Method for preparing a sulfurized alkaline earth metal dodecylphenate

Abstract

An overbased sulfurized alkaline earth metal alkylphenate is prepared by reacting an alkylphenol with an alkaline earth metal hydroxide or an alkaline earth metal oxide and sulfur in the presence of an alkylene glycol or dialkylene glycol, or ether thereof and in the presence of an oil of lubricating viscosity, and optionally further reacting the product thereof with carbon dioxide; thereby forming a sulfurized alkaline earth metal alkylphenate composition in oil. The composition is heated and subjected to steam stripping followed by filtration. The resulting product exhibits an improved rate and efficiency of filtration.

1 . A process for preparing a sulfurized alkaline earth metal alkylphenate, comprising:
 (a) reacting
 (i) an alkylphenol, wherein the alkyl group contains about 6 to about 24 carbon atoms, with: 
 (ii) an alkaline earth metal hydroxide or an alkaline earth metal oxide in an amount of about 0.4 to about 10 moles per mole of alkylphenol charged to the reaction; and 
 (iii) a sulfur source in an amount to provide about 0.8 to about 3 moles sulfur (as S) per mole of alkylphenol charged to the reaction; in the presence of 
 (iv) an alkylene glycol or dialkylene glycol, or ether thereof, in an amount of about 0.2 to about 2 moles per mole of alkylphenol charged to the reaction; and including in the reaction mixture 
 (v) an oil of lubricating viscosity; 
   and optionally further reacting the product thereof with:
 (vi) carbon dioxide; 
   thereby forming a sulfurized alkaline earth metal alkylphenate composition in oil;   (b) heating said alkylphenate composition to about 120 to 280° C.;   (c) supplying steam to said alkylphenate composition;   (d) removing said steam under reduced pressure; and   (e) filtering the resulting composition to provide, as the filtrate, a sulfurized alkaline earth metal alkylphenate in oil.   
     
     
         2 . The process of  claim 1  wherein the alkylphenol comprises p-dodecyl phenol. 
     
     
         3 . (canceled) 
     
     
         4 . The process of  claim 1  wherein the amount alkaline earth metal hydroxide or oxide is about 1 to about 5 moles per mole of alkylphenol charged to the reaction. 
     
     
         5 . The process of  claim 1  wherein the optional further reacting with carbon dioxide in optional step (vi) is conducted. 
     
     
         6 . The process of  claim 1  wherein the amount of alkaline earth metal hydroxide or oxide is suitable to provide a product with a total base number of about 200 to about 600 on an oil free basis. 
     
     
         7 . The process of  claim 1  wherein the amount of the alkaline earth metal hydroxide or oxide is suitable to provide a product with a total base number of about 100 to about 350. 
     
     
         8 . (canceled) 
     
     
         9 . The process of  claim 1  wherein the alkylene glycol or dialkylene glycol, or ether thereof, comprises ethylene glycol or propylene glycol. 
     
     
         10 . (canceled) 
     
     
         11 . (canceled) 
     
     
         12 . The process of  claim 1  wherein the oil of lubricating viscosity comprises a mineral oil. 
     
     
         13 . (canceled) 
     
     
         14 . The process of  claim 1  wherein the optional reaction with carbon dioxide is conducted and the amount of carbon dioxide supplied is about 10 to about 50 parts by weight per 100 parts by weight of alkylphenol charged to the reaction. 
     
     
         15 . The process of  claim 1  wherein the steam is supplied at superatmospheric pressure and at a temperature of about 120° C. to about 250° C. 
     
     
         16 . The process of  claim 1  wherein volatile materials are removed along with removal of the steam. 
     
     
         17 . The process of  claim 1  wherein the steam is removed at a pressure of about 1.3 to about 53 kPa (10 to 400 mmHg). 
     
     
         18 . The process of  claim 1  wherein the amount of steam is about 3 to about 36 parts by weight per 100 parts by weight of alkylphenol charged to the reaction. 
     
     
         19 . (canceled) 
     
     
         20 . The product prepared by the process of  claim 1 . 
     
     
         21 . A lubricant composition comprising an oil of lubricating viscosity and the product of  claim 20 . 
     
     
         22 . The lubricant composition of  claim 21  further comprising at least one of a supplemental overbased detergent, a dispersant, an antioxidant, a viscosity improver, an anti-wear agent, a pour point depressant, or an extreme pressure agent. 
     
     
         23 . A method for lubricating an internal combustion engine, comprising supplying thereto the lubricant composition of  claim 21 . 
     
     
         24 . A method for improving the filterability of an alkaline earth metal in a process comprising (a) reacting
 (i) an alkylphenol, wherein the alkyl group contains about 6 to about 24 carbon atoms, with:   (ii) an alkaline earth metal hydroxide or an alkaline earth metal oxide in an amount of about 0.4 to about 10 moles per mole of alkylphenol charged to the reaction; and   (iii) a sulfur source in an amount to provide about 0.8 to about 3 moles sulfur (as S) per mole of alkylphenol charged to the reaction; in the presence of   (iv) an alkylene glycol or dialkylene glycol, or ether thereof, in an amount of about 0.2 to about 2 moles per mole of alkylphenol charged to the reaction; and including in the reaction mixture   (v) an oil of lubricating viscosity;   
       and optionally further reacting the product thereof with:
 (vi) carbon dioxide; 
 
       thereby forming a sulfurized alkaline earth metal alkylphenate composition in oil; 
       (b) heating said alkylphenate composition to about 120 to 280° C.; 
       said improvement comprising: 
       (c) supplying steam to said alkylphenate composition; and 
       (d) removing said steam under reduced pressure; prior to 
       (e) filtering the resulting composition to provide, as the filtrate, a sulfurized alkaline earth metal alkylphenate in oil. 
     
     
         25 . The method of  claim 24  wherein the filtering is accomplished by use of a filter aid and the amount of said filter aid used is less than about 3 weight percent based on the final batch yield. 
     
     
         26 . (canceled) 
     
     
         27 . A method for reducing the amount of monomeric alkylphenol in the product of a process comprising (a) reacting
 (i) an alkylphenol, wherein the alkyl group contains about 6 to about 24 carbon atoms, with:   (ii) an alkaline earth metal hydroxide or an alkaline earth metal oxide in an amount of about 0.4 to about 10 moles per mole of alkylphenol charged to the reaction; and   (iii) a sulfur source in an amount to provide about 0.8 to about 3 moles sulfur (as S) per mole of alkylphenol charged to the reaction; in the presence of   (iv) an alkylene glycol or dialkylene glycol, or ether thereof, in an amount of about 0.2 to about 2 moles per mole of alkylphenol charged to the reaction; and including in the reaction mixture   (v) an oil of lubricating viscosity;   
       and optionally further reacting the product thereof with:
 (vi) carbon dioxide; 
 
       thereby forming a sulfurized alkaline earth metal alkylphenate composition in oil; 
       (b) heating said alkylphenate composition to about 120 to 280° C.; 
       said reduction arising from: 
       (c) supplying steam to said alkylphenate composition; and 
       (d) removing said steam under reduced pressure; prior to 
       (e) filtering the resulting composition to provide, as the filtrate, a sulfurized alkaline earth metal alkylphenate in oil.