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Method for preparing nitrogenous phosphate extreme-pressure anti-wear additive by vegetable-oil solid alkali method

A nitrophosphate, extreme pressure and anti-wear technology, used in additives, petroleum industry, lubricating compositions, etc., can solve problems such as non-recycling, corrosion of equipment, influence of amine value detection, etc., to reduce the use of toxic substances, reaction equipment, etc. The effect of low requirements and mild reaction conditions

Inactive Publication Date: 2011-08-03
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the selectivity of the catalyst KOH used in the reaction is poor, it cannot be recovered after the reaction, severely corrodes the equipment, and causes great pollution to the environment
At the same time, the remaining KOH reacts with the product to form potassium salt, which affects the detection of the amine value of the reaction product. If the method of washing with water is used to remove KOH and its potassium salt, a large amount of oily sewage will be produced, and the yield of the product will be reduced at the same time.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1) Synthesis of fatty acid diethanolamide

[0022] Put 50g of rapeseed oil and 5g of diethanolamine in a flask, and react at 110°C for 3 hours, and use solid base KF / Al 2 o 3 As a catalyst, the dosage is 1.5% of the mass of vegetable oil. After the reaction, the by-product glycerin is separated to obtain fatty acid diethanolamide. The yield of amide reaches 85.1%.

[0023] 2) Synthesis of nitrogen-containing phosphate extreme pressure anti-wear lubricant additives

[0024] Mix 50 g of the prepared fatty acid diethanolamide with 10 g of the phosphorylation reagent, react at 70° C. for 3 hours, and leave to stand to separate layers after the reaction. Take its oil phase to get the product. The yield of phosphate ester reached 69.6%. It was added to rapeseed oil methyl ester in an amount of 1%, and it was found by four-ball testing machine that its carrying capacity P B It is 603N, the wear spot diameter WSD is 0.624mm, and its rapeseed oil methyl ester (P B Compare...

Embodiment 2

[0026] 1) Synthesis of fatty acid diethanolamide

[0027] 50g of castor oil and 5g of diethanolamine were placed in a flask, and reacted for 3 hours under the condition of 120°C, with solid base Rb 2 O is a catalyst, and the dosage is 1.0% of the mass of vegetable oil. After the reaction, the by-product glycerol is separated to obtain fatty acid diethanolamide. The yield of amide reaches 80.9%.

[0028] 2) Synthesis of nitrogen-containing phosphate extreme pressure anti-wear lubricant additives

[0029] Mix 50 g of the prepared fatty acid diethanolamide with 10 g of the phosphorylation reagent, react at 80° C. for 3 hours, and leave to separate after the reaction. Take its oil phase to get the product. The yield of phosphate ester reached 70.7%. It was added to rapeseed oil methyl ester in an amount of 2%, and it was found by four-ball testing machine that its bearing capacity P B It is 732N, the wear spot diameter WSD is 0.535mm, and its rapeseed oil methyl ester (P B C...

Embodiment 3

[0031] 1) Synthesis of fatty acid diethanolamide

[0032] Put 50g of soybean oil and 10g of diethanolamine in a flask, react at 110°C for 4 hours, use solid alkali BaO as a catalyst, and use an amount of 3.5% of the mass of vegetable oil. After the reaction, separate the by-product glycerin to obtain fatty acid Diethanolamide. The yield of amide reaches 83.2%.

[0033] 2) Synthesis of nitrogen-containing phosphate extreme pressure anti-wear lubricant additives

[0034] Mix 50 g of the prepared fatty acid diethanolamide with 10 g of the phosphorylation reagent, react at 70° C. for 4 hours, and leave to separate after the reaction. Take its oil phase to get the product. The yield of phosphate ester reached 73.4%. It was added to rapeseed oil methyl ester in an amount of 2%, and it was found by four-ball testing machine that its bearing capacity P B It is 751N, the wear spot diameter WSD is 0.524mm, and its rapeseed oil methyl ester (P B Compared with 437N and WSD of 0.652m...

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Abstract

The invention relates to a method for preparing a nitrogenous phosphate extreme-pressure anti-wear additive by a vegetable-oil solid alkali method, which belongs to the technical field of a production process for lubricating oil additive. The nitrogenous phosphate extreme-pressure anti-wear additive is prepared by a two-step synthesis method by using vegetable oil as a raw material, wherein the two-step synthesis method comprises the following steps of: firstly, placing the vegetable oil and diethanol amine in a flask and synthesizing fatty acid diethanol amide by using solid alkali as a catalyst; and then mixing the prepared fatty acid diethanol amide and a phosphorylation reagent, and stirring the mixture for reaction to obtain the extreme-pressure anti-wear lubricating oil additive with fatty acid diethanol amide phosphate. The method has the advantages of wide source of the vegetable oil; the solid alkali is taken as the catalyst, therefore, the conversion rate can be improved by more than 80%; the solid-alkali catalyst can be separated only by sedimentation, therefore, the product does not need the washing process; the reaction process is simple, the reaction condition is mild, and the reaction time is short; and the method is environmentally friendly and overcomes the defect of poor biodegradation of the traditional lubricating oil additive.

Description

technical field [0001] The invention belongs to the technical field of lubricating oil additive production technology. In particular, it relates to a preparation method of a nitrogen-containing phosphate extreme-pressure anti-wear lubricating additive, which uses vegetable oil as a raw material, and then adopts a two-step synthesis method to prepare a fatty acid diethanolamide phosphate compound, which is an environmentally friendly lubricating oil additive. Background technique [0002] The purpose of using lubricating oil is to reduce mechanical friction and wear, improve mechanical efficiency, reduce energy consumption, and prolong the service life of machinery. Many parts are damaged due to wear and tear. Therefore, it is necessary to improve the lubrication performance to reduce friction, wear, and prevent sintering, and extreme pressure anti-wear additives are produced accordingly. Traditional extreme pressure anti-wear additives include sulfur-containing extreme pres...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10M137/04C07F9/09C10N30/06
Inventor 李为民任朋飞邱玉华郭登峰姚超
Owner CHANGZHOU UNIV