of wax, and subsequently chilling said emulsion to cause a precipitation ot' the Wax.

10. The process of tre-ating maize or corn oil, Which comprises the heating of said oil with steam or Water, to a temperature sul-H- ciently high to produce an emulsion and to cause part of the non-elnulsified oil to separate by gravity, upon cooling, from the-emulsied oil and Water, separating the non-emul- Sified oil from the emulsied oil and water, reheating With Water the emulsion so obtained, to a temperature sulliciently high to permit the balance of the non-emulsified oil to be separated, While hot, with a centrifuge, passing such emulsion through a centrifuge With Water to cause such separation` addinr an electrolyte that will break down the co loidal state of the emulsion last obtained, heating said emulsion to a temperature sufliciently high to cause a separation of Wax, and subsequently chilling lsaid emulsion to cause a precipitation of the wax.

1l. The process of treating maize or corn oil, which comprises the heating of said oil, with steam or Water, to a temperature sufliciently high to produce an emulsion and to cause part of the non-emulsified oil to scparate by gravity, upon cooling, from the emulsified oil and Water, separatin the nonemulsiied oil from the emulsilie oil and Water, reheating with Water the emulsion so obtained, to a temperature sufficiently high to permit the balance of the non-emulsilied oil to be separated, while hot, with a eentrifuge, passing such emulsion through a centrifuge with a substantially equal volume of hot Water to 'cause such separation, adding an electrolyte that Will break down the colloidal state of the emulsion last obtained, heating said emulsion to a temperature suiiciently high to cause a Separation of wax, and subsequently chilling said emulsion to cause a precipitation of the Wax.

12. The process of treating maize or corn oil, Which comprises the heating of said oil with Water to a temperature of substantially degrees centigrade so as to produce an emulsion and to cause part of the nonlemulsified oil to separate by gravity, upon cooling, from the emulsiied oil and Water, sel arating the non-emulsiied oil from the emulsied oil and Water, reheating with water the emulsion so obtained to a temperature of substantially 50 degrees centigrade to permit the balance of the non-emulsified oil to be separated, While hot, with a centrifuge, passing such emulsion, While hot, through a centrifuge with a substantially equal volume of hot water to cause such separation, and adding substantially five per cent. of sodium chlorid to the emulsion last obtained, heating said emulsion to a temperature of substantially 100 degrees centigrade to cause a separation of wax, and subsequently chilling said emulsion to cause a precipitation of the WaX and to cause a separation of the remaining oil from the brine.

Signed at Chicago this 18th day of Scl telnber, 1917.

CARLETON JOSEPH BARTON,

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