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Preparation method of boriding crystalline calcium sulfonate clearing agent

A technology of calcium sulfonate and detergent, which is applied in the direction of additives, petroleum industry, lubricating compositions, etc., can solve the problems of poor product stability, and achieve the effects of not easy to settle, good oil solubility and stability, and strong anti-wear performance

Inactive Publication Date: 2016-07-06
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN102295971 takes alkylbenzenesulfonic acid and CaO as raw materials, adds heptane and CaCl 2 , in the solvent system of methanol and water, the calcium sulfonate of this crystal form can be directly prepared in the next step, but the product has poor stability and cannot be used as a lubricating oil additive

Method used

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  • Preparation method of boriding crystalline calcium sulfonate clearing agent
  • Preparation method of boriding crystalline calcium sulfonate clearing agent
  • Preparation method of boriding crystalline calcium sulfonate clearing agent

Examples

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preparation example Construction

[0030] A preparation method of a boronated crystalline calcium sulfonate detergent, comprising the following steps in turn: mixing 100 parts by mass of an amorphous calcium sulfonate detergent with 10-60 parts by mass of base oil or a non-polar solvent, Stir at -70°C for 5-30 minutes, then sequentially add 20-100 parts by mass of polar solvent and 1-10 parts by mass of boron reagent, stir at 40-60°C for 5-30 minutes, then heat up to 70-120°C for reaction 0.5-5 hours, after the end, continue to heat up to 120-200°C to distill off the solvent to obtain boride crystalline calcium sulfonate detergent.

[0031] Wherein, the amorphous calcium sulfonate detergent comprises amorphous calcium carbonate, surfactant and base oil, the calcium content is 2-20wt%, the base number is 50-500mgKOH / g, and the average particle diameter of calcium carbonate nano-core is 10-200nm.

[0032] Wherein, the amorphous calcium sulfonate detergent comprises amorphous calcium carbonate, surfactant and bas...

Embodiment 1

[0044] In a 1L three-necked flask equipped with a mechanical stirrer and a reflux condenser, add calcium sulfonate detergent (TBN400mgKOH / g, 400g) and 150N base oil (200g), heat up to 50-60°C and stir for 10 minutes, then add methanol -Water (150ml-150ml) and boric acid (10g), continue to stir for 15 minutes, raise the temperature to 70-75°C for 2 hours, and then heat up to 150°C to evaporate the solvent to obtain a brown viscous product.

[0045] Infrared spectroscopy as a tool for qualitative and quantitative analysis of the crystal structure of calcium carbonate. Analyze raw material in embodiment 1 and IR spectrogram after conversion (see Figure 1a and Figure 1b ,in Figure 1a is the raw material IR diagram, Figure 1b It is the product IR picture) can be found: 722cm -1 and 860cm -1 The absorption peaks were shifted to 711cm -1 and 883cm -1 , 1400cm -1 The strong absorption peaks also become sharp, and these typical characteristic peak data indicate that the raw m...

Embodiment 2

[0048] In a 1L three-necked flask equipped with a mechanical stirrer and a reflux condenser, add calcium sulfonate detergent (TBN400mgKOH / g, 400g) and 100N base oil (150g), heat up to 50-60°C and stir for 10 minutes, then add methanol -Water (150ml-150ml) and boric acid (15g), continue to stir for 15 minutes, heat up to 70-75°C for 2 hours, after the end, heat up to 150°C to evaporate the solvent to obtain a brown viscous product.

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Abstract

A preparation method of a boriding crystalline calcium sulfonate clearing agent sequentially comprises the following steps of: mixing 100 parts by mass of an amorphous calcium sulfonate clearing agent and 10- 60 parts by mass of a base oil or a non-polar solvent; stirring a mixture for 5-30 minutes at the temperature between 40 DEG C and 70 DEG C; then adding 20-100 parts by mass of a polar solvent and 1-10 parts by mass of a boron reagent in order; stirring a mixture for 5-30 minutes at the temperature between 40 DEG C and 60 DEG C; then heating the mixture to the temperature between 70 DEG C and 120 DEG C and performing reaction for 0.5 to 5 hours; and continuously heating the mixture to the temperature between 120 DEG C and 200 DEG C after the reaction ends, performing distillation and removing the solvent, and obtaining the boriding crystalline calcium sulfonate clearing agent. The boriding crystalline calcium sulfonate clearing agent has a strong extreme pressure antiwear effect, can be used in the field of engine lubrication, solves the dependence of antiwear performance in oils on ZDDP, and alleviates the limitation of environmental emissions to S and P additives. The preparation method is green and environmental friendly, is high efficient and convenient, and is easy for industrialization.

Description

technical field [0001] The invention relates to a preparation method of a boride crystalline calcium sulfonate detergent. Background technique [0002] With the increasing popularization of high-power, high-load, and high-speed engines, internal combustion engine oils are also gradually becoming high-grade and multi-grade. In order to meet this lubrication requirement, modern lubricating oils often need to add more additives containing anti-wear elements such as sulfur and phosphorus to reduce friction and wear. On the other hand, the increasingly stringent environmental discharge requirements impose strict restrictions on elements such as sulfur and phosphorus. The traditional multi-effect antiwear agent zinc dialkyl dithiophosphate (ZDDP) is facing challenges. Finding ZDDP substitutes or other It has become an urgent task to carry out anti-wear multi-effect of additives. [0003] Sulfonate calcium salt detergent is the most widely used lubricating oil additive at home an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10M141/12C10M163/00C10N30/04C10N30/06
Inventor 马晓东刘功德曹聪蕊翟月奎
Owner PETROCHINA CO LTD
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