CN112625777B - Preparation method of lubricating oil antiwear dispersant - Google Patents
Preparation method of lubricating oil antiwear dispersant Download PDFInfo
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- CN112625777B CN112625777B CN201910905781.1A CN201910905781A CN112625777B CN 112625777 B CN112625777 B CN 112625777B CN 201910905781 A CN201910905781 A CN 201910905781A CN 112625777 B CN112625777 B CN 112625777B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M159/00—Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
- C10M159/12—Reaction products
- C10M159/16—Reaction products obtained by Mannich reactions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M155/00—Lubricating compositions characterised by the additive being a macromolecular compound containing atoms of elements not provided for in groups C10M143/00 - C10M153/00
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
Abstract
A preparation method of an antiwear dispersant for lubricating oil comprises the following steps: (1) preparation of non-phosphorus-sulfur type molybdate, (2) preparation of polyethylene polyamine containing molybdate by Mannich reaction, and (3) preparation of molybdenum modified antiwear dispersant. Among the preferred aminophenols are 4-aminophenol, 2-aminophenol and 4- (3-carbazolylamino) phenol; preferred molybdenum reagents are molybdenum carbamate, molybdenum trioxide, ammonium molybdate. The preparation method comprises the steps of firstly grafting a non-phosphorus-sulfur-molybdenum reagent onto aminophenol, then utilizing Mnnich reaction of the aminophenol and polyethylene polyamine to prepare a composite reagent bag containing molybdate-containing polyethylene polyamine modification, and then adding the composite reagent bag into various polyisobutylene maleic anhydrides according to requirements. The production process is simple and easy to operate, high in controllability, simple in post-treatment process and low in production cost, different series of molybdenum modified antiwear dispersant products can be prepared according to specific needs, and the products have excellent oil sludge dispersibility and wear resistance.
Description
Technical Field
The invention relates to a preparation method of a dispersant, in particular to a preparation method of an antiwear dispersant for lubricating oil, belonging to the field of lubricating oil additives.
Background
Friction, wear and lubrication are inevitable problems that must be properly solved in the design, manufacture, use and maintenance of automobiles. Studies have shown that 60% of engine failures are caused by wear and more than 30% of energy consumption is caused by friction. The current methods for improving the friction wear mainly comprise two methods: firstly, on the premise of keeping the fluid lubrication or mixed lubrication state, the shear stress is reduced by improving the rheological property of the lubricant (such as reducing the viscosity of oil products); and secondly, adding additives into the oil product to reduce the friction factor under the states of boundary lubrication and mixed lubrication. In engine oil, Zinc Dialkyl Dithiophosphate (ZDDP) and an ashless dispersant are taken as the two most important additives, and the ZDDP has good oxidation resistance and wear resistance; the ashless dispersant has good peptization and dispersion effects on solid particles such as carbon deposit, soot and the like of an engine, effectively ensures the low-temperature dispersion performance of internal combustion engine oil, particularly effectively solves the problem of low-temperature oil sludge of gasoline engine oil to prevent sludge and varnish accumulation, and along with the high standard requirements of environmental regulations, the progress of synthesis technology and the development requirements of engines, the new engine specification has increasingly strict requirements on sulfur, phosphorus and ashless quantity in oil products, so that the application of ZDDP is severely limited, the ashless dispersant is required to have good low-temperature dispersion performance, high-temperature detergency, corrosion inhibition, oxidation resistance, wear resistance and antifriction, and the structure of the ashless dispersant is changed from low-molecular weight, single-hanging and double-hanging to multi-functionalization and high-molecular weight. The multifunctional modification such as boronation, phosphorization, esterification, Mannich benzyl amination and the like is to achieve the purposes of increasing the product functions and improving the product performance by introducing functional groups or improving the structure of partial fragments of the product on the basis of the original product.
In recent years, oil-soluble organic molybdenum is a hot spot for research on lubricating oil additives due to excellent tribological properties such as oxidation resistance and wear resistance. The molybdenum additives commonly used on the market today are mainly molybdenum dialkyldithiophosphates (MoDTP), molybdenum dialkyldithiocarbamates (MoDTC) and non-thiophosphorus type organic molybdenum. Research shows that the phosphorus-sulfur type organic molybdenum additive has excellent friction reducing and wear resisting performance, but both compounds contain sulfur and phosphorus elements, harmful pollutants can be generated in the production and use processes, and severe corrosion can be generated to metal Cu and Pb. The non-sulfur-phosphorus type organic molybdenum additive has good anti-oxidation and anti-attrition performance, does not contain sulfur and phosphorus elements, and meets the requirement of environmental protection. The introduction of molybdenum into ashless dispersant can not only improve the antioxidant and antiwear properties of the dispersant, but also reduce the use of ZDDP. Patents EP2791293B1, US4239633, US 4259194, US 4265773, US 4272387 introduce sulfur-containing organomolybdenum into ashless dispersants; patents US4324672, US4261843, US4176073, US4176074 incorporate phosphorus-sulfur free molybdenum complexes into ashless dispersants such as molybdenimines, glycol molybdates, organic polyol molybdenum complexes, and the like. The molybdenum compounds in the above patents are simply physically mixed and no specific chemical reaction occurs, so that the solubility of molybdenum in the additive is very unstable and precipitation is easily generated. In addition, patents CN106478851A, CN106221862A, CN107760412, CN106867627A and the like adopt a segmentation method to enter molybdenum element, a large amount of solvent remains in the product, the grafting ratio of molybdenum is low, most of molybdenum belongs to physical suspension, precipitates are easy to generate, the reaction process is uncontrollable, and the post-treatment is complex.
Disclosure of Invention
Aiming at the defects of low molybdenum content, poor compatibility, complex reaction process, complex post-treatment process and the like of the existing molybdenum modified ashless dispersant, the invention provides a preparation method of an antiwear dispersant for lubricating oil.
The preparation method of the antiwear dispersant for lubricating oil provided by the invention comprises the following steps:
(1) adding aminophenol and a solvent into a reactor, introducing inert gas for protection in the whole process, stirring and mixing uniformly, heating to 50-80 ℃, then adding a molybdenum reagent into the reactor, continuously reacting for 4-8 hours, heating to 100-120 ℃, removing water by gas stripping, and removing the solvent by reduced pressure distillation to obtain non-phosphorus sulfur type molybdate, wherein the molar ratio of the aminophenol to the molybdenum reagent is 1 (0.3-0.8);
(2) adding the rare polyamine, the base oil and the non-phosphorus-sulfur type molybdate prepared in the step (1) into a reactor, simultaneously adding paraformaldehyde, stirring and mixing uniformly, heating to 80-90 ℃, continuously reacting for 2-3 hours, gradually heating to 130-150 ℃, and removing water by gas stripping to obtain the molybdate-containing polyethylene polyamine, wherein the mass ratio of the rare polyamine to the base oil is (0.005-0.2): 1; the mol ratio of the polydiene polyamine, the non-phosphorus sulfur type molybdate and the paraformaldehyde is 1: (0.3-1.2): (0.4 to 1.5);
(3) adding polyisobutylene maleic anhydride and base oil into a reactor, stirring and mixing uniformly, heating to 100-120 ℃, then dropwise adding the molybdate-containing polyethylene polyamine prepared in the step (2) into the reactor within 1-2 hours, continuously reacting for 2-4 hours, heating to 150-: 1, the molar ratio of the polyisobutylene maleic acid to the molybdate-containing polyethylene polyamine is 1: (0.3-0.8).
The preparation method of the lubricating oil antiwear dispersant provided by the invention is preferably as follows: in the step (1), the molar ratio of the aminophenol to the molybdenum reagent is 1 (0.5-0.65); in the step (2), the mass ratio of the polydiene polyamine to the base oil is (0.05-0.15) to 1, and the molar ratio of the polydiene polyamine, the non-phosphorus sulfur type molybdate and the paraformaldehyde is 1 (0.5-0.86) to (0.5-1.1); in the step (3), the molar ratio of the polyisobutylene maleic acid to the molybdate-containing polyethylene polyamine is 1 (0.45-0.63).
The preparation method of the lubricating oil antiwear dispersant provided by the invention is preferably as follows: heating to 65-75 ℃ in the step (1), wherein the reaction time is 6-7 hours; in the step (2), the temperature is gradually increased to 145-150 ℃.
The preparation method of the lubricating oil antiwear dispersant provided by the invention is preferably as follows: in the step (1), the aminophenol is one or more of 2-aminophenol, 3-aminophenol, 4-aminophenol, 2-diethylaminophenol, 3-methoxyacetaminophenol, 3-hydroxy-N, N-diethylaniline, 4-dimethylaminophenol, o-acetaminophenol, 4- [ (4-amino-m-tolyl) amino ] phenol, 4- (3-carbazolylamino) phenol, p-propylamino, 3-hydroxy-N, N-dimethylaniline, 2-methylaminophenol and p-methylaminophenol.
The preparation method of the lubricating oil antiwear dispersant provided by the invention is preferably as follows: the aminophenol is 4-aminophenol, 2-aminophenol or 4- (3-carbazolylamino) phenol.
The preparation method of the lubricating oil antiwear dispersant provided by the invention is preferably as follows: in the step (1), the molybdenum reagent is one or more of molybdenum carbamate, molybdenum trioxide, ammonium molybdate, molybdenum naphthenate, molybdate, alkyl molybdenum salicylate and nitrogen-containing molybdic acid compounds.
The preparation method of the lubricating oil antiwear dispersant provided by the invention is preferably as follows: the molybdenum reagent is molybdenum carbamate, molybdenum trioxide and ammonium molybdate.
The preparation method of the lubricating oil antiwear dispersant provided by the invention is preferably as follows: in the step (2), the polyamine is one or more of diethylenetriamine, triethylene tetramine, tetraethylene pentamine and hexaethylene heptamine.
The preparation method of the lubricating oil antiwear dispersant provided by the invention is preferably as follows: in the step (1), the solvent is one or more of petroleum ether, benzene, toluene, xylene, isooctane, dichloromethane, acetone and tetrahydrofuran.
The preparation method of the lubricating oil antiwear dispersant provided by the invention is preferably as follows: the number average molecular weight of the polyisobutylene maleic anhydride in the step (3) is 800-5000.
The invention also provides a lubricating oil antiwear dispersant, which is prepared by the preparation method of the lubricating oil antiwear dispersant.
The present invention can be described in detail as follows: the preparation method of the lubricating oil antiwear dispersant provided by the invention comprises the following steps:
(1) preparing non-phosphorus-sulfur type molybdate:
adding aminophenol and a solvent into a reactor according to a certain material ratio, introducing inert gas for protection in the whole process, stirring and mixing uniformly, heating to 50-80 ℃, then adding a molybdenum reagent into the reactor, continuously reacting for 4-8 hours, heating to 100-120 ℃, removing water by gas stripping, and removing the solvent by reduced pressure distillation to obtain the non-phosphorus-sulfur molybdate.
(2) Preparation of molybdate-containing polyethylene polyamine by Mannich reaction:
adding a certain amount of polyamine, base oil and the non-phosphorus sulfur type molybdate in the step (1) into a reactor, adding paraformaldehyde in a certain proportion, stirring and mixing uniformly, heating to 80-90 ℃, reacting for 2-3 hours, gradually heating to 130-150 ℃, and removing water by gas stripping to obtain the polyethylene polyamine containing molybdate.
(3) Preparation of molybdenum modified antiwear dispersant
Adding polyisobutylene maleic anhydride and base oil into a reactor according to a certain proportion, stirring and mixing uniformly, heating to 100-120 ℃, then dropwise adding the polyethylene polyamine containing molybdate in the step (1) into the reactor within 1-2 hours, reacting for 2-4 hours, heating to 150 ℃, stripping and removing water to obtain the molybdenum modified antiwear dispersant.
According to some embodiments of the present invention, the lubricating oil antiwear dispersant prepared by the method of the present invention has the following structural formula:
wherein R is polyisobutylene, and the molecular weight is 800-5000; n is an integer of 0 to 5; x is one or more mixtures in the following structural formula.
In the step (1), the aminophenol is one or a mixture of more than two of 2-aminophenol, 3-aminophenol, 4-aminophenol, 2-diethylaminophenol, 3-methoxyacetaminophenol, 3-hydroxy-N, N-diethylaniline, 4-dimethylaminophenol, o-acetaminophenol, 4- [ (4-amino-m-tolyl) amino ] phenol, 4- (3-carbazolylamino) phenol, p-propylamino-phenol, 3-hydroxy-N, N-dimethylaniline, 2-methylaminophenol and p-methylaminophenol.
In the step (1), the solvent is one or a mixture of more than two of petroleum ether, benzene, toluene, xylene, isooctane, dichloromethane, acetone and tetrahydrofuran.
In the step (1), the molybdenum reagent is one or a mixture of more than two of molybdenum carbamate, molybdenum trioxide, ammonium molybdate, molybdenum naphthenate, molybdate, alkyl molybdenum salicylate and nitrogen-containing molybdic acid compounds.
In the step (1), the molar ratio of the aminophenol to the molybdenum reagent is 1 (0.3-0.8).
In the step (2), one or a mixture of more than two of the polyethylene polyamine diethylenetriamine, triethylene tetramine, tetraethylene pentamine and hexaethylene heptamine.
In the step (2), the mass ratio of the multi-dilute polyamine to the base oil is 0.5-20%; the mol ratio of the polydiene polyamine, the non-phosphorus sulfur type molybdate and the paraformaldehyde is 1: (0.3-1.2): (0.4-1.5).
In the step (3), the number average molecular weight of the polyisobutylene maleic anhydride is 800-5000.
In the step (3), the ratio of the polyisobutylene maleic anhydride to the base oil is 50-80%, and the molar ratio of the polyisobutylene maleic acid to the molybdate-containing polyethylene polyamine is 1: (0.3-0.8).
The preparation method comprises the steps of firstly grafting a non-phosphorus-sulfur-molybdenum reagent onto aminophenol, then utilizing Mnnich reaction of the aminophenol and polyethylene polyamine to prepare a molybdic acid-containing polyethylene polyamine modified reagent complexing agent package, and then adding the reagent to various polyisobutylene maleic anhydrides according to requirements. The production process is simple and easy to operate, high in controllability, simple in post-treatment process and low in production cost, different series of molybdenum modified antiwear dispersant products can be prepared according to specific needs, and the products have excellent oil sludge dispersibility and wear resistance.
Drawings
FIG. 1 is a block diagram of a process for preparing an antiwear dispersant for lubricating oils according to the present invention
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Preparation of molybdenum acid ester containing polyene polyamine
Example 1
(1) Adding 109g of p-aminophenol (1 mol) and 200g of ethanol into a reactor, introducing inert gas for protection in the whole process, stirring and mixing uniformly, heating to 60 ℃, then adding 98g of ammonium molybdate (0.5 mol) into a four-neck flask, reacting for 5 hours continuously, heating to 110 ℃, carrying out nitrogen gas stripping to remove water, and carrying out reduced pressure distillation to remove the solvent ethanol to obtain the non-phosphorus-sulfur type molybdate.
(2) Adding 94.5g of tetraethylenepentamine, 100g of base oil and 94g of non-phosphorus sulfur type molybdate into a four-neck flask, simultaneously adding 2g of paraformaldehyde, stirring and mixing uniformly, heating to 84 ℃, reacting for 2 hours, gradually heating to 150 ℃, and removing water by nitrogen gas stripping to obtain the molybdate-containing tetraethylenepentamine A.
Example 2
(1) Adding 109g of 2-aminophenol (1 mol) and 200g of ethanol into a four-neck flask, introducing inert gas into the flask for protection in the whole process, stirring and mixing uniformly, heating to 60 ℃, then adding 72g of molybdenum trioxide (0.5 mol) into a reactor, reacting for 7 hours continuously, heating to 130 ℃, stripping nitrogen gas to remove water, and removing solvent ethanol by reduced pressure distillation to obtain the non-phosphorus sulfur type molybdate.
(2) Adding 73g of triethylene tetramine, 100g of base oil and 70g of non-phosphorus-sulfur type molybdate into a four-neck flask, simultaneously adding 1.8g of paraformaldehyde, stirring and mixing uniformly, heating to 90 ℃, reacting for 2 hours, gradually heating to 150 ℃, and removing water by nitrogen gas stripping to obtain molybdate-containing triethylene tetramine B.
Example 3
Adding 274g of 4- (3-carbazolyl amino) phenol and 300g of ethanol into a four-neck flask, introducing inert gas for protection in the whole process, stirring and mixing uniformly, heating to 65 ℃, then adding 108g of ammonium molybdate into a reactor, reacting for 6 hours, heating to 115 ℃, stripping nitrogen to remove water, and distilling under reduced pressure to remove the solvent ethanol to obtain the non-phosphorus-sulfur molybdate.
(2) Adding 94.5g of tetraethylenepentamine, 100g of base oil and 112g of non-phosphorus sulfur type molybdate into a four-neck flask, simultaneously adding 3.6g of paraformaldehyde, stirring and mixing uniformly, heating to 84 ℃, reacting for 2 hours, gradually heating to 150 ℃, and stripping off water by nitrogen gas to obtain the molybdate-containing tetraethylenepentamine C.
Preparation of antiwear dispersant for lubricating oil
Example 4
100g of polyisobutylene maleic anhydride (saponification value of 55mgKOH/g) with the molecular weight of 2300 and 60g of base oil are added into a 250ml four-neck flask, the mixture is stirred and mixed uniformly, the temperature is raised to 110 ℃, 18g of the molybdate-containing polyethylene polyamine A described in the embodiment 1 is added into the four-neck flask dropwise within 1 hour, the reaction is continued for 3 hours, and the temperature is raised to 150 ℃ for nitrogen gas stripping and water removal, so that the molybdenum modified antiwear dispersant A1 is obtained.
Example 5
80g of polyisobutylene maleic anhydride (saponification value of 55mgKOH/g) with the molecular weight of 2300 and 80g of base oil are added into a 250ml four-neck flask, the mixture is stirred and mixed uniformly, the temperature is raised to 115 ℃, 14g of the molybdate-containing polyethylene polyamine A described in the embodiment 1 is added into the four-neck flask dropwise within 1 hour, the reaction is continued for 2 hours, and the temperature is raised to 150 ℃ for nitrogen gas stripping and water removal, so that the molybdenum modified antiwear dispersant A2 is obtained.
Example 6
100g of polyisobutylene maleic anhydride (saponification value of 55mgKOH/g) with molecular weight of 2300 and 60g of base oil are added into a 250ml four-neck flask, the mixture is stirred and mixed evenly, the temperature is raised to 110 ℃, then 15g of the molybdate-containing polyethylene polyamine B in the embodiment 2 is dripped into the four-neck flask within 0.5 hour, the reaction is continued for 3 hours, and the temperature is raised to 150 ℃ for nitrogen gas stripping and water removal, so that the molybdenum modified antiwear dispersant B1 is obtained.
Example 7
120g of polyisobutylene maleic anhydride (saponification value of 90mgKOH/g) with molecular weight of 1000 and 40g of base oil are added into a 250ml four-neck flask, the mixture is stirred and mixed evenly, the temperature is raised to 110 ℃, then 23g of the molybdate-containing polyethylene polyamine B in example 2 is dripped into the four-neck flask within 0.5 hour, the reaction is continued for 3 hours, and the temperature is raised to 150 ℃ for nitrogen gas stripping and water removal, so that the molybdenum modified antiwear dispersant B2 is obtained.
Example 8
Adding 110g of polyisobutylene maleic anhydride (saponification value of 55mgKOH/g) with molecular weight of 2300 and 50g of base oil into a 250ml four-neck flask, stirring and mixing uniformly, heating to 110 ℃, then dropwise adding 16g of the polyethylene polyamine C containing molybdates described in example 3 into the four-neck flask within 0.5 hour, continuing to react for 2.5 hours, heating to 150 ℃, and stripping with nitrogen to remove water to obtain the molybdenum modified antiwear dispersant C1.
Example 9
Adding 110g of polyisobutylene maleic anhydride (saponification value of 90mgKOH/g) with molecular weight of 1000 and 50g of base oil into a 250ml four-neck flask, stirring and mixing uniformly, heating to 110 ℃, then dropwise adding 30g of the polyethylene polyamine C containing molybdates described in example 3 into the four-neck flask within 0.5 hour, continuing to react for 2.5 hours, heating to 150 ℃, and carrying out nitrogen gas stripping to remove water to obtain the molybdenum modified antiwear dispersant C2.
The molybdenum modified antiwear dispersants obtained in examples 4 to 9 were added to CH-4 test oil, respectively, to perform a sludge speck dispersion test; 1.5 percent of molybdenum modified antiwear dispersant is added into SM base oil, and the results of a MRS-1J type four-ball friction wear performance test are shown in Table 1. The result shows that the product has excellent oil sludge dispersibility and abrasion resistance.
TABLE 1
Claims (10)
1. A preparation method of an antiwear dispersant for lubricating oil is characterized by comprising the following steps:
(1) adding aminophenol and a solvent into a reactor, introducing inert gas for protection in the whole process, stirring and mixing uniformly, and heating to 50-80 DEG C o C, adding a molybdenum reagent into the reactor, continuously reacting for 4-8 hours, and heating to 100-120 DEG C o C, gas stripping to remove water, and reduced pressure distillation to remove the solvent to obtain non-phosphorus-sulfur type molybdate, wherein the molar ratio of the aminophenol to the molybdenum reagent is 1 (0.3-0.8);
(2) adding polyethylene polyamine, base oil and the non-phosphorus sulfur type molybdate prepared in the step (1) into a reactor, adding paraformaldehyde, stirring and mixing uniformly, and heating to 80-90 DEG C o C, after continuously reacting for 2-3 hours, gradually heating to 130-150 DEG C o C, stripping to remove water to obtain the polyethylene polyamine containing molybdic acid esters, whereinThe mass ratio of the polyethylene polyamine to the base oil is (0.005-0.2): 1; the mol ratio of the polyethylene polyamine, the non-phosphorus-sulfur type molybdate and the paraformaldehyde is 1: (0.3-1.2): (0.4 to 1.5);
(3) adding polyisobutylene maleic anhydride and base oil into a reactor, stirring and mixing uniformly, and heating to 100-120 DEG o C, dropwise adding the molybdate-containing polyethylene polyamine prepared in the step (2) into the reactor within 1-2 hours, continuing to react for 2-4 hours, and heating to 150-160- o And C, stripping to remove water to obtain the lubricating oil antiwear dispersant, wherein the mass ratio of the polyisobutylene maleic anhydride to the base oil is (0.5-0.8): 1, the molar ratio of the polyisobutylene maleic anhydride to the molybdate-containing polyethylene polyamine is 1: (0.3-0.8).
2. The method of preparing an antiwear dispersant for lubricating oils according to claim 1, wherein: in the step (1), the molar ratio of the aminophenol to the molybdenum reagent is 1 (0.5-0.65); in the step (2), the mass ratio of the polyethylene polyamine to the base oil is (0.05-0.15) to 1, and the molar ratio of the polyethylene polyamine, the non-phosphorus sulfur type molybdate and the paraformaldehyde is 1 (0.5-0.86) to (0.5-1.1); in the step (3), the molar ratio of the polyisobutylene maleic anhydride to the molybdate-containing polyethylene polyamine is 1 (0.45-0.63).
3. The method of preparing an antiwear dispersant for lubricating oils according to claim 1, wherein: heating to 65-75 ℃ in the step (1) o C, the reaction time is 6-7 hours; gradually heating to 145-150 ℃ in the step (2) o And C, the number average molecular weight of the polyisobutylene maleic anhydride in the step (3) is 800-5000.
4. A method for preparing an antiwear dispersant for lubricating oil according to any one of claims 1 to 3, characterized by: in the step (1), the aminophenol is one or more of 2-aminophenol, 3-aminophenol, 4-aminophenol, 2-diethylaminophenol, 3-methoxyacetaminophenol, 3-hydroxy-N, N-diethylaniline, 4-dimethylaminophenol, o-acetaminophenol, 4- [ (4-amino-m-tolyl) amino ] phenol, 4- (3-carbazolylamino) phenol, p-propylamino, 3-hydroxy-N, N-dimethylaniline, 2-methylaminophenol and p-methylaminophenol.
5. The method of preparing an antiwear dispersant for lubricating oils according to claim 4, wherein: the aminophenol is 4-aminophenol, 2-aminophenol or 4- (3-carbazolylamino) phenol.
6. The method for preparing an antiwear dispersant for lubricating oil according to claim 1, wherein: in the step (1), the molybdenum reagent is one or more of molybdenum carbamate, molybdenum trioxide, ammonium molybdate, molybdenum naphthenate, molybdate, alkyl molybdenum salicylate and nitrogen-containing molybdic acid compounds.
7. The method of preparing an antiwear dispersant for lubricating oils according to claim 6, wherein: the molybdenum reagent is molybdenum carbamate, molybdenum trioxide and ammonium molybdate.
8. The method of preparing an antiwear dispersant for lubricating oils according to claim 1, wherein: in the step (2), the polyethylene polyamine is one or more of diethylenetriamine, triethylene tetramine, tetraethylene pentamine and hexaethylene heptamine.
9. The method of preparing an antiwear dispersant for lubricating oils according to claim 1, wherein: the solvent in the step (1) is one or more of petroleum ether, benzene, toluene, xylene, isooctane, dichloromethane, acetone and tetrahydrofuran; the inert gas is nitrogen, carbon dioxide or helium.
10. A lubricating oil antiwear dispersant is characterized in that: which is prepared by the process for preparing an antiwear dispersant for lubricating oils according to any of claims 1 to 9.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4261843A (en) * | 1979-06-28 | 1981-04-14 | Chevron Research Company | Reaction product of acidic molybdenum compound with basic nitrogen compound and lubricants containing same |
| CA1125735A (en) * | 1978-09-18 | 1982-06-15 | Esther D. Winans | Molybdenum complexes of ashless nitrogen dispersants as friction reducing antiwear additives for lubricating oils |
| CN102796592A (en) * | 2011-05-27 | 2012-11-28 | 中国石油化工股份有限公司 | Organic molybdenum additive, preparation method thereof and lubricating oil composition containing additive |
| CN106867627A (en) * | 2015-12-11 | 2017-06-20 | 中国石油天然气股份有限公司 | The preparation method of soot dispersant |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6962896B2 (en) * | 2002-05-31 | 2005-11-08 | Chevron Oronite Company Llc | Reduced color molybdenum-containing composition and a method of making same |
| EP2935543A4 (en) * | 2012-12-21 | 2016-01-27 | Chevron Oronite Co | A post-treated molybdenum imide additive composition, methods of making same and lubricating oil compositions containing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1125735A (en) * | 1978-09-18 | 1982-06-15 | Esther D. Winans | Molybdenum complexes of ashless nitrogen dispersants as friction reducing antiwear additives for lubricating oils |
| US4261843A (en) * | 1979-06-28 | 1981-04-14 | Chevron Research Company | Reaction product of acidic molybdenum compound with basic nitrogen compound and lubricants containing same |
| CN102796592A (en) * | 2011-05-27 | 2012-11-28 | 中国石油化工股份有限公司 | Organic molybdenum additive, preparation method thereof and lubricating oil composition containing additive |
| CN106867627A (en) * | 2015-12-11 | 2017-06-20 | 中国石油天然气股份有限公司 | The preparation method of soot dispersant |
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