• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Graft copolymers are disclosed in which the backbone comprises a hydrocarbon polymer, such as an ethylene/ propylene copolymer and the grafted units are the residues of a monomer system comprising maleic acid or anhydride and one or more other monomers, the grafts being post-reacted with a polyamino compound. The graft copolymers impart combined detergent and viscosity index properties to lubricating oils and hydrocarbon motor fuels.
    公开号:SU1064870A3
    申请号:SU782696602
    申请日:1978-12-04
    公开日:1983-12-30
    发明作者:Ли Стамбау Роберт；Адриан Галлуццио Ричард
    申请人:Ром Энд Хаас Компани (Фирма)；
    IPC主号:
    专利说明:

    about
    4: 00 The invention relates to intramuscular compounds containing graft copolymers that are multifunctional additives for lubricating oils. In the oxidative breakdown of lubricating oils in internal combustion engines, they are formed. Partially oxidized motor fuel combustion by-products contain reactive intermediates, such as, for example, aldehydes, acids and hydroxy acids, which enter into complex condensation reactions, forming insoluble gummy materials (sludge and varnish). Lubricant compositions based on mineral lubricant mael with the addition of an oil-soluble copolymer dispersant additive — ethylene-vinyl acetate copolymer 1 or ethylene copolymer with straight chain olefins with terminal double bond 2-norbornene, hexadiene-1, C, etc. are known. 2. The disadvantages of the known compositions are There is a slight increase in dispersing properties. The purpose of the invention is to enhance the dispersing properties of the composition. The goal is achieved by the fact that a lubricating composition based on mineral lubricating oil with the addition of an oil-soluble copolymer dispersant, contains as an additive a copolymer of a saturated linear rubber-like polymer with a basic olefinic hydrocarbon chain with a monomer of maleic acid or maleic anhydride grafted to it and capable of liquefying a polymeric oil. their monome and polyamine compound having one primary or secondary amino group in the following ratio of components, wt.%: Copolymer 0.06-2.0 Mineral lubricating oil up to 100 The lubricating composition as a monomer capable of copolymerizing with maleic acid or maleic anhydride, contains alkyl esters of acrylic or methacrylic acid, styrene or at-methyl styrene. The backbone polymers can have a wide molecular weight range, for example, on the order of 10,000 to 20,000 (average molecular weight in terms of weight), the more common limit is 100,000,150,000. In general, graft copolymerization can lead to an increase in molecular weight, for example, up to 200,000-400,000 or even up to 500,000 or more. The choice of the molecular weight of the backbone polymer and the degree to which the molecular weight is allowed to increase during graft copolymerization mainly depends on the performance properties of the starting polymer and the shear stability required in the final product. Low molecular weight backbone base polymers, which are protected from a significant increase in molecular weight during grafting, can form more stable shear products of graft copolymerization and therefore require little subsequent degradation (or no need at all) in order to lower the molecular weight to providing good shear resistance. Lubricating oils containing the products offered may contain other additives to provide additional dispersing ability, adjust the viscosity and temperature characteristics, lower the pour point, high-temperature detergency, inhibit corrosion, anti-wear properties, antioxidant, anti-seize, anti-oxidant, dyeing properties or modifying friction . . Test methods dispersing ability. Asphaltene testing. This method of determining the dispersing ability of any polymer is based on the ability of the polymer to disperse asphaltenes in ordinary mineral oil. Asphaltenes are obtained by oxidizing naphthenic oil with air in the presence of trace amounts of iron salts as a catalyst, such as iron naphthenate. Preferably, the oxidation is carried out at approximately 72 hours, passing air through naphthenic oil in order to obtain a precipitate, which can be separated by centrifugation. This precipitate is freed from oil, extracted with pentane, then dissolved in chloroform, and the resulting solution is brought to a solid content of 2% (by weight or volume). If the Keobobdt 1O polymer is examined for dispersion activity, it is dissolved in standard oil, such as solvent-extracted. Neutral oil 100. Mixtures can be obtained which are approximately from 2 to 0.01% (or even less) of the polymer in oil. 10 ml of the sample mixture is processed. / At 2 ml of a standard solution of asphaltenes in chloroform. The sample and the reagent are thoroughly mixed in the sample tube, which is then placed in a forced-press furnace; with gO-lSO C, the volatile solvent is evaporated in the oven for 2 hours. Then the tube ohlachdayut and note the appearance of the sample. If the polymer has dispersing activity, then the oil will appear to be clear, although colored. Practice has shown that if the polymer does not have dispersing activity at concentrations below 2% in the specified test, it will not improve the cleanliness of the engine parts with actual testing. x engine. . Sequential crankcase ventilation test (VC). This engine test method evaluates crankcase engine oil for the presence of sludge and lacquer deposits obtained during engine operation at low and medium temperatures. In addition, this service indicates the crankcase's ability to be clean and in proper order. The test is conducted as follows. / The motor under test is completely disassembled, washed and reassembled as described. It is then placed on a test dynamometer equipped with appropriate instruments for determining speed, load and other conditions. The engine runs on certified fuel MS-08 in three cycles. In the first cycle, the engine runs for 120 minutes at. high output power and moderate temperatures of oil and water and poor air-fuel mixtures. In the second cycle, the drive works for another 75 minutes at high temperatures of oil and water. In the third cycle, the engine additionally runs for 45 minutes at low o6opiOTax, low temperatures of water and oil on a rich mixture of fuel and air. Four series are held every day. each lasting 4 hours, until the 48 series passes (192 engine work). At the end of the test, the engine is completely disassembled in order to determine the degree of wear and deposition of sludge, varnish and soot on the valves. In addition, the shutdown of crankcase ventilation valves / oil rings and oil strainer was determined. This test evaluates the dispersion characteristics of the sludge with lubricating oil under conditions of low and medium temperature operation. . Example 1. L. Preparation of a pre-twisted copolymer. . A sample of a copolymer of ethylene and propylene 50/50 in the amount of 350 g (Epkar50b company Tudrich Chemical companies) is loaded into a flask of 5 liters, containing 1050 g of o-dichlorobenzene. After purging with nitrogen, the contents of the flask are heated approximately up to and stirred using a metal stirrer such as Cu in order to form a homogeneous solution. During this stage and throughout the whole cycle, the flask is purged with nitrogen. A homogeneous solution is obtained within 2 hours. The polymer solution is then cooled to 80 ° C and 35., O g of methyl methacrylate (MMA) and 17.5 g of maleic anhydride (MAI) are added at this temperature. These monomers are thoroughly mixed. In solution for 35 minutes. A mixture of 1.75 g of initiator (tert-butyl perbenzoate) in 25 g of 0-dichlorobenzene is then added. Then the temperature is increased so that the reaction mixture is heated to 140 ° C for 45 minutes. Approximately when the grafting reaction starts, on. indicating an increase in viscosity: solution. The temperature of the solution is maintained at 140 ° C for 1 hour to do this. In order to complete the grafting reaction stage, to dilute 1500 g of neutral viscous oil 100. Then, the flow of nitrogen is stopped and the apparatus for stripping under vacuum is connected, equipped with a condenser and a receiver. The solution is stripped at a pressure of 1 mm Hg. The total stripping time is about 3 hours. Analysis of a polymer sample by IR spectroscopy confirms the presence of MMA and MAI in the resulting polymer product. A titration of the polymer solution indicates that 89.1% of the loaded MAN dovetailed to the polymer. Analysis of the distillate obtained by stripping shows that 88.5% of the loaded MMA was grafted. The grafted olefin polymer contains 8.9% MMA and 4.5% MAN. B. Getting a product of a tsego transform. 3500 g of a polymer solution with a concentration of 8.4% v, obtained in Part A, is loaded into a 5 L flask equipped with a thermometer, a stirrer, and nitrogen injected. Heating is carried out in a stream of nitrogen. Upon reaching 140c, 21.6 g of N- (Zr-aminopropyl) morpholine (NAnM) was added to the polymer solution. After 15 min, the viscosity of the solution increases. 2 hours after the NAPM is added, the viscosity of the solution returns to its original value, probably. due to the fact that the amino acid is converted into an imide. The solution is additionally heated with stirring for 16 hours, after which the nitrogen input is replaced by a condenser and a receiver, and a non-registered LAPM is vacuum distilled. Approximately 1 hour at a pressure of 2 mm Hg. Art. the entire unreacted NAIIM is removed. After stripping, the solution is homogenized at a pressure of 1120 atm in a Coib Saie 3 device with a triple pump of 2150 atm in order to lower the molecular weight of the polymer. An analysis of the sample of the product obtained showed that the Kjeldahl nitrogen content was 0.76%, which indicates a content of 6.1% LAPM in the polymer in the form of maleimide. Analysis by the method of IR-spectroscopy confirm the formation of imide, and the bands corresponding to the residual anhydride are practically absent. Using the method described above for testing the dispersibility of standard asphaltenes, 0.0625 g of polymer product was found to disperse about 4% asphaltenes at. SAE 10/40 oil is obtained by mixing 12.4% by weight of the final homogenization concentrate of the polymer imide, 1.5% by weight of commercial antiwear additive (dialkyl dithiophosphate of zinc) and, in addition, 2.0% magnesium sulfonate in the feedstock for lubricating oil from the mid-continental fraction, solvent purified. As a result, this oil contains 1.04% of a copolymer product. When testing VC on the engine described above, the following indicators were achieved after 200 hours of testing: 9.0 sludge, 8.3 varnishes and 7.2 varnishes on the piston skirt. EXAMPLE 2 The procedures of Example 1 are repeated in all cases, except for using L, L-dimethylaminopropylamine (K, K-DMAPA) in an amount of 22.5 g instead of N- (3-aminopropyl) morpholine. and the polymer product of part A is used in the form of a solution with a concentration of 9.8%. Analysis of the final product showed a Kjeldahl nitrogen content of 0.4%, which indicates the content of N, N-DMAP, expressed as maleimide, 6.1%. An IR analysis of the isolated polymer shows the formation of an imide and the absence of residual anhydride. Using the above test method for testing the dispersibility of standard asphaltenes, 0.0625 g of polymer product was found to disperse 0.4% of asphaltenes at 150% SAE 10/40 oil. receive, see 14.6% by weight of the product of final homogenization (1.43% of polymer in the final mixture), 1.5% by weight of commercial antiwear additive (zinc dialkyldithiophosphate) and, moreover, 2.0% of calcium sulfonate in the mid-continental purified solvent raw materials for the production of lubricating oil. When testing VC on the engine described above, the following indicators were achieved after 192 hours of testing: 9.6 sludge, 8.4 varnishes and 7.9 varnishes on the piston skirt. EXAMPLE 3 The procedure of Example 1 is repeated in all respects, except for using instead of N- (3-aminopropyl) morpholine, 4-aminomethylpyridine (AMP, 30.0 g) and using a polymer product, Polystyrene A. in the form of a 12.3% solution. Analysis of the final product showed the presence of nitrogen by Kjeldahl 0.82%, which indicates the content of the AMP, equal to 5.6%, expressed as maleimide. IR analysis confirmed the formation of imide and the absence of Residual anhydride. Using the standard test method described above for the dispersibility of asphaltenes, 0.125 g of polymer product is dispersed at 150 ° C to find 0.4% asphaltenes. SAE 10/40 oil is obtained by mixing 11.2% by weight of the product of final homogenization (1.35% of polymer in the final formulation of oil), 1.5% by weight of marketable antiwear additive of dialkyl dithiophosphate of zinc and, moreover, 2.0% of sulfonate calcium in the mid-continental solvent refined raw material for the production of lubricating oil. When tested on the engine described above, the following indicators were achieved through LB2 h: 9.7 sludge, 8.0 varnish and 7.4 varnish on the piston skirt. Example 4. Part A of Example 1 is repeated in all cases except for the fact that styrene (20.0 g) is used instead of MMA. The analysis shows that the graft copolymer contains 5.0% styrene and 4.5% MAI. The graft copolymer product is reacted with N- (3-aminopropyl) morpholine almost the same as described in Part B of Example 1. The final product contains about 6.0% of the shed product and exhibits dispersing ability when tested with asphaltene, as described above. . Examples 5-9. Part A of Example 1 is repeated in all respects, except that methyl acrylate (35-, O g) is used instead of MMA as a graftable monomer along with maleic anhydride; The graft copolymer product is then reacted with the amines listed in Table. 1, under conditions substantially identical to those described in Part B of Example 1, except that the target graft copolymers thus obtained are not homogenized in order to reduce the molecular weight (dispersibility does not depend on increasing stability under shear, given by homogenization) V In table. Figures 1 and 2 show the numerical characteristics of dispersing properties, which were obtained in tests with asphaltenes. All products after the interaction had dispersing activity. In addition, the products provided an increase in viscosity index imparted by the main chain polymer when used in lubricating oils. Table 1
    N, N-Dimethylaminopropylaminb
    N- (2-Aminoethyl) morpholine5
    L- (3-Aminopropyl) morpholine .4
    1- (2-Aminoethyl) -2-metip-2-imidazolin1
    N- (5-Aminopentyl) -2,5.-Dimethylpyrrole
    N-Phenol Urea1
    N- (2-Aminoethyl) morfsLIN3
    2.0
    1.0
    0.5
    0.25
    0.12
    0.06
    PRI me R s 10 - 16. Given in table. 1 amines (examples 10-16) interact with the product of example 1 part A according to the method, in all aspects identical to part B of example 1, with the exception that there is no homogenization. As can be seen from the table according to the test dispersing ability
    5 asphaltenes products provide a satisfactory dispersing ability of lubricant numbers. In addition, the products provide an improvement in viscosity index, mainly
    0. Thankful to the polymer of the main chain.
    权利要求:
    Claims (2)
    [1]
    1. LUBRICANT COMPOSITION based on mineral lubricating oil with the addition of an oil-soluble copolymer dispersant, which is different. in order to increase the dispersing properties of the composition, as an additive, it contains a copolymer of a saturated linear rubbery polymer with a basic olefinic hydrocarbon chain grafted with maleic acid or maleic anhydride monomer and capable of copolymerizing with them a monomer and a polyamine compound having one primary or secondary amino group in the following ratio of components, wt.%:
    Copolymer 0.06-2.0
    Mineral lubricating oil 'Up to 100
    [2]
    2. Composition by π. 1, characterized in that as a monomer capable of copolymerization with maleic acid or with maleic anhydride, it contains C and -C t2 - alkyl esters of acrylic or methacrylic acid., Styrene or ct-methylstyrene.
    »SU„ „1064870
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US05/857,079|US4160739A|1977-12-05|1977-12-05|Polyolefinic copolymer additives for lubricants and fuels|
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