CA2019916A1 - Process for deodorizing oils and fats - Google Patents

Process for deodorizing oils and fats

Info

Publication number
CA2019916A1
CA2019916A1 CA002019916A CA2019916A CA2019916A1 CA 2019916 A1 CA2019916 A1 CA 2019916A1 CA 002019916 A CA002019916 A CA 002019916A CA 2019916 A CA2019916 A CA 2019916A CA 2019916 A1 CA2019916 A1 CA 2019916A1
Authority
CA
Canada
Prior art keywords
oil
oils
fat
deodorized
steam
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
CA002019916A
Other languages
French (fr)
Inventor
Jose Huesa Lope
Maria Del Carmen Dobarganes Garcia
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Carburos Metalicos SA
Consejo Superior de Investigaciones Cientificas CSIC
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Publication of CA2019916A1 publication Critical patent/CA2019916A1/en
Abandoned legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/12Refining fats or fatty oils by distillation
    • C11B3/14Refining fats or fatty oils by distillation with the use of indifferent gases or vapours, e.g. steam

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)

Abstract

ABSTRACT A PROCESS FOR DEODORIZING OILS AND FATS A process for deodorizing oils and fats based on subjecting the products to be deodorized to a current of an inert gas, preferably nitrogen, under vacuum conditions in a pressure range from 1 to 8 mbars and at a temperature between 60°C and 270°C. This process, when compared to the conventional methods using steam currents, results in less power and water consumption, does not contaminate the environment and facilitates the recovery of byproducts.

Description

~ 1 2~

A PROCESS FOR DEODORIZING OILS ~ND ~AT~

D E S C ~ I P T I O N

The i.nvent.ion relates to a process for deodori.zi.ng oils and fats. In this description, the word "oil" has a wide meaning and includes any fatty liqui.ds of ve~etal or animal origin .
The deodorizin~ sta~e is one of the ~ost important i.n the process of refinin~ oils, because i.t has the ~reatest impact on the quality of the oil or fat substance bein~
refined and it gi.ves the products the desi.red organoleptic characteristics. 5ince deodorizi.n~ is part of the refinin~
process, it is proper to refer to said process in this description.
The oils are natural products of ve~etal origin (seeds and oily fruits~ or animal origin (fatty tissues, organs, etc.) that present a complex nature.
Practically all the oils are formed by glycerides, that is, glycerine esters with fatty acids (acids with a straight chain and between 12 and 24 carbon atoms, except for a few cases). Because the esterification i.s a revers-ible reaction, the oils contai.n not only tri~lycerides but also mono- and diglycerides formed by the action of certain enzymes, oxidizing processes, etc. that produce the hydroly-sis of these tri~lycerides. This results in the Pormation of mono- and di~lycerides, aæ well as free fatty acids.
In addition to these mono- and diglycerides, which are detrimental due to their emulsifying properties which ne~atively affect the processes to be descr.ibed later, the oils contain a number o~ other components. ~ome of these components, such as the toco~erols, sterols, carotenes, etc., due to their antioxidizin~, provi.taminic, etc., prop-erties, are beneficial while others, such as the free fatty acids, phospholipids, trace metals, humidity, etc., are harmful and must be eliminated.
In view of the foregoing, all oils and fats whether .............................. , .. , .. , .. ~.. ... ....... .... .... ........ .... ..... ....... ... . .
- 2 - 20~

of ve~etal or ani.mal origin (except for the vir~in oils), must under~o a series of prior treatments in order to be used in food or in i.ndustry. The process that includes all these treatments necessary for the separation of the harm-ful substances i.s called refin.in~.
Refinin~ is a necessary process in order to reduce to a mi.nimum all the oil contaminants which adversely affect its final auali.ty and negati.vely .impact on the effjciency of the operati.ons - some of them necessary - of fraction-ing, transesterification and hydrogenation. The refiningalso makes the oil capable of being used as a food or for other industrial applications.
The refining process can be accomplished by a number of systems, although most of them are no longer in use.
Practically, only the so-called traditional or chemical refining and the physical refining processes are used.
Hereinafter there is a schematic diagram identifying the differences between both types.

Physical Refining Crudl Oil Chemical Refining Degumming or Demucilagination I I
~ Neut~ralization Decoloration Dewaxing Filtration Sco~ring l Deco~oration 25 Neutralizing Deodorization Filt~ation Deodorization Brightening Consumer ............... .. .... .... . . .
- 3 - 20~

In the case of certain oils and fats, it is desirable to introduce other sta~es ln the process, such as hydrogen-ation, fractionin~, etc., depending on the nature of the oil.
With reference to chemical refining, it is important to point out that in the sta~e of degwnmin~ the oils it is possible to separate the following substances: phos-pholipids, proteins, trace metals, some pigments, carbo-hydrates, etc. The separation is usually accomplished in an acid medium, because it produces a more complete and rapid precipitation than performing the degumming operation with water.
The main purpose of neutralization is to separate the free fatty acids naturally present in the crude oils. There are various neutralization systems, although the most com-monly used are the neutralization with caustic alkalies and the neutralizing distillation.
The object of scourin~ is to remove the traces of soap that mi~ht have dissolvefl in the oil. It allows the separation of all alkaline substances (excess soaps and caustic soda) present in the oil, as well as trace metals, phospholipids and other impurities. The water used for scouring should be at a temperature of approximately 90YC
and is used in a rat.io that varies from 10 to 15%.
Once the oil is scoured, it i9 necessary to dry it in order to eliminate any residual humidity. This humidity could adversely affect the subsequent decoloration process because it deactivates the decoloring agents, such as earths and activated carbons.
Most of the pigments are eliminated in the decoloration process through the adsorption on decoloring earths or activated carbon.
The object of the deodorization stage is to eliminate the substances that give bad odor and taste to the oils.
Some of these substances have been identified as ketones, aldehydes, carbohydrates, terpenes, alcohols of very _ 4 _ 2~

different molecular weight and volatillty (most of them come from the oxidation and degradation of the fatty aclds), etc.
Later, we will refer a~ain to the conventional deodori7.ation process.
Regarding the physical refinin~ process, it is important to mention that the main difference between the traditional or chemical refinin~ process and the physical refinin~ process is that, in the former, the fatty acids are eliminated as soaps or pastes by means of an alkali during the neutralization stage, carrying with them other compounds or impurities such as phosphatides, trace metals, pigments, etc. and requiring less drastic decoloration conditions. In the physical refining process, however, the pretreatment stages prior to the neutralizing deodorization stage must be performed under more energetic conditions.
As indicated above, the process consists of the following stages: degumming, decoloration and neutralizing deodorization.
Owing to the fact that the oils must enter in the distillation apparatus free from any substance that is easily degradable with temperature, such as phosphatides, it is necessary to subject the oils to a prior demucilagination or de~ummin~ process.
Thls process is analo~ous to that Per~ormed duri.n~
the traditional refinin~ of the oils, with the exception that, in this case, it is a very long and energetic process in order to reduce the phospholipids content to a value of less than 0.2%.
The decoloration is performed in a similar manner as for chemical refining. The only difference is a greater consumption of decoloring earths due to the more energetic pretreatment required by the oil before undergoing the neutrali.zing deodorization process.
The physical refining process, in itself, consists of a distillation using steam to entrain the free fatty acids, as well as all those volatile substances that accompany oils and give them their typical odor and taste and to 2~ 3 Aestroy the thermolabile pigments.
The oil, once de~ummed and decolored, passes to an aerator. The oil, previously heated, is then introduced in the deodorizer where it is subject to an injected countercurrent of steam and remains under vacuum conditions and at an approximate temperature of 275C.
It can be seen from the previous description that both refinin~ processes include a deodorization stage, where the s~bstances that give the oils bad odor and taste are removed.
In practice, the removal of these substances is accomplished by the action of a countercurrent of dry steam under vacuum conditions and at a high temperature. The deodorization is possible under these conditions due to the large volatility difference between the triglycerides and the substances that give the oils the odor and taste. The vapour pressure of these compounds is so extremely low that a very high temperature would be required in order to remove them under atmospheric pressure conditions. The deodorization is accomplished more efficiently by combining the vacuum with steam entrainment. When the steam current passes through the oil, the distillation starts when the sum of the partial pressures of the vapour and of the volatile compounds reaches the pressure that exists on the oil surface. This occurs at a temperature lower than without the steam.
In order to obtain the maximum effici.ency of the deodorizati.on process, the steam must be injected in the oil in such a manner that a large number of small bubbles are formed with a very lar~e surface in relation to their wei~ht. In experiments, it has been observed that the saturation of the steam bubbles is so fast that it can be considered as complete at absolute pressures of ap-proximately 8 mbars.
There are losses incurred during the deodorization process. In addition to the weight loss caused by the removal of the small amounts of volatile Products ~less 2 ~

than 0.2%), there is a loss of triglycerides during this process because of the mechanical entrainment of the oil by the steam. The amount of oil entrained is a function of the velocity and density of the steam. The losses due to the hydrolysis of the oil by the steam are unavoidable.
In general, a deodorizing station consists of the following unit:
-Deodorizing device -Oil heating system -Vacuum system -Steam generator for producing the necessary steam flow.
-Condenser for volatile products -Oil coolers There is a wide variety of deodorizing facilities, which may be classified as discontinuous, semicontinuous and continuous. No greater details thereof will be given here.
It should be noted that, during the deodorizing process, the oils undergo a partial decoloration due to the loss of color of certain pigments at high temperature. The degree of decoloration depends on the previous bleaching pretreatment and the nature of the oil.
It should also be pointed out that the oils lose the natural antioxi.dizers durln~ their deodorization, which increase their tendency to become oxidlzed.
These known systems of deodorizing the oils by the use of steam present the following drawback:
-High energy consumption -High water consumption -Enviro~mental contamination -The byproducts may not be recovered economically.
The purpose of this invention is to provide an oil deodorization process that will eliminate the above mentioned drawbacks.
In this invention, the deodorization is achieved through a process characterized in that the oil to be .

- 7 - 2 ~ 3 deodorized is subjected to the action of an inert gas flow, preferably nitrogen, which will carry away the substances that impart bad odor and taste to the oil. The process takes place under vacuum conditions with pressures between 1 and 8 mbars, and at temperatures between 60C and 270C.
Preferably, the oil to be deodori.zed has been subjected to a prior de~umming, decoloration, neu-tralization and/or deaeration process.
According to another preferred feature, the inert gas is dispersed within the oil being deodorized, which results in a very good diffusion or distribution of the nitrogen throughout the oil mass.
The optimum inert gas flow value is preferably between 0.8 and 3 Nm3/hour per tonne of oil.
The process is also applicable to installations for continuous flow. In these cases, . there is a continuous incoming volume of oil to be deodorized and, therefore, a continuously outgoing volume of deodorized oil. This creates a continuous oil flow inside the deodorizing facility; in this invention, the nitrogen gas should preferably flow in the opposite direction to the oil flow.
The following conclusions have been reached from the tests and experiments performed using the process which is the subject of t;his invention:
a) The auality oP the olls deodor.tzed using the process of this invention is not only similar to that of the oils obtained using the traditional method, but also these oils have the advantage that they do not have products originating from the hydrolisis of the glycerides or, furthermore, products resulting from oxidation, such as peroxides.
b) The stability of the deodorized oils using the process of this invention is superior to that of the products refined using the traditional method; the reason for this is due to the higher unsaponifiable compounds content in the oils that have been refined with nitrogen.

- 8 ~

c) The utilization of nitro~en ls particularly advisable in the refining of hi~hly unsaturated oils, such as soy bean, sunflower, fish and other similar oils.
d) The process is applicable with utmost efficiency to the physical refining of oils (neutralizin~
deodorization stage).
e) The byproducts obtained with the process of this invention are of better quality than those obtained with the traditional method; besides lar~er amounts of such byproducts are obtained.
f) There is an important energy savin~, as well as a lower water consumption.
g) When the process is used in conjuction with vacuum pumps to obtain an adequate vacuum, the pollution in the deodorizing process disappears.
Several examples of the process of this invention are shown below. These examples are not to be considered as limitin~ the applications of the invention.

The raw material was olive oil, neutralized with caustic soda and decolored with Gador C earth. Its content of unsaponifiable compounds was 1.24%.
Thé steam generated in a container by the heat of a hot plate is injected in a deodorizin~ flask.
Alternatively, the nitrogen from a pressurized vessel is used as the carrier fluid in this process, with the effective diffusion being regulated by a porous device and a flow control valve with its corresponding flowmeter.
A number of tests were performed to study the effect of the different parameters that have an influence on the deodorizing process: time, temperature, pressure and flow rate of the carrier fluid. It was decided to leave the flowrate and pressure of the carrier fluid constant and to combine the time and temperature parameters. A flow of 30 ml/min of nitro~en gas or steam was selected for the carrier fluid, which resulted in good stirring of the oil in the deodorizer and a pressure of 4 mbars. Once these - ~ - 2~ 6 conditions were fixed, tests were performed by varyin~ the temperature between 180C and 270C and the time between 2 and ~ hours.
The control for the different tests was the amount of unsaponifiables in the oil and the or~anoleptic properties of the corresponding refined oils. Table I shows the average data for three such tests.
From the examination of this data it can be seen that the quality of the oils is similar in all cases, because no appreciable differences have been noted between them for most of the tests. What should be pointed out is that the content of unsaponifiable compounds is higher when nitrogen is used in place of steam. This is beneficial for the later stability of the oil. The purpose of using temperatures as high as 270QC was to prove that the fatty acids did not undergo isomerization (which was verified by the spec-trographs of the refined oils), so that the oils could undergo physical refining with this new system.
The amounts of impurities in the two oils to be tested were determined due to the poor quality of these oils. The following are the results:
Crude 1 Crude 2 Petroleum ether impurities 0.79/~ 0.0~%
Humidity 0.20% 0.10%
In view of the above results, the Crude 1 o:~l was purified prior to the tests due to its hl~h content of impurities. Such treatment was not considered necessary for Crude 2.
The purification was accomplished heating the oil to 70QC and adding to it a solution of 2/1000 of phosphoric acid and 4/1000 of water. The oil was stirred during 20 minutes and was then allowed to decant. The precipitate thus formed was then separated. A sample of the oil was taken and its acidity determined to proceed with the neu-tralization of both the free fatty acids and the residual mineral acid.
Once the acidity was known, the oil was heated a~ain - lo- 2~

to 70C and the amount of 18 Bé caustic soda required to neutraliæe the acidity, plus an excess of 10% was added to the oil. The oil was then stirred during 20 minutes, the pastes were separated by decantation and the oil was scoured with hot water. These scouring operations were repeated unti.l the wash waters did not show any alkaline reaction.
The oil once scoured and dried, was decolored with 0.5% of Gador C decoloring earth, heated to 80QC, stirred during 10 mi.nutes and filtered after this time had elapsed.
The oil was then subjected to the deodorizin~
process, with parallel tests performed usin~ steam and nitrogen under the followin~ conditions:

Conàition~ ressure 4 mbars; Tern~ 270QC; Time: 3 h; and Flowr;lte: 30 rnl/min.

TAE31,F :1 I

C rude 2 D~odor . 1 Deodor . 2 Deodor . 1 Deodor . 2 steam stearn nitro2en n .1 rogen ACIDITY 6.86 6.59 0.()5 0.08 0.08 0.05 K270 0.32 0.50 0.42 0.5 0.43 0.'52 PEROXIL3E NQ12.5 13.05 1 3.6 0 0 BELLIER NQ - - 15 12.5 14.5 12.'i 10 IODINE NQ 78.478.6 78.7 79 78.fi 78.9 REFRACT. Ind . - - 1 . 46 80 1 . 46 88 1 . 46 82 1 . 46 85 SAPONIF. NQ - - 195,3 184,5 195,1 194.3 UNSAPONIFIALLES
(HEXANE) 1,30 ~,32 0,65 0.132 0.72 0.86 15 ACIDS:
PALMITIC 1413,3 7 . 9 6 .1 7 7 PALMITOI.EIC 1.41.2 ~ .4 1 .2 ~ .4 ~ .2 MARGARIC 0.2C).2 0.2 0.2 0.2 0.2 M.ARGAROLEIC 0.30.4 0.3 0.2 0.2 0.3 20 STEARIC 2.52,3 2,3 2.6 2,4 2.6 OLEIC 7173.2 72.6 74.9 72.3 74.1 L,INOLEIC 86 . 6 7 6 . ~ 7 .1 6 . 2 I.INOL,ENIC 0,9().4 0.4 0.4 ().3 (1.:3 ARACHIDONIC 0.50.5 0.6 0.6 0.6 0~6 25 G~l:)OL,E:~(' 0,30.4 0.4 0.4 0. 4 0 4 BEHENIC 0,10,~ 0,~ 0,~ 0,~ 0,~
L,INOCERIC 0,80,8 0,3 0.4 0.7 0.4 POSITION: 10.9 3,1 3,~. 3 3,9 2 ~

The quality of the refined oils was as follows: Oil N 1 produced a refined product with acceptable almondlike organoleptic characteristics, both with steam and with nitrogen processes. Oil N~ 2 produced in both cases (with steam and with nitrogen) an acceptable refined product wi.th a very slight taste reminiscent of "Pickled olive" oils.
The content of polar compounds was determined for the refined oils. It was observed that the percenta~es of altered triglycerides, dimers and oxidi.zed compounds were lower than when nitrogen was used, except in the tests at 270C where there were similar percentages of altered triglycerides and dimers due to the high temperature. The amount of diglycerides was always lower when nitro~en was used.

TABLE III
.

Polar Crude 1 Crude 2 Deodor.l Deodor.2 Deodor.l Deodor.2 Compounds (%) Steam Steam N2 N2 Triglycerides Dlmers 0-3 0.1 2,4 3.4 1.3 1.4 Triglycerides Oxidized 1 1.5 0.9 1.6 0.6 0.8 Diglycerides 1.73.2 1.7 2 0.5 0.6 Free Fatty Acids 6.56.1 0.2 0.4 0.1 0.2 Total: 9.510.9 5.2 4 2.5 3 .......... ............... .... . .... . ....... ... . .. . . . .. . ...... . . .

- 13 _ 2~

....
The method described for Example 1 was applied to a sunflower oil under the followin~ conditions: Pressure: 4 mbars; Time: 3 hours; Steam or nitro~en flowrate: 30 ml/min.; Temperature: 180C and 220C. All the tests produced refined oils with the qualit~ and characteristics of refined seed oils.

Soy bean oil was used which, as the sunflower oil, is more sensitive to the refinin~ conditi.ons because of its higher content of unsaturated fats. The conditions were the same as for the previous example and the results were similar to those obtained with sunflower oil. The deodorised oil exhibited a significant decoloration.

Fish oil was used for the tests with animal fat oils because of two very important reasons: its special charac-teristics because it is a highly unsaturated oil and, therefore, very sensitive to the oxidation and isomerization agents, and also because of its recent significant importance in the preparation of dietetic products. This is due to its high PUFA (polyunsaturated fatty acids) content which are those that result in higher oil instability.
After a few prior tests, a fi.sh oil was used that had the following characteristi.cs:
TABLE IV
Acidity 3.6%
Phosphorus 172 ppm Unsaponifiables 1.1%
Insoluble Ketones 1.2%
Impurities 0.05%
Uumidity 0.2%
Sterols 9804 ppm ..... , ., .. ~ .. , ., . .. , ~, .... , ., , .,, ",, ., .. , .,, ... , . ........ . , .. . .. .... , ., ., " . . . . ............. .. ..
...... . .. . .. . ... . .... . . .. .. . . .

- 14 - 20~

TABLE V
Fatty Acids Content (Only the most significant percentages are included) AcidCrude Purified Decolored Deodorized 14:06.9 7.1 6.8 6.4 16:017.4 17.3 17.2 18.3 16:19.4 9.5 9.4 5.8 18:02.6 2.8 3.1 4.7 18:111.0 11.1 11.4 15.9 20:41.2 1.1 1.0 0.6 20:520.8 20.1 19.0 18.4 22:51.7 1.2 2.3 1.6 22:66.3 6.1 5.6 4.2 PUFA30.0 29.1 27.9 24.8 As it can be seen from the previous Table, the total PUFA (polyunsaturated fatty acids) content was significantly reduced when the process followed the described conditions. Therefore, after several tests trying to preserve the polyunsaturated acid content with negative results, it was decided to use an inert gas atmosphere. It was observed that, when the oil was processed in an inert ~as atmosphere, nitrogen, its content of polyunsaturates was not affected~ After several tests with positive results, the following conditions were selected as being optimum for the process:

- 15 - 2~

-Purification:
The oil was heated to 35-40C, with nitrogen gas flowing from the beginning of the test. Phosphoric acid was then added with stirring in a ratio of 2:1000. The stirring was maintained until the mixture reached a temperature of 60C. A 4% volume of an aqueous 5% sodium chloride solution was added and the stirring was suspended. A 6% volume of water was added, the solution was stirred and the oil was separated from the aqueous phase by decanting. All these operations were performed in a nitrogen atmosphere.
- Neutralization:
The oil was heated to 60QC and a soda solution of 24 Bé was added in sufficient quantity (with a 20% excess) to neutralize the acidity of the oil plus the remaining mineral acidity from the phosphoric acid that was previously added.
The mixture was maintained with stirring under a nitrogen atmosphere at 60~C during 30 minutes. After this time, the stirrin~ was stopped and a 25% volume of hot water was added; the mixture was stirred again during 10 minutes. After this time, the stirring was stopped and the solution was allowed to rest until it could be properly de-canted (usually from 15 to 20 minutes). The aqueous phase was then separated.
Care should be exercised to prevent the nitrogen gas in~ection from penetrating in the fatty phase; it should always remain above the surface of the oil because otherwise the nitrogen gas would become mixed with the pastes which would rise to the surface and make the separation very difficult.
-Scouring:
Since the soaps always constitute a poison for the decoloring earths and negatively affect the decoloration process, the neutralized oils were scoured in order to eliminate all traces of soap. A 25% volume of hot water was added and stirring took place during 10 minutes. The , .. ~ ........ .. .

2 ~

mixture was allowed to rest until it could be decanted and the scourin~ waters were removed. This operation was repeated until the water used in the scouring presented a neutral reaction.
-Decoloration:
Before the decoloration process, the oil was dried to eliminate any humidity remaining from the washing operations. For this purpose, the oil was heated to 60QC, under vacuum and a flow of nitrogen gas. Once the oil was dry, 1.5% of decoloring earth (Gador Type C) was added, as well as 0.2% of activated carbon (Ceca Type AG). The oil was held 60QC under stirring during 20 minutes and then filtered.
As indicated before, all the tests were performed in a nitrogen gas atmosphere, and the resulting oils had all the expected characteristics as can be seen from the following data. The data below corresponds to the average values obtained for the different tests performed:
Acidity 0.02%
~umidity ' . 05%
Impurities C 0.05%
Oxyacids ~ 0.05%
Phosphorus Negligible Unsaponifiables 0.65%
Gardner Color 3 - 4 ....... . . . . .

- 17 - 2~

Fatty Acids Content AcidCrude Purified Neutralized Decolored 14:0 6.9 7.1 7.4 6.9 lfi:0 17.4 17.8 18.0 17.0 16:1 ~.~ 10.1 9.6 9.6 1~:0 2.6 2.6 2.7 2.6 18:1 11.0 11.7 11.8 11.4 20:4 1.2 1.1 1.0 0.9 20:5 20.8 21.9 21.8 21.3 22:5 1.7 0.6 2.0 3.0 22:6 6.3 6.0 7.9 7.9 PUFA 30.0 29.6 32.7 33.1 None of the cases presented trans. isomerization.
The influence of the steam flow vs nitrogen gas flow in the different phases of the process was determined by studying the chromatograms corresponding to the fatty acid composition of the obtained oils and the presence of trans.
isomers, the formation of which we had tried to avoid. From the data shown in the above table, it can be seen that when a nitrogen gas atmosphere was used, the fatty acids did not undergo any transformation - either oxidizing nor polymeriz-ing - and the important acids were adequately protected.
This is contrary to what normally occurs during the conventional refining process. The formation of peroxides was thus avoided in all the phases.
-Deodorization:
The oil, once decolored, had a very good appearance but it still had the characteristic smell of fish oils. To solve this problem, the oil was subjected to a gentle deodorization. Given the tendency of these oils to polymerize at high temperatures, and since this tendency is more marked in the most important fatty acids (eicosapen-tanoic and docosahexanoic), the conditions of time and temperature were studied with more attention. Temperature steps between 60QC and llOQC were evaluated (because higher temperatures would produce polymerization), and time .... . ..... ....... . ..................... ....... ............. ... .... . . . . . .

- 18 - 20~

intervals between 60 and 240 minutes. The control of the tests was based on the iodine numbers and the or~anoleptic characteristics. From the results thus obtained, the conclusion was reached that it was possible to achieve acceptable products, without eliminatin~ the characteristic odor and taste of fish oils, by using temperatures between 80QC and 90QC and a time period of 2 hours. Polymers would appear if the conditions were more extreme.

2,880 Kg of "Lampante" olive oil, with 4.5Q acidity, were refined; once neutralized and decolored, a total of sixteen batches were prepared of 160 Kg each. Eight batches were treated with steam in the industrial deodorizer of the Instituto de la Grasa de Sevilla (Seville Fat Institute) pilot plant; the other eight batches were treated with a similar deodorizing device with provisions to accept the in~ection of nitrogen gas. The same following conditions were used in all cases: Pressure: 3 mbars; Time: 3 hours;
and Flowrate: 0.3 m3/hour.
The tests were as follows:
NQ of Tests Steam Nitrogen 1 test 180QC 180QC
3 tests 200QC 200QC
3 tests 220QC 220QC
1 test 240QC 240QC
In all the tests, except the one at 180QC, the refined oils had the characteristic almondlike taste of refined olive oils of quite good quality, both for the steam and the nitrogen tests. In the tests at 180QC it was noted for both cases (steam and nitrogen) that not enough deodorization time had been allowed. Another test was per-formed at this temperature but with a time period of 4 hours. This test produced a good quality refined oil.

Using the same conditions as for the previous example, a refinable olive oil of poor quality was 2~ ~ ~9~

deodorized. In thi,s case, the refined oil thus obtained had a taste slighty reminiscent of its origin of piled fermented olive, whereby the process time was increased to 4 hours and the results were very good.

Using the same conditions as for Exa~ple 5 and degummed, neutralized and decolored sunflower oils, two tests were performed at 180QC and 210C. Excellent results were obtained, with both steam and nitrogen.
Another series of tests was performed with sunflower oils, but only having been degummed and neutralized - not decolored. A deodorized oil of the same quality as the others was obtained. It was noted that it had lost its color.
The same results were obtained with soy bean oil except that, when the oil was deodorized without prior decoloration using a darker oil, the result was a deodorized oil with very good taste, color and odor.

The same equipment used for the previous tests was used for the physical refining tests, but in this case the vacuum was obtained with the CRYO-COND system of the firm Busch Ibérica. The ejector system was not util'ized in any case.
Four olive oils were used in these tests, wlth crudes having the characteristics shown in the following Table VI.
All the oils were purified and decolored before being subjected to the deodorization-neutralization process. The working conditions were the following:
Pressure: 2 mbars Temperature: 260QC
Time: 5 hours N2 Flowrate: 0.3 m3thour TABLE VI
PHYSICAL REFINING OF OLIVE OIL

Parameter Castilblanco de los A. Arcos de la Frontera Crude Steam N2 Crude Steam N2 5 Triglycerides Dimers - 0.6 0.4 - 0.2 0.2 Triglycerides Oxidized0.8 0.7 0.2 1.0 1.3 0.2 Diglycerides 4.8 4.2 4.2 5.3 4.5 4.1 10 Free Fatty Acids 4.3 0.2 0.15 9.85 0.2 0.;1 Peroxide Value 15.5 0.4 0.0 15.0 2.1 0.0 Pickled olives 1 Pickled ol.ives 2 15 Crude Steam N2 Crude Steam N2 Triglycerides Dimers 0.3 1.4 0.6 0.1 3.4 1.3 Triglycerides Oxidized 1.0 0.6 0.5 1.5 1.5 0.4 20 Diglycerides 1.7 0.9 0.8 3.2 3.2 2.7 Free Fatty Acids 6.8 0.12 0.08 6.G 0.08 0.0 Peroxide Value 12.5 0.8 0.0 13.5 0.6 0.0 .... ..... . ... ... .... . . . .. .. .. . .

- 21 - 2~9~1~

The results were positive and the characteristics of the refined oils, both when steam and nitrogen were used in the process, are shown in the previous Table. From the indicated values, it can be seen that the altered triglycerides, peroxide value, etc., were always lower when nitrogen was used instead of direc steam. In the same manner, the proportion of diglycerides was less because no steam hydrolysis occurred.
The physical refining of sunflower oil was performed using an oil that had been degummed and decolored before undergoing the neutralizing deodorization process. The conditions of the tests were the following: Vacuum: 3 Torr;
Temperature: 230C; and Time: 3 hours. The characteristics of the resulting oil are shown in Table VII.
TABLE VII
P~YSICAL REFINING OF SUNFLOWER OIL
Parameters Crude Refined Steam Nitrogen Dimers 1.1 0.2 Triglycerides Oxidized 6.6 3.0 1.1 Diglycerides 1.3 0.8 0.4 Free Fatty Acids 1.1 0.1 0.08 Peroxide Value99.5 0.14 0.0

Claims (9)

1.- A process for deodorizing oils and fats characterized in thatthe oil or fat to be deodorized is subjected to the action of a current of inert gas entraining the substances producing unpleasant odors and taste in the oil or fat, the process being conducted under vacuum conditions ranging from 1 to 8 mbars and temperatures between 60?C and 270?C.
2.- The process for deodorizing oils and fats, of Claim 1, characterized in that the oil or fat to be deodorized is subjected to the action of a current of nitrogen gas that entrains the substances producing unpleasant odors and taste in the oil or fat, the process being conducted under vacuum conditions ranging from 1 to 8 mbars and temperatures between 60?C and 270?C.
3.- The process of Claims 1 or 2, characterized in that the oil or fat to be deodorized has undergone a prior degumming process.
4.- The process of any one of Claims 1 to 3, characterized in that the oil or fat to be deodorized has undergone a prior decoloration process.
5.- The process of any one of Claims 1 to 4, characterized in that the oil or fat to be deodorized has undergone a prior neutralization process.
6.- The process of any one of Claims 1 to 5, characterized in that the oil or fat to be deodorized has undergone a prior deaeration process.
7.- The process of any one of Claims 1 to 6, characterized in that the flow of the nitrogen gas current is between a range from 0.8 to 3 Nm3 per hour per tonne of oil or fat.
8.- The process of any one of Claims 2 to 7, characterized in that said nitrogen gas current is subjected to dispersion.
9.- The process of any one of Claims 2 to 8, characterized in that the nitrogen gas circulates in a direction contrary to the direction of movement of the oil or fat.
CA002019916A 1989-06-29 1990-06-27 Process for deodorizing oils and fats Abandoned CA2019916A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ES8902284 1989-06-29
ES8902284A ES2013206A6 (en) 1989-06-29 1989-06-29 A process for deodorizing oils and fats.

Publications (1)

Publication Number Publication Date
CA2019916A1 true CA2019916A1 (en) 1990-12-29

Family

ID=8262802

Family Applications (1)

Application Number Title Priority Date Filing Date
CA002019916A Abandoned CA2019916A1 (en) 1989-06-29 1990-06-27 Process for deodorizing oils and fats

Country Status (8)

Country Link
EP (1) EP0405601A3 (en)
JP (1) JPH03263498A (en)
BR (1) BR9003055A (en)
CA (1) CA2019916A1 (en)
ES (1) ES2013206A6 (en)
IE (1) IE902363A1 (en)
IT (1) IT1241140B (en)
PT (1) PT94056A (en)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5241092A (en) * 1991-05-13 1993-08-31 Praxair Technology, Inc. Deodorizing edible oil and/or fat with non-condensible inert gas and recovering a high quality fatty acid distillate
US5315020A (en) * 1992-07-29 1994-05-24 Praxair Technology, Inc. Method of recovering waste heat from edible oil deodorizer and improving product stability
AU672858B2 (en) * 1992-12-03 1996-10-17 Unilever Plc Process for the refining of edible oils
ES2101500T3 (en) * 1993-01-18 1997-07-01 Unilever Nv MODIFICATION OF THE TASTE OF EDIBLE OILS.
CN1046192C (en) * 1994-03-30 1999-11-10 赵友苓 Method for prodn. of deodorized fish oil microcapsule
GR980100365A (en) * 1998-10-08 2000-06-30 Equipment complex for the production, preservation and maintenance of olive oil
US6476244B2 (en) 2000-02-23 2002-11-05 South Dakota Soybean Processors Process for preparing blown vegetable oil
EP1417288B1 (en) 2001-07-23 2018-08-29 Cargill, Incorporated Method and apparatus for processing vegetable oils
KR100665907B1 (en) 2005-02-28 2007-01-09 부경대학교 산학협력단 Removal process of off-flavors from fish oil
ES2332977B1 (en) 2008-07-22 2011-02-09 Consejo Superior De Investigaciones Cientificas (Csic) EDIBLE OLIVE OLIVE OIL CONCENTRATED IN TRITERPENIC ACIDS, PHYSICAL REFINING PROCEDURE USED FOR OBTAINING AND RECOVERY OF FUNCTIONAL COMPONENTS PRESENT IN THE CRUDE OIL.
RU2012106130A (en) * 2009-07-21 2013-08-27 Нестек С.А. DEODORIZED FOOD OIL OR FAT WITH LOW LEVELS RELATED TO MCPD AND METHOD FOR PRODUCING THEREOF USING AN INERT GAS

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR840499A (en) * 1937-09-07 1939-04-26 Chemische Fab Dr Kurt Albert Method and device for removing acidity from products such as cooked oils, balms and resins
US2508919A (en) * 1946-04-20 1950-05-23 Gen Mills Inc Soybean oil
NL173768C (en) * 1971-06-01 1984-03-01 Stork Amsterdam METHOD AND APPARATUS FOR VACUUM TREATING LIQUIDS WITH A GASEOUS STRIP MEDIUM
US4378317A (en) * 1980-01-10 1983-03-29 The Procter & Gamble Company Process to maintain bland taste in energy efficient oil deodorization systems
DE3839017A1 (en) * 1988-11-18 1990-05-23 Henkel Kgaa Process for separating off by distillation undesirable constituents of natural fats/oils and derivatives thereof

Also Published As

Publication number Publication date
EP0405601A2 (en) 1991-01-02
IT9020317A1 (en) 1991-11-16
JPH03263498A (en) 1991-11-22
IT9020317A0 (en) 1990-05-16
IT1241140B (en) 1993-12-29
EP0405601A3 (en) 1991-08-07
ES2013206A6 (en) 1990-04-16
BR9003055A (en) 1991-08-27
IE902363A1 (en) 1991-06-19
IE902363L (en) 1990-12-29
PT94056A (en) 1991-02-08

Similar Documents

Publication Publication Date Title
Sherwin Oxidation and antioxidants in fat and oil processing
US5091116A (en) Methods for treatment of edible oils
Wang et al. Refining high-free fatty acid wheat germ oil
US5696278A (en) Degumming of crude glyceride oils not exposed to prior enzymatic activity
Sleeter Effects of processing on quality of soybean oil
JP5955119B2 (en) Method for producing edible fats and oils
Smouse A review of soybean oil reversion flavor
EP1178103A1 (en) Purifying crude pufa oils
AU2001282054A1 (en) Purifying crude pufa oils
CN111349515B (en) Zero-reflection green precise moderate-processing grease composition and preparation method thereof
WO2010080019A2 (en) Refining of edible oil
CN102006780B (en) Process for refining a triglyceride oil
CA2019916A1 (en) Process for deodorizing oils and fats
EP0672096A1 (en) Process for the refining of edible oils.
JP2009102491A (en) Method for manufacturing alkali refined oil or purified oil obtained by the same
KR20090006293A (en) A process for refining fish oil and a process to deposit the refined fish oil
JP2014000012A (en) Manufacturing method of edible oil
US2308848A (en) Treatment of fats and oils
WO2019165065A1 (en) Edible oil refining
US2353229A (en) Hydrogenation of oil
Swoboda Chemistry of refining
List et al. Hydrogenation of soybean oil with copper-chromium catalyst: Preliminary plant-scale observations
US2349381A (en) Process of treating soybean oil
US1890585A (en) Method of stabilizing fats and oils
AU2022419565A1 (en) Process for removing impurities from vegetable oil

Legal Events

Date Code Title Description
EEER Examination request
FZDE Discontinued
FZDE Discontinued

Effective date: 20010227