Preparation and application of dialkyl dithiophosphate hydroxyl derivative and boric acid ester thereof

A technology of dialkyl dithiophosphoric acid and hydroxyl derivatives, which is applied in lubricating compositions, compounds of Group 5/15 elements of the periodic table, and the petroleum industry. Conditions and other issues, to achieve the effect of high thermal stability, good oil solubility, and low hydrolytic stability

Inactive Publication Date: 2013-01-23
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The research on organic borates containing only C, H, and O in the molecule as lubricating oil additives started earlier (see U.S. Patents US5759965, US5482591, US4584115 and US5062975, etc.), but this type of borate does not contain other substances except B. Active elements, so its function is relatively single, it is difficult to meet the needs of increasingly complex working conditions, which limits its application

Method used

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  • Preparation and application of dialkyl dithiophosphate hydroxyl derivative and boric acid ester thereof
  • Preparation and application of dialkyl dithiophosphate hydroxyl derivative and boric acid ester thereof
  • Preparation and application of dialkyl dithiophosphate hydroxyl derivative and boric acid ester thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add the appropriate amount of C 4 h 9 OH was added to the three-necked flask, and P was added in batches under vigorous stirring. 2 S 5 (the molar ratio of the two is 4:1), continue to stir at room temperature for 0.5h, then heat up to 90°C and continue to react for 3h. After the reaction solution is thoroughly clarified, an intermediate is obtained; take an appropriate amount of the above intermediate product in a three-necked flask, Add an equimolar amount of propylene oxide dropwise at room temperature, keep it warm for 0.5h, then gradually raise the temperature to 50°C, and continue the reaction for 2h to obtain di-n-butyl dithiophosphoric acid hydroxy derivative (a);

[0023] Add boric acid and the above product in a molar ratio of 1:3 into a reaction bottle equipped with a water separator, and add an appropriate amount of acidic resin as a catalyst and an appropriate amount of benzene as a water-carrying agent, and react at 70-80°C for 4-6 hours. After the wate...

Embodiment 2

[0026] Add an appropriate amount of dodecylphenol into a three-necked bottle, add an appropriate amount of toluene as a solvent, and add P in batches under vigorous stirring. 2 S 5 (the molar ratio of the two is 4:1), continue to stir at room temperature for 0.5h, and then heat up to 110°C to continue the reaction for 5h. After the reaction solution is thoroughly clarified, the toluene is evaporated to obtain an intermediate; take an appropriate amount of the above intermediate product in In a three-neck flask, add an equimolar amount of propylene oxide dropwise at room temperature, keep it warm for 0.5h, then gradually raise the temperature to 50°C, and continue the reaction for 3h to obtain a behenylphenol dithiophosphoric acid hydroxyl derivative;

[0027] Add boric acid and the above product in a molar ratio of 1:3 to a reaction bottle equipped with a water separator, and add an appropriate amount of acid resin as a catalyst and an appropriate amount of toluene as a water-...

Embodiment 3

[0029] This example is a tribological performance test.

[0030] Get example 1 and obtain the borate of di-n-butyl dithiophosphoric acid hydroxy derivative and di-n-butyl dithiophosphoric hydroxy derivative, take Mobil diester A51 as base oil on four-ball friction and wear testing machine to evaluate all The anti-wear and anti-friction performance of synthetic additives, the test conditions are: according to the GB / T 3142-82 standard method, the maximum non-seizing load P of the sample is measured B and sintering load P D To evaluate the extreme pressure performance; under the load of 392N, measure the wear spot diameter (WSD) of the sample according to the SH / T 0189-92 standard method to evaluate the anti-wear performance; under the load of 392N, according to the ASTM D5183-95 (1999) standard Methods The coefficient of friction (μ) of the samples under different loads was measured to evaluate the anti-friction performance. The test results are listed in Table 1 and Table 2....

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Abstract

The invention relates to preparation of a hydroxyl derivative (1) containing dialkyl dithiophosphate and boric acid ester (11) thereof. Both the hydroxyl derivative (1) and the boric acid ester (11) can be taken as environment-friendly lubricating oil additives, can be used for effectively improving the anti-friction quality of environment-friendly basic oil, and have certain anti-friction effects. A preparation method comprises the following steps of: making alcohol react with phosphorus pentasulfide under a certain reaction condition to generate dialkyl dithiophosphate; and reacting with epoxy propane to obtain the hydroxyl derivative containing a dialkyl dithiophosphate group, wherein boric acid ester can be generated by using the hydroxyl derivative and boric acid ester according to an appropriate chemical metering proportion. The method has the advantages of simple process, mild conditions and suitability for industrial production.

Description

Technical field: [0001] The present invention relates to the preparation of hydroxyl derivatives containing dialkyl dithiophosphoric acids and their borate esters, and their use as environmentally friendly lubricating oil load additives. It belongs to the field of lubricating oil. technical background: [0002] In order to meet the requirements of actual working conditions, various additives must be added to lubricating oil. For environmentally friendly lubricants, the performance of additives in base oils and their impact on the ecological environment must be considered. Since the base oil of biodegradable lubricants is very different from traditional mineral oil in terms of chemical structure and interfacial properties, and the biodegradability of the additive itself must be considered, most of the traditionally used lubricating oil additives cannot Directly used in biodegradable lubricants. [0003] According to the requirements of the German "Blue Angel" standard for ...

Claims

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Application Information

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IPC IPC(8): C07F9/17C10M137/10C10M139/00C10M141/12
Inventor 李久盛张立张梅
Owner PETROCHINA CO LTD
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