US2730538A - Sperm oil fractionation - Google Patents
Sperm oil fractionation Download PDFInfo
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- US2730538A US2730538A US326062A US32606252A US2730538A US 2730538 A US2730538 A US 2730538A US 326062 A US326062 A US 326062A US 32606252 A US32606252 A US 32606252A US 2730538 A US2730538 A US 2730538A
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- Prior art keywords
- oil
- tout
- wax
- sperm oil
- fraction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B11/00—Recovery or refining of other fatty substances, e.g. lanolin or waxes
Definitions
- the present invention relates in general to a new composition of matter and to the method of producing the same, and more particularly to a new liquid wax product and the method of obtaining the same from sperm oil and derivatives thereof.
- Another object of the present invention is to provide a method for treating crude sperm oil or derivatives thereof to produce a new liquid wax product.
- the drawing represents a schematic illustration of a fractionating tower which may be used in carrying out the method of the present invention.
- the present invention comprises the fractionation of sperm oil or derivatives thereof with a liquefied, normally gaseous hydrocarbon under specific operating conditions to produce a material which, after hydrogenation, may be used as a spermaceti substitute.
- Sperm oil is essentially composed of two types of chemical compounds.
- the triglyceride component constitutes .2S-30% of the crude oil while the remainder is made up of saturated and unsaturated wax esters, e. g. RCOOR.
- spermaceti is a saturated wax ester of the above type, wherein R' and R" are at least C14 or longer. As aforesaid, only about 6-8% spermaceti can be recovered from crudesperm oil.
- an overhead fraction 10-30% of the total oil is obtained which contains almost exclusively the Wax ester component of the oil, while the bottom fraction contains a reduced amount of wax ester and an increased amount of glyceride.
- the wax ester in the overhead fraction is a mixture of both saturates and unsaturates, and hence cannot be considered spermaceti.
- this product may be utilized very satisfactorily as a spermaceti substitute. It likewise nds considerable value, due to its low glyceride content, in the preparation of glyceridefree calcium soaps for greases.
- 10 designates a continuous, countercurrent fractionating tower of conventional design.
- the oil to be fractionated i. e. sperm oil, tout oil or hydrogenated tout oil
- the solvent may be any of the known normally gaseous hydrocarbons heretofore used by the art in the fractionation of fatty materials, as for example ethane, propane, isobutane, or butane, or mixtures thereof.
- propane is employed as the solvent.
- the temperature and pressure conditions within the tower must be such as to maintain the solvent in the liquid phase.
- the temperature may range from about 205 F. to about 215 F., although the preferred temperature is about 210 F.
- the pressure within the tower may likewise vary within relatively narow limits, i. e. from about 600 p. s. i. to about 700 p. s. i. Presures within the upper portion of this range are considered preferable.
- the solvent to oil ratio should be maintained within the range of about 20:1 to 25:1.
- the product, recovered from the overhead fraction in the fractionation of sperm oil, is a liquid wax ester fraction containing 10% glyceride or less. It is very light in color (FAC 1), is somewhat less viscous than the starting material, has an iodine value in the range of 55-65 and a free fatty acid content of 1.0-l.5%. A small amount of spermaceti will crystallize from the fraction after prolonged standing at room temperature. When hydrogenated in the usual manner, it may be used satisfactorily as a substitute for spermaceti in cosmetics.
- a method for the production of a liquid wax product which comprises: subjecting an oil selected from the group consisting of crude .sperm oil, tout oil and hydrogenated tout oil to the action of a liquefied, normally-gaseous hydrocarbon at a Atemperature within the range of 205 F. to 215 F., a pressure within the range of 600 to 700 p. s. i., and a hydrocarbon to oil ratio within the range of 20:1 to 25:1; and separating out a fraction of said oil by said treatment, said fraction having a high content of the wax ester component of said oil.
- a method for the production of a liquid wax product which comprises: contacting an oil selected from the group consisting of crude ⁇ sperm oil, tout oil and hydrogenated tout oil in a continuous, countercurrent fractionating zone with a liqueed, normally-gaseous hydrocarbon, the hydrocarbon to oil ratio ranging from 20:1 to 25:1; maintaining said zone at a temperature of from 205 F. to 215 F. and at a pressure of from 600 to 700 p. s. i.; and separating out an overhead fraction from said zone, said fraction having a high content of the wax ester component of said oil.
- a method as in claim 2 wherein the liquefied, normally-gaseous hydrocarbon is propane.
- a method of producing a substitute for spermaceti for use in cosmetics which comprises subjecting a sperm oil to countercurrent extraction in the liquid phase with a normally gaseous liquid hydrocarbon at a temperature of from 20S-215 F., a pressure of from 600-700 p. s. i., and a hydrocarbon to oil ratio of 20:1 to 25:1 whereby two phases are formed, one phase being relatively rich in wax esters and the other phase relatively rich in glycerides, separating the phases and hydrogenating the phase rich in wax esters,
Description
R. l. BRABETS ETAL SPERM OIL FRACTIONATION Filed DBG. l5, 1952 SPERMOIL FRACTIONATION TOWER PRoPANe c GLYc amos INvsN-rofzs ATTORNEY nited States Patent ice 2,730,538 SPERM OIL FRACTIONATION Robert I. Brabets, Hazelcrest, and Robert J. Hlavacek,
Berwyn, Ill., and Earle Fritz, East Chicago, Ind., as-
signors to Swift & Company, Chicago, lll., a corporation of Illinois Application December 15, 1952, Serial No. 326,062 4 Claims. (Cl. 260-409) The present invention relates in general to a new composition of matter and to the method of producing the same, and more particularly to a new liquid wax product and the method of obtaining the same from sperm oil and derivatives thereof.
Spermaceti, which is important to the cosmetic industry, is conventionally recovered by seeding and pressing of crude sperm oil. Y This operation is expensive and results in the recovery of about 7% spermaceti based on the weight of the crude oil. Due to this costly operation which results in a relatively small yield, it is desirable to provide an improved method for the recovery Yof spermaceti, or to provide a new product capable of serving as a substitute for the spermaceti.
' It is therefore an object of the present invention to provide a new product which may be less expensive to prepare and which may be eiectively used as a substitute for spermaceti.
Another object of the present invention is to provide a method for treating crude sperm oil or derivatives thereof to produce a new liquid wax product.
Additonal objects, if not specifically set forth herein, will be readily apparent to one skilled in the art from the following detailed description of the invention:
The drawing represents a schematic illustration of a fractionating tower which may be used in carrying out the method of the present invention.
Generally, the present invention comprises the fractionation of sperm oil or derivatives thereof with a liquefied, normally gaseous hydrocarbon under specific operating conditions to produce a material which, after hydrogenation, may be used as a spermaceti substitute.
More specifically, it has been found that, by subjecting crude sperm oil or a derivative thereof, such as tout oil (a by-product from the hot pressing of crude sperm oil), to the action of a liqueed, normally gaseous hydrocarbon in the manner disclosed below, an overhead fraction is obtained which is extremely high in both saturated and unsaturated wax content, and which contains a relatively small amount of glyceride.
Sperm oil is essentially composed of two types of chemical compounds. The triglyceride component constitutes .2S-30% of the crude oil while the remainder is made up of saturated and unsaturated wax esters, e. g. RCOOR.
2,730,538 Patented Jan. `10, 19.56
Spermaceti is a saturated wax ester of the above type, wherein R' and R" are at least C14 or longer. As aforesaid, only about 6-8% spermaceti can be recovered from crudesperm oil. By the present method, an overhead fraction 10-30% of the total oil) is obtained which contains almost exclusively the Wax ester component of the oil, while the bottom fraction contains a reduced amount of wax ester and an increased amount of glyceride. The wax ester in the overhead fraction is a mixture of both saturates and unsaturates, and hence cannot be considered spermaceti. However, by hydrogenation, this product may be utilized very satisfactorily as a spermaceti substitute. It likewise nds considerable value, due to its low glyceride content, in the preparation of glyceridefree calcium soaps for greases.
Referring now to the drawing, 10 designates a continuous, countercurrent fractionating tower of conventional design. The oil to be fractionated, i. e. sperm oil, tout oil or hydrogenated tout oil, is introduced into the top of the tower through line 11. This material then passes downwardly through the packed tower in contact with a rising column of solvent introduced into the tower through line l12. The solvent may be any of the known normally gaseous hydrocarbons heretofore used by the art in the fractionation of fatty materials, as for example ethane, propane, isobutane, or butane, or mixtures thereof. Preferably, propane is employed as the solvent. The temperature and pressure conditions within the tower must be such as to maintain the solvent in the liquid phase. Although these conditions may vary considerably for some fractionations, it is esential in carrying out the present method that they be maintained within relatively narrow limits. The temperature may range from about 205 F. to about 215 F., although the preferred temperature is about 210 F. The pressure within the tower may likewise vary within relatively narow limits, i. e. from about 600 p. s. i. to about 700 p. s. i. Presures within the upper portion of this range are considered preferable. The solvent to oil ratio should be maintained within the range of about 20:1 to 25:1. Under these conditions, the overhead fraction, removed from the tower through line 13 will be found to have a wax ester content of about 90% or better, while the bottom fraction removed through line 14 will be found to have a much smaller wax ester content and a correspondingly higher glyceride content. The following table illustrates typical runs at varying conditions within the specified ranges of operating conditions on sperm oil and tout oil, and clearly illustrates the results of such method. The data given is for the purpose of illustration only, and is not to be construed as placing any limitations on the scope of the present invention, other than those in the appended claims:
Table I Feedstock Operating Conditions Overhead Bottoms Composition Composition Olliijgesliatton (percent) (percent) Temp., Press. R ti Yield Yield Type F. (p. s. i.) a o (percent) (percent) Wax Glycer- Wax Glycer- Wax Glycer- Ester ide Ester 1de Ester ide 210- Crude Sperm Oil 30 610 20:1 15 82 18 85 25 75 Tout Oil gli? 700 25:1 11 95 5 89 65 35 Do 70 30 g1g- 700 25:1 55 92 8 57 43 The product, recovered from the overhead fraction in the fractionation of sperm oil, is a liquid wax ester fraction containing 10% glyceride or less. It is very light in color (FAC 1), is somewhat less viscous than the starting material, has an iodine value in the range of 55-65 and a free fatty acid content of 1.0-l.5%. A small amount of spermaceti will crystallize from the fraction after prolonged standing at room temperature. When hydrogenated in the usual manner, it may be used satisfactorily as a substitute for spermaceti in cosmetics.
Obviously, many modifications and variations of the invention as hereinbefore set forth may be made without departing from the spirit and scope thereof, and therefore only such limitations should be imposed as are indicated in the appended claims.
We claim:
l. A method for the production of a liquid wax product which comprises: subjecting an oil selected from the group consisting of crude .sperm oil, tout oil and hydrogenated tout oil to the action of a liquefied, normally-gaseous hydrocarbon at a Atemperature within the range of 205 F. to 215 F., a pressure within the range of 600 to 700 p. s. i., and a hydrocarbon to oil ratio within the range of 20:1 to 25:1; and separating out a fraction of said oil by said treatment, said fraction having a high content of the wax ester component of said oil.
2. A method for the production of a liquid wax product which comprises: contacting an oil selected from the group consisting of crude `sperm oil, tout oil and hydrogenated tout oil in a continuous, countercurrent fractionating zone with a liqueed, normally-gaseous hydrocarbon, the hydrocarbon to oil ratio ranging from 20:1 to 25:1; maintaining said zone at a temperature of from 205 F. to 215 F. and at a pressure of from 600 to 700 p. s. i.; and separating out an overhead fraction from said zone, said fraction having a high content of the wax ester component of said oil.
3. A method as in claim 2 wherein the liquefied, normally-gaseous hydrocarbon is propane.
4. A method of producing a substitute for spermaceti for use in cosmetics which comprises subjecting a sperm oil to countercurrent extraction in the liquid phase with a normally gaseous liquid hydrocarbon at a temperature of from 20S-215 F., a pressure of from 600-700 p. s. i., and a hydrocarbon to oil ratio of 20:1 to 25:1 whereby two phases are formed, one phase being relatively rich in wax esters and the other phase relatively rich in glycerides, separating the phases and hydrogenating the phase rich in wax esters,
References Cited in the le of this patent UNITED STATES PATENTS 2,077,837 Holwech Apr. 20, 1937 2,228,040 Voogt et a1 Ian. 7, 1941 2,505,338 Palmer Apr. 25, 1950 2,521,234 Leaders et al. Sept. 5, 1950
Claims (1)
- 2. A METHOD FOR THE PRODUCTION OF A LIQUID WAX PRODUCT WHICH COMPRISES: CONTACTING AN OIL SELECTED FROM THE GROUP CONSISTING OF CRUDE SPERM OIL, TOUT OIL AND HYDROGENATED TOUT OIL IN A CONTINUOUS, COUNTERCURRENT FRACTIONATING ZONE WITH A LIQUEFIED, NORMALLY-GASEOUS HYDROCARBON, THE HYDROCARBON TO OIL RATIO RANGING FROM 20:1 TO 25:1; MAINTAINING SAID ZONE AT A TEMPERATURE OF FROM 205* F. TO 215* F. AND AT A PRESSURE OF FROM 600 TO 700 P. S. I.; AND SEPARATING OUT AN OVERHEAD FRACTION FROM SAID ZONE, SAID FRACTION HAVING A HIGH CONTENT OF THE WAX ESTER COMPONENT OF SAID OIL.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US326062A US2730538A (en) | 1952-12-15 | 1952-12-15 | Sperm oil fractionation |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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US326062A US2730538A (en) | 1952-12-15 | 1952-12-15 | Sperm oil fractionation |
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US2730538A true US2730538A (en) | 1956-01-10 |
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US326062A Expired - Lifetime US2730538A (en) | 1952-12-15 | 1952-12-15 | Sperm oil fractionation |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3099561A (en) * | 1960-02-12 | 1963-07-30 | John E Thompson | Separation process |
US3142570A (en) * | 1962-12-31 | 1964-07-28 | John E Thompson | Separation process |
US20100055062A1 (en) * | 2006-11-21 | 2010-03-04 | L'oreal | Cosmetic composition comprising a proline derivative and/or a salt of the said derivative |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2077837A (en) * | 1935-02-04 | 1937-04-20 | Holwech Wilhelm | Process for the refining of sperm oil or wax |
US2228040A (en) * | 1936-11-28 | 1941-01-07 | Shell Dev | Process for stabilizing ester type oils against cold |
US2505338A (en) * | 1948-02-05 | 1950-04-25 | Kellogg M W Co | Refining fatty oils |
US2521234A (en) * | 1946-10-16 | 1950-09-05 | Swift & Co | Solvent fractionation of fatty material |
-
1952
- 1952-12-15 US US326062A patent/US2730538A/en not_active Expired - Lifetime
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2077837A (en) * | 1935-02-04 | 1937-04-20 | Holwech Wilhelm | Process for the refining of sperm oil or wax |
US2228040A (en) * | 1936-11-28 | 1941-01-07 | Shell Dev | Process for stabilizing ester type oils against cold |
US2521234A (en) * | 1946-10-16 | 1950-09-05 | Swift & Co | Solvent fractionation of fatty material |
US2505338A (en) * | 1948-02-05 | 1950-04-25 | Kellogg M W Co | Refining fatty oils |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3099561A (en) * | 1960-02-12 | 1963-07-30 | John E Thompson | Separation process |
US3142570A (en) * | 1962-12-31 | 1964-07-28 | John E Thompson | Separation process |
US20100055062A1 (en) * | 2006-11-21 | 2010-03-04 | L'oreal | Cosmetic composition comprising a proline derivative and/or a salt of the said derivative |
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