Condensed detergent and method of preparation

Abstract

This invention relates to a condensation-type detergent and its preparation method. The method uses alkylphenols, formaldehyde, salicylic acid, calcium hydroxide, and diluent oil as raw materials, and prepares the condensation-type detergent product through steps such as condensation reaction, neutralization reaction, and carbonation reaction. The condensation-type detergent product prepared by this invention is synthesized under conditions where alcohol compounds are used as accelerators, and unique additives are introduced, resulting in a condensation-type detergent product with an alkalinity of over 300 mg KOH / g and a calcium content of over 10.5% synthesized in a certain proportion. The product synthesized by this invention exhibits excellent high-temperature detergency and antioxidant properties, making it a high-performance lubricant additive.

Description

Technical Field

[0001] This invention belongs to the field of lubricating oil additive technology, specifically relating to a condensation-type detergent, and more specifically, to a method for preparing the detergent. Background Technology

[0002] Metal detergents are among the most important functional additives in lubricant formulations. They inhibit oil oxidation and deterioration under high-temperature engine operating conditions, reducing the formation of high-temperature deposits on the piston ring surface. Furthermore, they adsorb and encapsulate solid particulate contaminants, dispersing them within the lubricating oil, and wash away high-temperature deposits from the piston ring surface, ensuring a clean engine interior. Due to these unique functions, metal detergents have played a crucial role in the modern lubrication industry.

[0003] With increasingly stringent environmental regulations, the development of low-sulfur, low-phosphorus, and high-performance lubricants has become a major direction for lubricant development. Consequently, new requirements have been placed on lubricant additives, and low-phosphorus, low-sulfur, and high-performance additives will inevitably become a new trend in their development.

[0004] Among commonly used metal detergents, alkylbenzene sulfonate detergents are the most widely used. However, their sulfur content does not meet the requirements for low SAPS (low sulfur, low phosphorus, low ash) in additives, and alkylbenzene sulfonate detergents themselves lack antioxidant properties. In contrast, alkylphenol salt detergents and alkyl salicylate detergents do not contain sulfur or phosphorus, thus meeting the requirements for low SAPS (low sulfur, low phosphorus, low ash) in additives. However, while alkylphenol salts have some detergency, their detergency is relatively weak and they are difficult to carbonate to obtain high-base-value products. Alkyl salicylate detergents have excellent detergency, but their antioxidant properties are insufficient to meet the increasingly stringent requirements of oil products, limiting their application and making them difficult to widely use in the formulation of various engine oils. Summary of the Invention

[0005] The purpose of this invention is to provide a condensation-type detergent that solves the problems of insufficient cleaning and antioxidant properties in the prior art.

[0006] The technical solution adopted in this invention is:

[0007] This high-alkalinity condensation-type detergent product, with a total base value exceeding 300 mg KOH / g, is prepared by using alkylphenols, diluent oil, salicylic acid, formaldehyde solution, alkaline catalyst, calcium hydroxide, alcohol accelerator, solvent, and additives as raw materials, and through three reaction processes—condensation, neutralization, and carbonation—in a specific ratio. Compared to traditional alkylbenzene sulfonate and alkyl salicylate detergents, this product exhibits superior high-temperature detergency and antioxidant properties, meeting the requirements of high-grade and long-life engine oils, and is a high-performance lubricant additive.

[0008] A condensation-type detergent has the following structural formula:

[0009]

[0010] R represents an alkyl carbon chain.

[0011] The invention is further characterized by:

[0012] Furthermore, R is the C5-C of the alkyl carbon chain. 15 .

[0013] Another object of the present invention is to provide a method for preparing a condensation-type detergent, which uses the following raw materials:

[0014] Based on 100 parts by weight of alkylphenol, the following components are used: diluent oil: 90-150 parts, alkaline catalyst: 1-10 parts, salicylic acid: 15-25 parts, formaldehyde solution: 20-40 parts, solvent: 30-100 parts, accelerator: 20-50 parts, auxiliary agent: 2-10 parts, calcium hydroxide: 40-100 parts, carbon dioxide: 25-65 parts.

[0015] The specific method is as follows:

[0016] Step 1, Condensation reaction: Add alkylphenol, diluent oil, salicylic acid and alkaline catalyst to the reaction flask or reactor and stir. After heating to 80°C, add formaldehyde solution dropwise to carry out the condensation reaction. Maintain the reaction temperature between 90 and 120°C for 2 to 6 hours. After the condensation reaction is completed, pass nitrogen gas to strip the system and remove water. Then cool the system to 40 to 60°C to obtain the formaldehyde condensation product of alkylphenol and salicylic acid.

[0017] Step 2, neutralization reaction: Continue to add measured amounts of solvent, accelerator, auxiliary agent and calcium hydroxide to the reaction vessel, and maintain the temperature at 30-60℃ for 0.5-2.0 hours for the neutralization reaction;

[0018] Step 3, Carbonation reaction: Carbon dioxide gas is continuously introduced at a constant rate, and the temperature is maintained at 30-60℃ for the carbonation reaction. Calcium hydroxide is added in two equal portions. When the molar ratio of carbon dioxide introduced to calcium hydroxide reaches 0.7-0.9:1, the remaining calcium hydroxide is added, and carbon dioxide is continuously introduced. When the molar ratio of the total amount of carbon dioxide introduced to calcium hydroxide reaches 0.9-1.1:1, the carbon dioxide introduction is stopped, the carbonation reaction ends, and the crude product is obtained.

[0019] Step 4: The crude product is heated to remove the solvent, alcohol accelerator and water, then cooled and diluted with solvent, centrifuged to remove unreacted calcium hydroxide, and finally the solvent is removed by vacuum distillation to obtain a condensation-type detergent.

[0020] Alkylphenols are nonylphenol, dodecylphenol, or pentadecylphenol.

[0021] The formaldehyde solution is an industrial grade 37%, 44%, and 50% formaldehyde solution.

[0022] The diluent is one of Group I, II or III light base oils.

[0023] The alkaline catalyst is ammonia, sodium hydroxide solution, or potassium hydroxide solution.

[0024] The alcohol accelerator is a low-carbon alcohol.

[0025] The additives are dodecylbenzenesulfonic acid, dodecyl hydroxystearic acid, dodecenyl succinic acid, oleic acid, or stearic acid.

[0026] The solvent is No. 120 solvent oil with a distillation range of 80-120℃, No. 200 solvent oil with a distillation range of 140-200℃, straight-run gasoline with a distillation range of 80-180℃, xylene, or toluene.

[0027] The beneficial effects of this invention are:

[0028] Alkylphenol and salicylic acid undergo a phenol-formaldehyde condensation reaction in the presence of formaldehyde to yield a condensation product. This condensation product, with the aid of solvents and alcohol accelerators, and subsequent neutralization and carbonation reactions with the introduction of auxiliaries, yields a high-alkalinity condensation-type detergent. Compared to traditional alkylphenol salts and alkyl salicylates, this condensation-type detergent exhibits superior high-temperature detergency and antioxidant properties. More importantly, the raw materials for synthesizing this formaldehyde condensation-type detergent are readily available, and the process is simple; a three-step reaction starting with alkylphenol is sufficient to obtain the high-alkalinity condensation-type detergent.

[0029] The condensation-type detergent product involved in this invention has extremely excellent high-temperature detergency and antioxidant properties. It can be used to formulate medium and high-grade lubricating oils, meeting the performance requirements of low phosphorus, low sulfur, and even better detergency and antioxidant properties of oils. The product has good development prospects. Detailed Implementation

[0030] The present invention will now be described in detail with reference to specific embodiments.

[0031] The structural formula of a condensation-type detergent of the present invention is as follows:

[0032]

[0033] R represents an alkyl carbon chain, specifically the C5-C of the alkyl carbon chain. 15 .

[0034] Another technical solution of the present invention is a condensation-type detergent prepared by the following method:

[0035] A method for preparing a condensation-type detergent, using the following raw materials:

[0036] Based on 100 parts by weight of alkylphenol, the following components are used: diluent oil: 90-150 parts, alkaline catalyst: 1-10 parts, salicylic acid: 15-25 parts, formaldehyde solution: 20-40 parts, solvent: 30-100 parts, accelerator: 20-50 parts, auxiliary agent: 2-10 parts, calcium hydroxide: 40-100 parts, and carbon dioxide: 25-65 parts.

[0037] The specific method is as follows:

[0038] Step 1, Condensation reaction: The reaction is carried out in a four-necked flask or reactor equipped with an electric stirrer, thermometer and condenser. Alkylphenol, diluent oil, salicylic acid and alkaline catalyst are added to the four-necked flask or reactor. Stirring is started and the temperature is raised to 80°C. Formaldehyde solution is added dropwise to carry out the condensation reaction. The reaction temperature is maintained between 90 and 120°C for 2 to 6 hours. After the condensation reaction is completed, nitrogen gas is introduced for stripping to remove water from the system. The system is then cooled to 40 to 60°C to obtain the formaldehyde condensation product of alkylphenol and salicylic acid.

[0039] The molar ratio of alkylphenol to salicylic acid is approximately 3:1.

[0040] Step 2, neutralization reaction: Continue to add measured amounts of solvent, accelerator, auxiliary agent and calcium hydroxide to the reaction vessel, and maintain the temperature at 30-60℃ for 0.5-2.0 hours for the neutralization reaction;

[0041] Step 3, Carbonation reaction: Carbon dioxide gas is continuously introduced at a constant rate, and the temperature is maintained at 30-60℃ for the carbonation reaction. Calcium hydroxide is added in two equal portions. When the molar ratio of carbon dioxide introduced to calcium hydroxide reaches 0.7-0.9:1, the remaining calcium hydroxide is added, and carbon dioxide is continuously introduced. When the molar ratio of the total amount of carbon dioxide introduced to calcium hydroxide reaches 0.9-1.1:1, the carbon dioxide introduction is stopped, the carbonation reaction ends, and the crude product is obtained.

[0042] Step 4: The crude product is heated to remove the solvent, alcohol accelerator and water, then cooled and diluted with solvent, centrifuged to remove unreacted calcium hydroxide, and finally the solvent is removed by vacuum distillation to obtain a condensation-type detergent.

[0043] The alkylphenol is nonylphenol, dodecylphenol or pentadecylphenol, with nonylphenol being preferred.

[0044] The formaldehyde solution is an industrial-grade 37% formaldehyde solution, 44% formaldehyde solution, or 50% formaldehyde solution, with the 50% formaldehyde solution being preferred.

[0045] The diluent is any one of Group I, II or III light base oils such as MVI150, HVI150, HVI W150, etc.

[0046] Salicylic acid is industrial grade salicylic acid, sublimed salicylic acid, or pharmaceutical grade salicylic acid, with sublimed salicylic acid being preferred.

[0047] The alkaline catalyst is ammonia, sodium hydroxide solution, or potassium hydroxide solution, with sodium hydroxide solution being preferred.

[0048] The additives are long-chain carboxylic acids, such as dodecylbenzenesulfonic acid, dodecyl hydroxystearic acid, dodecenyl succinic acid, or oleic acid, stearic acid, etc., with dodecyl hydroxystearic acid being preferred.

[0049] For neutralization and carbonation reactions, industrially produced fine calcium hydroxide is preferred.

[0050] Alcohol accelerators are low-carbon alcohols such as methanol, ethanol, n-propanol, isopropanol, n-butanol, and isobutanol, with methanol being preferred.

[0051] The solvent used for the carbonation reaction is No. 120 solvent oil with a distillation range of 80-120℃, No. 200 solvent oil with a distillation range of 140-200℃, straight-run gasoline, xylene, toluene, or other organic solvents with a distillation range of 80-180℃, preferably No. 120 solvent oil.

[0052] The principle of this invention is as follows:

[0053] Alkylphenol and salicylic acid undergo a phenol-formaldehyde condensation reaction under the action of formaldehyde to obtain a condensation product. The condensation product, under the action of solvent and alcohol accelerator, and with the introduction of auxiliaries, can be neutralized and carbonated to obtain a high-alkalinity condensation-type detergent.

[0054] Alcohol accelerators act as carriers for both inorganic and organic phases, enabling the liquid and solid components in the reaction mixture to mix uniformly. Simultaneously, alcohol accelerators such as methanol and calcium hydroxide can generate calcium methoxide, which is encapsulated in micelles of the normal salt. It then reacts in situ with carbon dioxide to generate calcium carbonate, which is stably encapsulated in the micelles, resulting in a high-base-value condensation product.

[0055] The additives can form stable complex normal salt micelles with alkylphenol condensation products during the neutralization reaction. By adjusting the additives, the reaction system can be optimized, the size of the micelles can be improved, the viscosity of the product can be reduced, and the performance of the product can be improved.

[0056] This invention discloses a condensation-type detergent product with a calcium content of over 10.5% and an alkalinity of over 300 mg KOH / g. The product is free of sulfur and phosphorus. It exhibits excellent high-temperature detergency and antioxidant properties, making it a high-performance lubricant additive.

[0057] Example 1

[0058] In a 500 mL four-necked flask equipped with an electric stirrer, a condenser, and a thermometer, add 100.0 g nonylphenol, 100.0 g HVI 150 diluent oil, 21.0 g sublimed salicylic acid, and 2.0 g of 20% sodium hydroxide solution. Stir and heat to approximately 80°C. Add 36.5 g of 50% formaldehyde solution dropwise over 30 minutes using a dropping funnel. Maintain the reaction temperature at 105°C for phenol-formaldehyde condensation for 4 hours. Then, introduce N2 at a purge rate of 50 mL / min to remove water from the system via N2 stripping. The reaction ends when no more water distills from the condenser, yielding the condensation product. Then cool to 55°C.

[0059] Continue adding 60.0g of 120# solvent oil, 30.0g of accelerator methanol, 5.0g of dodecyl stearic acid, and 30.0g of calcium hydroxide to the four-necked flask, and carry out a neutralization reaction at 50℃ for 1.0 hour. Then, carbon dioxide gas is introduced at a rate of 100mL / min, and a carbonation reaction is carried out at 50℃. When the carbon dioxide gas flow rate reaches 7.0L, the remaining 30.0g of calcium hydroxide is added, and carbon dioxide gas is continued to be introduced. When the carbon dioxide gas flow rate reaches 18.0L, the carbonation reaction is complete.

[0060] The system was then heated to approximately 110°C to remove some of the solvent oil, methanol, and water. The temperature was then lowered to 60°C, and the crude product from the four-necked flask was transferred to a 1L beaker. Approximately 200mL of 120# solvent oil was added for dilution, and the mixture was centrifuged at 3500 rpm for 30 minutes to separate the unreacted calcium hydroxide residue. Finally, the solvent was removed by vacuum distillation at 160°C and 10kPa to obtain the product. The product had a base value of 315 mg KOH / g, a calcium content of 11.31%, and a kinematic viscosity (100°C) of 75.23 mm. 2 / s, turbidity 24.0 JTU.

[0061] Example 2

[0062] In a 500 mL four-necked flask equipped with an electric stirrer, a condenser, and a thermometer, add 100.0 g nonylphenol, 100.0 g MVI150 diluent oil, 21.0 g sublimed salicylic acid, and 4.0 g of 10% sodium hydroxide solution. Stir and heat to approximately 80°C. Add 36.5 g of 50% formaldehyde solution dropwise over 30 minutes using a dropping funnel. Maintain the reaction temperature at 110°C for phenol-formaldehyde condensation for 4 hours. Then, introduce N2 at a purge rate of 50 mL / min to separate water from the system through the condenser. The reaction ends when no more water distills from the condenser, yielding the condensation product. Then cool to 45°C.

[0063] Continue adding 80.0g of 120# solvent oil, 25.0g of accelerator methanol, 8.0g of dodecyl stearic acid, and 30.0g of calcium hydroxide to the four-necked flask, and carry out a neutralization reaction at 50℃ for 1.0 hour. Then, carbon dioxide gas is introduced at a rate of 100mL / min, and a carbonation reaction is carried out at 50℃. When the carbon dioxide gas flow rate reaches 8.0L, the remaining 30.0g of calcium hydroxide is added, and carbon dioxide gas is continued to be introduced. When the carbon dioxide gas flow rate reaches 19.5L, the carbonation reaction ends.

[0064] The system was then heated to approximately 110°C to remove some of the solvent oil, methanol, and water. The temperature was then lowered to 40°C, and the crude product from the four-necked flask was transferred to a 1L beaker. Approximately 200mL of 120# solvent oil was added for dilution, and the mixture was centrifuged at 3500 rpm for 30 minutes to separate the unreacted calcium hydroxide residue. Finally, the solvent was removed by vacuum distillation at 160°C and 10kPa to obtain the product. The product had a base value of 320 mg KOH / g, a calcium content of 11.56%, and a kinematic viscosity (100°C) of 65.32 mmHg. 2 / s, turbidity 22.0 JTU.

[0065] Example 3

[0066] In a 500 mL four-necked flask equipped with an electric stirrer, a condenser, and a thermometer, add 100.0 g nonylphenol, 100.0 g HVI 150 diluent oil, 21.5 g sublimed salicylic acid, and 2.0 g of 20% sodium hydroxide solution. Stir and heat to approximately 80°C. Add 40.0 g of 50% formaldehyde solution dropwise over 30 minutes using a dropping funnel. Maintain the reaction temperature at 105°C for phenol-formaldehyde condensation for 5 hours. Then, purge with N2 at a rate of 50 mL / min to remove water from the system via N2 stripping. The reaction ends when no more water distills from the condenser, yielding the condensation product. Then cool to 50°C.

[0067] Continue adding 60.0g of 120# solvent oil, 30.0g of accelerator methanol, 5.0g of dodecyl stearic acid, and 40.0g of calcium hydroxide to the four-necked flask, and carry out a neutralization reaction at 50℃ for 1.0 hour. Then, carbon dioxide gas is introduced at a rate of 100mL / min, and a carbonation reaction is carried out at 50℃. When the carbon dioxide gas flow rate reaches 9.5L, the remaining 40.0g of calcium hydroxide is added, and carbon dioxide gas is continued to be introduced. When the carbon dioxide gas flow rate reaches 24.0L, the carbonation reaction ends.

[0068] The system was then heated to approximately 110°C to remove some of the solvent oil, methanol, and water. The temperature was then lowered to 60°C, and the crude product from the four-necked flask was transferred to a 1L beaker. Approximately 200mL of 120# solvent oil was added for dilution. The mixture was centrifuged at 4000 rpm for 30 minutes to separate unreacted calcium hydroxide residue. Finally, the solvent was removed by vacuum distillation at 160°C and 10kPa to obtain the product. The product had a base value of 356 mg KOH / g, a calcium content of 12.75%, and a kinematic viscosity (100°C) of 78.35 mmHg. 2 / s, turbidity 18.0 JTU.

[0069] Example 4

[0070] In a 5.0L four-necked flask equipped with an electric stirrer, a condenser, and a thermometer, add 800.0g nonylphenol, 840.0g HVI150 diluent oil, 175.0g sublimed salicylic acid, and 16.0g of 20% sodium hydroxide solution. Stir and heat to approximately 80°C. Add 290.0g of 50% formaldehyde solution dropwise over 30 minutes using a dropping funnel. Maintain the reaction temperature at 105°C for phenol-formaldehyde condensation for 5 hours. Then, introduce N2 at a purge rate of 300mL / min to separate water from the system through the condenser. The reaction ends when no more water distills from the condenser, yielding the condensation product. Then cool to 50°C.

[0071] Continue adding 600.0g of 120# solvent oil, 250.0g of accelerator methanol, 40.0g of dodecyl stearic acid, and 320.0g of calcium hydroxide to the four-necked flask, and carry out a neutralization reaction at 50℃ for 1.0 hour. Then, carbon dioxide gas is introduced at a rate of 600mL / min, and a carbonation reaction is carried out at 50℃. When the carbon dioxide gas flow rate reaches 77.0L, the remaining 320.0g of calcium hydroxide is added, and carbon dioxide gas is continued to be introduced. When the carbon dioxide gas flow rate reaches 195.0L, the carbonation reaction ends.

[0072] The system was then heated to approximately 110°C to remove some of the solvent oil, methanol, and water. The temperature was then lowered to 60°C, and the crude product from the four-necked flask was transferred to a 5L beaker. Approximately 2000mL of 120# solvent oil was added for dilution. The mixture was centrifuged at 4000 rpm for 30 minutes to separate the unreacted calcium hydroxide residue. Finally, the solvent was removed by vacuum distillation at 160°C and 10kPa to obtain the product. The product had a base value of 348 mg KOH / g, a calcium content of 12.65%, and a kinematic viscosity (100°C) of 56.37 mm. 2 / s, turbidity 28.0 JTU.

[0073] Example 5

[0074] In a 500 mL four-necked flask equipped with an electric stirrer, a condenser, and a thermometer, add 100.0 g of dodecylphenol, 110.0 g of HVI 150 diluent oil, 17.6 g of sublimed salicylic acid, and 2.0 g of 20% sodium hydroxide solution. Stir and heat to approximately 80°C. Add 36.5 g of 50% formaldehyde solution dropwise over 30 minutes using a dropping funnel. Maintain the reaction temperature at 105°C for phenol-formaldehyde condensation for 4 hours. Then, purge with N2 at a rate of 50 mL / min to remove water from the system via N2 stripping. The reaction ends when no more water distills from the condenser, yielding the condensation product. Then cool to 55°C.

[0075] Continue adding 80.0g of 120# solvent oil, 40.0g of accelerator methanol, 5.0g of dodecyl stearic acid, and 30.0g of calcium hydroxide to the four-necked flask, and carry out a neutralization reaction at 50℃ for 1.0 hour. Then, carbon dioxide gas is introduced at a rate of 100mL / min, and a carbonation reaction is carried out at 50℃. When the carbon dioxide gas flow rate reaches 7.0L, the remaining 30.0g of calcium hydroxide is added, and carbon dioxide gas is continued to be introduced. When the carbon dioxide gas flow rate reaches 17.5L, the carbonation reaction is completed.

[0076] The system was then heated to approximately 110°C to remove some of the solvent oil, methanol, and water. The temperature was then lowered to 60°C, and the crude product from the four-necked flask was transferred to a 1L beaker. Approximately 200mL of 120# solvent oil was added for dilution, and the mixture was centrifuged at 3500 rpm for 30 minutes to separate the unreacted calcium hydroxide residue. Finally, the solvent was removed by vacuum distillation at 160°C and 10kPa to obtain the product. The product had an alkalinity of 308 mg KOH / g, a calcium content of 11.10%, a kinematic viscosity (100°C) of 87.38 mm² / s, and a turbidity of 52.0 JTU.

[0077] Example 6

[0078] In a 500 mL four-necked flask equipped with an electric stirrer, a condenser, and a thermometer, add 100.0 g of pentadecylphenol, 120.0 g of HVI 150 diluent oil, 15.5 g of sublimed salicylic acid, and 2.0 g of 20% sodium hydroxide solution. Stir and heat to approximately 80°C. Add 30.0 g of 50% formaldehyde solution dropwise over 30 minutes using a dropping funnel. Maintain the reaction temperature at 105°C for phenol-formaldehyde condensation for 4 hours. Then, purge with N2 at a rate of 50 mL / min to remove water from the system via N2 stripping. The reaction ends when no more water distills from the condenser, yielding the condensation product. Then cool to 55°C.

[0079] Continue adding 80.0g of 120# solvent oil, 40.0g of accelerator methanol, 5.0g of dodecenylsuccinic acid, and 35.0g of calcium hydroxide to the four-necked flask, and carry out a neutralization reaction at 50℃ for 1.0 hour. Then, carbon dioxide gas is introduced at a rate of 100mL / min, and a carbonation reaction is carried out at 50℃. When the carbon dioxide gas flow rate reaches 8.0L, the remaining 35.0g of calcium hydroxide is added, and carbon dioxide gas is continued to be introduced. When the carbon dioxide gas flow rate reaches 21.0L, the carbonation reaction is complete.

[0080] The system was then heated to approximately 110°C to remove some of the solvent oil, methanol, and water. The temperature was then lowered to 60°C, and the crude product from the four-necked flask was transferred to a 1L beaker. Approximately 200mL of 120# solvent oil was added for dilution, and the mixture was centrifuged at 3500 rpm for 30 minutes to separate the unreacted calcium hydroxide residue. Finally, the solvent was removed by vacuum distillation at 160°C and 10kPa to obtain the product. The product had a base value of 316 mg KOH / g, a calcium content of 11.68%, and a kinematic viscosity (100°C) of 95.36 mmHg. 2 / s, turbidity 65.5 JTU.

[0081] The performance evaluation results of the condensation-type detergents prepared by the preparation methods of Examples 1-6, and the commercially available alkylbenzene sulfonate calcium detergent T106 and alkyl salicylate calcium detergent T109 are shown in Table 1.

[0082] Table 1 Performance Analysis of Condensation-Type Detergents

[0083]

[0084] Note: T106 is alkylbenzene sulfonate calcium detergent, and T109 is alkyl salicylate calcium detergent. The lower the coking rate, the better the performance in cleaning gum and varnish under high temperature conditions, the lower the heat pipe oxidation rating, and the more difficult it is for oil samples to deposit on the equipment surface, indicating better high-temperature cleaning performance; the longer the oxidation induction period, the better the antioxidant effect.

[0085] As shown in the performance analysis in Table 1, the condensation-type detergent of the present invention exhibits higher alkalinity and lower viscosity in terms of physicochemical properties, and demonstrates excellent high-temperature detergency and antioxidant properties in terms of performance. It fundamentally and significantly improves the high-temperature detergency and antioxidant properties of existing metal detergents. The product can be used to formulate medium and high-grade lubricating oils, meeting the performance requirements of low phosphorus, low sulfur, and superior detergency and antioxidant properties of engine oils. The product has good development prospects.

Claims

1. A method for preparing a condensation-type detergent, characterized in that, The structural formula of the detergent is as follows: Wherein, R is the C5-C of the alkyl carbon chain. 15 ; The detergent is prepared using the following raw materials: Based on 100 parts by weight of alkylphenol, the following components are used: diluent oil: 90-150 parts, alkaline catalyst: 1-10 parts, salicylic acid: 15-25 parts, formaldehyde solution: 20-40 parts, solvent: 30-100 parts, accelerator: 20-50 parts, auxiliary agent: 2-10 parts, calcium hydroxide: 40-100 parts, carbon dioxide: 25-65 parts. The auxiliary agent is dodecylbenzenesulfonic acid, dodecyl hydroxystearic acid, dodecenyl succinic acid, or oleic acid or stearic acid; The specific preparation method of the detergent is as follows: Step 1, Condensation reaction: Add alkylphenol, diluent oil, salicylic acid and alkaline catalyst to the reaction flask or reactor and stir. After heating to 80°C, add formaldehyde solution dropwise to carry out the condensation reaction. Maintain the reaction temperature between 90 and 120°C for 2 to 6 hours. After the condensation reaction is completed, pass nitrogen gas to strip the system and remove water. Then cool the system to 40 to 60°C to obtain the formaldehyde condensation product of alkylphenol and salicylic acid. Step 2, neutralization reaction: Continue to add measured amounts of solvent, accelerator, auxiliary agent and calcium hydroxide to the reaction vessel, and maintain the temperature at 30-60℃ for 0.5-2.0 hours for the neutralization reaction; Step 3, Carbonation reaction: Carbon dioxide gas is continuously introduced at a constant rate, and the temperature is maintained at 30-60℃ for the carbonation reaction; calcium hydroxide is added in two equal portions. When the molar ratio of carbon dioxide introduced to calcium hydroxide reaches 0.7-0.9:1, the remaining calcium hydroxide is added, and carbon dioxide is continuously introduced. When the molar ratio of the total amount of carbon dioxide introduced to calcium hydroxide reaches 0.9-1.1:1, the carbon dioxide is stopped, the carbonation reaction ends, and the crude product is obtained. Step 4: The crude product is heated to remove the solvent, alcohol accelerator and water, then cooled and diluted with solvent, centrifuged to remove unreacted calcium hydroxide, and finally the solvent is removed by vacuum distillation to obtain a condensation-type detergent.

2. The method for preparing a condensation-type detergent as described in claim 1, characterized in that, The alkylphenol is nonylphenol, dodecylphenol, or pentadecylphenol.

3. The method for preparing a condensation-type detergent as described in claim 1, characterized in that, The formaldehyde solution is an industrial-grade 37% formaldehyde solution, a 44% formaldehyde solution, or a 50% formaldehyde solution.

4. The method for preparing a condensation-type detergent as described in claim 1, characterized in that, The diluent oil is one of Group I, II or III light base oils.

5. The method for preparing a condensation-type detergent as described in claim 1, characterized in that, The alkaline catalyst is ammonia, sodium hydroxide solution, or potassium hydroxide solution.

6. The method for preparing a condensation-type detergent as described in claim 1, characterized in that, The alcohol accelerator is a low-carbon alcohol.

7. The method for preparing a condensation-type detergent as described in claim 1, characterized in that, The solvent is No. 120 solvent oil with a distillation range of 80-120℃, No. 200 solvent oil with a distillation range of 140-200℃, straight-run gasoline with a distillation range of 80-180℃, xylene, or toluene.

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