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Preparation method of high-base number sulfurized alkylphenol salt

A technology for sulfurizing alkyl phenates and alkyl phenols, which is used in the petroleum industry, additives, lubricating compositions, etc. to achieve excellent high-temperature detergency and antioxidant properties.

Active Publication Date: 2015-07-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no introduction to further improving the high-temperature detergency of sulfurized alkyl phenate calcium. Since high-base value sulfurized alkyl phenate calcium is an important metal detergent, its high-temperature detergency directly determines the use of lubricating oil formulations. performance

Method used

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  • Preparation method of high-base number sulfurized alkylphenol salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039]In a 500ml three-necked flask equipped with a temperature control system and electric stirring, add 70 grams of dodecylphenol, 75 grams of 150SN neutral oil, stir for 15 minutes, then add 18 grams of sulfur, 9 grams of calcium oxide, and heat up to 90 ° C After 50 minutes of reaction, the color of the reaction material gradually became darker, and hydrogen sulfide gas was released. Pass the reaction tail gas into a 10% sodium hydroxide solution absorption device. After the reaction, the material is cooled to 30°C, and 80 grams of petroleum ether (distillation range is 90-120°C) is added, and then 50 grams of granular activated carbon (produced by Sinopharm Group, with a specific surface area of ​​900-1100m 2 / g) and 1000 grams of 20% ethanol aqueous solution preparation (stirring temperature is 20-30 ℃ when preparing the mixed solution, stirring for 1 hour), stirred at 30 ℃ for 4 hours, then the material was transferred to a separatory funnel After static layering, 251 ...

Embodiment 2

[0042] In a 500ml three-necked flask equipped with a temperature control system and electric stirring, add 80 grams of dodecylphenol, 75 grams of 150SN neutral oil, stir for 15 minutes, then add 19 grams of sulfur, 8.5 grams of calcium oxide, and heat up to 90 ° C After reacting for 50 minutes, the color of the reaction material gradually becomes darker, and hydrogen sulfide gas is released, and the reaction tail gas is passed into a 10% sodium hydroxide solution absorption device. After the reaction, the material is cooled to 27°C, 90 grams of No. 120 solvent gasoline are added, and then 50 grams of granular activated carbon (produced by Sinopharm Group, with a specific surface area of ​​900-1100m 2 / g) and 1100 grams of 30% ethanol aqueous solution preparation (stirring temperature is 20-30 ℃ when preparing mixed solution, stirring for 1 hour), control reaction temperature 25-30 ℃, should control stirring speed now, make oil The interface between the phase and the water phas...

Embodiment 3

[0045] In a 500ml three-neck flask equipped with a temperature control system and electric stirring, add 75 grams of dodecylphenol, 75 grams of 150SN neutral oil, stir for 20 minutes, then add 17 grams of sulfur, 9 grams of calcium oxide, and heat up to 90 ° C React for 40 minutes, at this time, the color of the reaction material gradually becomes darker, and hydrogen sulfide gas is released, and the reaction tail gas is passed into a 10% sodium hydroxide solution absorption device. After the reaction, the material is cooled to 25°C, 85 grams of n-heptane are added, and then 50 grams of granular activated carbon (produced by Sinopharm Group, with a specific surface area of ​​900-1100m 2 / g) and 900 grams of 20% ethanol aqueous solution preparation (stirring temperature is 20-30 ℃ when preparing the mixed solution, stirring for 1 hour), control the reaction temperature 25-30 ℃, should control the stirring speed this moment, make oil The interface between phase and water phase a...

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Abstract

The invention provides a high-base number sulfurized alkylphenol salt. The method of the invention comprises the following steps: (1) carrying out a sulfuration reaction of alkylphenol, oxides of alkaline earth metal and a sulfurizing reagent; (2) mixing and stirring the reaction product of step (1) with active carbon, and an aqueous solution of low molecular alcohol, separating and recovering an oil-phase product; (3) adding a dispersing aid and oxides of alkaline earth metal into the oil-phase product of step (2), introducing carbon dioxide, carrying out a carbonation reaction, and collecting the product. The high-base number sulfurized alkylphenol salt prepared by the method of the invention has excellent high temperature clearing performance and oxidation resistance.

Description

technical field [0001] The invention relates to a lubricating oil detergent, in particular to a preparation method of a high alkali value sulfurized alkyl phenate. Background technique [0002] High base value sulfurized alkyl phenate is a type of detergent developed earlier. Because the sulfur bridge is introduced into the alkylphenol molecule, it not only strengthens the polarity of the phenate, but also improves the cleaning performance, anti-oxidation performance and anti-wear performance. At the same time, due to the weak acidity of phenate, it is easily soluble in oil and has good oil solubility. The high alkalinity salt contains a large amount of inorganic base, which can neutralize the acidic substances in the lubricating oil. Salt has certain anti-oxidation stability, cleansing, acid neutralization and anti-wear effects, which can meet the needs of most medium and high-grade internal combustion engine oils. With a certain synergistic effect, it can be used to prepa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10M159/22C10N30/04
Inventor 刘依农段庆华
Owner CHINA PETROLEUM & CHEM CORP