CA1163228A - Method for refining oils and fats - Google Patents
Method for refining oils and fatsInfo
- Publication number
- CA1163228A CA1163228A CA000354550A CA354550A CA1163228A CA 1163228 A CA1163228 A CA 1163228A CA 000354550 A CA000354550 A CA 000354550A CA 354550 A CA354550 A CA 354550A CA 1163228 A CA1163228 A CA 1163228A
- Authority
- CA
- Canada
- Prior art keywords
- oil
- fat
- acid
- refining
- fats
- 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.)
- Expired
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Classifications
-
- 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
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
Abstract
ABSTRACT OF THE DISCLOSURE
The disclosure describes a method of refining an animal or vegetable oil or fat which is economical and which eliminates the washing step, thus avoiding the production of waste water and the accompanying environmental pollution. The method involves the following steps.
(a) mixing said oil or fat with an aqueous solution of an alkaline substance;
(b) separating the insoluble matter in the oil or fat from the resulting mixture;
(c) directly admixing the deacidified separated oil or fat from step (b) with an aqueous solution of an acid;
(d) treating the resulting admixture with an adsor-bent to adsorb coloring matter, impurities and salts formed during step (c);
(e) separating said adsorbent from said oil or fat, and (f) treating said oil or fat after step (e) by steam distillation.
The disclosure describes a method of refining an animal or vegetable oil or fat which is economical and which eliminates the washing step, thus avoiding the production of waste water and the accompanying environmental pollution. The method involves the following steps.
(a) mixing said oil or fat with an aqueous solution of an alkaline substance;
(b) separating the insoluble matter in the oil or fat from the resulting mixture;
(c) directly admixing the deacidified separated oil or fat from step (b) with an aqueous solution of an acid;
(d) treating the resulting admixture with an adsor-bent to adsorb coloring matter, impurities and salts formed during step (c);
(e) separating said adsorbent from said oil or fat, and (f) treating said oil or fat after step (e) by steam distillation.
Description
I ~ fi3~2~
This invention relates to methods for refining oils and fats.
Various methods have been developed for refining oils and fats. The alkali refining method is widely used and an im-portant method of refining oils and fats, since it has many advantages over the other methods. An important problem which recently becomes noticeable from the point of view of environ-mental pollution and saving materials is that the alkali refin-ing method produces a large amount of waste water.
In the conventional alkali refining method, crude or degummed oils and fats of animal and vegetable origin are con-tacted wi-th an aqueous alkaline solution. The free fatty acid in the oils and fats reacts with the alkaline solution and the oils and fats are deacidified to form soapstock consisting mainly of a fatty acid soap which is separated by centrifugation as illustrated in the flow sheet A.
After separating the soap from the oil the deacidified oil is then mixed and stirred with a large amount of hot water to achieve a sufficient contact of the oil with hot water.
The soap which is still present in the oil in an amount of about 100 - 1,000 ppm depending on the type and capacity of the centrifuge is shifted to the li~uid phase and is again centrifuged. To carry out this washing process only once is not enough, thus the operation must be repeated more than twice in order to remove soap exhaustively from the oil.
i il 6~28 FLOW SHEET A
Crude or degummed oils and fats o animal and vegetable origin ¦ ~ an aqueous alkaline ¦ solution deacidification centrifugation ¦ ~ soapstock ¦~ hot water mixing, stirring centrlfugation waste water ~
~ ~ hot water treatment for mixing, stirring step of washing discharge , ~ I ~ ~ith water centrifugation ~aste water ~ ¦
¦~ adsorbent decolorization - deodorization refined oil ~S - 2 -~ ~ fi~2~
Therefore a very large amount of waste water is produced in the washing process.
Since this waste water contains a considerable amount of impurities including soap and entrained oils, it is not per-mitted to discharge the waste water without treatment by the pressure floatation method or by the activated sludge process.
Therefore a large inves-tment is required for the equipment to treat the waste water.
A centrifuge or mixing and stirring apparatus requir-ed in the washing process is very expensive and the number of these apparatuses required depends on the number of times the washing treatment is carried out. Washing twice requires two sets of these apparatuses. Even the washing process which is used only in the oil refineries requires a large investment and it is a large economical burden to the processors. It is undesirable to use such a large amount of water from the point of view of saving materials and this is the first item to be reduced. Thus the conventional alkali refining method is be-coming gradually more disadvantageous.
The object of the present invention is to provide an economical method for the refining of oils and fats.
Another object of the invention is to provide a method for the refining of oils and fats which eliminates the washing step, thus avoiding the production of waste water and the accom-panyin~ environmental pollution.
A further object of the invention is to provide a method for refining oils and fats which eliminates the invest-ment for the apparatus required to wash the neutralized oils and fats with water and to treat the waste water.
Briefly, these objects and other objects of the inven-tion can be attained by providing a method of refining oils and fats wherein washing process is eliminated after the separation J I ~32~
of soapstock from the neutralized oils and fats.
This invention relates to a method of refining animal and vegetable oils and fats, and more particularly to a method of refining crude oils and fats of animal and vegetable origin or oils and fats which have been subjected to a conventional pre-treatment. Tne invention is characterized by deacidifying said oils and fats with an aqueous solution of alkaline compounds, separating the soapstock thus formed from the deacidified oils and fats by centrifuge, admixing said deacidified oils and fats directly with an aqueous solution of acids without washing the deacidified oils and fats with water after the separation of soapstock, drying if required, the resulting mixture, treating the mixture with an adsorbent and subjecting the oils and fats to a steam distillation treatment.
The inventors have studied oil refining methods which eliminate the washing steps after deacidification in the con-ventional alkali refining method, thus avoidin~ the production of waste water and realizing the present invention.
~ ~ 6~28 FLOW SHEET B
Crude or degummed oils and fats of animal and vegetable origin an aqueous alkaline solution deacidification I
centrifugation soapstock ¦~ an a~ueous acid solution 1 mixing, stirring step of treatment with acids <- adsorbent decolorization deodorization I
refined oil As lllustrated in Flow Sheet B, the method of refining animal and vegetable oils and fats according to the present in-vention omits the washing step which is used in the conventional alkali refining method, and replaces the washing step with a simple step of acid treatment. Therefore the refining process itself is simplified significantly. Since the centrifugal separation of oils from washing water which is carried out in the conventional washing step is eliminated in the refining method of the present invention, an expensive centrifugal mach-ine is not needed and no waste water is produced.
The method of refining oils and fats according to the invention comprises the following steps:
J ~ 6~2~
~1) treating the oils and fats with an alkaline solution (deacidification),
This invention relates to methods for refining oils and fats.
Various methods have been developed for refining oils and fats. The alkali refining method is widely used and an im-portant method of refining oils and fats, since it has many advantages over the other methods. An important problem which recently becomes noticeable from the point of view of environ-mental pollution and saving materials is that the alkali refin-ing method produces a large amount of waste water.
In the conventional alkali refining method, crude or degummed oils and fats of animal and vegetable origin are con-tacted wi-th an aqueous alkaline solution. The free fatty acid in the oils and fats reacts with the alkaline solution and the oils and fats are deacidified to form soapstock consisting mainly of a fatty acid soap which is separated by centrifugation as illustrated in the flow sheet A.
After separating the soap from the oil the deacidified oil is then mixed and stirred with a large amount of hot water to achieve a sufficient contact of the oil with hot water.
The soap which is still present in the oil in an amount of about 100 - 1,000 ppm depending on the type and capacity of the centrifuge is shifted to the li~uid phase and is again centrifuged. To carry out this washing process only once is not enough, thus the operation must be repeated more than twice in order to remove soap exhaustively from the oil.
i il 6~28 FLOW SHEET A
Crude or degummed oils and fats o animal and vegetable origin ¦ ~ an aqueous alkaline ¦ solution deacidification centrifugation ¦ ~ soapstock ¦~ hot water mixing, stirring centrlfugation waste water ~
~ ~ hot water treatment for mixing, stirring step of washing discharge , ~ I ~ ~ith water centrifugation ~aste water ~ ¦
¦~ adsorbent decolorization - deodorization refined oil ~S - 2 -~ ~ fi~2~
Therefore a very large amount of waste water is produced in the washing process.
Since this waste water contains a considerable amount of impurities including soap and entrained oils, it is not per-mitted to discharge the waste water without treatment by the pressure floatation method or by the activated sludge process.
Therefore a large inves-tment is required for the equipment to treat the waste water.
A centrifuge or mixing and stirring apparatus requir-ed in the washing process is very expensive and the number of these apparatuses required depends on the number of times the washing treatment is carried out. Washing twice requires two sets of these apparatuses. Even the washing process which is used only in the oil refineries requires a large investment and it is a large economical burden to the processors. It is undesirable to use such a large amount of water from the point of view of saving materials and this is the first item to be reduced. Thus the conventional alkali refining method is be-coming gradually more disadvantageous.
The object of the present invention is to provide an economical method for the refining of oils and fats.
Another object of the invention is to provide a method for the refining of oils and fats which eliminates the washing step, thus avoiding the production of waste water and the accom-panyin~ environmental pollution.
A further object of the invention is to provide a method for refining oils and fats which eliminates the invest-ment for the apparatus required to wash the neutralized oils and fats with water and to treat the waste water.
Briefly, these objects and other objects of the inven-tion can be attained by providing a method of refining oils and fats wherein washing process is eliminated after the separation J I ~32~
of soapstock from the neutralized oils and fats.
This invention relates to a method of refining animal and vegetable oils and fats, and more particularly to a method of refining crude oils and fats of animal and vegetable origin or oils and fats which have been subjected to a conventional pre-treatment. Tne invention is characterized by deacidifying said oils and fats with an aqueous solution of alkaline compounds, separating the soapstock thus formed from the deacidified oils and fats by centrifuge, admixing said deacidified oils and fats directly with an aqueous solution of acids without washing the deacidified oils and fats with water after the separation of soapstock, drying if required, the resulting mixture, treating the mixture with an adsorbent and subjecting the oils and fats to a steam distillation treatment.
The inventors have studied oil refining methods which eliminate the washing steps after deacidification in the con-ventional alkali refining method, thus avoidin~ the production of waste water and realizing the present invention.
~ ~ 6~28 FLOW SHEET B
Crude or degummed oils and fats of animal and vegetable origin an aqueous alkaline solution deacidification I
centrifugation soapstock ¦~ an a~ueous acid solution 1 mixing, stirring step of treatment with acids <- adsorbent decolorization deodorization I
refined oil As lllustrated in Flow Sheet B, the method of refining animal and vegetable oils and fats according to the present in-vention omits the washing step which is used in the conventional alkali refining method, and replaces the washing step with a simple step of acid treatment. Therefore the refining process itself is simplified significantly. Since the centrifugal separation of oils from washing water which is carried out in the conventional washing step is eliminated in the refining method of the present invention, an expensive centrifugal mach-ine is not needed and no waste water is produced.
The method of refining oils and fats according to the invention comprises the following steps:
J ~ 6~2~
~1) treating the oils and fats with an alkaline solution (deacidification),
(2) separating the insoluble matter,
(3) treating the oils and fats with an aqueous ~olution of acids, (~) treating the oils and fats with an adsorbent (decolorization), (5) treating the oils and fats by steam distilla-tion (deodorization More specifically, according to the invention, there is provided a method of refining an animal or vegetable oil or fat which comprises:
(a) mixing said oil or fat with an aqueous solution of an alkaline substance, (b) separating the insoluble matter in the oil or fat from the resulting mixture' (c) directly admixing the deacidified separated oil or fat from step (b) with an aqueous solution of an acid, (d) treating the resulting admixture with an adsor-bent to adsorh coloring matter, impurities and salts formed during step (c), (e) separating said adsorbent from said oil or fat and (f) treating said oil or fat after step (e) by steam distillation.
The particulars of these steps are described below.
1. Alkali treatment.
This step is a conventional deacidification step which is self-explanatory. The oils and fats of animal and vegetable origin are, if required, subjected to a pre-treatment such as physical removal of impurities from the oil by filtration or sedimen-tation, degumming with water, acids, alkalis and other che~micals. Gum conditioning with acids such as phosphoric acid I ~ ~3~8 may also be carried out in the conventional manner. This pre-treatment step is an optional one.
The alkali treatment is carried out by contacting oils and fats with an aqueous alkaline solution to neutralize the free fatty acid, to saponify, hydrate and coagulate the gummy substance and to decolorize the coloring matter in the oils and fats. ~lkali compounds such as caustic soda and soda ash are usually added to the oil. Soaps and coagulated gurnmy sub-stancesare suspended in the mixture as insoluble matter.
2. Separation of insoluble matter.
This step is a commonly used one in the conventional allcali refining method. The insoluble matter in the oil formed in the preceding step of alkali treatment is removed from the oil in the form of soapstock by means of centrifugation. This soapstock consists mainly of soap and contains entrained neutral oil and impurities such as gummy substance.
3. Treatment with an aqueous solution of acids.
In the usual alkali refining method, after step (2), the oil (hereinafter called as deacidified separated oil) is washed with a large amount of water. It is the characteristic of the present invention that step (3) be carried out directly without washing the deacidified separated oil with water.
The deacidified separated oil usually contains soap as described before in an amount of 100 to 1,000 ppm and a small amount of impurities such as mucilages. The deacidified sep-arated oil is treated with an aqueous solution of acids in this step (3) to hydrolyze the soap contained in the oil to form free fatty acid and salts. Impurities such as mucilages con-tained in the oil in a small amount are coagulated simultan-eously in the oil as the insoluble matter. Thus free fattyacid so formed dissolves in the oil and the impurities and salts remain in the oil as insoluble matter.
~ ~ 63228 The acids used in this step are organic or inorganic acids such as hydrochloric acid, sulfuric acid, phosphoric acid, oxalic acid, acetic acid, acetic anhydride, citric acid and tartaric acid or the combination of more than two kinds of these acids. Phosphoric acid is the most suitable consider-ing the influence on the material of the equipment and from an economical point of view. These acids are added to the de-acidified separated oil at a suitable concentration and the mixture is mixed or stirred at a temperature from room tempera-ture to 100C for a period of time varying from several secondsto several hours. If phosphoric acid is used, the concentration of the aqueous solution of acid is preferably about 75 - 85%, and if citric acid is used~ the concentration is preferably about 73-80%. Lower concentration of acids can also be used in this step but the con~entration of the acid solution is possibly as high as possible in view of subsequent step 4.
The wide interval of contact time is due to the differences of contact efficiencies among the mixers which are used. In short, it is necessary to establish an even and intimate contact between acids and soaps or mucilages in order to make sure that the reaction between them is rapid and sufficient.
The e~uipment or apparatus ~sed in the alkali refining method wherein oils are contacted with an alkali or water can also be used in this step. The contact between acids and soaps or mucilages can be accelerated by using a homogenizer.
The amount of an aqueous solution of acid to be added is calculated mainly from the amount of acid required to de-compose the soap contained in the deacidified separated oil and is established considering the amount of impurities such as mucilages in the oil. When the soap content in the oil is 1000 ppm or 100 ppm, the amount of 85% phosphoric acid re-quired is preferably about 380 ppm or 38.0 ppm and if 10~/o f - ~1 832?J8 acetic acid is used, preferably about 197 ppm or 19.7 ppm is required to decompose the soap. The amount of impurities should also be considered.
After the treatment involved in this step, if required, the oil is dried through a suitable drier to remove excess water from the oil before the treatment of the following step.
(a) mixing said oil or fat with an aqueous solution of an alkaline substance, (b) separating the insoluble matter in the oil or fat from the resulting mixture' (c) directly admixing the deacidified separated oil or fat from step (b) with an aqueous solution of an acid, (d) treating the resulting admixture with an adsor-bent to adsorh coloring matter, impurities and salts formed during step (c), (e) separating said adsorbent from said oil or fat and (f) treating said oil or fat after step (e) by steam distillation.
The particulars of these steps are described below.
1. Alkali treatment.
This step is a conventional deacidification step which is self-explanatory. The oils and fats of animal and vegetable origin are, if required, subjected to a pre-treatment such as physical removal of impurities from the oil by filtration or sedimen-tation, degumming with water, acids, alkalis and other che~micals. Gum conditioning with acids such as phosphoric acid I ~ ~3~8 may also be carried out in the conventional manner. This pre-treatment step is an optional one.
The alkali treatment is carried out by contacting oils and fats with an aqueous alkaline solution to neutralize the free fatty acid, to saponify, hydrate and coagulate the gummy substance and to decolorize the coloring matter in the oils and fats. ~lkali compounds such as caustic soda and soda ash are usually added to the oil. Soaps and coagulated gurnmy sub-stancesare suspended in the mixture as insoluble matter.
2. Separation of insoluble matter.
This step is a commonly used one in the conventional allcali refining method. The insoluble matter in the oil formed in the preceding step of alkali treatment is removed from the oil in the form of soapstock by means of centrifugation. This soapstock consists mainly of soap and contains entrained neutral oil and impurities such as gummy substance.
3. Treatment with an aqueous solution of acids.
In the usual alkali refining method, after step (2), the oil (hereinafter called as deacidified separated oil) is washed with a large amount of water. It is the characteristic of the present invention that step (3) be carried out directly without washing the deacidified separated oil with water.
The deacidified separated oil usually contains soap as described before in an amount of 100 to 1,000 ppm and a small amount of impurities such as mucilages. The deacidified sep-arated oil is treated with an aqueous solution of acids in this step (3) to hydrolyze the soap contained in the oil to form free fatty acid and salts. Impurities such as mucilages con-tained in the oil in a small amount are coagulated simultan-eously in the oil as the insoluble matter. Thus free fattyacid so formed dissolves in the oil and the impurities and salts remain in the oil as insoluble matter.
~ ~ 63228 The acids used in this step are organic or inorganic acids such as hydrochloric acid, sulfuric acid, phosphoric acid, oxalic acid, acetic acid, acetic anhydride, citric acid and tartaric acid or the combination of more than two kinds of these acids. Phosphoric acid is the most suitable consider-ing the influence on the material of the equipment and from an economical point of view. These acids are added to the de-acidified separated oil at a suitable concentration and the mixture is mixed or stirred at a temperature from room tempera-ture to 100C for a period of time varying from several secondsto several hours. If phosphoric acid is used, the concentration of the aqueous solution of acid is preferably about 75 - 85%, and if citric acid is used~ the concentration is preferably about 73-80%. Lower concentration of acids can also be used in this step but the con~entration of the acid solution is possibly as high as possible in view of subsequent step 4.
The wide interval of contact time is due to the differences of contact efficiencies among the mixers which are used. In short, it is necessary to establish an even and intimate contact between acids and soaps or mucilages in order to make sure that the reaction between them is rapid and sufficient.
The e~uipment or apparatus ~sed in the alkali refining method wherein oils are contacted with an alkali or water can also be used in this step. The contact between acids and soaps or mucilages can be accelerated by using a homogenizer.
The amount of an aqueous solution of acid to be added is calculated mainly from the amount of acid required to de-compose the soap contained in the deacidified separated oil and is established considering the amount of impurities such as mucilages in the oil. When the soap content in the oil is 1000 ppm or 100 ppm, the amount of 85% phosphoric acid re-quired is preferably about 380 ppm or 38.0 ppm and if 10~/o f - ~1 832?J8 acetic acid is used, preferably about 197 ppm or 19.7 ppm is required to decompose the soap. The amount of impurities should also be considered.
After the treatment involved in this step, if required, the oil is dried through a suitable drier to remove excess water from the oil before the treatment of the following step.
4. Treatment with adsorbent (decolorization).
This step is a conventional decolorization process.
The oil which is treated with acids in step (3) or the oil which is dried after the treatment of step (3) is treated with an ad-sorbent such as activated clay or activated carbon. The impuri-- 8a -,1 ~ 1 63228 ties which remain in the oil such as mucilages, salts formed by the reaction of acids with soaps and the coloring matter in the oil are substantially entirely adsorbed on the adsorbent and are removed from the oil. The manner of treatment, the condi-tions and the apparatus used for the conventional decoloriza-tion step can be applied to this step.
This step is a conventional decolorization process.
The oil which is treated with acids in step (3) or the oil which is dried after the treatment of step (3) is treated with an ad-sorbent such as activated clay or activated carbon. The impuri-- 8a -,1 ~ 1 63228 ties which remain in the oil such as mucilages, salts formed by the reaction of acids with soaps and the coloring matter in the oil are substantially entirely adsorbed on the adsorbent and are removed from the oil. The manner of treatment, the condi-tions and the apparatus used for the conventional decoloriza-tion step can be applied to this step.
5. Treatment by steam distillation (deodorization).
This step is also a conventional deodorization pro-cess. The fatty acid which became free by the acid treatment in step (3) is distilled entirely away from the oil accompanied by the odorous matter. The coloring matter in the oil is decom-posed simultaneously due to the heat and the oil is changed to lightly colored. Since the impurities such as mucilages have already been removed entirely from the oil, the oil does not color due to the presence of impurities. The conventional steam distillation method, apparatus and the conventional conditions can be applied to this step.
The above constitutes an embodiment of -the invention.
The effects and advantages of the present invention are that the washing step of the conventional al]cali refining method is eliminated and consequently expensive equipment and apparatus such as centrifuge are not required in this procedure. The im-purities and soaps which are removed from the oil by the conven-tional washing process are treated with acid in the deacidified separated oil and are removed entirely from the oil in the fol-lowing decolorization and deodorization steps~
In order to treat the oil with an aqueous solution of acids according to the present invention, only one mixing apparatus is required in a series of oil refining apparatus.
Two sets of apparatus such as centrifuge and mixer in a series of conventional oil refining apparatus is required for washing twice in the washing step. This means that the method of refin-ing oils and fats according to the invention is far superior to g _ ~ :~ 6:~2~
the conventional alkali refining method from an economical point of view.
The reduction of cost for the apparatus was estimated to be more than 100,000,000 yen in 1979, since the apparatus and the equipment for the washing step such as the centrifuge and the mixer became useless. This amount was calculated for an oil refinery having an average capacity in Japan, such as 200 tons per day. Moreover the running cost such as the cost for operation and maintenance of the apparatus and the cost for fixed assets such as space and building for these appara-tus are not necessary. Therefore, the method of the invention has an inestimable economical superiority over the usual methods.
The method of the invention is not accompanied by the generation of waste water and is a clean method which is effect-ive in protecting the environment from pollution. The method of the invention can reduce the comsumption of water, heat energy for heating washing water and the ener~y for the operation of the apparatus during the washing step. This method is highly suitable for the oil refining industry. The quality of the re-fined oils and fats produced by the method of the invention issubstantially the same as that of the oil produced by the con-ventional alkali refinin~ method and the yield of oil is superior to that produced by the conventional method.
If the washing process of the conventional alkali re-fining method is omitted and the amount of adsorbent is increas-ed to remove the soaps, impurities and coloring matter still present in the oil without treating the deacidified oil with an acid, the fact of omitting the washing step is still recommended in this method as in the method of the present invention. How-ever, this method requires a very large amount of adsorbentcompared with the method of the inven-tion. Therefore, a large amount of -the oil is lost with -the adsorbent and the disadvantage ~J ~ ~322~
caused by the increase of the cost of the adsorbent and by the decrease of the yield of the oil cancels the advantage of omitt-ing -the washing step. This method is not an economically signi-ficant method which is, as a matter of course, far inferior to the method of the invention.
The method of the present invention can be applied favourably to the refining of all kinds of vegetable and animal oils and fats such as soybean oil, rape seed oil, rice oil, corn oil, cotton seed oil, sunflower oil, safflower oil, sesame oil, peanut oil, palm oil, coconut oil, linseed oil, lard, beef tallow, mutton tallow, fish oil and the oils and fats of marine animals.
IIaving generally described this invention, a further understanding can be obtained by reference to certain specific examples which are provided herein for purposes of illustration only and are not intended to be limiting unless otherwise speci-fied.
Soyb~an oil was treated by the conventional al]cali refining method. A deacidified separated oil was obtained by separating soapstock from the oil using a centrifuge. The oil was divided into four samples and was used for the following tests. The characteristics of the deacidified separated oil is shown in Table 1.
Test 1 (Method of the present invention (1~) 40 ppm by weight of 85% phosphoric acid was added to the deacidified separated oil and the acid treatment was carried out by stirring the mixture for 5 minutes at a temperature of 80C. Then 0.3% by weight of activated clay was added to the oil treated with acid, and the oil was decolorized under reduced pressure at 105C for 15 minutes and the activated clay was separated from the mixture. The decolorized oil thus obtained ~ :~ 83228 was subjected to deodorization under vacuum at 250C for 45 minutes to give the refined oil.
Test 2 (Method accordinq to the present invention (2)) This test was carried out under the same conditions as in Test 1 except that the amount of phosphoric acid was changed to 80 ppm.
Test_3 (Comparison test (1): conventional method) The deacidified separa-ted oil was washed with 20%
of hot water against the oil and centrifuged. After the wash-ing a double decolorization and deodorization were carried outunder the condition described in Test 1.
Test 4 (Comparison test (2)) The deacidified separated oil was directly decolorized and deodorized under the conditions described in Test 1 without acid treatment and washing.
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rl I :~ 63228 The characteristics of the oil at each step in the tests 1 - 4 are shown in Table 1.
As evident from the results of the tests shown in Table 1, the refining method of the invention (in the tests 1 and 2) can give a refined oil having substantially the same characteristics and quality as that of the oil obtained by the conventional method (test 3) by treating merely the deacid-ified separated oil with phosphoric acid without washing with water. As the conditions of decolorization and deodorization in the method of the invention need not be changed from that of the conventional method, they have no influence on the yield of refined oil. The method of the invention is rather superior to the conventional method in the yield of refined oil, since the latter loses neutral oil entrained in the washing water.
When the deacidified separated oil is directly decolor-ized and deodorized without acid treatment and washing with water (in test 4), soaps and phospholipids are not sufficient-ly removed. Therefore the quality of the refined oil is bad.
It was found in the test that activated clay was re-quired in an amount of 0.8% which was more than twice the clayrequired in the method of the invention, in order to improve the quality of the refined oil in test 4 to the level of the quality of the oil obtained in tests 1 and 2. The increase of the cost for refining the oil by this method compared with that of the method of the invention was about 1000 yen per ton of the oil.
Rape seed oil was treated conventionally with the alkaline solution and the soap stock was centrifuged. 431 ppm by weight of 30% aqueous solution of citric acid was added to a deacidified separated oil having an acid value of 0.06, a soap content of 205 ppm and a phospholipid content of 283 ppm. The ~ I ~322~
mixture was stirred for 30 minutes at a temperature of 50C.
Then 0.6% by weight of activated clay was added to the oil, and the oil was decolorized at 105~C for 15 minutes. The activated clay was separated from the oil. The oil was deodorized under reduced pressure at 250C for 45 minutes to give a refined oil.
It has an acid value of 0.05, a color of 6Yx0.5R and a phos-pholipid content of 5 ppm. The quality of the refined oil was substantially the same as that in a conventionally refined oil.
Corn oil was deacidified by the conventional alkali treatment and the soap stock was centrifuged to obtain the de-acidified separated oil. 604 ppm by weight of a 20% aqueous solution of hydrochloric acid was added to the deacidified separated oil having an acid value of 0.08, a soap content of 990 ppm, and a phospholipid content of 368 ppm. Tne mixture was stirred for 5 minutes at a temperature of 80C. Then 0.6% by weight of activated clay was added to the oil, and the oil was decolorized at 105C for 15 minutes. After the activated clay was separated from the oil, the oil was deodorized under reduc-ed pressure at 260C for 60 minutes to give a refined oil. It has an acid value of 0~07, a color of 6Yx0.6R and a phospholipid content of 13 ppm. The quality of the refined oil was substan-tially the same as that of conventionally refined oil.
. _ Beef tallow was deacidified by the conventional alkali treatment and the soap stock was separated from the tallow to give a deacidified separated tallow having an acid value of 0.06, a soap content of 205 ppm and a phospholipid content of 54 ppm.
45 ppm by weight of 98% acetic acid was added to the tallow and the mixture was agitated at high speed by a Dispermill (made hy Hosokawa Iron Works) for 30 seconds at a temperature of 90C. 2% by weight of activated clay was added to the oil, and * Trademark I ~ 63~2P~
was decolorized under reduced pressure at a temperature of 100C for 30 minutes. The oil was deodorized under vacuum at a temperature of 250C for 90 minutes. The refined oil obtained had an acid value oE 0.02, a color of lYxO.lR and a trace of phospholipid.
The refining method of the invention can eliminate the washing step after deacidification and separation of soap stock from the deacidified oil in the usual alkali refining method as clearly shown in the examples and can give a refined oil with a good yield having the same quality as that of the conventionally refined oil.
Since the economical burden to the processors is very small for the acid treatment of the present invention compared with the advantage of omitting the washing step, the method of the invention is far superior to the conventional method. The refining method of the invention does not produce waste water and saves the consumption of valuable water, thus making an important contribution to the oil refining industry.
This step is also a conventional deodorization pro-cess. The fatty acid which became free by the acid treatment in step (3) is distilled entirely away from the oil accompanied by the odorous matter. The coloring matter in the oil is decom-posed simultaneously due to the heat and the oil is changed to lightly colored. Since the impurities such as mucilages have already been removed entirely from the oil, the oil does not color due to the presence of impurities. The conventional steam distillation method, apparatus and the conventional conditions can be applied to this step.
The above constitutes an embodiment of -the invention.
The effects and advantages of the present invention are that the washing step of the conventional al]cali refining method is eliminated and consequently expensive equipment and apparatus such as centrifuge are not required in this procedure. The im-purities and soaps which are removed from the oil by the conven-tional washing process are treated with acid in the deacidified separated oil and are removed entirely from the oil in the fol-lowing decolorization and deodorization steps~
In order to treat the oil with an aqueous solution of acids according to the present invention, only one mixing apparatus is required in a series of oil refining apparatus.
Two sets of apparatus such as centrifuge and mixer in a series of conventional oil refining apparatus is required for washing twice in the washing step. This means that the method of refin-ing oils and fats according to the invention is far superior to g _ ~ :~ 6:~2~
the conventional alkali refining method from an economical point of view.
The reduction of cost for the apparatus was estimated to be more than 100,000,000 yen in 1979, since the apparatus and the equipment for the washing step such as the centrifuge and the mixer became useless. This amount was calculated for an oil refinery having an average capacity in Japan, such as 200 tons per day. Moreover the running cost such as the cost for operation and maintenance of the apparatus and the cost for fixed assets such as space and building for these appara-tus are not necessary. Therefore, the method of the invention has an inestimable economical superiority over the usual methods.
The method of the invention is not accompanied by the generation of waste water and is a clean method which is effect-ive in protecting the environment from pollution. The method of the invention can reduce the comsumption of water, heat energy for heating washing water and the ener~y for the operation of the apparatus during the washing step. This method is highly suitable for the oil refining industry. The quality of the re-fined oils and fats produced by the method of the invention issubstantially the same as that of the oil produced by the con-ventional alkali refinin~ method and the yield of oil is superior to that produced by the conventional method.
If the washing process of the conventional alkali re-fining method is omitted and the amount of adsorbent is increas-ed to remove the soaps, impurities and coloring matter still present in the oil without treating the deacidified oil with an acid, the fact of omitting the washing step is still recommended in this method as in the method of the present invention. How-ever, this method requires a very large amount of adsorbentcompared with the method of the inven-tion. Therefore, a large amount of -the oil is lost with -the adsorbent and the disadvantage ~J ~ ~322~
caused by the increase of the cost of the adsorbent and by the decrease of the yield of the oil cancels the advantage of omitt-ing -the washing step. This method is not an economically signi-ficant method which is, as a matter of course, far inferior to the method of the invention.
The method of the present invention can be applied favourably to the refining of all kinds of vegetable and animal oils and fats such as soybean oil, rape seed oil, rice oil, corn oil, cotton seed oil, sunflower oil, safflower oil, sesame oil, peanut oil, palm oil, coconut oil, linseed oil, lard, beef tallow, mutton tallow, fish oil and the oils and fats of marine animals.
IIaving generally described this invention, a further understanding can be obtained by reference to certain specific examples which are provided herein for purposes of illustration only and are not intended to be limiting unless otherwise speci-fied.
Soyb~an oil was treated by the conventional al]cali refining method. A deacidified separated oil was obtained by separating soapstock from the oil using a centrifuge. The oil was divided into four samples and was used for the following tests. The characteristics of the deacidified separated oil is shown in Table 1.
Test 1 (Method of the present invention (1~) 40 ppm by weight of 85% phosphoric acid was added to the deacidified separated oil and the acid treatment was carried out by stirring the mixture for 5 minutes at a temperature of 80C. Then 0.3% by weight of activated clay was added to the oil treated with acid, and the oil was decolorized under reduced pressure at 105C for 15 minutes and the activated clay was separated from the mixture. The decolorized oil thus obtained ~ :~ 83228 was subjected to deodorization under vacuum at 250C for 45 minutes to give the refined oil.
Test 2 (Method accordinq to the present invention (2)) This test was carried out under the same conditions as in Test 1 except that the amount of phosphoric acid was changed to 80 ppm.
Test_3 (Comparison test (1): conventional method) The deacidified separa-ted oil was washed with 20%
of hot water against the oil and centrifuged. After the wash-ing a double decolorization and deodorization were carried outunder the condition described in Test 1.
Test 4 (Comparison test (2)) The deacidified separated oil was directly decolorized and deodorized under the conditions described in Test 1 without acid treatment and washing.
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/ ~ ~ ~ ~ ~o / ~ ~ ~ ~ ~ O ~ '~ O
/ O rl 11~ 0 rl d O ,1 ~-1 (d ,1 rl O ~d / ~) ~.) O ~ t) O rS~ c) O O O O
/ ~1 ~ I ~ 4 f~ U u~ ~ U Ql ~1 ~ ... .__ ,1 ~ O O N a) ~1 O ~: ~) .,1 N
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o (1~ rlrl-rl a~ ~ O rl 0 3 ~ O ~ O
.
O O
rl I :~ 63228 The characteristics of the oil at each step in the tests 1 - 4 are shown in Table 1.
As evident from the results of the tests shown in Table 1, the refining method of the invention (in the tests 1 and 2) can give a refined oil having substantially the same characteristics and quality as that of the oil obtained by the conventional method (test 3) by treating merely the deacid-ified separated oil with phosphoric acid without washing with water. As the conditions of decolorization and deodorization in the method of the invention need not be changed from that of the conventional method, they have no influence on the yield of refined oil. The method of the invention is rather superior to the conventional method in the yield of refined oil, since the latter loses neutral oil entrained in the washing water.
When the deacidified separated oil is directly decolor-ized and deodorized without acid treatment and washing with water (in test 4), soaps and phospholipids are not sufficient-ly removed. Therefore the quality of the refined oil is bad.
It was found in the test that activated clay was re-quired in an amount of 0.8% which was more than twice the clayrequired in the method of the invention, in order to improve the quality of the refined oil in test 4 to the level of the quality of the oil obtained in tests 1 and 2. The increase of the cost for refining the oil by this method compared with that of the method of the invention was about 1000 yen per ton of the oil.
Rape seed oil was treated conventionally with the alkaline solution and the soap stock was centrifuged. 431 ppm by weight of 30% aqueous solution of citric acid was added to a deacidified separated oil having an acid value of 0.06, a soap content of 205 ppm and a phospholipid content of 283 ppm. The ~ I ~322~
mixture was stirred for 30 minutes at a temperature of 50C.
Then 0.6% by weight of activated clay was added to the oil, and the oil was decolorized at 105~C for 15 minutes. The activated clay was separated from the oil. The oil was deodorized under reduced pressure at 250C for 45 minutes to give a refined oil.
It has an acid value of 0.05, a color of 6Yx0.5R and a phos-pholipid content of 5 ppm. The quality of the refined oil was substantially the same as that in a conventionally refined oil.
Corn oil was deacidified by the conventional alkali treatment and the soap stock was centrifuged to obtain the de-acidified separated oil. 604 ppm by weight of a 20% aqueous solution of hydrochloric acid was added to the deacidified separated oil having an acid value of 0.08, a soap content of 990 ppm, and a phospholipid content of 368 ppm. Tne mixture was stirred for 5 minutes at a temperature of 80C. Then 0.6% by weight of activated clay was added to the oil, and the oil was decolorized at 105C for 15 minutes. After the activated clay was separated from the oil, the oil was deodorized under reduc-ed pressure at 260C for 60 minutes to give a refined oil. It has an acid value of 0~07, a color of 6Yx0.6R and a phospholipid content of 13 ppm. The quality of the refined oil was substan-tially the same as that of conventionally refined oil.
. _ Beef tallow was deacidified by the conventional alkali treatment and the soap stock was separated from the tallow to give a deacidified separated tallow having an acid value of 0.06, a soap content of 205 ppm and a phospholipid content of 54 ppm.
45 ppm by weight of 98% acetic acid was added to the tallow and the mixture was agitated at high speed by a Dispermill (made hy Hosokawa Iron Works) for 30 seconds at a temperature of 90C. 2% by weight of activated clay was added to the oil, and * Trademark I ~ 63~2P~
was decolorized under reduced pressure at a temperature of 100C for 30 minutes. The oil was deodorized under vacuum at a temperature of 250C for 90 minutes. The refined oil obtained had an acid value oE 0.02, a color of lYxO.lR and a trace of phospholipid.
The refining method of the invention can eliminate the washing step after deacidification and separation of soap stock from the deacidified oil in the usual alkali refining method as clearly shown in the examples and can give a refined oil with a good yield having the same quality as that of the conventionally refined oil.
Since the economical burden to the processors is very small for the acid treatment of the present invention compared with the advantage of omitting the washing step, the method of the invention is far superior to the conventional method. The refining method of the invention does not produce waste water and saves the consumption of valuable water, thus making an important contribution to the oil refining industry.
Claims (8)
1. A method of refining an animal or vegetable oil or fat which comprises:
(a) mixing said oil or fat with an aqueous solution of an alkaline substance;
(b) separating the insoluble matter in the oil or fat from the resulting mixture;
(c) directly admixing the deacidified separated oil or fat from step (b) with an aqueous solution of an acid;
(d) treating the resulting admixture with an adsor-bent to adsorb coloring matter, impurities and salts formed during step (c);
(e) separating said adsorbent from said oil or fat, and (f) treating said oil or fat after step (e) by steam distillation.
(a) mixing said oil or fat with an aqueous solution of an alkaline substance;
(b) separating the insoluble matter in the oil or fat from the resulting mixture;
(c) directly admixing the deacidified separated oil or fat from step (b) with an aqueous solution of an acid;
(d) treating the resulting admixture with an adsor-bent to adsorb coloring matter, impurities and salts formed during step (c);
(e) separating said adsorbent from said oil or fat, and (f) treating said oil or fat after step (e) by steam distillation.
2. The method according to claim 1, wherein after step (c) and before step (d) the resulting admixture is dried to remove excess water.
3. The method according to claim 1, wherein said oil or fat is subjected to a pre-treatment to remove impurities.
4. The method according to claim 1, wherein said pre-treatment includes filtration, sedimentation and degumming with water, acids and alkalis.
5. The method according to claims 1, 2 or 3, wherein step (b) is carried out by centrifugation.
6. The method according to claim 1, wherein the acid in step (c) is selected from the group consisting of hydrochloric acid, sulfuric acid, phosphoric acid, oxalic acid, acetic acid, acetic anhydride, citric acid, tartaric acid and mixtures thereof.
7. The method according to claim 6, wherein after ad-mixing the acid, the mixture is stirred at a temperature from room temperature to 100°C for a period of time varying from several seconds to several hours.
8. The method according to claim 6, wherein said adsor-bent is selected from the group consisting of activated clay or activated charcoal.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7912779A JPS564698A (en) | 1979-06-25 | 1979-06-25 | Purification of oll and fat |
| JP79127/1979 | 1979-06-25 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1163228A true CA1163228A (en) | 1984-03-06 |
Family
ID=13681266
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000354550A Expired CA1163228A (en) | 1979-06-25 | 1980-06-23 | Method for refining oils and fats |
Country Status (6)
| Country | Link |
|---|---|
| JP (1) | JPS564698A (en) |
| CA (1) | CA1163228A (en) |
| DE (1) | DE3023589A1 (en) |
| FR (1) | FR2459828A1 (en) |
| GB (1) | GB2058121B (en) |
| NL (1) | NL8003649A (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4609500A (en) * | 1981-10-15 | 1986-09-02 | Cpc International Inc. | Refining of oil and product thereof |
| JP2003313578A (en) * | 2002-04-25 | 2003-11-06 | Kanegafuchi Chem Ind Co Ltd | Method for purifying oils and fats |
| JP2005264077A (en) * | 2004-03-19 | 2005-09-29 | Nisshin Oillio Group Ltd | Conjugated trienoic acid-containing fat-and-oil composition and manufacturing method therefor |
| US8232419B2 (en) | 2008-10-02 | 2012-07-31 | The Dallas Group Of America | Triacylglycerol purification by a continuous regenerable adsorbent process |
| JP6219147B2 (en) * | 2013-12-02 | 2017-10-25 | 花王株式会社 | Method for producing refined fish oil |
| JP6726657B2 (en) * | 2015-03-02 | 2020-07-22 | 株式会社カネカ | Method for producing edible oil and fat |
| JP6987445B2 (en) * | 2017-09-29 | 2022-01-05 | 日清オイリオグループ株式会社 | Cooking oil manufacturing system and cooking oil manufacturing method |
| CN116355690B (en) * | 2023-02-22 | 2023-09-05 | 山东亿科化学有限责任公司 | Biodiesel raw material pretreatment process |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2510379A (en) * | 1948-08-31 | 1950-06-06 | Pittsburgh Plate Glass Co | Preparation of break-free glyceride oils |
| DE1186162B (en) * | 1959-09-21 | 1965-01-28 | Pellerins Margarinfabrik Ab | Process for removing small amounts of soap and alkali from refined fats |
| CH387851A (en) * | 1959-09-21 | 1965-02-15 | Pellerins Margarinfabrik Ab | Process for removing small amounts of soap and alkali from alkali-refined fat and fatty oil |
| US3943155A (en) * | 1974-05-13 | 1976-03-09 | The Procter & Gamble Company | Simultaneous refining and dewaxing of crude vegetable oil |
| JPS5573793A (en) * | 1978-11-30 | 1980-06-03 | Showa Sangyo Co | Purification of oil and fat |
-
1979
- 1979-06-25 JP JP7912779A patent/JPS564698A/en active Granted
-
1980
- 1980-06-23 CA CA000354550A patent/CA1163228A/en not_active Expired
- 1980-06-24 NL NL8003649A patent/NL8003649A/en not_active Application Discontinuation
- 1980-06-24 FR FR8014009A patent/FR2459828A1/en active Granted
- 1980-06-24 DE DE19803023589 patent/DE3023589A1/en not_active Ceased
- 1980-06-25 GB GB8020761A patent/GB2058121B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| GB2058121B (en) | 1983-09-21 |
| GB2058121A (en) | 1981-04-08 |
| NL8003649A (en) | 1980-12-30 |
| FR2459828B1 (en) | 1984-04-27 |
| FR2459828A1 (en) | 1981-01-16 |
| JPS6243476B2 (en) | 1987-09-14 |
| DE3023589A1 (en) | 1981-01-22 |
| JPS564698A (en) | 1981-01-19 |
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