RU2195478C2 - Method of refining fats and oils of furry animals - Google Patents

Abstract

FIELD: fat-and-oil industry. SUBSTANCE: refining of fats and oils of furry animals for cosmetics, medicinal branches, and domestic chemistry is accomplished by hydration, neutralization, and water washing followed by additionally mixing with water at ratio between 5:1 and 20:1. Resulting mixture is affected for 3-5 min by ultrasound with frequency 15-22 kHz and intensity 0.2-0.5 W/sq.cm and then evacuated at 60-90 C and residual pressure 665-13300 Pa to essentially full removal of moisture. Method is characterized by complete absence of foreign smells and low values of peroxide number and weight portions of moisture and volatile components. EFFECT: increased stability and preserved consumer's properties. 2 tbl, 27 ex

Description

 The invention relates to the oil industry, specifically to the processing technology of fats and oils of fur animals, and in particular to a method of refining the latter.

 In the pharmaceutical industry, cosmetics and perfumes, as well as household chemicals, as a rule, fats and fatty components are used that are similar in composition to human skin fat. Fats of fur animals (mink, fox, polar fox, etc.), which are mixtures of complex composition - glycerides of higher saturated saturated and unsaturated acids, a complex of oil-soluble vitamins F, A, D, K, phospholipids, sterols, waxes, pigments and other useful substances are the most valuable biologically active components for these purposes. An assessment of the world practice of using fat from fur animals shows that these products are widely used in such developed countries as France, USA, Germany. Moreover, the last decade of work has intensified, as evidenced by the growing number of publications and patents.

 The main raw material for producing deodorized fats and oils of fur animals is the fatty waste of animal husbandry. In order to remove impurities and those related substances from fat that reduce the quality and technological properties of products, raw fat is subjected to refining or processing, which is a complex set of various physical and chemical processes, the use of which allows you to selectively affect the accompanying substances.

 The classical method of refining fats consists of several main stages: melting the fat fraction from the crude fat in order to separate from protein and mechanical impurities, hydration, alkaline neutralization, drying (deodorization).

 The process of hydration of fats is carried out in order to extract the accompanying substances: phosphatides, sterols, tocopherols, pesticides, wax, etc. from oils and fats by washing the latter with water. After the hydration process, the acid number of fats of fur animals decreases by 0.4-0.6 mg KOH / 1 g of product, the color intensity decreases significantly, and mechanical impurities are removed. Upon completion of the hydration process, the oil (fat) is subjected to alkaline neutralization in order to remove free fatty acids. Aqueous solutions of alkalis are used to neutralize, free acids in the form of alkali metal salts ("soaps") are removed from oil (fat). Then the fat (oil) is washed several times with water to remove residual saponified fatty acids and vacuum to remove moisture and an unpleasant odor of volatile fat components.

 There are many ways to evacuate fats and oils of fur animals. Evacuation is often carried out in film evaporators at a residual pressure of 1 mm Hg. (133 Pa) [French Patent 2629468 MKI C 11 B 1/00, 3/00, claimed. 04/01/88, publ. 10/06/89, РЖ Chemistry 10, 10Р 2044 П, 1990; Graig A., Casimir D. Int. Conf. Fats, Auckland, 12-17 Febr., 1989. - [Wellington], 1989 - p. 27 (RJ Chemistry 1, 1P 1330, 1990); Sioberg P. Int. Conf. Fats, Auckland, 12-17 Febr., 1989. - [Wellington], 1989 - p. 28 (РЖ Chemistry 1, 1P 1333, 1990); patent of Czechoslovakia, cl. 23a 1 (C 11 B 1/12), 153133, claimed 05/20/71, publ. 05/15/74. (RJ Chemistry 7, 7P 613 P, 1976)]. Multistage low-temperature distillation has proven itself quite well, which makes it possible to isolate volatile impurities from oils that determine its taste and smell. To do this, sequential evaporation of the oil is carried out in special conical shaped devices providing a high degree of turbulence, which makes it possible to isolate volatile impurities without their partial destruction [Graig A., Casimir D. Int. Conf. Fats, Auckland, 12-17 Febr., 1989. - [Wellington], 1989 - p. 27 (RJ Chemistry 1, 1P 1330, 1990)]. It is also known that sufficiently effective deodorization of oil is achieved by contact with steam in a thin layer in the column [Sioberg P. Int. Conf. Fats, Auckland, 12-17 Febr., 1989. - [Wellington], 1989 - p. 28 (RJ Chemistry 1, 1P 1333, 1990)].

 The main disadvantage of the above refining methods is the increase in the peroxide number of oils and fats, which leads to a deterioration in product quality before the expiration of the guaranteed storage period.

 In our opinion, the most promising refining method is the method by which before distillation, oils and fats are treated in a constant magnetic field with magnetic induction of 0.8-1.2 T at a linear flow rate in the field of 1.5-2.0 m / s [Patent of Russia 2100427 (РЖ Chemistry 12, 12Р 1233П, 1998)]. The method provides for deaeration, heating, distillation and cooling of the processed mass. Unfortunately, this method is effective in deodorizing edible oils and fats that do not have a pronounced specific odor. Oils and fats of fur animals, as a rule, even after deodorization by known methods retain a rather sharp specific smell that is difficult to mask even by perfumes, which creates significant difficulties in the further use of oils and fats of fur animals in household products, cosmetics and perfumery.

Thus, the refining methods discussed above in relation to oils and fats of fur animals have the following significant disadvantages:
- preservation of a rather sharp specific smell;
- an increase in the peroxide value, which leads to a deterioration in the quality of oil and fat during storage.

A known method of refining fats of fur animals [A.S. 806751, USSR MKI S11 3/16, BI, 1981, 7, p. 119] by treating them with steam, ultrasound and vacuum, characterized in that in order to reduce fat loss, the latter is heated to 140-150 ^o C, mixed with steam in a ratio of 10-20: 1, using superheated steam with the same temperature; the resulting mixture is successively passed through a sound field (ultrasound) with a frequency of 10-12 kHz and an intensity of 0.2-0.5 W / cm ² for 1-2 minutes, then a pulsating jet is fed into a vacuum space, the residual pressure of which is maintained at level 3-10 mmHg (399-1330 Pa) (prototype method). The main disadvantage of this method is the high process temperature of 140-150 ^o With, accelerating the oxidation of fats. Despite the low loss of fat or oil of fur animals during the refining process, the quality of the products obtained does not meet the requirements of the technical conditions (Table 1). It is known that the refining process at a temperature of more than 100 ^o With leads to a sharp increase in the peroxide value. In addition, the authors of the work [Pat. France 2629468 С 11 В 1/00, 3/00 of 04/01/08] consider that the valuable properties of fats of fur animals containing fatty acids (linoleic, linolenic, arachidonic), which are part of vitamin F, are lost when the latter is heated above 100 ^o C. The most optimal process at 85-95 ^o C. Moreover, the resulting oil (fat) has an unpleasant sharp, not characteristic for oils of fur animals, smell.

 In order to eliminate the disadvantages of the known methods of processing oils and fats of fur animals used in perfumes, cosmetics, household products, the task was to develop an effective method for refining oils and fats of fur animals.

The problem is solved in that the fats and oils of fur animals after the main stages of refining, i.e. hydration, alkaline neutralization, washing with water by known methods, are additionally mixed with water in a ratio of 5: 1 to 20: 1, the resulting mixture is sequentially exposed to ultrasound with a frequency of 15-22 kHz and an intensity of 0.2-0.5 W / cm ² for 3-5 minutes, then vacuum at a temperature of 60-90 ^o C and a residual pressure of 665-13300 Pa to almost complete removal of moisture. The resulting fat or oil meets the requirements of technical specifications TU 9154-007-23333879-96 (see table. 1). The quality indicators of mink oil obtained by the prototype method are also shown there.

 The high efficiency of the proposed refining method is confirmed by the following examples.

Example 1. 100 g of mink oil after hydration, alkaline neutralization, washing with water by known methods is additionally mixed with water in the ratio oil: water = 5: 1. The resulting mixture is affected by ultrasound with a frequency of 15 kHz and an intensity of 0.2 W / cm ² for 3 minutes. The resulting emulsion is evacuated at a temperature of 60 ^{° C.} and a residual pressure of 665 Pa until the moisture is almost completely removed. The mink oil sample obtained in quantitative yield complies with the requirements of TU 9154-007-23333879-96. The peroxide value is 0.028. The moisture and volatiles content is 0.02%.

 Example 2. Analogously to example 1, a mink oil sample is refined.

Experiment Conditions:
oil to water ratio 5: 1
ultrasound frequency - 22 kHz
ultrasound intensity - 0.5 W / cm ²
processing time - 3 min
vacuum temperature - 90 ^o C
residual pressure - 13300 Pa
The peroxide value of the obtained oil sample is 0.028. The moisture and volatiles content is 0.02%.

 Example 3. Analogously to example 1, a mink oil sample is refined.

Experiment Conditions:
oil to water ratio 10: 1
ultrasound frequency - 22 kHz
ultrasound intensity - 0.5 W / cm ²
processing time - 5 min
vacuum temperature - 90 ^o C
residual pressure - 13300 Pa
The peroxide value of the obtained oil sample is 0.028. The moisture and volatiles content is not more than 0.02%.

 Example 4. Analogously to example 1, a mink oil sample is refined.

Experiment Conditions:
oil to water ratio 10: 1
ultrasound frequency - 15 kHz
ultrasound intensity - 0.5 W / cm ²
processing time - 5 min
vacuum temperature - 70 ^o C
residual pressure - 665 Pa
The peroxide value of the obtained sample is 0.028. The moisture and volatile substances content is not more than 0.02%.

 Example 5. Analogously to example 1, a mink oil sample is refined.

Experiment Conditions:
oil to water ratio 20: 1
ultrasound frequency - 15 kHz
ultrasound intensity - 0.5 W / cm ²
processing time - 5 min
vacuum temperature - 70 ^o C
residual pressure - 665 Pa
The peroxide value of the obtained oil sample is 0.028. The moisture and volatiles content is not more than 0.02%.

 Example 6. Analogously to example 1, a mink oil sample is refined.

Experiment Conditions:
oil to water ratio 20: 1
ultrasound frequency - 22 kHz
ultrasound intensity - 0.2 W / cm ²
processing time - 3 min
vacuum temperature - 90 ^o C
residual pressure - 13300 Pa
The peroxide value of the obtained oil sample is 0.028. The moisture and volatiles content is not more than 0.02%.

 Examples 7-12. Similar to examples 1-6, refined samples of fox fat are refined.

 The peroxide values of the obtained samples do not exceed 0.028; residual moisture and volatility not more than 0.02%.

 Examples 13-18. Similar to examples 1-6, refined samples of Arctic fox fat.

 The peroxide values of the obtained samples do not exceed 0.028; residual moisture and volatility not more than 0.02%.

 Examples 19-24. Similarly to examples 1-6, mink fat samples are refined.

 Example 25. Analogously to example 1, a mink oil sample is refined.

Experiment Conditions:
oil to water ratio 1: 1
ultrasound frequency - 15 kHz
ultrasound intensity - 0.5 W / cm ²
processing time - 5 min
vacuum temperature - 120 ^o C
residual pressure - 13300 Pa
The peroxide value of the obtained sample is 0.042, which in accordance with GOST 8285-74 means: "the sample is fresh, not subject to storage."

 Example 26. Analogously to example 1, a mink oil sample is refined.

Experiment Conditions:
oil to water ratio 1: 2
ultrasound frequency - 22 kHz
ultrasound intensity - 0.8 W / cm ²
processing time - 6 min
vacuum temperature - 100 ^o C
residual pressure - 665 Pa
The obtained sample has the following main characteristics: peroxide value 0.036, humidity 0.12, which does not meet the requirements of technical conditions (see tables 1 and 2).

 Example 27. Analogously to example 1, a mink oil sample is refined.

Experiment Conditions:
oil to water ratio 25: 1
ultrasound frequency - 22 kHz
ultrasound intensity - 0.15 W / cm ²
processing time - 10 min
vacuum temperature - 60 ^o C
residual pressure - 665 Pa
The resulting sample has a sharp odor that is not characteristic of mink oil, which does not meet the technical requirements.

 All samples of fats and oils of fur animals, obtained in accordance with examples 1-24, meet the requirements of technical conditions (see table 1).

 The conditions for refining fats and oils of fur animals by the proposed method are optimal, because provide samples of oils and fats of the required quality.

 The use of smaller or larger amounts of water in relation to oil or fat, a decrease or increase in the time of ultrasonic treatment, an increase or decrease in its intensity, a change in the vacuum regimes is not economically feasible, and, most importantly, does not provide samples of deodorized oils and fats of fur animals of the required quality ( examples 25-27).

The above examples confirm the fact that the processing of the wet technological mass of fats and oils of fur animals with ultrasound with a frequency of 15-22 kHz and an intensity of 0.2-0.5 W / cm ² for 3-5 minutes before the vacuum process allows to achieve a significantly high degree refining in comparison with the known methods, as evidenced by test report 2788 of 12/02/99, the Testing Laboratory Center of the State Committee for Sanitary and Epidemiological Surveillance of the Republic of Tatarstan (copy attached).

 The use of ultrasonic treatment of mixtures of oils and fats with water in the stated proportions led to an unexpected (non-obvious) result: the removal of impurities that give a sharp nonspecific odor, a sharp decrease in peroxide value and moisture, and thereby increase the stability of fats and oils of fur animals.

Thus, in comparison with the known refining methods, the proposed method has significant advantages, namely, it allows to obtain fats and oils of fur animals
- almost odorless;
- with low values of peroxide values and humidity, which helps to maintain high quality products for a long time.

 Industrial applicability. The claimed method of deodorizing fats and oils of fur animals is planned to be applied in the production of oils and fats of fur animals, in particular, in the conditions of the pilot production of IOFH im. A.E. Arbuzov KSC RAS, having the necessary equipment and production facilities.

Claims (1)

The method of refining fats and oils of fur animals by moistening, sonication and vacuum, characterized in that the fats and oils after hydration and neutralization are mixed with water in a ratio of 5: 1 to 20: 1, respectively, and the resulting mixture is sonicated with a frequency 15-22 kHz and an intensity of 0.2-0.5 W / cm ² for 3-5 minutes, then vacuum at a temperature of 60-90 ^o C and a residual pressure of 665-13300 Pa to completely remove moisture.

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