US3629307A - Refining process for crude glyceride oil - Google Patents

Refining process for crude glyceride oil Download PDF

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Publication number
US3629307A
US3629307A US828926A US3629307DA US3629307A US 3629307 A US3629307 A US 3629307A US 828926 A US828926 A US 828926A US 3629307D A US3629307D A US 3629307DA US 3629307 A US3629307 A US 3629307A
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United States
Prior art keywords
oil
crude
soap stock
mixture
free fatty
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Expired - Lifetime
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US828926A
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English (en)
Inventor
Morris Anthony Marino
Frederic John Birkhaug
George Edward Sadek
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Unilever Bestfoods North America
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Unilever Bestfoods North America
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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
    • C11B3/00—Refining fats or fatty oils
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • C11B3/06—Refining fats or fatty oils by chemical reaction with bases

Definitions

  • This invention relates to an improved process of alkali refining a glyceride oil and more particularly to a process in which it is not necessary to degum or otherwise pretreat the glyceride oil prior to the alkali refining treatment.
  • a problem which arises in the purification of glyceride oils is that crude glyceride oils tend to have high contents of such materials as free fatty acids, phosphatides (phospholipids), and particulate matter, and they are often relatively viscous. Since free fatty acids, phosphatides and particula'te matter are undesirable in many edible products, crude glyceride oils are refined to remove these undesirable materials.
  • a glyceride oil particularly an edible glyceride oil, is conventionally refined by treating it with an aqueous solution of sodium hydroxide or sodium carbonate.
  • the alkali ice treatment improves the color of the oil. It precipitates the phosphatides, neutralizes any remaining free fatty acids by forming soaps, and entraps the particulate matter in the soaps.
  • Alkali refining is usually only one of several steps that are designed to place the oil in a form that is acceptable to the consumer.
  • Other treatment such as bleaching, hydrogenating, Winterizing and deodorizing are usually employed for improving quality.
  • the alkali refining step tends to be practiced to disadvantage when the glyceride oil contains free fatty acids at higher levels. Larger amounts of soap are formed and are accompanied by serious oil losses, because the neutral oils are entrained or occluded in the soap. This is especially true when the glyceride oil contains surface active emulsifying agents such as phosphatides. In general, the oil loss, during the refining of such oils, is on the same order of magnitude as the amount of free fatty acids originally present in the glyceride oil.
  • a further object of the invention is to provide an improved process for refining a gummy glyceride oil whereby lower refining losses due to saponification and entrapment of neutral oil in the separated soap stock occur.
  • a still further object of the invention is to provide an improved process for alkali refining a viscous glyceride oil that contains substantial quantities of free fatty acids, gummy material and particulate matter.
  • a specific object of the invention is to develop an improved process of alkali refining a viscous corn oil which contains substantial quantities of free fatty acids, gummy material and particulate matter.
  • the invention in one embodiment thereof is a process of refining a glyceride oil that contains free fatty acids as impurities, which comprises mixing an aqueous sodium hydroxide solution with the oil to form a mixture; allowing the mixture to react until the free fatty acids are converted into a soap stock phase, to form an oilwater-soap stock composition; dehydrating the composition to form a dehydrated oil-soap stock mixture; conveying' the dehydrated mixture into a pressurized centrifuge, and therein simultaneously rehydrating and centrifugally separating the soap stock from the refined oil.
  • FIG. 1 is a flow diagram illustrating the process.
  • This process is applicable to a viscous glyceride oil which contains gummy materials such as phosphatides, dissolved protein fragments, and, as well, other particulate matter such as, for example, cellulose, starch, inorganic insolubles, and the like.
  • the process is, of course, also applicable to a glyceride oil which does not contain these impurities. But it is most advantageously applied to a glyceride oil containing these naturally-occurring materials, since the process of the present invention removes these materials along with the free fatty acids, with a minimal loss of glyceride oil. This is surprising in View of the fact that phosphatides are surface active agents that ordinarily solubilize glyceride oil in soap stock, and increase oil losses.
  • the preferred sodium hydroxide solution for use in the practice of this invention has a concentration of at least Baum. This reduces the amount of water which must be removed in the dehydration step.
  • the concentration of the sodium hydroxide solution is within the range from about 10 Baum to about 32 Baum.
  • the total amount of sodium hydroxide added to the glyceride oil is preferably not more than about 0.3% more than that necessary to neutralize the free fatty acids present. Most preferably, the excess of sodium hydroxide falls within the range from about 0.1% to about 0.3% above theoretical. The use of this amount of sodium hydroxide minimizes saponification of the glyceride oil, while ensuring neutralization of the free fatty acids.
  • the mixing is preferably accomplished by flowing together streams of sodium hydroxide solution and glyceride oil in a pipe containing bafiles and a mechanical agitator. As the mixture flows through the pipe the bafiles and the agitator insure thorough mixing.
  • the total residence time and temperature in the pipe are preferably those mentioned above. This allows sufiicient time in the preferred temperature range, for the sodium hydroxide to react with the free fatty acids.
  • the resulting oil-water-soap stock composition is then dehydrated by vacuum drying.
  • the vacuum drying is done by spraying the composition continuously into a chamber that is continuously evacuated.
  • the water and volatile gases are removed as vapors, and the dehydrated oil-soap stock mixture, which is much less volatile than the water, collects at the lower end of the chamber, and is pumped out.
  • the temperature of the chamber and its contents should be maintained within the range from about 150 F. to about 200 F., so that the vapor pressure of the water is high enough for eflicient water removal.
  • the dehydrated oilsoap stock mixture should contain no more than about 3.0% by weight of water.
  • the oil-soap stock mixture preferably is transported into a pressurized centrifuge, where it is rehydrated and centrifuged simultaneously.
  • the rehydrating agent preferably water
  • the rehydrating agent is generally heated to least about 165 F., prior to the rehydration.
  • suitable rehydration agents include water and water solutions of neutral or weakly acidic or basic materials which do not react with the oil. Examples of such materials include salts, for example sodium chloride, sodium sulfate, sodium silicate, potassium acetate, and the like and weak organic acids such as citric acid.
  • the preferred glyceride oil for use in the practice of this invention is a viscous non-degummed (crude) corn oil.
  • a crude corn oil, prior to refining, generally contains an amount of free fatty acid falling within the range from about 1% to about 7%, an amount of gummy material (phosphatides, dissolved protein, etc.) falling within the range from about 1% to about 4%, an an amount of particulate matter falling within the range from about 0.1% to about 1.0% all of the precentage figures being by weight based on the total weight of the crude corn oil.
  • the oil and a 15 Baum sodium hydroxide solution were each preheated to F. and flowed together in a bafiied pipe equipped with a mechanical agitator and then through the pipe.
  • the pipe was maintained at 180 F.
  • the battles and the agitator in the pipe insured good mixing of the oil and the caustic.
  • a 0.2% excess of sodium hydroxide was maintained over that amount necessary to saponify the free fatty acids.
  • the average residence time for the mixture in the pipe was about 2 minutes.
  • the crude oil-alkali mixture after passage through the baffled pipe, was continuously spray dried under vacuum.
  • the entire spray drier was maintained at a temperature of approximately F.
  • the temperature was controlled by passing steam through sealed coils contained within the spray drier.
  • a pressure of between about 24 inches and 28 inches of mercury was maintained within the spray drier.
  • the dehydrated, spray-dried mixture was delivered to a pressurized centrifuge.
  • the discharge pressure (light phase) of the pressurized centrifuge was periodically adjusted for efficient separation, and was maintained within the range from about 40 p.s.i.g. to about 70 p.s.i.g.
  • the inlet pressure to the centrifuge was adjusted at and maintained within the range from about 90 p.s.i.g. to about 110 p.s.i.g., so as to provide a pressure dilferential across the centrifuge of at least 25 p.s.i.
  • Each sampling operation consisted of removing a series of 5 samples, one sample each of crude corn oil, dehydrated mixture, crude oil-alkali mixture, refined corn oil, and soap stock. Each of the 4 crude corn oil samples was analyzed to determine its free fatty acid content. Each of the 4 dehydrated mixtures was analyzed to determine its water content.
  • dehydrating the composition to provide a dehydrated oil-soap stock having a Water content of no more than 3.0% by weight based on the total weight of the oil-soap stock supply;
  • a process as in claim 5 wherein said pressurized centrifuge has a light phase discharge and an inlet and operates with a discharge pressure at the light phase discharge which falls Within the range from about 25 p.s.ig. to about p.s.i.g. and with an inlet pressure which falls within the range from about 75 p.s.i.g. to about 150 p.s.i.g.
  • discharge pressure falls within the range from about 40 p.s.i.g. to about 70 p.s.i.g. and said inlet pressure falls within the range from about 90 p.s.ig. to about p.s.i.g.
  • a process as in claim 9 wherein said crude corn oil, prior to refining contains an amount of free fatty acids falling within the range from about 1% to about 7%, an amount of gummy material falling within the range from about 1% to about 4% and an amount of particulate matter falling within the range from about 0.1% to about 1%, said percent figures being weight percent based on total weight of the crude corn oil.
  • dehydrating the composition by spray drying under vacuum at a temperature falling within the range from about F. to about 200 F. to provide a dehydrated oil-soap stock having a water content of no more than 3.0% by weight based on the total weight of the oil-soap stock supply;

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)
US828926A 1969-05-29 1969-05-29 Refining process for crude glyceride oil Expired - Lifetime US3629307A (en)

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US82892669A 1969-05-29 1969-05-29

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US (1) US3629307A (enrdf_load_stackoverflow)
JP (1) JPS4912563B1 (enrdf_load_stackoverflow)
BR (1) BR7019349D0 (enrdf_load_stackoverflow)
GB (1) GB1301731A (enrdf_load_stackoverflow)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4569796A (en) * 1982-06-29 1986-02-11 Lever Brothers Company Process for refining triglyceride oils
US5308372A (en) * 1984-01-18 1994-05-03 Daniels Ralph S Vegetable oil processing to obtain nutrient by-products
US6632952B1 (en) 1984-01-18 2003-10-14 Carrie Lee Mahoney Agricultural oil processing using potassium hydroxide
US20130109873A1 (en) * 2008-09-10 2013-05-02 Poet Research, Inc. Oil composition and method of producing the same
US9695449B2 (en) 2008-09-10 2017-07-04 Poet, Llc Oil composition and method of recovering same

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6290721U (enrdf_load_stackoverflow) * 1985-11-27 1987-06-10
JP2009108145A (ja) * 2007-10-27 2009-05-21 Kaneka Corp 脱酸油脂の製造方法またはそれによって得られる精製油脂

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4569796A (en) * 1982-06-29 1986-02-11 Lever Brothers Company Process for refining triglyceride oils
US5308372A (en) * 1984-01-18 1994-05-03 Daniels Ralph S Vegetable oil processing to obtain nutrient by-products
US6632952B1 (en) 1984-01-18 2003-10-14 Carrie Lee Mahoney Agricultural oil processing using potassium hydroxide
US20130109873A1 (en) * 2008-09-10 2013-05-02 Poet Research, Inc. Oil composition and method of producing the same
US9695449B2 (en) 2008-09-10 2017-07-04 Poet, Llc Oil composition and method of recovering same
US10526623B2 (en) 2008-09-10 2020-01-07 Poet Research, Inc. Oil composition and method of recovering same
US11359218B2 (en) * 2008-09-10 2022-06-14 Poet Research, Inc. Oil composition and method of recovering same

Also Published As

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JPS4912563B1 (enrdf_load_stackoverflow) 1974-03-26
BR7019349D0 (pt) 1973-01-11
DE2025739A1 (de) 1970-12-03
GB1301731A (enrdf_load_stackoverflow) 1973-01-04

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