DE2452027A1 - Plastic edible fat prodn - by hydrogenation of an animal fat-unsatd vegetable oil mixt under specified conditions - Google Patents

Abstract

Animal fats (I) are converted to plastic edible fats by mixing 1 pt. of the molten (I) with 0.4-9 pts. of a lightly unsatd. vegetable oil and hydrogenating the mixt. at 180-220 degrees C using an H2 excess press. of =2 Kp/cm2 and an Ni catalyst whole activity is =35 degrees C so that the polyunsatd. fatty acids of (I) and (II) are selectively hydrogenated and a partial transesterification of (I) with (II) occurs. The process enables a prod. having an m. pt. of i9-40 degrees C and a hardness of 130-140 g/cm to be produced which are free from the characteristic smell and taste of (I) and which is stable during further processing esp. to margarine. Pre-determination of end-prod. props. possible. No pre-refining of (I) reqd.

Description

METHOD OF PROCESSING ANIMAL RESCUE INTO PLASTIC EDIBLE FAT The present invention relates to the technology for the production of fats, in particular on processes for processing animal fats into plastic (e.g.

spreadable) edible fat.

The natural animal fats (pork fat, beef tallow, enochene fat etc.) have specific features that reduce their utility value. to These peculiarities include peculiar, often unpleasant smells, sebum Taste, high meltability, unsatisfactory consistency and rapid rancidity (oxidative spoilage), significant fluctuations in the physico-chemical parameters (of the melting point, of hardship and others) that self for one and the same kind of animal fat can be observed.

The specific smell of animal fats depends on the type of Animal, the feed ration and the degree of oxidative spoilage. Through treatment with direct steam under vacuum (deodorization), volatile additions are achieved that give animal fat a specific smell. However comes there is a rapid reversion when the deodorized fat is used further the specific smell, which affects the taste properties of the products, in which animal fat has been used, has a negative effect. The cause of the Reversion of the smell consists in the slight oxidation of the linolenic, archidonic and other polyunsaturated fatty acids found in the triglycerides of animal Fats are contained in small amounts (up to 3%). With deeper oxidation of the animal bed when stored in the air they gain the typical smell and Taste of the "rancid" fats.

The sebum taste, the unsatisfactory consistency and the high The elutability of animal fats is due to their fatty acid and triglyceride composition traced back. For comparison, Tables 1 and 2 show the fatty acid composition (Table 1) and the triglyceride composition e (Table 2) of the pig fat, of sunflower oil and selectively hydrogenated (hardened ") sunflower oil, used in the production of margarine.

Table 1 Fatty acid composition of the samples,% fatty acids Pig fat hydrogenated sunflower-sunflower seed oil linolenic acid and other polyunsaturated Acids 0.8 0.0 0.0 linoleic acid 7.9 6.9 72.1 oleic acid and other monounsaturated Acids 45.4 79.3 18.1 Palmitic Acid and Other Saturated Acids 45.9 13.8 9.8 Table 2 Triglyceride composition of the groups of samples,% triglycerides pig fat hydrogenated sunflower oil 1 2 3 tri-saturated 9.8 0.8 8-symmetrical dunsaturated 37.5 6.4 1 2 3 Symmetrical unsaturated 2.0 3.6 Asymmetrical monosaturated 7.5 26.7 Symmetrical mono-saturated 36.0 12.1 Triunsaturated 7.2 50.4 As from Table 1 shows that the pork fat contains about 46% high molecular weight saturated fatty acids, these acids mainly in the form of tri-saturated and disaturated triglycerides are concentrated (Table 2), which have a high melting point (43 to 71 ° C). Just the presence of significant amounts of high melting point Triglycerides cause the sebum taste and the inhomogeneous consistency of the pork fat and the other animal fats A no less essential disadvantage of animal fats Fetter of what was mentioned above is, after all, the instability of their physico-chemical Characteristic values.

Corresponding information is given in Table 3.

Table 3 Type of fat No. of the sample Melting point, hardness, g / cm 0, pork fat 1 29.0 16 2 29.8 34 3 37.5 180 4 40.0 177 Beef tallow 1 42.5 230 2 44.0 350 3 47.0 690 4 48.4 770 bone fat 1 36.3 68 2 37.4 86 It is evident that a and the same fat, e.g. pork fat, has a different melting point and can have a different hardness. Also exists for different animal fats have a different ratio between the melting point and the Hardness.

It is understandable, therefore, that when one of the other disadvantages The animal fats also refrains from using the animal fats as a component of a fat product due to the instability of its physico-chemical parameters is extremely difficult. This conclusion is supported by the information in the table 4 illustrates in which the physically -chemical characteristics of Mixtures of different animal fats with one and the same selectively hydrogenated ("Hardened") sunflower oil are listed.

Table 4 Characteristic values of the mixture. Animal content of the mixture cal animal fat,% te with hydrogenated oil 0 5 10 15 20 40 1. Pig fat. Melting point 28.9 ° C, hardness 13 g / cm Melting point, ° C 32.6 33.3 32.9 32.3 31.0 29.3 Hardness, g / cm 220 199 193 159. 165 116 2. Pig fat. Melting point 40.0 ° C, hardness 230 g / cm melting point, ° C 32.6 33.3 33.4 33.9 34.1 35.9 hardness, g / cm 220 240 230 236 257 266 3. Beef tallow. Melting point 44.1 ° C, hardness 270 g / cm, melting point, ° C 32.6 33.9 34.4 34.6 35.5 37.7 hardness, g / cm 220 203 205 209 215 219 4. Beef tallow. Melting point 47.0 ° C, hardness 690 g / cm Melting point, ° C 32.6 34.6 35.6 38.2 37.0 42.0 Hardness, g / cm 220 244 265. 297 301 418 As from the information in the table 4, it allows the animal fats to be mixed with the hydrogenated fats Oils don't get an end product with certain properties because of the melting point and the hardness of the mixtures both from the ratio between the animal fat and the hydrogenated oil as well as the characteristics of the animal fat itself are. Consequently, under the conditions of large-scale bed manufacture, where it comes down to the finished product with relatively constant properties every time the recipe of the mixture changes as soon as the properties change of animal fat have changed.

In addition, the mixing of the high-melting line leads to unsatisfactory results Animal fat hardness with the hydrogenated vegetable oil (or any other fat or not oil) To obtain a product different from the specific Odor and the sebum taste of animal fat is free and the necessary Has relationship between the melting point and the hardness. Indeed it will be like shown in Table 4, the blending does not increase in proportion the melting point and the hardness of the end product or the hardness increases significantly slower than the melting point. This phenomenon is due to that by mixing the triglyceride composition of the animal Fat is not changed, which is why the animal content of the mixture is high enough Fat the unsaturated and triglycerides triglycerides the consistency of the product affect unfavorably.

Thus it is for the production of plastic edible fat without specific smell and sebum based taste based on animal fat, the required melting point (31 to 370C) and the required hardness (160 to 400 g / cm), necessary: a) the polyunsaturated from the animal fat Fatty acids, which are responsible for the smell and the ability of the same to be rapidly oxidative Spoilage are responsible for removing, and b) a molecular remodeling of the animal fat in mixtures with other fats or oils for the purpose of a more uniform Distribution of fatty acids in the triglycerides carry out, which makes its plasticity increases and the sebum taste disappears.

The well-known process for the hydrogenation purification of animal fats consists of small amounts of polyunsaturated fatty acids (linolenic acid, etc.) therein, d a 13 the animal fat under increased hydrogen pressure, for example 5 to 10 atm, and elevated temperatures of 200 to 2300C in the presence of copper-chromium catalysts treated.

Such treatment results in a practically complete conversion the linolenic acid and the other polyunsaturated acids in linoleic, oleic and Stearic acid, as a result of which the animal fat loses its specific smell and becomes significant becomes more resistant to the oxidative action of the medium.

However, this leads to undesired trans isomerization of the oleic acid of animal fat and the formation of undesirable isomers of linoleic acid animal fat (conjugated dienes). On the whole, these reactions lower the isomerization while unsaturated acids slightly increase the biological value of animal fat its melting point does not drop and the tallowy taste is retained. Another The disadvantage of this process is the need for careful refining of animal fat before and after the catalytic treatment. The pre-refining is necessary so that free fatty acids are removed from animal fat react with the copper-earm catalyst to form copper soaps. the Refining is absolutely necessary because in each case in the fat after the catalytic treatment copper remains in the form of soap or colloidal particles, what because of the specific properties of EupSers, which is a promoter of oxidation of fat is inadmissible.

It should also be noted that the removal of the copper is only it is achieved through special refining of the fat with solutions of complexing substances will.

Then the animals treated in this way are subjected Fats mixing with specially selected oils and fats and a subsequent one Transesterification in the presence of alkaline catalysts such as sodium methylate, sodium ethylate, metallic sodium, etc. The transesterification results in a molecular remodeling of the Mixture of fats brought about, whereby the sebum disappears, the melting point decreases and the plasticity of the end product increases.

However, such a process of transesterification with alkaline adheres Catalysts have certain defects. It is especially necessary to the animal fat or the mixture of fats and oils (if one uses the previous mixing) of free fatty acids and moisture in order to avoid significant fat loss during the transesterification and significant consumption of the expensive catalyst to the maximum to free.

Then it is necessary to carry out the transesterification process in such a way that that the molecular remodeling does not involve statistical distribution of the fatty acids under the triglycerides is completed. This is necessary because in the event Due to the statistical distribution of the fatty acids, the hardness of the end product is always minimal will be, while the melting point drops only insignificantly. In practice that is said partial transesterification cannot be carried out in the presence of alkaline catalysts, why the transesterified plastic fat obtained has too high a melting point and an insufficient one Has hardness. This disadvantage of the interesterified fat is caused by mixing it up with the corresponding non-transesterified hard (natural or hydrogenated) vegetable oil balanced by obtaining a fat mixture with the required properties.

The described conventional technological scheme of processing of animal fats to plastic edible fat has the following major disadvantages: 1) Multistage (the hydrogenation and the transesterification are performed as separate operations carried out); 2) Complicated technology (use of two specific catalysts for carrying out the selective hydrogenation of animal fat and separately the subsequent transesterification); 3) Increased requirements for pre- and intermediate refining (cleaning) of fats and oils; 4) The need for the components of the fat mixture which forms the end product, plastic fat, depending on the To select properties of animal fat and interesterified fat.

There is an attempt known to the technology of processing to perfect animal fats (Spanish Patent No. 193123, from 1951). The procedure consists in that you get a mixture of Vegetable oil and animal fat with hydrogen at a pressure of 10 kp / cm2 and a temperature of 250 ° C in the presence of a nickel catalyst and 2 to 5% sodium methylate or sodium ethylate treated.

In the same patent it is suggested that instead of sodium methylate or Sodium ethylate tin or zinc to be used, each in an amount of 2 up to 5%, based on the weight of the mixture of oil and fat, can be added.

A test of this method has shown that once the mixing the nickel catalyst with the sodium methylate or sodium ethylate and the subsequent Hydrogenation under the conditions mentioned to a very rapid and complete Poisoning of the nickel catalyst, a complete destruction of the sodium methylate or of sodium methylate and severe destruction (saponification) of the mixture of oil with fat leads. It is practically impossible to produce plastic edible fat after this Variant of the procedure. On the other hand comes when the sodium methylate is replaced or of sodium ethylate by tin or zinc itself in such large quantities as they specified in the patent), the transesterification practically did not take place during In addition to the oil, the animal fat is also deeply hydrogenated.

As a result, a high-melting and tallowy end product is obtained. It is also essential that due to the difficulty of subsequent removal of zinc, especially tin, this product is not approved for nutritional purposes can be.

The purpose of the present invention is to remedy the disadvantages mentioned the known technology for processing animal edible fats.

In accordance with the purpose, the task was set which in the development of a process for the production of plastic edible fat animal fats existed, which makes it possible at the same time the selective hydrogenation of the polyunsaturated fatty acids of animal fat and its partial transesterification to be carried out with selectively hydrogenated vegetable oil in the presence of a heterogeneous catalyst.

The problem posed was achieved by a method for processing animal fats to plastic edible fat by mixing it with vegetable oil and subsequent treatment with hydrogen on nickel catalyst, the ore in accordance with is characterized in that the molten edible animal fat with a highly unsaturated edible vegetable oil mixed in a ratio that to 1 part of the animal pette 0.4 to 9 parts of said oil are omitted, and the obtained Mixture at a temperature of 180 to 220 ° C under a hydrogen pressure not exceeding 2 kgf / cm² and the activity of the catalyst not exceeding 35 ° C hydrogenated. Under the conditions mentioned, it is mainly selective Hydrogenation of the polyunsaturated fatty acids of animal fat, for selective Hydrogenation of the highly unsaturated fatty acids in vegetable oil and for partial Transesterification of animal fat with this oil.

Among the highly unsaturated vegetable oil is any vegetable oil and to understand any mixture of vegetable oils, which is at least 30% Contain linoleic acid and a maximum of 30% saturated fatty acids.

We understand the technical term "polyunsaturated fatty acids" the fatty acids which contain three or more double bonds in the carbon chain. The term "highly unsaturated fatty acids" means all fatty acids which contain more than one double bond in the carbon chain e.

When it comes down to it, a plastic low-melting fat with a melting point of 31 to 330C can be any animal Edible fat or a mixture of the corresponding animal fats are used, whose melting point (of the individual fat or a mixture of fats) is 430C must not exceed. Thereby the ratio between the animal fat and the vegetable oil chosen so that the melting point of this mixture does not exceed the required melting point of the end product, the plastic fat. So it is, for example, to obtain a plastic fat with a melting point of 32 + 100 desired that the melting point of the starting mixture of the animal Fat with the vegetable oil is in a range of 15 to 300C.

For the production of a plastic fat with a melting point of 32 + 1 ° C and a content of trans isomers of the monounsaturated fatty acids of not more than 45% it is desirable that 1 to 1 part of the animal fat is added 3 parts of the vegetable oil are omitted.

Under the word "part" by which the ratio of the components is expressed are, in the present case, both parts by weight and parts by volume to understand the components in the mixture. In other words, the dosage of the Components of the mixture both according to the weight methods and according to the volumetric Methods are controlled.

According to the invention, the hydrogenation with a nickel catalyst carried out, the activity of which does not exceed 350C. To the nickel catalysts include powdered catalysts whose main active component is nickel, for example Nickel obtained from the nickel formate or nickel carbonate, nickel, deposited on diatomaceous earth or other carriers involved in accelerating the reaction used by acids and bases, nickel with copper as a promoter, as well as others Nickel catalysts with salts as promoters with the exception of lead, tin, zinc and metals or metalloids whose presence in food is impermissible is.

It is desirable that the activity of the one used in the present invention Catalyst is in a range from 20 to 300C. The activity of the catalysts which one is determined according to the method used in the O1 and fat industry consists in determining the melting point of 50 g of sunflower oil, which during 60 minutes at a temperature of 22006 under normal pressure, at one speed of the hydrogen of 3 1 / min passed through the oil layer in the presence of 0.15% Catalyst, converted to metallic nickel, has been hydrogenated to form a catalyst to obtain the activity mentioned, it is sufficient to use any of the and fat industries used nickel catalysts in the conventional process the hydrogenation of refined bleeds and fats to be used several times.

According to the present invention, the process is used for the selective Hydrogenation of the edible vegetable oils applied concentration of nickel in the raw material (0.08 to 0.25%) based on the activity of Catalyst, the temperature of the process, the hydrogen pressure, the melting point of the animal fat and the melting point of the mixture of the animal bed with the vegetable oil is determined.

Manufacture guarantees compliance with the above conditions of plastic hydroesterified fat, in which the specific properties of the animal fat does not come to light.

Lowering the temperature of the process below 1800C is undesirable, because they are due to a significant reduction in the rate of transesterification on nickel catalysts is accompanied.

Raising the temperature of the process above 2200C is undesirable as a result of the acceleration of the side reactions of thermal decomposition, hydrolysis, and the polymerisation of fats and oils. .

As mentioned above, the hydrogen pressure must not exceed 2 kp / cm2. It is expedient to keep this in a range of 0.1 to 1.0 kgf / cm2, which is such a Relationship between the rate of hydrogenation and the rate of transesterification guaranteed at the time of production of plastic fat with predetermined Melting point, the degree of transesterification of animal fat is close to 1.

In the present case, the degree of transesterification is understood to mean that Ratio of the concentration of palmitic acid in the 2-position of the triglycerides of the Mixture of fat and oil to concentrate the palmitic acid in this mixture.

The selectivity decreases under a hydrogen pressure of more than 2 kp / cm2 of hydrogenation, while the overall rate of hydrogenation is the rate the transesterification significantly exceeds. On the whole, the pressure increase worsens the consistency and taste of the end product.

The use of catalysts with an activity above 350C exerts the same influence on the course of the process and the quality of the finished product as well as increasing the hydrogen pressure.

The speed of the process is determined by the said ratio the components, the temperature, the pressure, the amount and activity of the catalyst certainly.

The present invention makes it possible from animal fats and vegetable oils, plastic edible fats with a melting point of 29 to 400C and to obtain a hardness of 130 to 140 / cm depending on the specific smell and Flavor of the animal fat are free, stable during further processing and for use in the manufacture of margarine, culinary fats and special fat products (for baking bread, for sugar confectionery, food concentrates) suitable.

Of those obtained by the process of the invention Fats are of particular interest plastic fats with a melting point of 32 + 100, which are mainly used for making Largarine.

The invention makes it possible to process animal fats with vegetable oils in a one-step technological process of hydroesterification perform, in which the following is achieved at the same time: a) hydrogenation of the polyunsaturated Fatty acids of animal fat, which removes the specific smell of the animal fat and prevents its reversion; b) selective hydrogenation of the highly unsaturated fatty acids in vegetable oil, which leads to the achievement of a melting point and a hardness of the finished product ensures that as plastic edible fat referred to as; c) partial transesterification of animal fat and vegetable oil, thereby eliminating the greasy taste of the end product and its homogeneity and plasticity is increased.

According to the invention, the edible animal fat is dissolved in the highly unsaturated one Oil. This, as well as the combination of other conditions, are subject to the present Invention practically only hydrogenated its polyunsaturated acids, their content in animal fats is low and does not exceed 3S, which is sufficient for that the specific smell of fat disappears, the possibility of one Reversion of this odor is eliminated, the melting point of animal fat remains unchanged and at the same time the resistance of the animal fat it is guaranteed against the oxidative effect of the medium (air) 0 at the same time Under the conditions mentioned, the highly unsaturated ones are hydrogenated selectively Fatty acids of the vegetable oil, whereby the required degree of hardness of the fatty product is achieved.

In addition to the reactions mentioned, it occurs under the conditions of Implementation of the process according to the invention for the partial transesterification of the animal Fat it and the vegetable oil, resulting in greater homogeneity and plasticity of the End product, to disappear, in the same of the tallowy taste of the animal Fat leads.

A major advantage of the proposed method is that all chemical transformations listed above take place in the presence of a catalyst, which is also easily available and suitable for multiple use.

Another advantage of the invention is the possibility of plastic Edible fats with a given melting point and a given hardness regardless of the melting point and hardness of the starting animal fat. That is enough it, the animal fat with the strongly unsaturated (51 in a ratio to mix so that the melting point of the starting mixture is below the required Melting point of the end product is, and then combined in one process hydrogenation and to carry out transesterification according to the invention.

One advantage of the proposed method is the possibility of animal Edible fats not only of the top grades, but also of the lower grades, including to process fats that have a specific smell and a specific feed smell Own color. There is no need for a previous deep refining of this Fats.

A no less important advantage of the invention is the ability to animal edible fat with a melting point of 32 + 100 and a hardness of at least 160 / cm with a reduced content of transmonounsaturated fatty acids (max 45%), which are undesirable from a biological point of view, to get what the relatively low degree of hydrogenation of the vegetable oil and the low degree of catalytic isomerization of oleic acid of animal fat is guaranteed.

The invention makes it possible to use the unified process of hydrogenation and transesterification (the process of hydroesterification) on an industrial scale to be carried out according to both the periodic and the continuous process.

The method of processing animal fats from Standard from plastic edible fat is made using retrofits of oil and Fat factories performed as follows.

A previously prepared homogeneous mixture (a solution) of the animal Fats and vegetable oils, the quality of which corresponds to that of food one continuously to the first at a rate of 5 to 8 tons per hour Reactor of the continuously operated plant, which for example consists of three reactors each of 6 m3 of work content, which is carried out with turbo or other stirrers, barboteur, internal or external heat exchange devices as well as with standard monitoring meters are equipped.

At the same time one leads the same first one from a separate container An intimately mixed suspension of finely divided nickel catalyst in the reactor to the starting mixture of animal fat and oil. The concentration of the Catalyst, converted to nickel, in the suspension is kept in one area from 1 to 5% by weight.

The length of the catalyst suspension fed to the reactor is dimensioned so that the concentration of nickel in the raw material to be hydrogenated is constant is maintained in the range of 0.08 to 0.4% by weight. In the process of continuous Hydrogenation is the pressure in the reactors of the plant in a range from 0.1 to 2 kp / cm2 held, in with this the / hydrogen pneumatically stirred and / in the system with a speed of 500 to 1000 m3 / h in the circuit guided will. Monitoring the completion of the hydrogenation process (hydro-esterification) is carried out by measuring the melting point, the refractive index and the Hardness of the product emerging from the last reactor in the plant. The temperature in the reactors of the plant is maintained in a range of 200 + 200C. The end grease coming from the last reactor of the plant, which contains 0.08 to 0.4s0 nickel, is cooled to a temperature around 1000C by passing the fat through the heat exchanger directs.

Then the cooled fat is placed on horizontal or vertical filter presses (of the "Niagara" type, etc.) continuously filtered. The filtered fat is then subjected to alkaline neutralization, washed, on a periodic or continuously operated refining plant (for example on the separation plants "Laval") and periodic or continuous deodorization conventional plants (for example of the "Die Smet" type) among those for the processes subjected to refining and deodorization under conventional conditions.

The hydrogenation (hydro-esterification) of mixtures of animal fats with the vegetable oils under the above conditions can also be used after the Construction carried out analogous periodically operated hydrogenation reactors will. In this case one brings the homogeneous mixture of animal fat and of vegetable oil into one periodically operated reactor (for example from the company t'Blau-Nocks ") and heated with barbotage of hydrogen and stirring to a temperature of 170 to 1800C, then leads the same reactor a suspension of the catalyst in the abovementioned quantity and of the abovementioned activity and leads to the temperatures and hydrogen pressures mentioned in the invention for 1 to 3 hours by the hydroesterification by following the process according to the The index of refraction, the hardness and the melting point of the fat it monitors.

The process is terminated after the required characteristics of the plastic edible fat it has been achieved.

Then the fat obtained is cooled as described above, filtered, refined and deodorized.

Carrying out the unified process of selective hydrogenation and the partial transesterification of mixtures of animal fats with vegetable oils illustrated according to the invention with reference to Examples 1-7. Examples 8-10 are for Comparison listed.

Example 1.

Pork fat 1st grade, which has a melting point of 28.50C, an acid number of 0.6 mg of KOH is mixed in an apparatus with a stirrer with refined Sunflower oil, which has an acid number of. 2 mg KOH. On one part by weight each Pork fat you take one part by weight of sunflower oil and get a mixture, which one Acid number of 0.4 mg KOH, a melting point of 240C and has a hardness e of 0 g / cm. The fatty acid composition of the mixture is characterized by the following information: linolenic acid and other polyunsaturated Acids 0.3%, linoleic acid 38.9%, oleic acid and other monounsaturated acids 39.1%, Palmitic acid 13.7%, other saturated acids 8.0%. 6 tons of said mixture is brought into a large-scale, periodically operated hydrogenation reactor 11 m3 total capacity, with a 'pure stirrer', a hydrogen barboteur Coiled tubes are provided for heating and cooling the raw material. Then heated man * with stirring and barbotage with hydrogen at a rate of 100 m3 / h (pressure = 0.1 kg / cm2) the starting raw material to a temperature of 170 to 175 ° C and brings a suspension of nickel-copper catalyst at this temperature in the starting raw material. The activity of the catalyst is 22.4 ° C. the Suspension of the catalyst is introduced in an amount that the concentration of the nickel in the mixture to be processed is 0.2%. The catalyst was by joint deposition of the nickel and copper carbonates in a nickel / Eupfer ratio of 3: 1, subsequent reduction of the co-deposited carbonates in sunflower oil and exercising by hydrogenating the sunflower oil several times until achieved an activity of 22.4 ° C.

* Pressure mix After the catalyst suspension has been charged the reactor contents are heated to a temperature of 215 + 50C and are carried out at this Temperature, a hydrogen pressure of 0.1 kp / cm2 and a speed of Barbotage with hydrogen of 100 m3 / h the process of hydro-esterification 1.5 hours proceeding by terminating the process after the refractive index of the obtained hydroesterified fat, measured at a temperature of 600C, 1.4539 + 0.0001 has reached.

When the process is complete, the product is pumped into the container for unfiltered fat, then diverts the fat from this container via the Heat exchanger for the filter press to separate the catalyst. The one from the filter press The removed catalyst is collected in the container to be used again to V catalyst and the filtered fat in the containers for the filtered fat. The fat obtained, which has an acid number of 0.7 mg KOH, is then subjected to the continuous refining on a separation plant and the continuous Deodorization.

The refined and deodorized plastic fat has the following characteristics to: melting point 31,500; Hardness 190 yom; Content of trans isomers 41.0%; salary of conjugated dienes 0%; Fatty acid composition: polyunsaturated acids 0%; diunsaturated acids 7.7; monounsaturated acids 69.2ffi; Palmitic acid 14.5%; other saturated acids 9.1%.

According to the values of selective enzymatic hydrolysis of fat it was found that the palmitic acid between the 1-, 2- and 3-position in the Triglycerides is statistically distributed.

The obtained plastic fat is free from the smell and the taste of pork fat. When storing this fat for 30 days at one temperature from 4 to 200C no reversion of the pig fat odor was detected.

The fat is suitable for making margarine.

Example Q.

1st grade pork fat with a melting point of 29.50C and an acid number 0.4 mg of KON are mixed with refined cottonseed oil as in Example 1. 1 part by volume of animal fat is taken and 1.5 parts by volume of oil are obtained a mixture that has a melting point of 24.7 ° C in the absence of hardness.

The mixture obtained is in an amount of 6 tons per hour the 1st reactor of a continuously operated hydrogenation plant fed from three reactors connected in series, which are described in Example 1 are described, consists. The treatment is carried out at an overpressure of the hydrogen vnn 0.8 to 1.0 kp / cm2 in the presence of C), 1%% nickel in the form of suspended Nickel-copper catalyst with an activity of 350C. The catalyst became as described in Example 1 prepared. The speed of the barbotage of the parallel hydrogen fed to each reactor of the plant is 750 m3 / h. The process is based on the melting point of the fat emerging from the last reactor in the plant monitored, the product obtained, which contains the suspended catalyst, subjected one analogous to Example 1 of the filtration, refining and deodorization.

The refined and deodorized plastic hydroesterified fat is free from the specific smell and taste of pork fat, stable in storage and has a melting point of 32.7 ° C and a hardness of 340 g / cm. The others Characteristic values of the fat obtained are as follows: content of trans isomers 35.0%; Conjugated diene content 0%; Fatty acid composition: polunsaturated acids 0%; diunsaturated acids 15.79 monounsaturated acids 53.7%; Palmitic acid 23.6%; other saturated acids 750%.

The ratio of the concentration of palmitic acid in the e 2 position the triglycerides of fat to the total palmitic acid content of the fat 1.03.

The fat is suitable for making margarine, culinary Fats, food concentrates, etc.

Example 3.

A mixture of melting point 27.3 ° C, which is 1 part Pork fat the top quality (melting point 37,500), 1 part pork fat of the first kind (with a melting point of 28.70C) and contains 3 parts of sunflower oil, is subjected to catalytic treatment analogous to Example 2, but in the presence of 0.12% nickel in the form of a nickel-copper catalyst with an activity of 30 ° C.

The hydro-esterified plastic edible fat has the following characteristics: Melting point 31.9 ° C; Hardness 250 g / cm; Content of trans isomers 28So, acid composition: polyunsaturated acids 0%; diunsaturated acids 8.9%; monounsaturated acids 68.4% o; Palmitic acid 12.1%; other saturated acids 9.6%.

The ratio of the concentration of palmitic acid in the 2-position the triglycerides of the fat to the total palmitic acid content of this fat 1.2.

Example 4.

A mixture with a melting point of 260C, which contains 1 part of pork fat, 1.5 parts of sunflower oil was processed as described in Example 2, but in the presence of a nickel catalyst on kieselguhr, which is made from nickel formate, deposited on this support. The activity of the catalyst was 32 ° C.

The plastic fat obtained had the following characteristics: a melting point 32.7 ° C; Hardness 210 g / cm; Content of trans- Isomers 36%; Fatty acid composition: diunsaturated acids 7.6%; monounsaturated acids 69.5%; Palmitic acid 9.9%; other Saturated acids 8.7, The degree of transesterification was (according to the information on distribution of palmitic acid) 1.3. In the starting mixture, the ratio of the concentration was the palmitic acid in the 2-position of the ionoglycerides, separated after the enzymatic Hydrolysis of the sample of the mixture, to the concentration of the palmitic acid in the triglycerides this sample 2.

Example 5.

A mixture containing 1 part pork fat, 1 part tree wool seed oil and 0.5 i'eiX contains sunflower oil, was processed analogously to Example 2. The obtained product had a melting point of 32.9 ° C. and a hardness of 250 g / cm on. From the intensity of the intramolecular and intermolecular transesterification can judge according to the information in Table 5, in which the content of each fatty acid in the triglycerides (TG) and in the 2-position of the monoglycerides (MG) in the starting mixture and is shown in the final product, the plastic fat.

Table 5 Fatty acid composition,% Example diunsaturated monounsaturated Stearic Palmitin Acids Acid Acid Acid MG / TG MG / TG MG / TG MG / TG mixture 41.6 / 35.8 = 1.2 23.1 / 31.2 = 0.7 2.2 / d, 2 = 0.3 36.1 / 24.8 = = 1.4 end product 14.9 / 13.6 = 1.1 54.2 / 53.2 = 1.0 6.2 / 8.6 = 0.7 26.0 / 24.6 = = 1.1 As can be seen from Table 5, in the process of hydro-esterification according to the invention, the MG / TG ratio is in close to 1, suggesting an intense transesterification of triglycerides among the above conditions described.

Example 6.

1 part beef tallow melting point 47,400 was mixed with 3 parts soybean oil mixed and the resulting mixture, which has a melting point of 38.50C, subjected to hydroesterification analogously to Example 1. The hydroesterified obtained Fat had an elevated melting point of 36.7 ° C. and a hardness of 270 g / cm. Simultaneously Thus, as can be seen from Table 6, the intensity of the transesterification was high enough.

Table 6 fatty acid composition,% Example 6 diunsaturated monounsaturated Stearic-Palmitic Acids Te Acids Acid Acid MG / TG MG / TG MG / TG MG / TG Starting mixture 54.5 / 44.5 = 1.2 32.0 / 26.8 = 1.2 3.1 / 10.9 = 9.3 / 17.8 = = 0.3 = 0.5 final product 15.9 / 15.5 = 1.0 56.8 / 55.4 = 1.0 10.4 / 11.0 = 16.9 / 18.1 = = 1.0 = 0.9 Example 7.

4 parts of pork fat with a melting point of 34 ° C. were mixed with 1 Part of beef tallow with a melting point of 46 ° C and 10 parts of sunflower oil. The melting point the starting mix of the fats and the oil was 33,400. The process is as in Example 1 described carried out. The hydro-esterification occurs over a period of time carried out that is sufficient for the manufacture of a product that has a melting point of 35.200, has a hardness of 370 g / cm. The fat contains 42.5% tranæ isomers; 8.3% diunsaturated fatty acids; 63.8% monounsaturated fatty acids and 27.9 /% saturated Fatty acids and is suitable for the production of culinary fats.

Example b.

A mixture of pork fat and sunflower oil obtained according to Example 1 one brings in an amount of 1 kg in a laboratory working periodically A hydrogenation reactor with a capacity of 2 liters, which is equipped with a turbo stirrer, an adjustable electric heater, provided and for a working pressure of 10 kp / cm2 definitely who is. The process is carried out at the temperature used in Example 1 and in Presence of the catalyst used in Example 1, but under a hydrogen pressure of 3 kp / cm2 carried out without barbotage of the gas. The process is as in Example 1 when reaching a refractive index of 1.4539 + 0.0001 (measured ended at a temperature of 600C).

The filtration, refining and deodorization of the final product is made carried out on periodically working laboratory-like systems from the plastic fat according to Example 1, a fat is obtained which has a melting point of 34.0 ° C and a hardness of 150 2 / cm. The low hardness with increased Melting point, which characterizes the product obtained, as well as its tallowy taste make this fat unsuitable for making margarine.

Example 9.

In a laboratory reactor (according to example 8th) treats a mixture of pork fat and obtained analogously to Example 1 Sunflower oil under a hydrogen pressure of 1 kp / cm2 at a temperature of 165 to 17,000 in the presence of 0.25% catalyst according to Example 1. As a result of decreased The temperature of the process becomes the desired value of the refractive index (at 600C) 1.4539 + 0.0001 only reached after 3.5 hours. The fat obtained does not have a specific smell of pork fat, nor does it have a pronounced one tallowy taste, contains 28S trans isomers, but exhibits a melting point from 32.5 ° C insufficient hardness (170 g / cm) and separates on storage a fraction that is liquid and high melting at room temperature.

In terms of technology, the fat meets the requirements for manufacturing requirements imposed by margarine are not.

Example 10.

In a laboratory-like reactor (according to Example 8) one leads the processing of a mixture obtained analogously to Example 1 at one temperature of 210 + 50C under a hydrogen pressure of 1 kp / cm2 in the presence of 0.15% nickel in the form of catalyst according to Example 1 through. Overall, one leads one behind the other 5 experiments with catalysts with an activity of 22 to 4600. In each Attempt is the process when reaching a refractive index (determined at ;, a temperature of 600C) of 1.4539 + 0.0001. The analysis results of the 5 samples of fat are listed in Table 7.

Table 7 Activity Refractive Melting Point Hardness of the transesterification des Cata- coefficient of fat, fat, degree of Pallysators, at 600C ° C g / cm mitic acid ° C (MG / TG) 22.4 1.4540 31.3 270 1 28.6 1.4538 31.7 260 1 30.0-1.4539 31.6 230 1.2 40.0 1.4538 33.4 170 1.5 46.4 1.4540 34.3 200 1.6 If all the fats obtained on the whole belong to the plastic edible fats, no specific smell of pork fat and show no tendency after reversion of this odor, deteriorates their technological properties (the ratio between the melting point and the hardness at the specified depth of hydrogenation) with the increasing activity of the Catalyst. This is particularly evident when looking for the Hydrogenation of vegetable oils typical catalysts used, their activity in ranges from 40 to 4600. The deterioration in technological property comes as an increase in sebum Taste, as a tendency towards separation in liquid and solid fraction and is aimed at lowering the degree of transesterification traced back. Thus, when a catalyst is used, miA is one activity from 22 to 300C the MG / TG coefficient, which is the distribution of palmitic acid between 2-position of the triglycerides and 1, 3-position of the triglycerides, 1 up to 1.2. Such a coefficient indicates a high degree of transesterification. With catalysts however, with an activity of 40 to 460C, the MG / TG coefficient is 1.5 to 1.6, i.e. is close to the coefficient mentioned for the starting mixture, which indicates a low degree of transesterification and consequently a low relative Transesterification rate suggests.

Thus, Examples b-10 show the procedure below Failure to comply with the technological conditions specified in the present invention such as pressure, temperature, activity of the catalyst. This non-compliance has to do with The result is that one arrives at a product that resembles the high-quality plastic Edible fats does not meet the requirements.

Claims (8)

PATENT CLAIMS: Process for processing animal fats into plastic edible fat by mixing them with vegetable oil and in the presence of a subsequent treatment with hydrogen / nickel catalyst that one melted edible animal fat with highly unsaturated edible vegetable oil mixed in a ratio that to 1 part of animal fat 0.4 to 9 parts of the vegetable oil mentioned are omitted, and the mixture obtained at one temperature from 180 to 220 ° C, a hydrogen overpressure of at most 2 kp / cm2 and an activity of the catalyst not hydrogenated above 350C, with it being under the stated conditions mainly for the selective hydrogenation of the polyunsaturated fatty acids of the animal Fat, for the selective hydrogenation of the highly unsaturated fatty acids in vegetable oil and there is partial transesterification of the animal fat with this oil. 2. The method of claim 1, d a d u r c h g e -k e n n z e i c It does not mean that a vegetable oil is used which contains at least 30% linoleic acid and Contains a maximum of 30% saturated fatty acids. 3. The method according to claim 1 and 2, d a d u r c h g e -k e n n z It is important to note that mixtures of the above oils are used. 4. The method according to claim 1-3, d a d u r c h g e -k e n n z e i c h n e t that a mixture of animal fats is used. 5. The method according to claim 1-4, d a d u r c h g e -k e n n z e i c h n e -t that one can produce fat with a melting point of 32 + 100 a starting mixture of the animal fat with the vegetable oil used, the one Has a melting point of not more than 300C. 6. The method according to claim 1-5, d a d u r c h g e -k e n n z e i c h n e t that for the production of fat with a melting point of 32 + 100, which contains at most 45S trans isomers of the monounsaturated fatty acids, a mixture used, which 1 part of animal fat with a melting point not exceeding 430C and contains 1 to 3 parts of the vegetable oil. 7. The method according to claim 1-6, d a d u r c h g e -k e n n z e i c h n e t that a catalyst with an activity of 22-300C is used. 8. The method according to claim 1-7, d a d u r c h g e -k e n n z e i c h n e t that the process is carried out at a pressure of 0.1 to 1.0 kgf / cm2.