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Dialkyl dithio organic molybdenum as well as preparation method and application thereof

A technology of dialkyldithioorganomolybdenum and dialkyldithio, which is applied in the field of dialkyldithioorganomolybdenum and its preparation, can solve the problems of harsh reaction conditions and poor solubility, and achieve simple separation High efficiency, excellent anti-friction and anti-wear properties, and mild reaction conditions

Pending Publication Date: 2020-11-03
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the preparation method of dialkyldithioorganomolybdenum lubricating additives mainly selects inorganic molybdenum sources such as molybdenum oxide, ammonium molybdate, sodium molybdate, molybdenum dichloride, etc., which have poor solubility in organic solvents. , mainly based on heterogeneous reaction, in order to improve the conversion rate of molybdenum source, so harsh reaction conditions are required

Method used

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  • Dialkyl dithio organic molybdenum as well as preparation method and application thereof
  • Dialkyl dithio organic molybdenum as well as preparation method and application thereof
  • Dialkyl dithio organic molybdenum as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] This embodiment provides a method for preparing dialkyldithioorganomolybdenum, comprising the following steps:

[0041] Add 4.53g of molybdenum acetylacetonate MoO to 10.25g of butyl octyl dithiophosphoric acid in absolute ethanol under stirring 2 (acac) 2 (The molar ratio of butyl octyl dithiophosphoric acid to molybdenum acetylacetonate is 2:1), react at room temperature for 8 hours. After the reaction was terminated, the solvent and by-products were spun off to obtain 9.85 g of a brownish-red oily liquid (M202) of butyl-octyl molybdenum dithiophosphate (M202), with a yield of 92.18%, wherein the molybdenum content was 10.86%.

[0042] The above reaction equation:

[0043]

[0044] Implementation effect: see figure 1 , which is an infrared spectrum analysis schematic diagram of the product of Example 1, and the analysis results are as follows: IR (cm -1 ): 2959, 2927, 2874 (-CH 2 -, -CH 3 ); 1585(P=S); 1262(P-O); 1019(P-S,); 905(Mo=O);

Embodiment 2

[0046] This embodiment provides a method for preparing dialkyldithioorganomolybdenum, comprising the following steps:

[0047] Add 4.45g molybdenum acetylacetonate MoO to 10.50g of diisooctyl dithiophosphoric acid in absolute ethanol under stirring 2 (acac) 2 (the molar ratio of diisooctyl dithiophosphoric acid to molybdenum acetylacetonate is 2:1), react at 60°C for 2 hours. After the reaction was terminated, 10.85 g of a brownish-red oily liquid (M204) of molybdenum diisooctyldithiophosphate was obtained after the solvent was removed under reduced pressure, with a yield of 93.86%, wherein the molybdenum content was 9.78%.

[0048] The above reaction equation:

[0049]

[0050] Implementation effect: see figure 2 , which is an infrared spectrum analysis schematic diagram of the product of Example 2, and the analysis results are as follows: IR (cm -1 ):2919,2951(-CH 2 -, -CH 3 ); 1495(P=S); 1229(P-O); 1011(P-S); 906(Mo=O);

Embodiment 3

[0052] This embodiment provides a method for preparing dialkyldithioorganomolybdenum, comprising the following steps:

[0053] Add 3.26g molybdenum acetylacetonate MoO to 2.60g of di-n-butylamine in dehydrated ethanol solution under stirring 2 (acac) 2 , add 0.76g CS dropwise while stirring at 0°C 2 (di-n-butylamine, molybdenum acetylacetonate and CS 2 The molar ratio is 2:1:2), and reacted at room temperature for 12 hours after the dropwise addition was completed. After the reaction was terminated, the solvent was removed under reduced pressure to obtain 5.16 g of brownish-red oily paste (MoDTC4) of molybdenum dialkyldithiocarbamate (MoDTC4), with a yield of 95.56%, wherein the molybdenum content was 14.35%.

[0054] The above reaction equation:

[0055]

[0056] Implementation effect: see image 3 , which is a schematic diagram of the infrared spectrum analysis of the product of Example 3, and the analysis results are as follows: IR (cm -1 ): 2958, 2931, 2870 (-CH ...

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Abstract

The invention provides dialkyl dithio organic molybdenum as well as a preparation method and application thereof. The dialkyl dithio organic molybdenum has a simple structural formula as shown in thefollowing formula I or formula II: wherein R1 and R2 are respectively C3-C50 straight-chain or branched-chain alkyl. The dialkyl dithio organic molybdenum is prepared by reacting dialkylamine and / or dialkyl dithiophosphoric acid with an organic molybdenum source and carbon disulfide at the temperature of 0-100 DEG C for 1-72 hours. The prepared dialkyl dithio organic molybdenum can be used as an anti-wear and anti-friction additive of lubricating grease, and has better oil solubility and tribological properties, so that the dialkyl dithio organic molybdenum is a good anti-friction and anti-wear agent. The preparation process is green and environment-friendly, mild in reaction condition, simple in process and high in yield, has a relatively good application prospect, and is suitable for popularization and application.

Description

technical field [0001] The invention belongs to the technical field of lubricating oil additives, and relates to a dialkyldithioorganomolybdenum and its preparation method and application, in particular to a dialkyldithioorganomolybdenum, its preparation method and its application in lubricating oils . Background technique [0002] Friction and wear are one of the main factors causing energy loss, material loss or destruction. Organic molybdenum is a kind of multi-effect lubricating additive with many advantages such as extreme pressure, anti-wear, anti-friction and anti-oxidation. , Weapon shell lubricating coating and other fields. Such additives can significantly improve the anti-wear and anti-friction performance of lubricants, effectively reduce friction and wear on the surface of the friction pair, and have good high-temperature oxidation resistance, which can improve the mechanical efficiency of the engine and improve the fuel economy of the car. [0003] The most ...

Claims

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Application Information

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IPC IPC(8): C07F11/00C10M139/00C10N30/06
CPCC07F11/005C10M139/00C10M2227/066
Inventor 王娇任天辉
Owner SHANGHAI JIAO TONG UNIV
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