RU2798574C1 - Method for producing a multifunctional additive for motor gasoline - Google Patents

Abstract

FIELD: fuel additives.

SUBSTANCE: methods for producing multifunctional additives for motor gasoline, which includes three stages: the interaction of diethanolamine and vegetable oils at a molar ratio of reagents from 3.0 to 1.0 to 3.6 to 1.0, a temperature of 120 to 180 C; interaction of diethanolamine and fatty acids at a molar ratio of reagents from 0.9:1.0 to 1.1:1.0, temperature from 30 to 70 C; and mixing the reaction products obtained in stages 1 and 2, in a mass ratio of 1.0:1.0 to 20.0:1.0 at a temperature of 30 to 70 C. The invention relates to methods for producing multifunctional additives. A method is also proposed that includes carrying out two stages in the course of joint synthesis in one apparatus: the interaction of diethanolamine and vegetable oils at a molar ratio of reagents from 3.0:1.0 to 3.6:1.0, a temperature of 120 to 180° C; and the interaction of an excess amount of diethanolamine, which did not react in the first stage, and fatty acids added in the second stage, at a molar ratio of reagents from 0.9:1.0 to 1.1:1.0, a temperature of 30 to 70° C.

EFFECT: obtaining a multifunctional additive that exhibits anti-corrosion properties and possesses detergent and anti-friction efficiency.

12 cl, 5 tbl, 15 ex

Description

The invention relates to methods for producing multifunctional additives for motor gasoline and makes it possible to obtain an additive with anti-corrosion, anti-friction and detergent properties.

A known method for producing a fuel additive includes the step of heating a mixture of mixed fatty acid esters, monohydroxylamines, dihydroxyalkylamines or a mixture thereof and an ester with a low molecular weight, while the ratio of amine to ester is from 10 to 1 (US application No. 20020134007 "Method for improving Properties of Low-Temperature Solutions of Gasoline Friction Modifiers). The disadvantage of the invention is the lack of anti-corrosion and detergent properties of the additive obtained by the method.

A known method for producing a composition, including the interaction of a fatty acid with diethanolamine, in which the reaction is carried out with a molar excess of diethanolamine relative to the fatty acid and at a pressure below 50,000 Pa, at a temperature of from 120 to 160 ° C (US application No. 20200332207 A1 "Composition used as a friction modifier). The composition obtained in accordance with this method has insufficient anti-friction properties, manifested in the ability to improve the fuel efficiency of the internal combustion engine, does not improve the cleaning properties of motor gasoline in relation to intake valves, and is characterized by the absence of the claimed and confirmed anti-corrosion effect on the properties of fuels.

A known method for producing fatty acid salts, including mixing a mixture of oleic and palmitic acids (70:30), adding monoethanolamine at a temperature of 80-90, adding synthetic fatty acids (RF Patent No. 2037503 "Activator-dispersant of rubber compounds"). The disadvantage of this method is the significant content of free fatty acids in the product, which, not completely burning out during operation of a gasoline internal combustion engine, can interact with engine oil and additives contained in it, leading to a significant deterioration in the lubricity of the oil.

A known method for producing additives (RF Patent No. 2235119 "Detergent additive for motor gasoline"), according to which distilled tall oil or a tall oil fatty acid fraction with diethanolamine, taken in a molar ratio of acid: amine, equal to 3:1, is mixed in a mixer with external heating and the solvent is alkylbenzenes in an amount of 0.5 to 1.5 times the weight of tall oil. Next, an azeotropic distillation of the resulting reaction water is carried out for 1-4 hours. After completion of the reaction, the solvent is partially distilled off. Nitrogen purge through the reaction mixture can be used to accelerate the distillation of the solvent. The disadvantages of this method are the manifestation of insufficient detergent and anti-corrosion properties of the additive, as well as the absence of the claimed anti-friction action.

The technical result to which the created invention is directed, consists in a method for obtaining a multifunctional additive for motor gasoline from available raw materials, which exhibits anti-corrosion properties and has detergent and anti-friction efficiency.

The technical result is achieved by the fact that the proposed method for producing a multifunctional additive to motor gasoline consists of three stages: the interaction of diethanolamine and vegetable oils at a molar ratio of reagents from 3.0 to 1.0 to 3.6 to 1.0, a temperature of 120 to 180°C; interaction of diethanolamine and fatty acids at a molar ratio of reagents from 0.9 to 1.0 to 1.1 to 1.0, temperature from 30 to 70°C; mixing the reaction products obtained in stages 1 and 2, in a mass ratio of 1.0 to 1.0 to 20.0 to 1.0 at a temperature of 30 to 70°C.

The technical result is also achieved by the fact that the proposed method for obtaining a multifunctional additive to motor gasolines consists of two stages in the course of joint synthesis in one apparatus: the interaction of diethanolamine and vegetable oils at a molar ratio of reagents from 3.0 to 1.0 to 3.6 to 1.0, temperature from 120 to 180°C, interaction of an excess amount of diethanolamine, which did not react in the first stage, and fatty acids added in the second stage, at a molar ratio of reagents from 0.9 to 1.0 to 1.1 to 1.0, temperature from 30 to 70°C.

When diethanolamine and vegetable oil interact, diethanolamides of fatty acids contained in vegetable oil are predominantly formed. When diethanolamine and fatty acids interact, ammonium salts of diethanolamine and fatty acids are formed.

In the course of research, it was found that the use of the method in accordance with the present invention allows to obtain a multifunctional additive consisting of a synergistic composition of two derivatives of fatty acids: amides and ammonium salts. Amides are an effective antifriction component, which, along with the improvement of antifriction properties, has a positive effect on the detergency and anticorrosion ability of the fuel, however, in working concentrations from 50 mg / kg to 500 mg / kg, the amide is able to reduce corrosion to 1 point (traces) according to the modified ASTM D665 method (GOST 19199). At the same time, ammonium salts of fatty acids show themselves as an effective additive with anti-corrosion properties, whose working concentration to achieve a score of 0 points (no corrosion) does not exceed 50 mg/kg. At the same time, due to the strong surface-active properties with a significant excess of ammonium salts above their optimal application concentration (not higher than 50 mg / kg), an increase in the emulsifying ability of gasolines is possible (the formation of stable emulsions when alloyed gasoline interacts with water) and the manifestation of corrosion of the steel rod after due to a significant increase in the conductivity of the aquatic environment due to the high concentration of ammonium ions of diethanolamine, which causes the presence of an upper limit on the concentration of involvement of these substances. Considering the stated limitation, it is important that there is a synergistic effect between the two components of the additive obtained in accordance with the method of the present invention: amides provide most of the detergent and anti-friction action of the additive, while at the same time possessing some anti-corrosion properties, which makes it possible to reduce the consumption of anti-corrosion additive, which improves protective properties of gasolines up to the level of 0 points (no corrosion) and at the same time positively affects the washing and antifriction properties.

At the same time, for the manifestation of this synergistic effect, it is extremely important to carry out the production process under the conditions in accordance with the present invention, since they are most conducive to obtaining a multifunctional additive with a given level of functional properties.

The reaction between diethanolamine and vegetable oil according to the present invention is carried out at a molar ratio of reagents from 3.0 : 1.0 to 3.6 : 1.0, therefore, fatty acid diethanolamides are predominantly formed with a minimum residual amount of fatty acid glycerides. The reaction is carried out at a temperature of from 120 to 180°C with continuous stirring. Purification of the target product from unreacted raw materials, excess diethanolamine and by-products is not carried out, therefore, in addition to diethanolamides of fatty acids, the product of the interaction of diethanolamine and vegetable oil contains glycerol, unreacted diethanolamine, and may also contain tri-, di- and monoglycerides of fatty acids. The reaction between diethanolamine and vegetable oil according to the present invention can be introduced in catalytic and non-catalytic versions. The use of a catalyst accelerates the course of the reaction, which is expressed in the possibility of reducing the duration and temperature of the reaction while maintaining a high level of functional properties. As a catalyst, alkaline compounds are used, mainly hydroxides and carbonates of alkali and alkaline earth metals, such as sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium bicarbonate, potassium bicarbonate, calcium bicarbonate, in a mass fraction of 0.01 to 0.5%.

The reaction between diethanolamine and fatty acid according to the present invention is carried out at a molar ratio of reagents from 0.9: 1.0 to 1.1: 1.0 with the formation of the target product - ammonium salt of diethanolamine and fatty acid. The reaction is carried out at a temperature of 30 to 70°C with continuous stirring. Purification of the target product from unreacted raw materials, by-products and solvent is not carried out.

The third stage of the method according to the present invention is the preparation of a multifunctional additive from the reaction products of diethanolamine with vegetable oil and diethanolamine with fatty acid. The additive is prepared by mixing the components in the required proportions at a temperature of 30 to 70°C with continuous stirring.

The method according to the present invention can be carried out in a single technological process in which the stage of synthesizing the anti-corrosion component is combined with the stage of mixing the components so that the first stage is the reaction between diethanolamine and vegetable oil, proceeding under the conditions according to the present invention, with the exception that the ratio of reagents can be changed in order to introduce an excess of diethanolamine into the reaction mass, which, after the reaction between diethanolamine and vegetable oil, will remain unreacted and will be sent as part of the entire product of the first stage to the second stage. The second and final step of the process is the reaction between diethanolamine and a fatty acid according to the present invention, except that the diethanolamine used is the excess amount taken from the first step and remaining after the reaction. The reaction mixture after the second stage of this process is equivalent in its physicochemical, operational and functional properties to an additive of a similar composition obtained by mixing the solvent with the reaction product of diethanolamine and vegetable oil and the product of the interaction of diethanolamine and fatty acid, obtained during two separate synthesis processes.

Preferably, the interaction reaction of diethanolamine and vegetable oil is carried out from 2 to 10 hours at a pressure of 1 to 5 atm, the reaction of the interaction of diethanolamine and fatty acid is carried out from 0.5 to 2.0 hours, and the mixing of the reaction products is from 0.5 to 2 .0 hours.

Preferably, rapeseed, sunflower, olive, soybean oils, as well as mixtures thereof, are used as vegetable oil.

Preferably, tall oil fatty acids (FTA), vegetable oil fatty acids (FFA), oleic acid (OK) are used as fatty acids.

To improve mass transfer processes, the reaction of interaction between diethanolamine and fatty acid is carried out in a solvent, the proportion of which is from 10 to 78% of the total mass of the mixture.

Preferably, at the final stage, the solvent is additionally added in such a way that its mass fraction is 10 - 78%.

Preferably, various hydrocarbon fractions are used as a solvent, boiling off in the temperature ranges corresponding to gasoline from 30 to 200°C and kerosene from 120 to 300°C, including commercial fuels; narrow cuts used as solvents and for other purposes, such as Nefras, aromatic solvent, polyalkylbenzene solvent (PAB), low viscosity hydrocarbon base for drilling fluids (RMBM); individual hydrocarbons and mixed fractions thereof, such as toluene, p-xylene, o-xylene, m-xylene, a mixture of xylenes, cumene, ethylbenzene; other components and fractions similar in their physical and chemical properties and composition. In addition to hydrocarbon fractions, various higher alcohols and their mixed fractions can be used as a solvent, such as n-butanol, iso-butanol, iso-pentanol, alcohol-ether concentrate, 2-ethylhexanol, butyl alcohol distillation residue (KORBS).

Preferably, at the final stage, an antioxidant and a demulsifier are added to the mixture in such a way that the mass fraction of each component does not exceed 1%.

As demulsifiers, industrially produced demulsifiers used in oil dehydration processes and which are non-ionic surfactants based on block copolymers of propylene and ethylene oxides, their derivatives with amines, polybasic alcohols, phenol-formaldehyde and alkylphenol-formaldehyde resins can be used.

Preferably, commercially available antioxidants based on hindered alkyl-substituted phenols or alkyl-substituted aromatic amines, including Mannich bases, are used as the antioxidant.

The implementation of the invention is illustrated by the following examples.

Example 1

The first stage of the process is carried out by adding 200.00 g of sunflower oil and 71.27 g of diethanolamine (molar ratio 1 to 3) to the first three-necked round-bottom flask of 500 ml, equipped with a mechanical stirrer, reflux condenser and thermometer, heating the contents of the flask to 150 ° C and exposure at a given temperature for 5 hours. After that, the heating is turned off and the flask is allowed to cool to room temperature. Purification of the reaction mass from unreacted raw materials, excess diethanolamine and by-products is not carried out, therefore, the entire resulting product is the target.

The second step of the process is carried out by adding to a second 500 ml three-necked round-bottom flask equipped with a mechanical stirrer, reflux condenser and thermometer, 100.0 g of vegetable oil fatty acids, 36.56 g of diethanolamine and 136.56 g of toluene (molar ratio of fatty acids to DEA 1 to 1, the proportion of the solvent is 50% by weight of the mixture), heating the contents of the flask to 50°C and holding at a given temperature for 1 hour with constant stirring. After that, the heating is turned off and the flask is allowed to cool to room temperature. Purification of the target product from unreacted raw materials, by-products and solvent is not carried out.

The third stage of the process is carried out by adding to a third three-necked 500 ml round bottom flask equipped with a mechanical stirrer, reflux condenser and thermometer, 136.25 g of the reaction product of diethanolamine and vegetable oil obtained in stage 1, 27.50 g of the reaction product of diethanolamine and fatty acid obtained in stage 2, 86.25 g of toluene: heating the contents of the flask to 50°C and holding at a given temperature for 1 hour with constant stirring. After that, the heating is turned off and the flask is allowed to cool to room temperature. The resulting mixture is the target product - a multifunctional additive obtained in accordance with the method according to this invention.

Example 2

The production method according to example 2 is similar to the method according to example 1, but vegetable oils, fatty acids and solvents indicated in table 1 were used as raw materials, and the conditions for carrying out the process steps correspond to table 2. In this case, the method according to example 2 was carried out in a metal autoclave , equipped with a mechanical stirrer and an inert gas (nitrogen) supply line to maintain elevated pressure. All three stages were carried out in one apparatus sequentially with the unloading of the products of the previous stage and cleaning of the reactor.

Example 3

The production method according to example 3 is similar to the method according to example 1, but vegetable oils, fatty acids and solvents indicated in table 1 were used as raw materials, and the conditions for carrying out the process steps correspond to table 2. In this case, the method according to example 2 was implemented in a metal reactor , with a volume of 200 l, equipped with a system for mixing and heating the contents of the reactor, as well as windows for loading raw materials. In addition to the components described in example 1, the method according to example 3 uses a NaOH catalyst in an amount of 0.15 wt. %, which is loaded into the reactor in the first stage, as well as a demulsifier and an antioxidant, which are added to the mixture in the third stage in an amount of 0.1 % wt. every. All three stages were carried out in one apparatus sequentially with the unloading of the products of the previous stage and cleaning of the reactor.

Example 4

The production method according to example 4 is similar to the method according to example 2, but vegetable oils, fatty acids and solvents indicated in table 1 were used as raw materials, and the conditions for carrying out the process stages correspond to table 2. Also in example 4, Na2CO3 catalyst is used in an amount of 0 .2% of the mass, which is loaded into the reactor in the first stage

Example 5

The production method according to example 5 is similar to the method according to example 1, but vegetable oils, fatty acids and solvents indicated in table 1 were used as raw materials, and the conditions for carrying out the process stages correspond to table 2. At the third stage, a demulsifier and an antioxidant were added, in an amount of 0 .5% wt. every.

Example 6

The first stage of the process is carried out by adding 129.02 g of rapeseed oil and 50.66 g of diethanolamine (molar ratio 1 to 3, as well as an excess of DEA to carry out the reaction on stage 2), heating the contents of the flask to 120°C and holding at a given temperature for 10 hours. After that, the heating is turned off and the flask is allowed to cool to a temperature of 50°C.

The second stage of the process is carried out by adding at a constant temperature of 50°C to the same flask 12.81 g of fatty acids of tall oil, 57.25 of kerosene, and also an antioxidant in the amount of 0.1% of the mass. After that, the heating is turned off and the flask is allowed to cool to room temperature. The resulting mixture is the target product - a multifunctional additive obtained in accordance with the method according to this invention

Examples 7-15.

The preparation method according to examples 7-15 is similar to the method according to example 6, but vegetable oils, fatty acids and solvents indicated in table 1 were used as raw materials, and the conditions for carrying out the process steps correspond to table 2.

The methods of examples 7 and 8 were carried out in a metal autoclave equipped with a mechanical stirrer and an inert gas (nitrogen) supply line to maintain an elevated pressure. All three stages were carried out in one apparatus sequentially with the unloading of the products of the previous stage and cleaning of the reactor.

The method according to example 13 was implemented in a metal reactor with a volume of 200 liters, equipped with a system for mixing and heating the contents of the reactor, as well as windows for loading raw materials. All three stages were carried out in one apparatus sequentially with the unloading of the products of the previous stage without cleaning the reactor.

The method according to example 11 was implemented in a metal reactor with a volume of 10 m ³ equipped with a mixing and heating system for the contents of the reactor, as well as nozzles for loading raw materials and unloading products. All three stages were carried out in one apparatus sequentially with the unloading of the products of the previous stage without cleaning the reactor.

In addition to the components described in example 4, the methods of examples 7-15 can use a catalyst added in the first stage of the process, and a demulsifier and antioxidant added in the second stage of the process. The amount and type of catalyst, demulsifier and antioxidant are in accordance with Table 2.

Table 1 - The composition of the components for the preparation of a multifunctional additive. Example number Oil type LCD type Solvent type 1 Sunflower oil JKRM Toluene 2 Rapeseed oil JKRM IWBR 3 Sunflower oil ZhKTM SEC 4 Soybean oil ZhKTM Kerosene 5 Rapeseed oil OK A PUB 6 Rapeseed oil ZhKTM Kerosene 7 Soybean oil ZhKTM Kerosene 8 Rapeseed oil OK A PUB 9 Rapeseed oil OK AI-95 10 Sunflower oil JKRM Kerosene eleven Sunflower oil JKRM KORBS 12 Olive oil ZhKTM IWBR 13 Sunflower oil OK M-xylene 14 Rapeseed oil JKRM n-butanol 15 Soybean oil ZhKTM SEC

Table 2 - Conditions for obtaining a multifunctional additive Example number 1 2 3 4 5 6 7 8 9 10 eleven 12 13 14 15 The ratio of the product of the interaction of diethanolamine (DEA) and vegetable oils to the product of the interaction of diethanolamine (DEA) and fatty acids in the final additive 4.95 1.50 5.77 1.00 20.00 7.71 1.76 4.55 20.00 7.75 1.00 2.20 5.12 3.35 6.64 Stage 1 - Interaction of diethanolamine (DEA) and vegetable oils Molar ratio of DEA to oil 3.0 3.3 3.0 3.6 3.0 3.0 3.3 3.0 3.0 3.0 3.6 3.0 3.0 3.0 3.0 Temperature, °C 150 170 130 180 120 150 120 150 170 180 140 150 140 150 160 Pressure, MPa 1.0 4.0 2.0 5.0 1.0 1.0 1.0 1.0 4.3 5.0 1.0 1.0 1.0 1.0 3.0 Duration, h 5.0 4.0 5.0 2.0 10.0 5.0 10.0 5.0 4.0 2.0 3.0 4.5 5.0 5.0 5.0 Type of catalyst and mass fraction of its input - - NaOH
0.15 _{Na2CO3 _}
0.2 - - KOH
0.5 - - _{Ca2CO3 _}
0.1 K ₂ CO ₃
0.3 - - Ca(OH) ₂
0.01 - Stage 2 - Interaction of diethanolamine (DEA) and fatty acids (for examples 6-13, mixing with the product of the first stage occurs simultaneously) Molar ratio of DEA to FA 1.0 1.0 1.1 0.9 1.0 1.0 1.0 1.0 1.1 1.0 0.9 1.0 1.0 1.0 1.0 Temperature, °C 50 40 70 thirty 50 50 thirty 50 50 70 50 60 35 55 60 Duration, h 1.0 1.5 0.5 2.0 1.0 1.0 2.0 1.0 1.0 0.5 1.5 1.0 2.0 1.0 1.0 Mass fraction of solvent, % 50.0 78.0 10.0 50.0 16.7 22.9 20.0 49.5 14.9 22.5 10.0 78.0 31.8 47.9 39.6 Stage 3 - Mixing the interaction products obtained in stages 1 and 2 Temperature, °C 50 70 thirty thirty 50 - - - - - - - - - - Duration, h 1.0 0.5 2.0 2.0 1.0 - - - - - - - - - - Mass fraction of solvent, % 34.5 0.0 78.0 10.0 36.0 - - - - - - - - - - Auxiliary components Mass fraction of demulsifier, % 0.0 0.0 0.1 0.0 0.5 0.0 0.0 0.5 0.1 0.0 1 0.0 0.2 0.0 0.3 Mass fraction of antioxidant, % 0.0 0.0 0.1 0.0 0.5 0.1 0.0 0.0 0.0 0.5 1 0.0 0.0 0.1 0.1 ^{1 As a demulsifier in examples 3,9 and 15, a demulsifier based on ethoxylated and hydroxypropylated amine was used, in examples 5, 8, 11,13 - based on ethoxylated and hydroxypropylated polybasic alcohol
2 As an antioxidant in examples 3, 5, 11, 14, an antioxidant based on 2,6-ditretbutyl-4-methylphenol was used, in examples 6, 10, 15 - based on 2,2-methylene-bis (4-methyl-6 -tertbutylphenol)a}

The additives obtained by the methods of examples 1-15 were used to prepare prototypes of the fuel composition of motor gasoline by introducing the additive into gasoline at a given concentration, presented in table 3, and stirring until complete dissolution. Samples of the motor gasoline fuel composition prepared in this way were tested for the presence of a functional anti-corrosion and anti-friction action, as well as the absence of a negative effect on the properties of motor gasoline in terms of the most important indicators: emulsification and the amount of resins. The test results are presented in table 3.

The anticorrosion properties of prototypes of the fuel composition of motor gasoline were evaluated according to the modified method ASTM D665 (GOST 19199), which is generally accepted in world practice. This method gives a qualitative assessment of the protective properties of fuels, and also allows you to establish the dependence of the anti-corrosion effectiveness of additives on their concentration in the fuel. The essence of the method lies in the qualitative assessment of the corrosion damage of a polished steel rod immersed during the test in a water-fuel emulsion. Each rod is given a score in points, according to which the maximum degree of corrosion (more than 5% of the rod surface is covered with corrosion products) is estimated at 3 points (severe corrosion); the surface of the rod, free from traces of corrosion (clean rod), is estimated at 0 points (absence); intermediate states are assigned 1 (traces of corrosion) or 2 (moderate corrosion) points.

There are no standard test methods to determine the anti-friction properties of the fuel composition of motor gasoline, therefore, as the most reliable way to confirm the presence and magnitude of these properties, the change in fuel efficiency, power (and torque), as well as acceleration dynamics for motor gasolines with and without additives is determined. These tests are technically complex, require a large amount of sample, and are difficult to apply to the analysis of a large number of samples. To indirectly determine the anti-friction properties, it uses the method for determining anti-wear properties on a high-frequency vibration stand (HFRR - apparatus with high frequency reciprocating motion). A similar methodology (for example, GOST ISO 12156-1) is used for diesel fuels as a standard method for evaluating the anti-wear properties of fuels. At the same time, in accordance with this method, the test is carried out at a temperature of 60°C, therefore, in order to correctly assess the anti-friction effectiveness of the multifunctional additive according to the invention, gasoline cannot be used as the base fuel, but it must be replaced with a diesel fuel fraction, which is the hydrocracking diesel fraction. , as having relatively low antiwear properties and the effect of the presence of an additive in which is most pronounced.

The ASTM D1094 method is used to evaluate the tendency of gasolines to form an emulsion with water. According to this method, 20 ml of water is added to 80 ml of the fuel composition in a graduated cylinder, the mixture is stirred for 2 minutes. The mixture then settles and the emulsion is evaluated after 5 minutes. The evaluation of the test is carried out on a scale from 1 to 3, where: 1 - complete absence of emulsion and / or precipitation in any layer or on the surface of the fuel layer; 2 - the same as 1, except for small air bubbles or small water droplets in the fuel layer; 3 - emulsions, deposits in any layer or on the fuel layer, droplets in the water layer or adhering to the walls of the cylinder, except for the walls above the fuel layer. The phase interface is also additionally evaluated on a scale from 1 to 4. The test results reflect the state of the phase interface and an estimate of the degree of separation.

The tendency of gasolines to form resins is determined according to the standard method GOST 32404 with the simultaneous determination of the amount of washed and unwashed resins.

Table 3 - Test results of the fuel composition with additives Example number base fuel 1 2 3 4 5 6 7 8 9 10 eleven 12 13 14 15 Additive input concentration, mg/kg - 334 300 1000 300 600 280 180 400 410 600 105 1000 300 400 500 Corrosion of a steel bar according to ASTM D665, points 3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Wear scar diameter according to GOST ISO 12156-1, µm ¹ 508 316 322 308 342 258 294 392 326 231 210 430 279 314 310 256 Resins according to GOST 32404, mg/100 cm ³ Unwashed 12 14 13 12 13 21 15 10 12 28 34 10 16 13 13 24 washed less than 0.5 less than 0.5 less than 0.5 less than 0.5 less than 0.5 less than 0.5 less than 0.5 less than 0.5 less than 0.5 less than 0.5 less than 0.5 less than 0.5 less than 0.5 less than 0.5 less than 0.5 less than 0.5 Water interaction according to ASTM D1094, rating 1/1 1/1 1/1 1/1 1/1 1/1 1/1 1/1 1/1 1/1 1/1 1/1 1/1 1/1 1/1 ¹ To determine the diameter of the wear scar, the diesel fraction of hydrocracking was taken as the base fuel

It can be seen from the data in Table 3 that using the multifunctional additive produced by the method of the present invention, it is possible to achieve an ASTM D665 steel rod corrosion index of 0 without adversely affecting the properties of gasolines such as emulsification and tendency to form gums.

To reliably establish the presence of detergent and antifriction properties of a multifunctional additive on the properties of motor gasoline, motor-bench tests were carried out on a 4Ch8.2 / 7.56 gasoline engine (four-stroke, four-cylinder, in-line, sixteen-valve, with two camshafts, marking of the manufacturer VAZ -21126) with gasoline injection into the intake manifold as part of a test bench. The tests consisted in taking the speed and load characteristics of the engine running on the base fuel or the fuel composition of motor gasoline with an additive, carrying out the stage of accumulation of deposits for 30 hours and re-taking the speed and load characteristics of the engine. In addition to the characteristics at the beginning and end of the cycle, the power of mechanical losses of the engine is determined, which is carried out by forcing the crankshaft of the engine using an external energy source, as well as weighing the intake valves to determine the mass of deposits formed on them. Two fuel compositions of motor gasolines with a multifunctional additive took part in the motor-bench tests: the additive obtained by the method according to example 1 at a concentration of 334 mg/kg, and the additive obtained by the method according to example 6 at a concentration of 280 mg/kg. The results of comparative motor-bench tests are presented in tables 4-5.

Table 4 - Results of determining the mass of deposits on the intake valves Parameter Dimension Fuel Base gasoline Fuel composition with additive (example 1) Fuel Composition with Additive (Example 6) Mass difference mg 58.6 31.5 34.3 Average sediment intensity mg/mh 1.96 1.19 1.14 Reduced deposits relative to base gasoline % - 39.3 41.8

Table 5 - Influence of a multifunctional additive on engine performance Name of indicator Additive according to example 1 Additive according to example 6 Instantaneous effect value ¹ , % The value of the accumulated effect ² , % Instantaneous effect value ¹ , % The value of the accumulated effect ² , % Reduced specific effective fuel consumption up to 0.9 up to 3.4 up to 1.2 up to 2.0 Increasing torque and effective power up to 4.6 up to 3.2 up to 3.6 up to 6.2 Reducing carbon monoxide emissions - up to 9.0 up to 7.3 up to 9.7 Reducing carbon dioxide emissions up to 2.3 up to 6.5 up to 2.6 up to 6.4 Reducing emissions of unburned hydrocarbons up to 2.4 up to 7.2 up to 2.4 up to 7.1 Reducing nitrogen oxide emissions up to 1.2 up to 3.9 up to 8.9 up to 11.5 Reducing the power of mechanical losses in the motor up to 10.5 up to 15.0 up to 6.4 up to 12.2 ¹ Instantaneous effect - comparison of indicators before operating time on base gasoline and before operating time on gasoline with an additive
² Cumulative effect - comparison of indicators before operating time on base gasoline and after operating time on gasoline with an additive

From the results of motor-bench tests presented in tables 4-5, it can be seen that the involvement of a multifunctional additive according to the invention in the composition of motor gasoline gasolines can reduce the amount of deposits on intake valves by 39-42%, as well as achieve power, efficiency and environmental benefits in terms of compared with the base gasoline presented in Table 5, which makes it possible to characterize the additive as an effective detergent and anti-friction agent and, in combination with the test results in Table 3, confirms its multifunctional nature.

Claims (17)

1. A method for producing a multifunctional additive for motor gasoline, consisting of three stages: - interaction of diethanolamine and vegetable oils at a molar ratio of reagents from 3.0:1.0 to 3.6:1.0, temperature from 120 to 180°C, - interaction of diethanolamine and fatty acids at a molar ratio of reagents from 0.9:1.0 to 1.1:1.0, temperature from 30 to 70°C, - mixing the reaction products obtained in stages 1 and 2, in a mass ratio of 1.0:1.0 to 20.0:1.0 at a temperature of 30 to 70°C. 2. The method according to p. 1, characterized in that the reaction of interaction of diethanolamine and fatty acid is carried out in a solvent, the proportion of which is from 10 to 78% of the total mass of the mixture. 3. The method according to p. 1, characterized in that the mixing of the interaction products is from 0.5 to 2.0 hours. 4. A method for producing a multifunctional additive for motor gasoline, consisting of two stages in the course of joint synthesis in one apparatus: - interaction of diethanolamine and vegetable oils at a molar ratio of reagents from 3.0:1.0 to 3.6:1.0, temperature from 120 to 180°C, - interaction of an excess amount of diethanolamine, which did not react in the first stage, and fatty acids added in the second stage, at a molar ratio of reagents from 0.9:1.0 to 1.1:1.0, a temperature of 30 to 70 ° C. 5. The method according to paragraphs. 1 and 4, characterized in that at the final stage, a solvent is additionally added to the mixture in such a way that its mass fraction is from 10 to 78%. 6. The method according to paragraphs. 1 and 4, characterized in that the first stage is carried out in the presence of an alkaline catalyst at its mass fraction from 0.01 to 0.50%. 7. The method according to paragraphs. 1 and 4, characterized in that at the final stage, an antioxidant and a demulsifier are additionally added to the mixture so that the mass fraction of each component does not exceed 1%. 8. The method according to paragraphs. 1 and 4, characterized in that the reaction of the interaction of diethanolamine and vegetable oil is carried out from 2 to 10 hours at a pressure of 1 to 5 atm, the reaction of the interaction of diethanolamine and fatty acid is carried out from 0.5 to 2.0 hours. 9. The method according to paragraphs. 1 and 4, characterized in that rapeseed, sunflower, olive, soybean oils, as well as mixtures thereof, are used as vegetable oil. 10. The method according to paragraphs. 1 and 4, characterized in that fatty acids of tall oils, fatty acids of vegetable oils, oleic acid are used as fatty acids. 11. The method according to paragraphs. 2, 4, characterized in that various hydrocarbon fractions are used as a solvent, boiling off in the temperature ranges corresponding to gasoline from 30 to 200°C and kerosene from 120 to 300°C, including commercial fuels; narrow cuts such as Nefras, aromatic solvent, polyalkylbenzene solvent, low viscosity hydrocarbon base for drilling fluids; individual hydrocarbons and mixed fractions thereof, such as toluene, p-xylene, o-xylene, m-xylene, a mixture of xylenes, cumene, ethylbenzene; higher alcohols and their mixed fractions, such as n-butanol, iso-butanol, iso-pentanol, alcohol-ether concentrate, 2-ethylhexanol, distillation residue of butyl alcohols. 12. The method according to claim 6, characterized in that hydroxides and carbonates of alkali and alkaline earth metals, such as sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium bicarbonate, potassium bicarbonate, calcium bicarbonate, are used as an alkaline catalyst.