Method for producing depressant-dispersant additive for diesel fuel

Abstract

FIELD: fuel additives.SUBSTANCE: invention relates to the field of additives for improving the performance characteristics of diesel fuel. A method for producing a depressant-dispersant additive for diesel fuel is proposed, during which the first component is obtained, which is an alkylphenol-formaldehyde resin, by boiling monoalkylphenol with formaldehyde in the form of formalin, paraform or trioxane, in the presence of a hydrocarbon solvent and an acid catalyst at a temperature of 80 to 150 °C for 5-6 hours. The obtained first component is mixed with the solvent in a mass ratio of 1:1. A second component is obtained, which is a product of the interaction of a carboxylic acid and a mono- or dialkylamine, by heating a mixture of a carboxylic acid and a mono- or dialkylamine at a temperature of 195 to 200 °C for 5-6 hours. The obtained second component is mixed with a solvent, represented by a mono- or mixed solvent, in a mass ratio of 1:1. The reaction mass of the first component and solvent is mixed with the reaction mass of the second component and solvent in a mass ratio of 1:[1-10].EFFECT: improving the properties of a set of operational characteristics of diesel fuel when using the obtained depressant-dispersant additive.17 cl, 2 dwg, 1 tbl, 9 ex

Description

[0001] The invention relates to methods for producing depressant-dispersant additives for diesel fuel and can be used in the chemical and oil refining industries.

[0002] Pour point depressant / dispersant additives play a key role in improving the performance of diesel fuel, especially at low temperatures. The primary function of these additives is to prevent the formation of paraffin crystals, which can cause fuel thickening and clog fuel filters.

[0003] The use of these additives directly impacts the comprehensive properties of diesel fuel, enhancing its stability and thermodynamic efficiency. Thanks to these additives, diesel fuel maintains fluidity and allows for uniform flow through fuel lines, ensuring stable engine operation even in extreme climatic conditions, including northern and high-altitude regions. This, in turn, significantly improves the reliability and efficiency of diesel engines, reducing the likelihood of failures and downtime. However, problems associated with the unsatisfactory performance of dispersants in pour point depressant additives remain relevant.

[0004] In particular, poor quality dispersants often fail to effectively disperse paraffins in fuel, which reduces its flowability and increases the risk of freezing in fuel lines. As a result, equipment operation becomes less reliable, which can lead to increased maintenance costs due to the need to frequently increase dispersant concentrations or completely replace them. This is not only economically ineffective but also complicates fuel and equipment management.

[0005] To solve the above problems, dispersants of depressant-dispersant additives for diesel fuel are being developed.

[0006] For example, a dispersant of a depressant-dispersant additive for diesel fuel selected as a prototype is known, which is either an alkylphenol formaldehyde resin or amine salts and / or amides, which are products of the reaction of aliphatic or aromatic amines, preferably long-chain aliphatic amines, with aliphatic or aromatic mono-, di-, tri- or tetracarboxylic acids or their anhydrides. [EP 1116780 B1, publication date: 31.08.2005]

[0007] A disadvantage of the prototype is the low effectiveness of the pour point depressant / dispersant additive for diesel fuel, which includes the prototype dispersant, in improving the overall performance characteristics of diesel fuel. Diesel fuel performance characteristics affected by the use of the dispersant may include pour point, viscosity, water and solids content, and oxidation stability of diesel fuel. The prototype's low effectiveness is due to the fact that the dispersant can only be represented by a single main component and, as a result, cannot have a comprehensive effect on the physicochemical processes occurring in the fuel. This also limits the flexibility of using such a dispersant in diesel fuel compositions with different compositions and qualities.

[0008] In this regard, it is necessary to develop a dispersant that would provide a comprehensive effect on improving the performance characteristics of diesel fuel.

[0009] The technical problem that the invention is aimed at solving is the need to develop a dispersant depressant-dispersant additive that eliminates existing disadvantages.

[0010] The technical result that the invention is aimed at achieving consists in improving the properties of a set of operational characteristics of diesel fuel when using the developed dispersant as part of a depressant-dispersant additive.

[0011] The essence of the invention is as follows.

[0012] A method for producing a dispersant depressant-dispersant additive for diesel fuel, during which:

[0013] - the first component, which is an alkylphenol formaldehyde resin, is obtained by boiling monoalkylphenol with formaldehyde in the form of formalin, paraformaldehyde or trioxane in the presence of a hydrocarbon solvent and an acid catalyst at a temperature of 80 to 150 °C for 5-6 hours;

[0014] - mix the first component with a solvent, represented by a mono- or mixed solvent, in a mass ratio of 1:1;

[0015] - a second component is obtained, which is a product of the interaction of a carboxylic acid and a mono- or dialkylamine, by heating a mixture of a carboxylic acid and a mono- or dialkylamine at a temperature of 195 to 200 °C for 5-6 hours;

[0016] - mix the second component with a solvent, represented by a mono- or mixed solvent, in a mass ratio of 1:1;

[0017] - mix the reaction mass of the first component and solvent (PM1) and the reaction mass of the second component and solvent (PM2) in a mass ratio of PM1:PM2 = 1:[1-10].

[0018] The target product of the invention is a dispersant depressant-dispersant additive for diesel fuel, which effectively reduces the waxing temperature of the fuel and improves its fluidity, which is very important for operation in cold climates, where paraffin thickening of the fuel can seriously affect the operation of engines.

[0019] The dispersant is a 50% solution of two main components. These components provide significant improvement in fuel performance, especially at low temperatures.

[0020] Using a 50% ratio in the dispersant ensures a balance between activity and solubility, allowing for effective action on paraffin structures and uniform distribution in diesel fuel. This ratio simplifies integration into existing dosing systems without significant modifications. Furthermore, a 50% solution maintains mixture stability, preventing stratification and coagulation, which is particularly important for maintaining consistent low-temperature fuel properties.

[0021] The process for producing the first component, an alkylphenol-formaldehyde resin, involves the polycondensation of monoalkylphenol with formaldehyde. The formation of alkylphenol-formaldehyde resin involves the formation of complex structures, where formaldehyde forms methylene bridges that link phenolic rings. This process creates a stable polymer network, which imparts the resin the necessary mechanical and physicochemical properties. The final product—alkylphenol-formaldehyde resin—provides the basis for the improved performance characteristics necessary for the effective performance of a pour point depressant additive in diesel fuel.

[0022] The polycondensation reaction of monoalkylphenol with formaldehyde is carried out in the presence of a hydrocarbon solvent, which ensures high reactivity and a complete process, as well as a catalyst, which accelerates polycondensation and stabilizes intermediate compounds, promoting the formation of a denser and stronger polymer network.

[0023] The hydrocarbon solvent used to obtain the first component can be selected from a group including benzene, toluene, xylene, heptane, and octane. These solvents provide the environment for the polycondensation reaction due to their high solubility and stability. Each of them promotes the effective penetration and interaction of the reactants, maintaining the desired viscosity of the mixture, and also facilitates heat transfer, which is critical for uniform reaction and the production of a high-quality polymer product.

[0024] The catalyst used to produce the first component can be selected from the group consisting of p-toluenesulfonic acid, hydrochloric acid, oxalic acid, maleic acid, and succinic acid. These catalysts accelerate the polycondensation reaction and promote the stabilization of intermediate compounds, ensuring the active combination of phenolic and formaldehyde monomers into a dense polymer network. Each of these catalysts plays a key role in increasing the efficiency and rate of the reaction, helping to create a strong and stable resin structure, which significantly improves its performance properties in the dispersant composition. The most preferred catalyst is p-toluenesulfonic acid, which, as an aromatic organic acid, has an affinity for the first component of the dispersant due to the presence of an aromatic ring, and for the second component of the dispersant due to the presence of an acidic function.Its presence in the final product does not reduce its functional properties, while other catalysts can act as antagonists to the target properties of the dispersant.

[0025] The monoalkylphenol used to obtain the first component may be a mixture of monoalkylphenols in which the alkyl group contains from 1 to 20 carbon atoms, or may be a pure monoalkylphenol in which the alkyl group contains N=1÷20 carbon atoms, since the use of industrially produced individual monoalkylphenols is more preferable.

[0026] In this case, it is preferable to use pure monoalkylphenol, in which the alkyl group contains N=3-15 carbon atoms, which allows for an optimal combination of the reactive and physical properties of the resin itself, such as stability and compatibility with other diesel fuel components. Even more preferable is the use of pure monoalkylphenol, in which the alkyl group contains N=7-12 carbon atoms, which provides an additional balance between flexibility and stability of the resulting product, allowing the resulting alkylphenol formaldehyde resin to maintain its properties over a wider range of operating temperatures. The presence of various alkyl substituents introduces irregularity into the additive, which helps keep the paraffins dispersed, preventing crystallization and improving fuel flow.

[0027] Formaldehyde, used to prepare the first component, can be present in various forms, such as formalin, paraformaldehyde, or trioxane, allowing for flexible selection of starting reagents based on availability and cost-effectiveness. Formaldehyde ensures a rapid and uniform reaction due to its aqueous dispersion, but requires control to avoid side reactions with water. Paraformaldehyde allows for the reaction to be carried out without water, ensuring controlled release of formaldehyde upon heating, reducing the risk of side reactions. Trioxane, as a cyclic trimer, provides a gradual release of formaldehyde, ensuring stable and uniform polymerization under less aggressive conditions.

[0028] When obtaining the first component, monoalkylphenol, formaldehyde, hydrocarbon solvent and catalyst are taken in the following weight ratio: monoalkylphenol: from 0.9 to 1.1 parts; formaldehyde: from 0.09 to 0.13 parts; hydrocarbon solvent: from 0.9 to 1.1 parts; catalyst: from 0.005 to 0.02 parts.

[0029] The addition of 0.9 to 1.1 parts of monoalkylphenol creates a stable base for uniform reaction with formaldehyde. Formaldehyde addition in a ratio of 0.09 to 0.13 parts ensures an optimal degree of polymerization without excessive oversaturation or undersaturation. Furthermore, the addition of 0.9 to 1.1 parts of solvent ensures uniform polymer formation, while the addition of 0.005 to 0.02 parts of catalyst prevents potential side reactions and degradation of intermediate products.

[0030] The first component is obtained by boiling monoalkylphenol with formaldehyde in the presence of a hydrocarbon solvent and catalyst. The process is carried out at temperatures ranging from 80 to 150°C for 5-6 hours, allowing for precise control of this chemical process and achieving complete polymerization. Lower temperatures can lead to incomplete polycondensation, resulting in the formation of oligomers that are less effective as dispersants. Exceeding this temperature limit can lead to degradation of the resulting polymer, which will break the chains and degrade the mechanical properties of the dispersant.

[0031] Also, during the production of the first component by boiling monoalkylphenol with formaldehyde in the presence of a hydrocarbon solvent and catalyst, water is formed. The resulting water can be removed by azeotropic distillation at temperatures ranging from 80 to 130°C. This accelerates the polycondensation reaction, shifts potential equilibria toward polymer formation, and improves monomer interactions. The result is a more concentrated and structured polymer network, improving the physical stability and performance properties of the resin, making it ideal for use as a dispersant.

[0032] After obtaining the first component, it is mixed with a solvent, represented by a mono- or mixed solvent, in a mass ratio of 1:1.

[0033] The process for producing the second component, which is a reaction product of a carboxylic acid and a mono- or dialkylamine, involves a reaction between the functional groups of the carboxylic acids and amines. This results in the formation of substituted amines with unique properties necessary for dispersant function in diesel fuel.

[0034] The carboxylic acid used to produce the second component may be selected from the group consisting of ethylenediaminetetraacetic acid (EDTA), the product of EDTA alkylation at the nitrogen atoms with monochloroacetic acid, aromatic tetracarboxylic acids represented by benzene and naphthalene tetracarboxylic acids, nitrilotriacetic acid, and products of exhaustive or partial C-alkylation of malonic or succinic acids with haloacetic acid. These acids provide active functional groups that create stable bonds with mono- or dialkylamines, promoting the formation of strong and polar interactions necessary for dispersion activity.Each of the mentioned acids increases the polarity and reactivity of the component, which plays a critical role in improving the ability of the dispersant to maintain a homogeneous phase in diesel fuel, thereby increasing the overall effectiveness of the depressant-dispersant additive in preventing paraffin crystallization and improving fuel flowability.

[0035] The mono- or dialkylamine used to produce the second component can be a mixture of mono- and dialkylamines containing amines with alkyl groups ranging from 5 to 30 carbon atoms, or a mixture of pure mono- and dialkylamines containing amines with alkyl groups ranging from 5 to 30 carbon atoms, providing a broad balance between solubility and viscosity. This variety of chain lengths allows for the dispersant to be actively adapted to the existing hydrocarbon composition of the fuel. Shorter chains ensure easy distribution of the additive in the fuel, improving initial fluidity and lowering the pour point. Longer chains, in turn, provide additional viscosity and structural stability, helping to minimize the tendency to form paraffin crystals and maintain stability under extreme temperature conditions.

[0036] In a more preferred embodiment, the mono- or dialkylamine used to produce the second component can be a mixture of pure mono- and dialkylamines containing amines with an alkyl group length of N=8÷25 carbon atoms. This ensures optimal polarity and solubility achieved through proper integration of chemical bonds, allowing the component to effectively perform its function in the diesel fuel matrix. This, in turn, helps prevent paraffin crystallization and improves the low-temperature properties of the fuel.

[0037] Optimal properties can be achieved by using a mixture of pure mono- or dialkylamines for the second component, containing amines with an alkyl group length of N=12–18 carbon atoms. Such chains are capable of forming a stable and flexible matrix in the fuel, preventing paraffin crystallization, keeping them dispersed, and improving lubricating properties. This allows the fuel to maintain fluidity and stability at low temperatures without losing efficiency and performance.

[0038] To obtain the second component, the carboxylic acid and mono- or dialkylamine are used in a molar ratio of the carboxyl function of the carboxylic acid (CF) to each amine of the mixture of mono- and dialkylamines (A), equal to CF:A = [1-4]:1. This optimizes the interaction between them, ensuring the formation of stable amide bonds. Taking an amount of amines insufficient in relation to the carboxyl functions of the carboxylic acid required further neutralization of the reaction mixture, which consisted of introducing an additional amount of amine or amine mixture into the reaction mixture in an amount equal to the number of unreacted carboxyl groups.

[0039] The reaction to obtain the second component is carried out at a temperature of 195 to 200°C for 5-6 hours. If the temperature or time parameters deviate from these limits, insufficient reactivity of the components may occur, leading to decreased product efficacy due to incomplete realization of the required chemical structure or excessive side reactions.

[0040] After obtaining the second component, it is also mixed with a solvent, represented by a mono- or mixed solvent, in a mass ratio of 1:1.

[0041] A mono- or mixed solvent used for mixing the first and second components after each component has been produced can be selected from a group including polyalkylbenzene, an aromatic hydrocarbon fraction, aromatic petroleum naphtha, or diesel fuel. The primary purpose of the mono- or mixed solvent is to maintain product homogeneity and efficiency. The use of solvents from this group also improves fluidity and ensures uniform distribution of the additive components in the fuel mixture. In particular, polyalkylbenzenes impart aromaticity, which increases their solubility and improves interaction with fuel hydrocarbons. Aromatic petroleum naphthas, in turn, reduce the viscosity of the mixture, promoting better fuel flow in the fuel system and thereby minimizing the risk of solidification or paraffin deposit formation.Aromatic hydrocarbon fractions and diesel fuel provide excellent dispersant solubility for pour point depressant (PDP) components and high compatibility with the PDP and fuel components. These solvents are also widely available and have low toxicity. As a result, the use of these solvents optimizes the low-temperature performance of diesel fuel and ensures reliable fuel system operation in extreme climatic conditions.

[0042] The final step in producing a pour point depressant / dispersant additive is mixing the reaction mixture of the first component and solvent (PM1) with the reaction mixture of the second component and solvent (PM2) in a mass ratio of PM1:PM2 = 1:[1-10]. Maintaining this mass ratio is critical, as deviations from the optimal proportions can weaken the dispersant's effect on the low-temperature properties of diesel fuel and affect its functionality, making the additive, which contains the dispersant, less effective when mixed with diesel fuel. An incorrectly selected ratio can lead to uneven distribution of the components, which will impair the interaction of the dispersant with the fuel and reduce the overall stability of the mixture.To achieve maximum efficiency, these reaction masses can be mixed at a ratio of PM1:PM2 = 1:[2-7], which optimizes the mutual influence of the components on improving the low-temperature properties of diesel fuel, achieving maximum dispersancy. However, depending on the final application, the ratio can also be PM1:PM2 = 1:[3-5], providing the necessary flexibility in adapting to various operating conditions and fuel requirements. Selecting the optimal ratio is important for maintaining a balance between paraffin dissolution and retention, as well as for ensuring stable and uniform dispersion of the dispersant in the fuel, thereby preventing unwanted deposits and improving overall diesel engine performance in various climatic conditions.

[0043] The dispersant can be obtained by mixing the reaction mass of the first component and the solvent and the reaction mass of the second component and the solvent at a temperature of 50 to 70 °C, which ensures that the homogenization reaction occurs completely, resulting in the formation of a spatial structure stabilized by the electrostatic forces of the polar components included in the commercial form of the dispersant.

[0044] Thus, the resulting dispersant, depending on the ratio in which the aforementioned reaction masses were mixed together, will have a ratio of the first component (K1) and the second component (K2) equal to K1:K2 = 1:[1-10], or equal to K1:K2 = 1:[2-7], K1:K2 = 1:[3-5].

[0045] The proposed dispersant-depressant-dispersant additive composition demonstrates its ability to significantly lower the pour point of diesel fuel, improve its flowability, and prevent the formation of paraffin structures that can clog fuel filters and lines. This makes it particularly useful in extreme climatic conditions. The processes for producing and mixing the components are adaptable to existing industrial methods, demonstrating compliance with industrial applicability and high efficiency criteria, facilitating their easy implementation and use in practice.

[0046] The invention can be made from known materials using known means, which indicates its compliance with the patentability criterion of “industrial applicability”.

[0047] The invention is characterized by a previously unknown set of essential features from the prior art, distinguished in that:

[0048] when performing the method for producing a dispersant depressant-dispersant additive for diesel fuel:

[0049] - the first component, which is an alkylphenol formaldehyde resin, is obtained by boiling monoalkylphenol with formaldehyde in the form of formalin, paraform or trioxane in the presence of a hydrocarbon solvent and an acid catalyst at a temperature of 80 to 150 °C for 5-6 hours;

[0050] - mix the first component with a solvent, represented by a mono- or mixed solvent, in a mass ratio of 1:1;

[0051] - a second component is obtained, which is a product of the interaction of a carboxylic acid and a mono- or dialkylamine, by heating a mixture of a carboxylic acid and a mono- or dialkylamine at a temperature of 195 to 200 °C for 5-6 hours;

[0052] - mix the second component with a solvent, represented by a mono- or mixed solvent, in a mass ratio of 1:1;

[0053] - mix the reaction mass of the first component and solvent (PM1) and the reaction mass of the second component and solvent (PM2) in a mass ratio of PM1:PM2 = 1:[1-10].

[0054] The combination of essential features of the invention allows for a significant improvement in the performance characteristics of the fuel due to the following mechanisms and properties.

[0055] The first component, an alkylphenol-formaldehyde resin obtained by polycondensation of monoalkylphenol with formaldehyde, forms a strong polymer network, which helps keep paraffin particles suspended and prevents their crystallization. This property reduces the risk of diesel fuel thickening at low temperatures. The polymer structure also enhances the fuel's resistance to physical and thermal stress.

[0056] The second component, a product of the interaction of a carboxylic acid and a mono- or dialkylamine, forms amide and ester bonds, which have both polar and non-polar properties. Polar groups improve solubility and solvent power for various compounds, including hydrocarbon components of the fuel. This interaction enhances the lubricating properties of diesel fuel, improving flow and reducing friction in the fuel system, which reduces engine wear.

[0057] The K1:K2 component weight ratio of 1:[1-10] allows for variable component proportions to achieve optimal performance under specific operating conditions. Maintaining this ratio ensures a balance between fuel stability (provided by resin K1) and fluidity (provided by component K2). This ensures maximum effectiveness in preventing wax formation and maintaining fuel fluidity at various temperatures and engine loads.

[0058] This ensures the achievement of a technical result consisting in improving the properties of a set of operational characteristics of diesel fuel when using the developed dispersant as part of a depressant-dispersant additive.

[0059] The invention has a set of essential features previously unknown in the prior art, which indicates its compliance with the patentability criterion of “novelty”.

[0060] The prior art discloses a dispersant depressant-dispersant additive for diesel fuel, which is either an alkylphenol formaldehyde resin or amine salts and / or amides, which are products of the interaction of aliphatic or aromatic amines, preferably long-chain aliphatic amines, with aliphatic or aromatic mono-, di-, tri- or tetracarboxylic acids or their anhydrides.

[0061] However, the prior art does not know a dispersant for a pour point depressant additive for diesel fuel, which is a 50% solution of two components in a mass ratio with each other of 1:[1-10], wherein the first component is represented by an alkylphenol formaldehyde resin, and the second component is represented by a product of the interaction of a carboxylic acid and a mono- or dialkylamine, and which at the same time provides flexibility in the use of such a dispersant in diesel fuel compositions with different compositions and qualities, due to the possibility of varying the amount of one or another component in the dispersant composition, and also provides better implementation of the dispersant into the fuel composition as part of a pour point depressant additive, due to the presence of a solvent in its composition.

[0062] In view of this, the invention meets the patentability criterion of “inventive step”.

[0063] The invention is explained by the following figures.

[0064] Fig. 1 - Conditions for obtaining a dispersant depressant-dispersant additive for diesel fuel.

[0065] To illustrate the possibility of implementation and a more complete understanding of the essence of the invention, an embodiment of it is presented below, which can be changed or supplemented in any way, while the present invention is in no way limited to the presented embodiment.

[0066] The dispersant was obtained as follows:

[0067] - the first component was obtained and mixed with a solvent;

[0068] - the second component was obtained and mixed with the solvent;

[0069] - the reaction mass of the first component and solvent and the reaction mass of the second component and solvent were mixed.

[0070] The process of obtaining the dispersant is carried out using equipment that includes a reactor with a container equipped with a mechanical stirrer, a heater, a device for azeotropic distillation of water and a thermometer.

[0071] Below are examples of how to obtain a dispersant.

[0072] Example 1.

[0073] To obtain the first component, the following raw materials were placed in a reactor vessel: monoalkylphenol (MP), represented by pure monoalkylphenol in which the alkyl group contained 10 carbons located in both the para- and ortho-positions of the phenolic ring; formaldehyde in the form of paraformaldehyde; a hydrocarbon solvent (octane); and a catalyst (maleic acid). The raw materials were taken in the following weight ratio: 1.1 parts MAP, 0.1 parts formaldehyde, 1.1 parts hydrocarbon solvent, and 0.01 parts catalyst.

[0074] The mixture of raw components was then boiled at 150°C. While heating the mixture, upon reaching 80°C, azeotropic distillation of the water formed during the reaction began. Upon reaching 130°C, azeotropic distillation ceased, and boiling of the mixture continued until it reached 150°C. The boiling process lasted for 5 hours. Upon completion of the boiling process, the hydrocarbon solvent was distilled off. The hydrocarbon solvent was distilled off in two stages: the first at atmospheric pressure, and the second at subatmospheric pressure (10-30 mmHg) to remove residual hydrocarbon solvent. Upon completion of the hydrocarbon solvent distillation process, the first component was obtained.After this, the first component was mixed with a solvent, represented by polyalkylbenzene with a final boiling point of no higher than 340 °C, in a mass ratio of the first component to the solvent of 1:1, and the resulting reaction mass was removed from the reactor vessel.

[0075] To obtain the second component, a carboxylic acid represented by nitrilotriacetic acid and a mixture of pure mono- and dialkylamines containing amines with an alkyl group length of 18 carbon atoms were placed in a reactor vessel. These components were taken in an equimolar ratio of each amine (A) of the mixture of pure mono- and dialkylamines to each carboxyl function (CF) of the carboxylic acid, CF:A = 1:1. The above-mentioned components were then heated to a temperature of 200 °C for 6 hours with constant stirring, thereby obtaining the second component. Subsequently, the second component was mixed with a solvent represented by polyalkylbenzene with a final boiling point of no higher than 340 °C, in a weight ratio of the first component to the solvent of 1:1.

[0076] To obtain a dispersant, the reaction mass of the first component and solvent (PM1) was placed in a container with the reaction mass of the second component and solvent (PM2) in a ratio of PM1:PM2 = 1:4 and the resulting mixture was heated to a temperature of 70 °C with constant stirring, thus homogenizing the components of the dispersant.

[0077] Examples 2-9 for obtaining the dispersant were carried out similarly to Example 1 in accordance with the data indicated in the table presented in Fig. 1. The process of obtaining the dispersant for each of Examples 2-9 was accompanied by the following changes.

[0078] At the stage of obtaining the first component, the mass ratio of the raw materials was changed, in particular, monoalkylphenol, formaldehyde, hydrocarbon solvent and catalyst were taken in the following mass ratios:

[0079] – monoalkylphenol was taken in an amount of 0.9 to 1.1 parts;

[0080] – formaldehyde was taken in an amount from 0.09 to 0.13 parts;

[0081] – hydrocarbon solvent was taken in an amount of 0.9 to 1.1 parts;

[0082] – the catalyst was taken in an amount from 0.005 to 0.02.

[0083] Also, at the stage of obtaining the first component, the type of monoalkylphenol was changed. In particular, in addition to pure monoalkylphenol, in which the alkyl group contained N=10 carbons (C 10 ), pure monoalkylphenol was also used, in which the alkyl group contained N=1÷20 carbons (C N ), and also used a mixture of monoalkylphenols in which the alkyl group contained from 1 to 20 carbons (C 1-20 ).

[0084] Also during the production of the first component, the formaldehyde was modified. Specifically, in addition to formaldehyde in the form of paraformaldehyde (P), formaldehyde in the form of formalin (F) or trioxane (T) was also used.

[0085] Also, during the first component production stage, the type of hydrocarbon solvent used was varied. Specifically, in addition to octane (O), benzene (B), toluene (T), xylene (X), or heptane (H) were also used as hydrocarbon solvents.

[0086] Also, during the production of the first component, the catalyst type was changed. Specifically, in addition to maleic acid (M), p-toluenesulfonic acid (p-T), hydrochloric acid (HCl), oxalic acid (Ox), or succinic acid (S) were also used as catalysts.

[0087] In addition, at the stage of obtaining the first component, the reaction temperature was changed in the range from 80 to 150 °C and the duration of this reaction was changed in the range of 5-6 hours.

[0088] Additionally, during the first component production stage, the temperature for azeotropic distillation of water formed during the boiling of the raw materials was varied. Specifically, in addition to azeotropic distillation, the temperature range from 80 to 130°C was varied.

[0089] When diluting the first component, the solvent type of the first component was varied. Specifically, in addition to polyalkylbenzene (PAB) with a final boiling point no higher than 340°C, aromatic hydrocarbon fraction (AHF), aromatic naphtha A150 / 330 (AN), or diesel fuel (DF) were also used as the first component solvent.

[0090] At the stage of obtaining the second component, the amounts of carboxylic acid and mono- or dialkylamine used were varied. Specifically, in addition to taking the carboxylic acid and mono- or dialkylamine in an equimolar ratio of each amine (A) of the mixture of mono- and dialkylamines to each carboxyl function (CF) of the carboxylic acid, they were also taken in a molar ratio of CF:A = [1-4]:1, that is, when the amount of amines was insufficient in relation to the carboxyl functions of the carboxylic acid, which in this case required further neutralization, which consisted of introducing an additional amount of amine or a mixture of amines into the reaction mixture in an amount equal to the number of unreacted carboxyl groups.

[0091] Also, during the second component production stage, the type of carboxylic acid used was varied. Specifically, in addition to nitrilotriacetic acid (NTA), other carboxylic acids used included ethylenediaminetetraacetic acid (EDTA), the product of EDTA alkylation at nitrogen atoms with monochloroacetic acid (EDTA-M), aromatic tetracarboxylic acids represented by benzene and naphthalene tetracarboxylic acids (BTC and NTC), or products of exhaustive or partial C-alkylation of malonic or succinic acids with haloacetic acid (HA or HA).

[0092] Also, at the stage of obtaining the second component, the type of mono- or dialkylamine used was changed. In particular, in addition to a mixture of pure mono- and dialkylamines, which contain amines with an alkyl group length of N = 18 carbon atoms (C 18), a mixture of pure mono- and dialkylamines was also used, in which amines with an alkyl group length of N=5÷30 carbon atoms (C) are present. N ), or a mixture of mono- and dialkylamines, which contain amines with an alkyl group length of 5 to 30 carbon atoms (C 5-30 ).

[0093] At the stage of obtaining the second component, the reaction temperature was changed in the range from 195 to 200 °C and the duration of this reaction was changed in the range of 5-6 hours.

[0094] When diluting the second component, the type of solvent for the second component was varied. Specifically, in addition to polyalkylbenzene (PAB) with a final boiling point no higher than 340°C, aromatic hydrocarbon fraction (AHF), aromatic naphtha A150 / 330 (AN), or diesel fuel (DF) were also used as the second component solvent.

[0095] When obtaining a dispersant by mixing the reaction mass of the first component and solvent (PM1) and the reaction mass of the second component and solvent (PM2), the amount of reaction masses was changed within the ratio PM1:PM2 = 1:[1-10], and the temperature of the homogenization reaction was also changed within the range of 50-70 °C.

[0096] The dispersants obtained according to Examples 1-9 had the following physicochemical characteristics:

[0097] Appearance Transparent liquid from orange to red color without signs of stratification, suspension, sediment and surface film Density at 20 °C, kg / m3, no more than 850-930 Kinematic viscosity mm2 / s at 50 °C, mm2 / s, no more than 5,0-20,0 Flash point, °C, not less than 61

[0098] Also, the dispersants obtained in Examples 1-9 were used to prepare a depressant-dispersant additive for introduction into diesel fuel and to determine its low-temperature performance characteristics.

[0099] Improvement of low-temperature performance characteristics of diesel fuel is due to such indicators as sedimentation stability, determined according to STO 11605031-041-2010 (method of JSC VNII NP), and the filter plugging point (CFPP), determined according to GOST 22254-92. To test low-temperature performance characteristics, an additive was added to the base diesel fuel in an amount of 400 mg / kg of base diesel fuel, containing 200 mg of the dispersing component obtained according to examples 1-9, and 200 mg of a commercially available depressant of industrial production. The test results are presented in the table shown in Fig. 2.

[0100] The test results show that diesel fuel containing the additive of the described composition has a full range of performance properties that make it suitable for use in winter conditions at sub-zero temperatures.

[0101] This ensures the achievement of a technical result consisting in improving the properties of a set of operational characteristics of diesel fuel when using the developed dispersant as part of a depressant-dispersant additive.

Claims

1. A method for producing a dispersant depressant-dispersant additive for diesel fuel, during which: - the first component, which is an alkylphenol-formaldehyde resin, is obtained by boiling monoalkylphenol with formaldehyde in the form of formalin, paraform or trioxane, in the presence of a hydrocarbon solvent and an acid catalyst at a temperature of 80 to 150 °C for 5-6 hours; - the first component is mixed with a solvent, represented by a mono- or mixed solvent, in a mass ratio of 1:1; - a second component is obtained, which is a product of the interaction of a carboxylic acid and a mono- or dialkylamine, by heating a mixture of a carboxylic acid and a mono- or dialkylamine at a temperature of 195 to 200 °C for 5-6 hours; - the second component is mixed with a solvent, represented by a mono- or mixed solvent, in a mass ratio of 1:1; - mix the reaction mass of the first component and solvent (PM1) and the reaction mass of the second component and solvent (PM2) in a mass ratio of PM1:PM2 = 1:[1-10].

2. The method according to paragraph 1, characterized in that, when obtaining the first component, monoalkylphenol, formaldehyde, hydrocarbon solvent and catalyst are taken in the following mass ratio: monoalkylphenol: 0.9 to 1.1 parts; formaldehyde: from 0.09 to 0.13 parts; hydrocarbon solvent: 0.9 to 1.1 parts; catalyst: from 0.005 to 0.02 parts.

3. The method according to claim 1, characterized in that the monoalkylphenol used to obtain the first component is a mixture of monoalkylphenols in which the alkyl group contains from 1 to 20 carbon atoms or is a pure monoalkylphenol in which the alkyl group contains N=1-20 carbon atoms.

4. The method according to claim 3, characterized in that the monoalkylphenol used to obtain the first component is a pure monoalkylphenol in which the alkyl group contains N=3-15 carbon atoms.

5. The method according to claim 4, characterized in that the monoalkylphenol used to obtain the first component is a pure monoalkylphenol in which the alkyl group contains N=7-12 carbon atoms.

6. The method according to claim 1, characterized in that the hydrocarbon solvent used to obtain the first component is selected from the group including benzene, toluene, xylene, heptane and octane.

7. The method according to claim 1, characterized in that the catalyst used to obtain the first component is selected from the group consisting of p-toluenesulfonic acid, hydrochloric acid, oxalic acid, maleic acid and succinic acid.

8. The method according to claim 1, characterized in that when boiling monoalkylphenol with formaldehyde in the presence of a hydrocarbon solvent and a catalyst, azeotropic distillation of water is carried out at a temperature of 80 to 130 °C.

9. The method according to claim 1, characterized in that when mixing the first component with the solvent, the solvent is selected from a group including polyalkylbenzene, an aromatic hydrocarbon fraction, aromatic petroleum or diesel fuel.

10. The method according to paragraph 1, characterized in that, when obtaining the second component, the carboxylic acid and mono- or dialkylamine are taken in a molar ratio of each amine of the mixture of mono- and dialkylamines (A) to each carboxyl function of the carboxylic acid (CF) constituting CF:A = [1-4]:

1.

11. The method according to claim 1, characterized in that the carboxylic acid used to obtain the second component is selected from the group comprising ethylenediaminetetraacetic acid (EDTA), the product of alkylation of EDTA at nitrogen atoms with monochloroacetic acid, aromatic tetracarboxylic acids represented by benzene and naphthalenetetracarboxylic acids, nitrilotriacetic acid and products of exhaustive or partial C-alkylation of malonic or succinic acids with haloacetic acid.

12. The method according to claim 1, characterized in that the mono- or dialkylamine used to obtain the second component is represented by a mixture of mono- and dialkylamines in which amines with an alkyl group length of 5 to 30 carbon atoms are present, or is represented by a mixture of pure mono- and dialkylamines in which amines with an alkyl group length of N=5-30 carbon atoms are present.

13. The method according to claim 12, characterized in that the mono- or dialkylamine used to obtain the second component is represented by a mixture of pure mono- and dialkylamines, in which amines with an alkyl group length of N=8-25 carbon atoms are present.

14. The method according to claim 13, characterized in that the mono- or dialkylamine used to obtain the second component is a mixture of pure mono- and dialkylamines, in which amines with an alkyl group length of N=12-18 carbon atoms are present.

15. The method according to claim 1, characterized in that when mixing the second component with the solvent, the solvent is selected from a group including polyalkylbenzene, an aromatic hydrocarbon fraction, aromatic petroleum or diesel fuel.

16. The method according to paragraph 1, characterized in that the reaction mass of the first component and solvent (PM1) and the reaction mass of the second component and solvent (PM2) are mixed in a mass ratio of PM1:PM2 = 1:[2-7].

17. The method according to paragraph 16, characterized in that the reaction mass of the first component and solvent (PM1) and the reaction mass of the second component and solvent (PM2) are mixed in a mass ratio of PM1:PM2 = 1:[3-5].

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