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Preparing process and usage of thiophosphate

A technology of phosphorothioate and phosphorus trichloride, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, lubricating compositions, etc., can solve the problems of increased cost, difficulty in synthesis, and complex molecular structure of compounds and other problems, to achieve the effect of good anti-wear and high extreme pressure performance

Inactive Publication Date: 2003-02-12
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In recent years, there have been many reports on the synthesis of new ashless extreme pressure anti-wear lubricating oil additives and their tribological properties, such as patents CN1036593C, US5395538, etc., pointing out that some heterocyclic derivatives of thiophosphoric acid are useful as lubricating oil additives. Excellent extreme pressure and anti-wear properties, but these compounds have complex molecular structures and are difficult to synthesize, which increases the cost of product development

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add n-butanethiol (0.45mol), 40mL pyridine and 45mL benzene in a 250mL three-necked flask, stir mechanically and cool to below 10°C with an ice-salt bath, then add phosphorus trichloride (0.15mol) dropwise, and drop it over in 1 hour. Continue to stir at room temperature for a certain period of time, then heat and reflux in a water bath for 2 hours, cool the reaction solution to room temperature naturally, add 80mL 10.0% NaHCO 3 (mass fraction) washed with aqueous solution, the separated oil layer was washed twice with water, added a certain amount of anhydrous sodium sulfate to dry for a period of time, the product obtained was distilled under normal pressure to remove the solvent benzene, then distilled under reduced pressure, and collected fractions at 194 to 196 ° C to obtain The transparent liquid is tri-n-butyl tetrathiophosphate (additive 1).

Embodiment 2

[0029] Add n-octanol (0.30mol), 25mL pyridine and 30mL benzene into a 250mL three-necked flask, stir mechanically and cool to below 10°C with an ice-salt bath, then add phosphorus trichloride (0.10mol) dropwise. After continuing to stir for a certain period of time, heat and reflux in a water bath for 2 hours, and add 80 mL of 10.0% NaHCO after cooling the reaction solution to room temperature naturally 3 (mass fraction) washed with aqueous solution, the separated oil layer was washed twice with water, added a certain amount of anhydrous sodium sulfate to dry for a period of time, the resulting product was distilled under normal pressure to remove the solvent benzene, and then distilled under reduced pressure to remove other impurities to obtain tri-n-octyl Alkyl monothiophosphate (Additive 2).

Embodiment 3

[0031] Add n-octyl mercaptan (0.30mol), 25mL pyridine and 30mL benzene into a 250mL three-necked flask, stir mechanically and cool to below 10°C with an ice-salt bath, then add phosphorous trichloride (0.10mol) dropwise. Continue stirring for a certain period of time, then heat and reflux in a water bath for 2 h, and add 80 mL of 10.0% NaHCO after the reaction solution is naturally cooled to room temperature 3 (mass fraction) washed with aqueous solution, the separated oil layer was washed twice with water, added a certain amount of anhydrous sodium sulfate to dry for a period of time, the resulting product was distilled under normal pressure to remove the solvent benzene, and then distilled under reduced pressure to remove other impurities to obtain tri-n-octyl Alkyl tetrathiophosphate (Additive 3).

[0032] Table 1 lists the infrared analysis results of the products obtained in the above examples.

[0033] The infrared spectrum analysis result of table 1 synthetic ...

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Abstract

A novel thiophosphate can be used as the extreme pressure antiwear additive of new-type non-ash lubricating oil for improving the friction-reducing antiwear performance and load-bearing capability ofthe lubricant using atoleine as basic oil.

Description

Technical field: [0001] The invention relates to a phosphorothioate and its preparation method and application. Background technique: [0002] As we all know, zinc dialkyldithiophosphate (ZDDP) has good anti-oxidation, anti-corrosion and anti-wear properties, and has been widely used in lubricating oils such as internal combustion engine oil, gear oil and hydraulic oil for a long time. But there are also some shortcomings in practical applications. For example, ZDDP anti-wear hydraulic oil has a corrosive effect on hydraulic systems containing silver and lead components, and its hydrolysis stability, emulsification resistance and oxidation stability are far from meeting the requirements of the development of modern hydraulic systems; ZDDP contained in internal combustion engine oil Zn is deposited in the internal combustion engine in the form of ZnO during the combustion process, which has an adverse effect on engine operation. Therefore, the development of new ashless mul...

Claims

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Application Information

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IPC IPC(8): C07F9/165C10M137/10
Inventor 刘维民何万仁巩清叶张泽抚薛群基
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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