RU2496860C1 - Method for sorption-alkali oil refinement - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: method involves adding bleaching clay to oil, holding and separating phases. Before adding sorbent, the oil is heated to temperature of 90-120°C. Holding is carried out at residual pressure of 0.2×10^-3 MPa for 35-50 minutes. The bleaching clay is pretreated with 25% alkali alcohol solution in amount of 5-25% of the weight of the bleaching clay with evaporation of alcohol by drying. The bleaching clay is used in amount of 1-3% of the weight of the oil. Phase separation is carried out by filtering.

EFFECT: invention reduces content of phospholipids, the weight ratio of chlorophylls and free fatty acids, reduces the colour value and acid number, wax remains in the oil and maximum output of triacylglycerides is provided.

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Description

The invention relates to the field of technology of fats and perfumes and cosmetics and can be used in the purification of vegetable oils with their subsequent use in cosmetics.

A classic method for refining vegetable oils is known, including the stages of filtration, hydration, neutralization, adsorption refining, deodorization, winterization [N. Harutyunyan. Fat processing technology / N. S. Harutyunyan, E. P. Kornena, A.I. Yanova et al. - 3rd ed. - M.: Pishchepromizdat, 1999. - 452 p.: Ill.]. This method allows you to clean vegetable oils from all related substances, leaving only triacylglycerides. For the use of vegetable oils in cosmetics, most of the accompanying substances turn out to be valuable biologically active substances, which does not make sense to remove from the oil, it is necessary to remove pigments, odorizing substances from the oils, partially remove free fatty acids. The disadvantage of this method is the formation of a large amount of waste and losses, containing related substances removed from the oil, as well as neutral fat. In addition, you need high-performance equipment, high energy consumption, as a result, the resulting raffinate is of low quality.

There is a technology of alkaline (physical) refining of oils when combining the process of removing free fatty acids, odorizing substances and oxidation products [N. Harutyunyan The technology of processing fat / N.S. Harutyunyan, E.P. Kornen, A.I. Yanova and others. - 3rd ed. - M.: Pishchepromizdat, 1999. - 452 p.: Ill.]. For the implementation of this method requires careful preparation of oils for distillation, including deep hydration and bleaching. If necessary, the hydration module is understaffed with a separate self-unloading separator and a drying unit for phosphatide emulsion. The disadvantage of this method is the high temperature of oil heating, as a result, the oils darken and the superheated oil loses its quality characteristics.

Closest to the claimed is a method of sorption purification of unrefined vegetable oils from impurities using sorbents [Lobanov VG, Karakay MS, Scherbakova EV Method for sorption purification of unrefined vegetable oils. RF patent 2209234]. The method includes introducing into the oil a suspension of bleached earth and part of the oil, thoroughly mixing for 28-32 minutes, holding at a temperature of 25-30 ° C for 70-72 hours and decantation. Moreover, the amount of bleaching earth used is proportional to the amount of volumetric sludge of the original oil and is 0.5-2% by weight of the processed oil. The invention allows to obtain a product with a reduced content of oxidation products, phospholipids, waxes and free fatty acids. A significant drawback of this method is the removal of wax substances, which are a valuable component of cosmetics, an increase in the amount of waste and loss of neutral fat.

The objective of the invention is to improve the quality of vegetable oils for use in cosmetics by combining the process of sorption and neutralization. The technical result is to reduce the content of phospholipids, the mass fraction of chlorophylls (i.e., reduce the color number), free fatty acids (i.e., reduce the acid number), but at the same time waxes are preserved in the oil and the maximum yield of triacylglycerides is ensured. The technical result is achieved by the fact that in the method of sorption-alkaline refining of oils, including the introduction of bleaching clay into the oil, aging, phase separation, the oil is heated to a temperature of 90-120 ° C before applying the sorbent, exposure is carried out at a residual pressure of 0.2 × 10 ^{- 3} MPa, over a period of 35-50 minutes, and bleaching clay, pre-treated with 25% alcohol solution of alkali in the amount of 5-25% to bleaching clay, followed by removal of the alcohol by drying, is used in an amount of 1-3% to oil, and separation is carried out by filter tion.

The mechanism of the sorption-alkaline refining process is fundamentally different from the generally accepted one in that the neutralization of free fatty acids occurs at the solid / liquid interface, which allows:

- reduce the content of free fatty acids and other undesirable related substances;

- reduce the loss of neutral fat and a valuable fraction of waxes;

- preserve the unique properties of the oil and ensure its high quality as an ingredient in the fat phase of cosmetics, which is achieved by reducing acid and color numbers.

As a sorbent in sorption-alkaline refining, bleaching clay is used in a concentration of 1-3% pre-treated with an alcoholic solution of sodium hydroxide in an amount of 5-25% with respect to the starting oil, followed by evaporation of ethyl alcohol by heating. The oil is treated with an adsorbent at a temperature of 90-95 ° C for 35-50 minutes under a vacuum of 0.2 × 10 ^-3 MPa with constant stirring. The sorbent was separated from the oil by mechanical filtration.

The most widespread and versatile applications in the oil and fat industry were found in the Filtrol series bentonite clays. The main brands of bleaching earths are intended for the adsorption purification of oils after the stages of refining, as well as for the adsorption of pigments, phospholipids from hydrated oils and hydrogenated fats, directed respectively to physical refining and (or) deodorization.

Calcium bentonites of the Filtrol series have an average oil absorption of 30%, a moisture content of 15-16% and a bulk density of 510-740 kg / m ³ .

The advantage of this method is the combination of alkaline neutralization processes with sorption, which allows you to adjust the quantitative composition of the components by changing the ratio of bleaching clay and alkali, vegetable oils: phospholipids, triacylglycerides, waxes, free fatty acids, chlorophyll.

The method is as follows: as a sorbent, bleaching clay is used in an amount of 1-3% to oil, which is treated with an alcoholic solution of sodium hydroxide with a concentration of 25% in an amount of 5-25% to the cultivated land, followed by evaporation of ethyl alcohol from the earth by evaporation. A sample of rapeseed oil (100 g) in a unit with a stirrer is heated to 90-95 ° C with stirring, sorbent is added in an amount of 1-3%, the reaction mass is kept for 35-50 minutes with constant stirring under vacuum 0.2 × 10 ^-3 MPa, then the sorbent is separated from the oil by filtration.

To confirm the claimed technical solutions are examples. The ratio of the mass fraction of the sorbent and the mass fraction of alkali to the starting oil used in the examples are presented in table 1.

Table 1
The ratio of the mass fractions of the sorbent and alkali in the experiments The main characteristics of the experiments Experience No. 1 Experience No. 2 Experience No. 3 Prototype Mass fraction of sorbent,% one 2 3 2 Mass fraction of alkali,% 5 fifteen 25 -

Experiment 1. The bleaching clay is treated with a 25% alcohol solution of sodium hydroxide, the mass fraction of which is 5% of the initial clay mass, followed by evaporation of ethyl alcohol by heating. A 100 g sample of unrefined rapeseed oil is heated in the apparatus with stirring to a temperature of 90-95 ° C, 1% adsorbent is added and the reaction mass is kept for 35-50 minutes under a vacuum of 0.2 × 10 ^-3 MPa and temperature control. Next, the sorbent is separated from the oil by filtration.

Experience 2. The bleaching clay is treated with a 25% alcohol solution of sodium hydroxide, the mass fraction of which is 15% of the initial mass of clay, followed by evaporation of ethyl alcohol by heating. A 100 g sample of unrefined rapeseed oil is heated at the installation with stirring to a temperature of 90-95 ° C, 2% adsorbent is added and the reaction mass is kept for 35-50 minutes under a vacuum of 0.2 × 10 ^-3 MPa and temperature control. Next, the sorbent is separated from the oil by filtration.

Experiment 3. The bleaching clay is treated with a 25% alcohol solution of sodium hydroxide, the mass fraction of which is 25% of the initial clay mass, followed by evaporation of ethyl alcohol by heating. A 100 g sample of unrefined rapeseed oil is heated at the installation with stirring to a temperature of 90-95 ° C, 3% adsorbent is added and the reaction mass is kept for 35-50 minutes under a vacuum of 0.2 × 10 ^-3 MPa and temperature control. Next, the sorbent is separated from the oil by filtration.

Experience 4. For comparison, we carry out the prototype method in parallel. A 100 g sample of unrefined rapeseed oil is heated at the installation with stirring to a temperature of 35 ° C, a 2% sorbent is added, which is a suspension of bleached earth and part of the oil, the reaction mass is kept for 28-32 minutes with constant stirring under vacuum and control temperature. Next, the sorbent is separated from the oil by filtration.

The final results of the experiments are presented in table 2.

table 2 The composition of rapeseed oil lipids Name of lipids Unrefined little Experience 1 Experience 2 Experience 3 Prototype Phospholipids,% in terms of stearoleolecithin 0.9 0.6 0.45 0.2 0.75 Chlorophyll mg / kg 20,0 7.2 4,5 5,0 14.0 Free fatty acids, mg KOH / g 1,5 1.3 0.7 0.5 1.4 Triacylglycerides,% 98.2 98.38 97.85 97.1 96.45 Wax% 1,2 1.15 1.06 0.98 0.21

Analyzing the results presented in table 2, we can conclude that the proposed technology can reduce the content of phospholipids, the mass fraction of chlorophylls (i.e., reduce the color number), free fatty acids, but waxes are preserved in the oil and the maximum yield of triacylglycerides is ensured .

Claims (1)

The method of sorption-alkaline refining of oils, including the introduction of bleaching clay into the oil, aging, phase separation, characterized in that before applying the sorbent, the oil is heated to a temperature of 90-120 ° C, exposure is carried out at a residual pressure of 0.2 × 10 ^-3 MPa the course of time is 35-50 minutes, and bleaching clay, pre-treated with 25% alcohol solution of alkali in an amount of 5-25% to bleaching clay, followed by removal of the alcohol by drying, is used in an amount of 1-3% to oil, and separation is carried out by filtration.