Preparation method of calcium sulfonate salt with low alkali value

A technology of low-basic calcium sulfonate and alkylbenzenesulfonic acid, which is applied in the field of preparation of low-basic calcium sulfonate, can solve the problems of poor, incomplete, and easy layering reactions between phases and phases. Achieve fast speed, reduce product turbidity, and low reaction temperature

Active Publication Date: 2009-12-16
LIAONING BODA CHEM
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  • Abstract
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Problems solved by technology

Patent CN1114349A introduces a preparation method for synthesizing alkylbenzene sulfonate. The process includes steps such as sulfonation, purification, neutralization, and distillation desolventization. In this patent, a demulsifier is added to assist in adding water to separate layers, but adding a demulsifier As a result of the emulsion, the product will eventually contain a demulsifier. Since the neutral calcium sulfonate salt is a heterogeneous reaction in the preparation of downstream products with intermediate value and high alkali value calcium sulfonate, the demulsifier will cause poor mixing between phases and easily stratified resulting in slower or incomplete responses

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  • Preparation method of calcium sulfonate salt with low alkali value

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example 1

[0011] Add 200g of alkylbenzene, with an average molecular weight of 340-360, to a container equipped with a thermometer, an electric heating mantle, and a stirrer, add 150g of oleum with 20% sulfur trioxide dropwise, and control the temperature between 35-50°C, drop After adding, keep it warm for 1-4 hours, add 70g of water, and the temperature of adding water should be lower than 60°C. After adding water, purging with nitrogen, the purging temperature is 30-50°C, and absorbing tail gas with 10% sodium hydroxide aqueous solution, the pH value range of the purged gas is preferably 5.5-7.0, add 130g of 75SN, add Toluene 70g, stirred evenly, moved to a separatory funnel, static layered for 2-15 hours, separated the upper layer of crude sulfonic acid, added 20 grams of diatomite filter aid to filter, obtained refined sulfonic acid liquid, diluted sulfonic acid After testing, the acid value is 69.0mgKOH / g, and the free acid is 0.15%. Take 200g of this diluted sulfonic acid, add 1...

example 2

[0013] Add 126g of alkylbenzene to the container equipped with thermometer, electric heating mantle and stirrer, the molecular weight is about 300-320, add dropwise with 122g of oleum with 7.5% sulfur trioxide, and control the temperature between 50-80°C, After the dropwise addition, keep warm for 1-4 hours, add 40g of water, and the temperature of the water should be lower than 60°C. After adding water, purging with nitrogen, the purging temperature is 50-65°C, and absorbing tail gas with 10% sodium hydroxide aqueous solution, the pH value range of the purged gas is preferably 5.5-7.0, add 150SN 95g, add 15g of cyclohexane, stirred evenly, moved to a separatory funnel, static layered for 2-15 hours, separated the crude sulfonic acid in the upper layer, added 14g of diatomite filter aid to filter, and obtained refined alkylbenzenesulfonic acid, diluted After testing, the acid value of the final sulfonic acid is 85.0mgKOH / g, and the free acid is 0.13%. Take 265g of this diluted...

example 3

[0015] Add 100g of alkylbenzene in the container that thermometer, electric heating mantle, stirrer are housed, the carbon chain of alkylbenzene is C22-C24, molecular weight 380-400, drips with 100g of fuming sulfuric acid containing 10% sulfur trioxide, temperature Control it between 35-50°C, keep it warm for 1-4 hours after the dropwise addition, add 50g of water, and the temperature of adding water should be lower than 60°C. After adding water, purging with nitrogen, the purging temperature is 50-60°C, and absorbing tail gas with 10% sodium hydroxide aqueous solution, the pH value range of the purged gas is preferably 5.5-7.0, add 500SN50g, add solvent Oil (distillation range 90°C-120°C) 30g, stirred evenly, moved to a separatory funnel, static layered for 2-15 hours, separated the upper layer of crude sulfonic acid, added 12 grams of diatomaceous earth filter aid to filter, and obtained refined The sulfonic acid solution has an acid value of 72.2mgKOH / g and a free acid con...

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Abstract

The invention relates to a preparation method of calcium sulfonate salt with low alkali value. The preparation method comprises the following steps that: synthesis alkylbenzene with the molecular weight between 300 and 450 is sulfonated by oleum, a certain amount of water is added after sulfonation for 2-5 hours, then nitrogen gas is used for purging, an inert solvent and base oil are used for dilution, then standing and stratification are carried out to obtain coarse sulfonic acid of an upper layer, an alkali filter aid is used for filtration to obtain synthesis alkyl benzene sulphonate diluted by a purifying solvent, the total acid value of the synthesis alkyl benzene sulphonate is 60 to 120mgKOH/g, and the concentration of free acid is controlled below 0.2%; and then, a sodium hydroxide water solution is used for carrying out a neutralization reaction, then solid calcium chloride is added to carry out a double-decomposition reaction, and finally, stratification, water washing and distillation are carried out to obtain low-alkali-value synthesis alkyl benzene calcium sulfonate salt which does not contain or contains trace sulfate radicals and chlorine radicals and has good antirust performance and superior cleaning performance.

Description

technical field [0001] The invention relates to a preparation method of calcium sulfonate with low alkali value, and the product is used in the field of lubricating oil additives. Background technique [0002] Calcium sulfonate with low base number is a commonly used lubricating oil additive. It not only has good detergency, but also has ideal antirust performance. Under the high-temperature operation of the supercharged diesel engine, it has particularly excellent performance in controlling the cleanliness of the piston, and has good compatibility with other lubricating oil additives. It is widely used in compound formulations of medium and high-grade internal combustion engine oils. Calcium sulfonate with low base value can also be used to prepare medium and high base value calcium sulfonate, which is widely used in internal combustion engine oil. [0003] The commonly used preparation method of low base value calcium sulfonate is: alkylbenzene is sulfonated with a sulfo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/32C07C303/06C07C303/44C07C309/30C10M135/10C10N30/04C10N30/12C10N40/25
Inventor 肖宇华吴艳娜关建平许华峰刘明张宏舟
Owner LIAONING BODA CHEM
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