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High-hydrolysis stability organic ammonium borate extreme-pressure antiwear additive and preparation method thereof

A technology of hydrolytic stability and ammonium borate salt, which is applied in the fields of additives, organic chemistry, chemical instruments and methods, etc., and can solve the problems of poor hydrolytic stability of boron-containing additives and failure of product storage performance to meet requirements, etc.

Active Publication Date: 2013-05-22
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Due to the poor hydrolytic stability of boron-containing additives, the storage performance of the product cannot meet the requirements

Method used

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  • High-hydrolysis stability organic ammonium borate extreme-pressure antiwear additive and preparation method thereof
  • High-hydrolysis stability organic ammonium borate extreme-pressure antiwear additive and preparation method thereof
  • High-hydrolysis stability organic ammonium borate extreme-pressure antiwear additive and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0049] This embodiment relates to a highly hydrolytically stable ammonium organoborate extreme pressure anti-wear additive and a preparation method thereof, the method comprising the following steps:

[0050] Step 1, in the there-necked flask of the bromine of 24.6g 4-dodecylbenzene and 17.5g, add 2g catalyst, after reacting in ice-water bath for half an hour, add 2g acid-binding agent (potassium hydroxide) aqueous solution, heated to reflux for 12 hours, the organic layer was washed with sodium thiosulfate solution until the aqueous layer was transparent, dried over anhydrous magnesium sulfate, and the organic solvent was evaporated under reduced pressure to obtain a yellow oily intermediate (4-dodecylbromobenzene) 30.91 g, yield 95.2%;

[0051] Step 2: Add 0.1 g of catalyst to 30.91 g of 4-dodecylbromobenzene anhydrous tetrahydrofuran solution, cool to -78°C, add 5.9 g of n-butyllithium, and slowly add excess 43.73 g of boric acid after 0.5 h Tributyl ester, the reaction te...

Embodiment 2

[0059] This example relates to a highly hydrolytically stable organic borate ammonium salt extreme pressure anti-wear additive and its preparation method.

[0060] Its method comprises the following steps:

[0061] Step 1, in the there-necked flask that 24.6g4-dodecylbenzene and 17.5g bromine are housed, add 2g catalyst, after reacting in ice-water bath for half an hour, add 2g acid-binding agent (potassium hydroxide) aqueous solution again, Heated to reflux for 12 hours, the organic layer was washed with sodium thiosulfate solution until the aqueous layer was transparent, dried over anhydrous magnesium sulfate, and the organic solvent was evaporated under reduced pressure to obtain 30.91 g of a yellow oily intermediate (4-dodecylbromobenzene). Yield 95.2%;

[0062] Step 2: Add 0.1 g of catalyst to 30.91 g of 4-dodecylbromobenzene anhydrous tetrahydrofuran solution, cool to -78°C, add 5.9 g of n-butyllithium, and slowly add excess 43.73 g of boric acid after 0.5 h Tributyl est...

Embodiment 3

[0067] This embodiment relates to a highly hydrolytically stable ammonium organoborate extreme pressure anti-wear additive and a preparation method thereof, the method comprising the following steps:

[0068] Step 1, in the there-necked flask that 33g4-octadecylbenzene and 17.5g of bromine are housed, add 2g catalyst, after reacting in ice-water bath for half an hour, then add 2g acid-binding agent (potassium hydroxide) aqueous solution, heat Refluxed for 12 hours, the organic layer was washed with sodium thiosulfate solution until the aqueous layer was transparent, dried over anhydrous magnesium sulfate, and the organic solvent was evaporated under reduced pressure to obtain 38.9 g of a yellow oily intermediate (4-octadecylbromobenzene), which produced Rate 94.99%;

[0069] Step 2: Add 0.1 g of catalyst to 30 g of 4-octadecylbromobenzene anhydrous tetrahydrofuran solution, cool to -78°C, add 4.7 g of n-butyllithium, and slowly add excess 33.72 g of tributyl borate after 0.5 h...

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Abstract

The invention provides a high-hydrolysis stability organic ammonium borate extreme-pressure antiwear additive and a preparation method of the additive. The structural formula of the additive is shown as in formula (I). The invention further relates to a preparation method of the additive; and according to the preparation method, the additive is prepared from alkylbenzene, bromine, tributyl borate and alkylamine. The additive prepared by the preparation method disclosed by the invention can be independently added into lubricating oil to obtain a lubrication system with good antiwear performance and extreme pressure resistance, so that PB value of the lubricating oil is increased by 30%-110% and the wear scar diameter is reduced by 30%-50%. The additive prepared by the preparation method disclosed by the invention can be further compounded with other lubricating oil additives for use so as to achieve a synergistic interaction effect. The additive prepared by the preparation method disclosed by the invention has good antiwear performance and extreme pressure resistance, as well as excellent corrosion resistance, anti-oxidation performance and the like, and has good application prospect.

Description

technical field [0001] The invention relates to an organic compound and a preparation method thereof, in particular to a highly hydrolytically stable organic borate ammonium salt extreme pressure anti-wear additive and a preparation method thereof. Background technique [0002] Due to increasingly stringent environmental protection requirements, the well-known high-efficiency multifunctional additive ZDDP will be restricted in use because it is easy to poison the automobile exhaust treatment catalyst and increase particulate matter emissions; the commonly used sulfurized isobutylene extreme pressure additive is also easy to The use of malodorous volatiles will also be restricted; machinery and equipment used in agriculture, forestry and fishery must use biodegradable lubricants due to ecological protection restrictions. Therefore, the development of ZDDP substitutes, sulfurized isobutylene substitutes and lubricating additives with low toxicity and high biodegradation rate h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10M139/00C07F5/02C10N30/06
Inventor 李志鹏李秀峰张雅文任天辉
Owner SHANGHAI JIAO TONG UNIV
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