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Carbamic acid molybdenum lubricating grease additive, its preparation method and application

A molybdenum carbamate, lubricating grease technology, applied in the directions of additives, lubricating compositions, chemical instruments and methods, can solve the problems of phosphorus-containing solubility, easy oxidation, etc., achieve excellent anti-friction and anti-wear performance, simplify production process, The effect of reducing production costs

Active Publication Date: 2012-01-11
太平洋联合(北京)石油化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a lubricating grease additive to overcome the shortcomings of phosphorus in current additives, low solubility and easy oxidation

Method used

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  • Carbamic acid molybdenum lubricating grease additive, its preparation method and application
  • Carbamic acid molybdenum lubricating grease additive, its preparation method and application
  • Carbamic acid molybdenum lubricating grease additive, its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Put 22.5g of water, 20.5g of 2-(ethylhexyl)-tridecylamine, 51.1g of ditridecylamine, 7.8g of naphthenic base oil, and 33.2g of ammonium molybdate in a 500ml round bottom flask , mix and stir evenly and cool to 16°C, then pressurize to 830mmHg, add 17.5g of carbon disulfide dropwise, heat to 65°C and reflux for 3 hours, depressurize to 800mmHg to evaporate water, then pump at low speed to complete vacuum, and heat up to 125°C Continue to react for 1.5 hours, cool to 70°C, filter to obtain molybdenum dialkyldithiocarbamate lubricating grease additive (numbering is P-1002-01), the yield is 89.6%, and its mass percentage Mo is measured by RIPP % is 6%, S% is 6.5%, and N% is 1.4%.

Embodiment 2

[0031] Put 22.5g of water, 24.9g of 2-(ethylhexyl)-tridecylamine, 45.7g of ditridecylamine, 7.8g of naphthenic base oil, and 33.2g of ammonium molybdate in a 500ml round bottom flask , mix and stir evenly and cool to 17°C, then pressurize to 840mmHg, add 17.5g of carbon disulfide dropwise, heat to 70°C and reflux for 3.5 hours, depressurize to 790mmHg to evaporate water, then pump at low speed to complete vacuum, and heat up to 130°C Continue to react for 2 hours, lower the temperature to 70° C., and filter to obtain molybdenum dialkyldithiocarbamate lubricating grease additive (numbering is P-1002-02). The yield is 88.9%, and its mass percentage Mo is measured by RIPP. % is 6.4%, S% is 5.5%, and N% is 1.5%.

Embodiment 3

[0033] Put 22.5g of water, 41.7g of 2-(ethylhexyl)-tridecylamine, 25.1g of ditridecylamine, 7.8g of naphthenic base oil, and 33.2g of ammonium molybdate in a 500ml round bottom flask , mix and stir evenly and cool to 18°C, then pressurize to 850mmHg, add 17.5g of carbon disulfide dropwise, heat to 72°C and reflux for 4 hours, depressurize to 780mmHg to evaporate water, then pump at low speed to complete vacuum, and heat up to 132°C Continue to react for 2.5 hours, cool to 70°C, filter to obtain molybdenum dialkyldithiocarbamate lubricating grease additive (numbering is P-1002-03), the yield is 88.7%, and its mass percentage Mo is measured by RIPP % was 5.9%, S% was 6.8%, and N% was 1.4%.

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Abstract

The invention relates to a lubricating grease additive, which has a structure as shown in a general formula, wherein R1, R2, R3 and R4 are selected from C4-C15 straight chain and branched chain alkyl group; R1 is different from R2; R3 is the same with R4; R1 and R2 can be the same with or different from R3 and R4; Z equals to 1-3, W equals to 1-3; and x+y=3-7. The invention also provides a methodfor preparing the above additive by a reaction of a dialkylamine mixture, comprising the following steps of: mixing water, the dialkylamine mixture, cycloalkyl base oil and molybdenum resource with uniformly stirring, cooling to 15-20DEG C, pressurizing to 830-900mmHg, adding dropwisely carbon disulfide, heating up to 60-80DEG C, followed by reflux reaction for 3-5 hours, reducing pressure to 760-800mmHg for water evaporation, completely vacuumizing at low speed, heating to 120-140DEG C, continuously reacting for 1-3 hours, cooling, and filtering. The additive provided by the invention contains no phosphorus, and has not only excellent antifriction and anti-wear performance but also improved oil dissolving performance and antioxidation performance.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a molybdenum dialkyldithiocarbamate lubricating oil additive and its preparation method and application. Background technique [0002] Organomolybdenum compounds are well-known additives in lubricating formulas. They have excellent tribological properties and are widely used in internal combustion engine oils, gear oils, greases and some industrial oils. The limit of phosphorus (P) content in automobile exhaust is more stringent, and the research and application of P-free molybdenum dialkyldithiocarbamate has become an inevitable trend. [0003] However, in the prior art, molybdenum dialkyldithiocarbamate synthesized by a single symmetrical amine and a single asymmetric amine does not have the desired solubility, especially at low temperatures, it is easy to separate from the lubricating composition, forming flocs or precipitation , reducing its effectiveness. In t...

Claims

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Application Information

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IPC IPC(8): C10M135/18C10M177/00C07F11/00C10N50/10
Inventor 张桂林
Owner 太平洋联合(北京)石油化工有限公司
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