Classifications

• • 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
  • C10M159/20—Reaction mixtures having an excess of neutralising base, e.g. so-called overbasic or highly basic products
  • C10M159/24—Reaction mixtures having an excess of neutralising base, e.g. so-called overbasic or highly basic products containing sulfonic radicals

Definitions

• the subject of the present invention is a process for the preparation of overbased metal detergent-dispersants, in particular for lubricating oils.
• the Applicant has found a method for obtaining metal detergent-dispersant additives of TBN (Total Basic Number - Standard ASTM D 2896) greater than 200, in a simple and rapid manner, in the presence of alkylene glycol in small quantities and in the absence of monoalcohol.
• TBN Total Basic Number - Standard ASTM D 2896
• the carbonation operation can be carried out in one or more times, by introducing the necessary quantity defined above of alkaline earth compound and alkylene glycol, in one or more times, each introduction of alkaline compound. earthy and alkylene glycol being followed by a carbonation operation.
• sulfurized alkylphenate denotes any solution containing from 30 to 80% by weight, preferably from 40 to 70% by weight of a sulfurized alkylphenate in a dilution oil which may or may not be the same as that used. implemented to carry out the process which is the subject of the invention.
• alkylbenzene sulfonate will denote any solution containing from 40 to 95% by weight, preferably from 55 to 85% by weight of an alkylbenzene sulfonate in a dilution oil which may or may not be the same than that used to carry out the process which is the subject of the invention.
• sulfurized alkylphenates which can be used, mention may be made of those obtained by sulfurization with sulfur of an alkylphenol preferably carrying one or more C 9 -C 15 alkyl substituents (such as nonyl, decyl, dodecyl or tetradecylphenols). presence of an alkaline earth base and an alkylene glycol, optionally followed by carbonation with carbon dioxide.
• alkylbenzene sulfonates which can be used, there may be mentioned the salts of sulfonic acids (of molecular weight preferably greater than 400) natural obtained by sulfonating synthetic oil or cuts obtained by the sulfonation of alkylbenzenes déri- v a n t olefin or olefin polymers of C 15 - C 30 and alkaline earth metals such as calcium, barium, magnesium. ..
• the alkaline-earth compound to be used can consist of oxides or hydroxides of calcium, barium, magnesium ... taken alone or as a mixture; the metal from which the alkaline earth alkylbenzene sulfonate and the alkaline earth alkylphenate used may or may not be the same as that or those contained in the alkaline earth compound.
• the amount of oil that can be used is such that the amount of oil present in the final product (including that from the sulfurized alkylphenate and the starting alkylbenzene sulfonate) is between 20 and 60%, from preferably between 25 and 55% of said product.
• alkylene glycols which can be used, mention may very particularly be made of glycol; these can optionally be present in mixture with up to 200% by weight of a monoalcohol such as ethylhexanol, tridecyl alcohol, C 8 -C 14 oxo alcohols and in general , the alcohols having a boiling point higher than 120 ° C and preferably higher than 150 ° C.
• a monoalcohol such as ethylhexanol, tridecyl alcohol, C 8 -C 14 oxo alcohols and in general , the alcohols having a boiling point higher than 120 ° C and preferably higher than 150 ° C.
• Another variant of the process which is the subject of the invention consists in preparing, in situ before the carbonation operation, the alkaline earth metal alkyl benzene sulfonate by the action of an oxide or a hydroxide of said alkali metal. - earthy on an alkylbenzene sulfonic acid as defined above, in the presence of oil and optionally alkylene glycol, at a temperature between 40 and 110 ° C, the amount of alkali metal oxide or hydroxide- earthy and of oil to be used being such that the alkylbenzene sulfonate obtained has a TBN less than or equal to 150, preferably less than or equal to 50.
• the process which is the subject of the invention is very particularly advantageous for preparing detergent-dispersants with a TBN greater than or equal to 250 and having a large percentage by weight of calcium or barium (at least 9%).
• the process which is the subject of the invention is also advantageous for preparing detergent-dispersants with a TBN greater than 200 and containing at least 2% by weight of magnesium and optionally at least 0.5% by weight of calcium.
• magnesium oxide any type of magnesium oxide can be used, however, "active" magnesium oxide is preferred.
• active magnesium oxide denotes magnesium oxide Mg 0 with a specific surface greater than or equal to 80 m2 / g, for example between 100 and 170m2 / g.
• magnesium oxide Mg 0 with a specific surface greater than or equal to 80 m2 / g, for example between 100 and 170m2 / g.
• Maglite DE marketed by Merck
• Feumag marketed by Rhône-Poulenc Industries
• the present invention also relates to detergents-dispersants of high alkalinity obtained by the process described above. These have the advantage of very good compatibility with viscous oils as well as a very low rate of sediment. They can be added to lubricating oils in amounts depending on the TBN of said detergent-dispersants, and depending on the future use of said oils; thus for a petrol engine oil, the amount of detergent-dispersant of TBN 200 - 300 for example to be added, is generally between 1 and 3.5%; ; for a diesel engine oil, it is generally between 1.8 and 5%; for a marine engine oil, this can be up to 25%.
• the lubricating oils which can thus be improved can be chosen from a wide variety of lubricating oils, such as lubricating oils of naphthenic base of paraffinic base and of mixed base, other hydrocarbon lubricants, for example lubricating oils derived from coal, and synthetic oils, for example alkylene polymers, polymers of the alkylene oxide type and their derivatives, including the alkylene oxide polymers prepared by polymerizing alkylene oxide in the presence water or alcohols, for example ethyl alcohol, esters of dicarboxylic acids, liquid esters of phosphorus acids, alkylbenzenes and dialkyl benzenes, polyphenyls, alkyl biphenyl ethers, polymers of silicon .
• lubricating oils such as lubricating oils of naphthenic base of paraffinic base and of mixed base, other hydrocarbon lubricants, for example lubricating oils derived from coal, and synthetic oils, for example alkylene polymers, polymers of the
• Additional additives may also be present in said lubricating oils alongside the detergent-dispersants obtained according to the process of the invention; mention may, for example, be made of antioxidant, anti-corrosion additives, ashless dispersant additives, etc.
• reaction medium After having readjusted the amount of glycol to its initial value, the reaction medium is carbonated at 145 ° C. using C0 2 for 25 minutes under 260 mm Hg and then 35 minutes at atmospheric pressure. Water is eliminated by carrying with it a little glycol. 2nd phase (elimination of glycol)
• the overbased and carbonated medium is brought to a temperature of 184 ° C. under 30 mm Hg for 1 hour.
• the glycol distills.
• the medium is filtered to remove the sediments and a solution is recovered in 100 N oil of overbased detergent-dispersant which is degassed and the characteristics are shown in Table I.
• Example 1 to 3 The operation described in Examples 1 to 3 is carried out under the same conditions, starting from a 60% solution in 100 N oil of a sulfurized dodecylphenate and calcium carbonate, said solution containing 5.25% of calcium and 2.6% C0 2 and has a TBN of around 148.
• glycol is removed (2nd phase) and the detergent-dispersant solution is filtered (3rd phase) as before Use examples 1 to 3.
• Example 7 The operation described in Example 7 is carried out in the presence of a TBN 200 base stock prepared in Example 7 consisting of a 44/56 mixture of calcium sulphurized dodecylphenate / magnesium alkylbenzene sulphonate.
• Glycol is also used in admixture with decanol.
• Example 7 The operation described in Example 7 is carried out by carrying out the carbonation operation at 140 ° C. at atmospheric pressure for approximately 4 hours without the addition of water.
• Example 7 The operation described in Example 7 is carried out by carrying out the carbonation operation for 2 hours at 160 ° C, adding water after having cooled the medium to 110 ° C and continuing the carbonation for another 2 hours at 110 ° C.
• the medium is heated to 50 ° C. and lime and then glycol are introduced over 30 minutes.
• the medium is heated at 80 ° C. for 30 minutes and a 60% solution in 100 N dilution oil of calcium sulphurized dodecylphenate is introduced, said solution containing 5.5% of calcium being free of C0 2 and with a TBN of around 153.
• the medium is brought to and maintained at 145 ° C. under 260 mm Hg for 20 minutes to completely eliminate the reaction water.
• the eliminated water always carries with it a little glycol.
• the medium is carbonated at 145 ° C. using C0 2 for 25 minutes under 260 mm Hg and then for 35 minutes at atmospheric pressure.
• glycol is removed (3rd phase) and the detergent-dispersant solution is filtered (4th phase) as previously in Examples 1 to 3.
• Example 12 The product of Example 12 is added to an SAE 50 oil with a paraffimic tendency so as to obtain a solution containing 125 millimoles of calcium +. magnesium.
• the solution is stored for 15 days at 20 ° C; we see that the solution remains clear.
• This mixture is brought for 25 days to 80 ° C., then is added to an SAE 30 oil so as to have a concentration of 6.6% by weight of mixture (A).
• the solution is stored for 5 days at 80 ° C.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Organic Chemistry (AREA)
• Lubricants (AREA)

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Citations (6)

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• 1978
  • 1978-06-26 FR FR7818947A patent/FR2429833A1/fr active Granted
• 1979
  • 1979-06-14 AT AT79400391T patent/ATE356T1/de not_active IP Right Cessation
  • 1979-06-14 EP EP79400391A patent/EP0006796B1/de not_active Expired
  • 1979-06-14 DE DE7979400391T patent/DE2961227D1/de not_active Expired
  • 1979-06-21 MX MX798106U patent/MX5734E/es unknown
  • 1979-06-22 CA CA330,645A patent/CA1124227A/fr not_active Expired
  • 1979-06-25 ES ES481865A patent/ES481865A1/es not_active Expired
  • 1979-06-25 BR BR7903980A patent/BR7903980A/pt not_active IP Right Cessation
  • 1979-06-26 JP JP54079793A patent/JPS6056200B2/ja not_active Expired
  • 1979-06-26 ZA ZA793197A patent/ZA793197B/xx unknown
• 1982
  • 1982-02-19 US US06/350,282 patent/US4412927A/en not_active Expired - Lifetime

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