RU2638294C1 - Method of producing lubricant oil additives - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: in an oil suspension with a content of calcium hydroxide and water in a weight ratio to oil of 1:0.43-0.49:0.02-0.03, respectively, at 70-90°C, ethylene glycol and dodecylphenol or nonylphenol are introduced with the molar ratio of alkyl phenol: ethylene glycol: calcium hydroxide 1:0.84-0.96:1.46-1.56 for the formation of complex salts of calcium alkylphenolate and their neutralization. The formed complex salts are condensed at 120-130°C with a 40% non-methanol solution of formaldehyde or acetaldehyde, taken in an amount of 0.25-0.51 moles. The condensed product is carbonated by passing CO₂ through it at a rate of 53-80 ml/min for 2.5-3 hours. The volatile components are driven and the resulting additive is cleaned of impurities.

EFFECT: additive improvement.

3 cl, 1 dwg, 2 tbl, 8 ex

Description

The invention relates to the field of petrochemistry, in particular to a method for producing an alkaline alkylphenol additive for lubricating oils.

One of the most promising types of alkaline ash detergents are alkaline alkyl phenolic additives, which are colloidal dispersions of metal carbonate of the second group of the periodic table (mainly barium, calcium and magnesium).

A known method of producing oil-soluble calcium phenolate based on the condensation product of alkyl phenol with formalin. This patent proposes to involve in the lubricating composition an oil-soluble calcium phenolate obtained by the reaction of 1 mole of alkyl phenol and 1-2 moles of CH ₂ O in the presence of a catalyst at a temperature of 10 ÷ 90 ° C, followed by modification of the resulting product by condensation with a reagent containing calcium (oxide, hydroxide ), at temperatures above 30 ° C. The disadvantage of this method is the low alkaline number of the obtained additive (and83256183, class С10М 1/08, publ. 06/14/1966).

In US Pat.

where X is --CHO or -CH ₂ OH, Y - -CH ₂ - or -CH ₂ OCH ₂ -, R ¹ is a hydrocarbon radical containing from 1 to 60 hydrocarbon atoms, and m is from 0 to 10, at least 1 aryl radical contains R ¹ Deputy, the total number of hydrocarbon atoms in all R ¹ groups must be at least 7.

Among the disadvantages of the method for producing lubricating oil additives described in this patent is the use of a large amount of formaldehyde involved in the synthesis, which means the risk of obtaining a gummy product, the use of less reactive magnesium oxide instead of calcium hydroxide, and the low alkaline number of the resulting product.

In the patent US 3951830 (CL C10M 159/22, publ. 04/20/1976) it is proposed to obtain highly alkaline salts of alkyl phenol containing both -CH ₂ - and -S-bridges connecting alkylphenol molecules. For this, the sulfuric alkylphenol is treated with formaldehyde, diluted with mineral oil, and in the presence of calcium hydroxide and promoters (acetic acid and methanol) are carbonated at elevated temperatures. The content of sulfate ash in the resulting product is about 17% of the mass.

Patent RU 2398814 (class C10M 159/22, published September 10, 2010) describes a method for producing a modified ultra-alkaline alkyl phenol additive for lubricating oils, in which at the first stage they interact (C ₈ -C ₁₈ -alkylphenol, elemental sulfur and oxide or calcium hydroxide in the presence of ethylene glycol at a molar ratio of calcium oxide or hydroxide: ethylene glycol equal to 1: 0.2-0.5 Then, in the second stage, in the presence of modifying additives, the resulting product is reacted with an additional amount of oxide or hydro calcium hydroxide and ethylene glycol at a molar ratio of 1: 0.2-0.6, followed by treatment with carbon dioxide at a carbon dioxide transmission rate of 0.02-0.04 mol / min mol of phenol. The disadvantage of this method is the presence in the composition of the resulting sulfur additive, i.e. its insufficient environmental properties.

Closest to the proposed method, selected as a prototype, is a method for producing an additive for lubricating oils, according to which an additive for lubricating oils is produced by condensing alkyl phenol with a 37% formaldehyde solution in the presence of a catalyst, followed by treatment of the resulting product with alkaline earth metal hydroxide in medium of diluent oil, while C ₈ , C ₉ , C ₁₂ , C ₁₈ - alkyl phenols are used as alkyl phenol with a molar ratio of alkyl phenol to formaldehyde of 1: 0.6-1.3. The process is carried out in the presence of a solvent, an acidic or alkaline catalyst is used as a catalyst, and calcium hydroxide is used as an alkaline earth metal hydroxide. Carbonation is additionally carried out by passing carbon dioxide through the obtained product in the presence of a promoter. In accordance with this method, a sulfur-free alkyl phenol additive with an alkaline number of at least 200 mg KOH / g is obtained. The disadvantage of this method is the use of a large amount of solvent, which pollutes the environment. When carrying out the process at temperatures above 85 ° C, the technology proposed in the patent is also fire hazard (RU 2582124, class C10M, 159/00, publ. 04/20/2016).

The objective of the invention is to develop a method for producing an alkyl phenolic alkaline additive for lubricating oils with detergent, antioxidant, anticorrosive properties, improved color (not higher than 4 according to GOST 20284-74) and meeting modern environmental requirements for additives that have the abbreviation "Low SAPS additives".

To solve this problem, a method for producing an acylphenol additive to lubricating oils by neutralizing an alkaline earth metal hydroxide with calcium alkyl phenolates, their subsequent condensation with an aliphatic aldehyde in the presence of a catalyst, and carbonation of the obtained condensation product by passing through it in the presence of a carbon dioxide promoter, characterized in that in an oil suspension with the content of calcium hydroxide and water in a weight ratio to oil equal to 1: 0.43-0.49: 0.02-0.03, respectively, pr at a temperature of 70-90 ° C, ethylene glycol and dodecylphenol or nonylphenol are introduced at a molar ratio of alkyl phenol: ethylene glycol: calcium hydroxide 1: 0.84-0.96: 1.46-1.56 with the formation of complex salts of calcium alkyl phenolate and their neutralization, then in the reaction mixture with the complex salts of calcium alkyl phenolate formed is slowly introduced through a metering device at a temperature of 120-130 ° C. a 40% methanol-free formaldehyde solution or acetaldehyde in an amount of 0.25-0.51 mol and a condensation reaction is carried out, the condensed product at a temperature e 170-180 ° C is subjected to carbonation with neproreagiruyuschimi amounts condensation step calcium hydroxide as catalyst and ethylene glycol as a promoter, passing therethrough CO ₂ at a rate 53-80 ml / min for 2.5-3 hours, followed by distilling off volatile components and water; and purification of the obtained additive from mechanical impurities insoluble in the hydrocarbon medium.

The method of producing alkylphenol additives is carried out in several stages as follows:

- at the first stage, a neutralization reaction is carried out, which consists in first preparing a suspension of mineral oil with calcium hydroxide, to which, when heated, water is added to facilitate the neutralization reaction and reduce the viscosity of the reaction mass; then ethylene glycol is introduced and, when reacted with calcium hydroxide, alkyl phenol is introduced; the neutralization reaction proceeds with the formation of complex salts of calcium alkyl phenolate;

- at the second stage, a condensation reaction of the obtained complex salts with an aldehyde is carried out;

- at the third stage, the carbonation of the product obtained after condensation is carried out in the presence of the remaining amounts of unreacted calcium hydroxide and ethylene glycol in the first stages; for this, at a temperature of 170-180 ° C, CO _{2 is} passed through the reaction mass at a rate of 53-80 ml / min for 2.5-3 hours, after which the volatile components are distilled off and the additive is purified, for example, by dissolution in gasoline followed by centrifugation and (or) by filtration, gasoline is distilled off.

A method for producing an alkyl phenol additive can alternatively be carried out by fractional administration of an amount of calcium hydroxide and ethylene glycol as follows:

- in the first stage of neutralization, calcium hydroxide and ethylene glycol are introduced in a stoichiometric amount sufficient to obtain complex salts of calcium alkyl phenolate;

- in the second stage, the condensation reaction of the obtained complex salts with the aldehyde is carried out, as in the first method;

- in the third stage, calcium hydroxide and ethylene glycol are additionally introduced before carbonation, then they are carbonated at a temperature of 170-180 ° C, a CO ₂ transmission rate _of 53-62 ml / min, for 2.5-3 hours. Then, volatile components and water are distilled off and clean the additive.

The following are examples of the production of alkyl phenol additives by the two methods described above.

Example 1 (method one)

At the first stage of the synthesis of the alkyl phenol additive, 85 g of I-20A oil is poured into a 4-necked flask with a volume of 500 ml, the mixing device is turned on, 42 g (0.57 mol) of calcium hydroxide are poured. With constant stirring and heating to 90 ° C, water — 2 g (0.11 mol) and ethylene glycol — 21.7 g (0.35 mol) are introduced into the reaction mixture. Then, at a temperature of 90-95 ° C, 100 g of dodecylphenol (0.38 mol) was added to the reaction mixture, after which the temperature of the reaction mixture was raised to 125 ° C.

In the second stage of the synthesis, a condensation reaction is carried out. For this purpose, a 40% methanol-free aqueous formaldehyde solution is prepared. For this, paraforms are dissolved in distilled water and heated to a temperature of 80-90 ° C in a water bath with periodic stirring. Next, the mixture was kept at this temperature for 1 hour until the paraform was completely dissolved in water. For synthesis, a solution with a shelf life of not more than 1 day is used.

At a temperature of 125 ° C, a 40% formalin solution in the amount of 19.8 g (0.25 mol) is freshly prepared with a shelf life of not more than 1 day. Then the temperature rises to 175 ° C.

In the third stage of synthesis at 175 ° C, the carbonation of the product obtained in the first two stages is carried out. To do this, pass through the reaction mass CO ₂ at a rate of 64 ml / min for 2.5 hours. After carbonation and after distillation of the volatiles, the obtained alkyl phenol additive is purified from mechanical impurities by dissolution, for example, in gasoline, followed by centrifugation or filtration and distillation gasoline from the finished additive.

Example 2 (method one)

The neutralization reaction is carried out as described in Example 1.

At the stage of condensation, acetaldehyde is dosed into the product obtained after neutralization in an amount of 11.7 g (0.27 mol) at a temperature of 130 ° C.

Carbonation is carried out at a temperature of 180 ° C (CO _{2 is} fed into the reactor at a rate of 53 ml / min for 3 hours). Then, the supply of CO ₂ to the reactor is stopped, and volatile components and water are distilled off. The obtained alkyl phenolic additive is purified from mechanical impurities, as described in Example 1.

Example 3 (method one)

For the neutralization reaction in the first stage of the synthesis of the alkyl phenol additive, 150 g of I-20A oil are poured into a 4-necked flask with a volume of 500 ml, 75 g (1.01 mol) of calcium hydroxide are poured, and the resulting suspension is heated with constant stirring. At a suspension temperature of 25-35 ° C., 3 g (0.17 mol) of water are added, and at a temperature of 70-75 ° C. 30.4 g (0.49 mol) of ethylene glycol are added.

When the temperature reaches 90-95 ° C, 150 g of nonylphenol (0.69 mol) are added to the reaction mixture, after which they begin to raise the temperature to 125 ° C.

At the condensation stage at a temperature of 125 ° C, formalin (in accordance with GOST 1625-89) in the amount of 38.5 g (0.51 mol) is metered into the reaction mixture.

The product obtained in the first two stages, carbonate at a temperature of 170 ° C for 4.2 hours (flow rate of CO ₂ 80 ml / min). Then, the supply of CO ₂ to the reactor is stopped, and volatile components and water are distilled off. The obtained alkyl phenolic additive is purified from mechanical impurities, as described in Example 1.

Example 4 (method one)

For the neutralization reaction in the first stage of the synthesis of an alkyl phenol additive, 75 g of I-20A oil and 2.5 g (0.01 mol) of dodecylphenol are poured into a 4-necked flask with a volume of 500 ml to reduce viscosity, 45 g (0.61 mol) are added calcium hydroxide and begin to heat the resulting suspension with constant stirring. At a suspension temperature of 25-35 ° C, 2 g (0.11 mol) of water are added, and at a temperature of 70-75 ° C, 20.2 g (0.33 mol) of ethylene glycol are added. At a temperature of 90-95 ° C, 100 g of dodecylphenol (0.38 mol) is introduced into the reaction mixture, then the reaction mixture is heated to 120 ° C.

The condensation is carried out at 120 ° C, freshly prepared 40% methanol-free aqueous formalin solution, obtained as described in Example 1, in the amount of 23.5 g (0.31 mol) is metered into the reaction mixture.

The product obtained in the first two stages, carbonate at a temperature of 175 ° C for 2.5 hours (flow rate of CO ₂ 64 ml / min). Then, the supply of CO ₂ to the reactor is stopped, and volatile components and water are distilled off. The obtained alkyl phenolic additive is purified from mechanical impurities, as described in Example 1.

Example 5 (method two)

For the neutralization reaction in the first stage of the synthesis of the alkyl phenol additive, 20 g of I-20A oil is poured into a 4-necked flask with a volume of 500 ml, the mixing device is turned on, 20 g (0.27 mol) of calcium hydroxide is poured and heating of the resulting suspension with constant stirring is started. At a suspension temperature of 25-35 ° C., 2 g (0.11 mol) of water are added, and at a reaction temperature of 70-75 ° C., 15 g (0.20) of ethylene glycol are added. Upon reaching a temperature of 90-95 ° C, 100 g of nonylphenol (0.45 mol) is introduced into the reaction mixture.

The condensation is carried out at a temperature of 130 ° C. A 40% methanol-free aqueous solution of formalin, obtained as described in Example 1, in the amount of 25.8 g (0.34 mol) is metered into the reaction mixture.

Before carbonation at a temperature of 130 ° C, 22 g (0.30 mol) of calcium hydroxide, 7 g (0.11 mol) of ethylene glycol and 80 g of I-20A mineral oil are introduced.

The product obtained in the first two stages, carbonate at a temperature of 175 ° C for 3 hours (feed rate of CO ₂ 53 ml / min). Then, the supply of CO ₂ to the reactor is stopped, and volatile components and water are distilled off. The obtained alkyl phenolic additive is purified from mechanical impurities, as described in Example 1.

Example 6 (method two)

For the neutralization reaction in the first stage of the synthesis of the alkyl phenol additive, 20 g of I-20A oil is added to a 4-necked flask with a volume of 500 ml, the stirring device is turned on, 20 g (0.27 mol) of calcium hydroxide is poured and heating of the suspension obtained with constant stirring. At a suspension temperature of 25-35 ° C., 2 g (0.11 mol) of water are added, and at a reaction temperature of 70-75 ° C., 15 g (0.20 mol) of ethylene glycol are added. Upon reaching a temperature of 90-95 ° C, 100 g of the mixture containing 50% nonylphenol and 50% dodecylphenol in total (0.41 mol) are introduced into the reaction mixture.

Condensation is carried out at a temperature of 130 ° C, formalin is dosed into the reaction mixture according to GOST 1625-89 g in an amount of 25.8 g (0.34 mol).

Before carbonation at a temperature of 130 ° C, 22 g (0.30 mol) of calcium hydroxide, 7 g (0.11 mol) of ethylene glycol and 80 g of I-20A mineral oil are introduced.

The product obtained in the first two stages, carbonate at a temperature of 180 ° C for 3 hours (feed rate of CO ₂ 62 ml / min). Then, the supply of CO ₂ to the reactor is stopped, and volatile components and water are distilled off. The obtained alkyl phenolic additive is purified from mechanical impurities, as described in Example 1.

Example 7 (method two)

For the neutralization reaction in the first stage of the synthesis of the alkyl phenol additive, 20 g of I-20A oil is poured into a 4-necked flask with a volume of 500 ml, 17 g (0.23 mol) of calcium hydroxide are poured and heating of the resulting suspension with constant stirring is started. - At a suspension temperature of 25-35 ° C., 2 g (0.11 mol) of water are added, and at a reaction temperature of 70-75 ° C., 15 g (0.20) of ethylene glycol are added. Upon reaching a temperature of 90-95 ° C, 100 g of dodecylphenol (0.38 mol) is introduced into the reaction mixture.

The condensation is carried out at a temperature of 125 ° C. A 40% methanol-free aqueous solution of formalin, prepared as described in Example 1, in an amount of 23.5 g (0.31 mol) is metered into the reaction mixture.

Before carbonation at a temperature of 125 ° C, 28 g (0.38 mol) of calcium hydroxide, 7 g (0.11 mol) of ethylene glycol and 65 g of I-20A mineral oil are introduced.

The product obtained in the first two stages, carbonate at a temperature of 175 ° C for 3 hours (feed rate of CO ₂ 53 ml / min). Then, the supply of CO ₂ to the reactor is stopped, and volatile components and water are distilled off. The obtained alkyl phenolic additive is purified from mechanical impurities, as described in Example 1.

Example 8 (method two)

For the neutralization reaction in the first stage of the synthesis of the alkyl phenol additive, 20 g of I-20A oil is poured into a 4-necked flask with a volume of 500 ml, 17 g (0.23 mol) of calcium hydroxide are poured and heating of the resulting suspension with constant stirring is started. At a suspension temperature of 25-35 ° C., 2 g (0.11 mol) of water are added, and at a reaction temperature of 70-75 ° C., 15 g (0.20) of ethylene glycol are added. Upon reaching a temperature of 90-95 ° C, 100 g of a mixture containing 70 wt. % dodecylphenol and 30 weight. % nonylphenol (0.40 mol total).

Condensation is carried out at a temperature of 120 ° C, formalin (GOST 1625-89) is metered into the reaction mixture in an amount of 30 g (0.40 mol).

Before carbonation at a temperature of 120 ° C, 28 g (0.38 mol) of calcium hydroxide, 7 g (0.11 mol) of ethylene glycol and 65 g of mineral oil I-20A are introduced.

The product obtained in the first two stages, carbonate at a temperature of 180 ° C for 3 hours (feed rate of CO ₂ 53 ml / min). Then, the supply of CO ₂ to the reactor is stopped, and volatile components and water are distilled off. The obtained alkyl phenolic additive is purified from mechanical impurities, as described in Example 1.

It should be emphasized that the proposed method is carried out in contrast to the known methods without the use of a solvent, which simplifies and reduces the cost of the technology.

The addition of water in the preparation of a suspension of mineral oil and calcium hydroxide promotes ionization and calcium hydroxide, which facilitates the neutralization reaction and reduces the viscosity of the reaction mass.

Slow dosed introduction of the aldehyde into the reaction mixture at the condensation stage avoids foaming and a strong decrease in temperature. In addition, such an aldehyde feed does not allow resins to form, as predominantly non-condensed complex salts enter the condensation reaction.

A slow temperature rise with the distillation of volatile components after the condensation stage prepares the reaction mass for carbonation. Removing water prevents the formation of a by-product of carbonic acid. At a selected temperature regime above 165 ° C, the reaction mass has a small viscosity and is easier to carbonate. At a lower temperature, passing CO ₂ through the reaction mass can be difficult due to the high viscosity of the reaction mass.

The transmission rate of carbon dioxide is selected so that there is no "slip" of carbon dioxide. Fast carbonation leads to the formation of a large amount of calcium carbonate, the excess of which precipitates; the alkaline number decreases, and the dried potential sludge (HPS) of the additive increases.

The low transmission rate of CO ₂ leads to additional energy costs for heating the reaction mass.

Below in the table. 1 shows the downloads of the starting materials for examples of the proposed method for producing alkylphenol additives.

The detergent properties of the additive obtained in examples 1-8 were evaluated by the degree of contamination of the piston in points at the installation of PZV according to GOST 5727-53. Corrosion resistance was determined according to GOST 20502-75.

Stability in the induction period of sedimentation (NPO) with 1% of the mass. the obtained additive was determined according to GOST 11063-77.

The quality of the obtained additive was determined by its transparency, color and the amount of sludge at the bottom of the tubes. The transparency of the additive was determined by measuring the value of the optical permeability coefficient (T) at a wavelength of 750 (T ₇₅₀ ) on a KFK-2 photoelectrocalorimeter in a 1 cm thick cuvette. The IPL — dried potential sludge — was determined by drying the precipitate in a test tube after centrifugation of a 10% solution additive in nephras C-2 with a separation factor of 3900 g.

The color for a 10% additive solution in Nefras C2 80/120 was determined according to GOST 20284-74

In the table. 2 shows the basic physicochemical and functional properties of the resulting additive. From the data of table 2 it follows that all samples synthesized by the proposed method have high alkalinity, good performance, corresponding to additives with the abbreviation "Low SAPS additives".

Using the IR method, we analyzed a sample of the obtained alkyl phenol additive in a KBr tablet in the region of 400–4000 cm ^–1 . The spectrum is shown in Fig. one.

The following bands were recorded in the IR spectrum:

- there is an absorption band characteristic of stretching vibrations υ С-О in the molecule of calcium phenolate 1250-1280 cm ^-1 ;

- absorption bands of 870, 910 cm ^{-1 are} characteristic of deformation vibrations of 1, 2, 4 substituted benzene rings, a band of 830 cm ^-1 can be attributed to deformation vibrations of 1.4 benzene rings. These bands indicate the formation of an alkyl phenol condensation product. An absorption band of 1075 cm ^{−1 is} characteristic of stretching vibrations of the CO bond in the calcium glycolate molecule.

A wide absorption band in the region of 2500–3700 cm ^–1 with a maximum at 3450 cm ^–1 is characteristic of OH stretching vibrations in the alkyl phenol molecule. A wide absorption band in the region of 1300-1600 cm ^-1 with a maximum at 1460 cm ^-1 can be attributed to stretching vibrations of CO ₃ ^-2 , absorption bands of 860 cm ^-1 , 1300-1600 cm ^-1 to deformation vibrations of CO ₃ ^-2 . Attention was drawn to the fact that the wider the absorption band in the region of 1300-1600 cm ^-1 , the more the reaction mass absorbed carbon dioxide.

IR spectral analysis confirms the production of an alkyl phenol additive with the formation of a carbonated condensation product of alkyl phenol and aldehyde, and also confirms the presence of calcium and calcium glycolate in the molecule in the following structural formulas:

и/или

and / or

,

,

where n is the number of calcium carbonate molecules that make up the alkyl phenol additive in the form of a colloidal dispersion, n = 1 ... 10, R is nonyl and / or dodecyl.

Claims (6)

1. A method of producing an acilphenol additive for lubricating oils by neutralizing calcium alkyl phenolates with an alkaline earth metal hydroxide, then condensing them with an aliphatic aldehyde in the presence of a catalyst and carbonating the obtained condensation product by passing through it in the presence of a carbon dioxide promoter, characterized in that in an oil suspension containing hydroxide calcium and water in a weight ratio to oil equal to 1: 0.43-0.49: 0.02-0.03, respectively, at a temperature of 70-90 ° C ethylene glycol is introduced and up to ecylphenol or nonylphenol at a molar ratio of alkyl phenol: ethylene glycol: calcium hydroxide 1: 0.84-0.96: 1.46-1.56 to form complex salts of calcium alkyl phenolate and neutralize them, then into the resulting reaction mixture with formed complex salts of calcium alkyl phenolate at a temperature of 120-130 ° C, a 40% methanol-free formaldehyde solution or acetaldehyde is introduced in an amount of 0.25-0.51 mol slowly and a condensation reaction is carried out, the condensed product is subjected to carbonation at a temperature of 170-180 ° C non-reactive amounts of calcium hydroxide as a catalyst and ethylene glycol as a promoter at the condensation stage, passing CO ₂ through it at a rate of 53-80 ml / min for 2.5-3 hours, followed by distillation of the volatile components and water and purification of the obtained additive from mechanical impurities insoluble in a hydrocarbon medium. 2. A method of producing an acylphenol additive to lubricating oils by neutralizing calcium alkyl phenolates with an alkaline earth metal hydroxide, then condensing them with an aliphatic aldehyde in the presence of a catalyst and carbonating the obtained condensation product by passing through it in the presence of a carbon dioxide promoter, characterized in that in the oil suspension containing hydroxide calcium and water in a weight ratio to oil equal to 1: 0.2-0.85: 0.02-0.1, respectively, nonylphenol or a mixture is introduced at a temperature of 70-90 ° C dodecylphenol and nonylphenol, taken as a percentage of 50:50 or 30:70, ethylene glycol and calcium hydroxide in a molar ratio of alkyl phenol: ethylene glycol: calcium hydroxide as 1: 0.43-0.96: 0.56: 1.50 with the formation of complex salts of calcium alkyl phenolate and their neutralization, then formalin or formaldehyde in an amount of 0.31-0.40 mol and at a temperature of 120-130 ° C is slowly introduced through a dosing device into the resulting reaction mixture with formed complex salts of calcium alkyl phenolate and a condensation reaction is carried out, condensed product They are carbonated at a temperature of 170-180 ° C, while calcium hydroxide as a catalyst and ethylene glycol as a promoter are additionally introduced with a total molar ratio of alkyl phenol: ethylene glycol: calcium hydroxide as 1: 0.67-0.81: 1.24-1 , 60, passing CO ₂ through it at a rate of 53-62 ml / min for 2.5-3 hours, followed by distillation of the volatile components and water and purification of the obtained additive from mechanical impurities insoluble in the hydrocarbon medium. 3. Additive alkaline alkyl phenol obtained according to paragraphs. 1, 2, having in the base basis carbonitic complex salts of calcium alkyl phenolates of structural formulas

where n is the number of molecules from 1 to 10, and R is nonyl and / or dodecyl.

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