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A kind of preparation method and application of branched chain alkyl phosphonic acid dialkyl ester

A branched-chain dialkyl phosphonate and dialkyl phosphite technology, which is applied in the field of preparation of extreme pressure and anti-wear agents for lubricating oils, to achieve good catalytic activity, easy industrial implementation, and simple preparation process

Active Publication Date: 2021-09-03
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

By consulting the literature, the reverse Markov addition reaction of α-olefin dimerization product vinylidene olefin and dialkyl phosphite to prepare branched chain alkyl phosphonate dialkyl ester and its application as extreme pressure and antiwear additive in lubricating oil Research has rarely reported

Method used

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  • A kind of preparation method and application of branched chain alkyl phosphonic acid dialkyl ester
  • A kind of preparation method and application of branched chain alkyl phosphonic acid dialkyl ester
  • A kind of preparation method and application of branched chain alkyl phosphonic acid dialkyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Dimerization reaction: Add 15.429 g (137.5 mmol) of n-octene into a three-necked flask equipped with a magnetic stirrer, according to the molar ratio of zirconocene dichloride: methylaluminoxane: α-olefin is 1:10:275 , 0.146 g (0.5 mmol) of zirconocene dichloride and 2.901 g (5 mmol) of methylaluminoxane were sequentially added into the glove box. Stir the reaction at 25°C for 12 hours. After the reaction is completed, add water to quench the reaction, wash with water, extract with petroleum ether, dry with anhydrous sodium sulfate, and distill under reduced pressure to obtain 14.972g of octene dimerization product. The purity of the product was measured by gas chromatography. is 95.26%.

[0032] n-octene dimerization reaction equation:

[0033]

[0034] Catalyst preparation: take MnSO 4 ·H 2 O 8.451g (0.05mol), (NH 4 ) 2 HPO 4 Add 19.809g (0.15mol) and 90.000g (5mol) of deionized water into the hydrothermal reactor, stir thoroughly, and mix evenly; place the ...

Embodiment 2

[0039] Dimerization reaction: Add 11.572 g (137.5 mmol) of n-hexene into a three-necked flask equipped with a magnetic stirrer, according to the molar ratio of zirconocene dichloride: methylaluminoxane: α-olefin is 1:10:275, In the glove box, 0.146 g (0.5 mmol) of zirconocene dichloride and 2.901 g (5 mmol) of methylaluminoxane were sequentially added. Stir the reaction at 25°C for 12 hours. After the reaction is complete, add water to quench the reaction, wash with water, extract with petroleum ether, dry with anhydrous sodium sulfate, and distill under reduced pressure to obtain 11.036 g of hexene dimerization product. The product purity is measured by gas chromatography. is 96.37%.

[0040] The reaction equation of n-hexene dimerization:

[0041]

[0042] Catalyst preparation: take Mn(NO 3 ) 2 8.948g (0.05mol), (NH 4 ) 2 HPO 4 Add 33.015g (0.25mol) and 72.000g (4mol) of deionized water into the hydrothermal reactor, stir well, and mix evenly; place the configured...

Embodiment 3

[0047] Dimerization reaction: Add 19.287g (137.5mmol) of n-decene into a three-necked flask equipped with a magnetic stirrer, according to the molar ratio of zirconocene dichloride:methylaluminoxane:α-olefin is 1:10:275 , 0.146 g (0.5 mmol) of zirconocene dichloride and 2.901 g (5 mmol) of methylaluminoxane were sequentially added into the glove box. Stir the reaction at 25°C for 12 hours. After the reaction is completed, add water to quench the reaction, wash with water, extract with petroleum ether, dry with anhydrous sodium sulfate, and distill under reduced pressure to obtain 18.919g of decene dimerization product. The purity of the product was measured by gas chromatography. is 97.10%.

[0048] The reaction equation of n-decene dimerization:

[0049]

[0050] Catalyst preparation: take MnCl 2 6.292g (0.05mol), (NH 4 ) 2 HPO 4 Add 52.824g (0.40mol) and 45.000g (2.5mol) of deionized water into the hydrothermal reaction kettle, stir thoroughly, and mix evenly; plac...

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Abstract

The invention discloses a preparation method and application of branched chain alkyl phosphonic acid dialkyl ester. The invention uses vinylidene olefin, a dimerization product of α-olefin, and dialkyl phosphite as raw materials, and carries out reverse Markov addition reaction in the presence of a solid catalyst to prepare branched chain alkylphosphonic acid dialkyl. The solid catalyst is prepared by using soluble manganese salt as manganese source and diammonium hydrogen phosphate as phosphorus source through hydrothermal method-high temperature roasting. The catalyst has good catalytic activity for the synthesis of branched chain alkyl phosphonic acid dialkyl esters by reverse Markov addition reaction, the yield of branched chain alkyl phosphonic acid dialkyl esters can reach more than 90%, and the purity can reach 95%. above. The preparation process of the catalyst used in the method of the invention is simple, easy to separate, recycle and implement industrially, and the obtained dialkyl branched chain alkyl phosphonate has excellent extreme pressure and antiwear performance as an extreme pressure and antiwear agent for lubricating oil.

Description

technical field [0001] The invention belongs to the technical field of preparation of extreme pressure and antiwear agents for lubricating oils, and in particular relates to the synthesis of a branched chain alkyl dialkyl phosphonate and its application as extreme pressure and antiwear agents for lubricating oils. Background technique [0002] Phosphorus is a commonly used active element in lubricating oil, and phosphorus-containing compounds are used as extreme pressure and antiwear additives, which can effectively improve the extreme pressure and antiwear performance of lubricating oil. Phosphates or phosphites are commonly used phosphorus-containing extreme pressure antiwear additives. Among them, dialkyl phosphite, such as di-n-butyl phosphite (T304), as a common anti-wear additive has received widespread attention in practical application research. Short-chain dialkyl phosphite has certain extreme pressure and antiwear properties, but due to its active chemical propert...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/40B01J27/187C10M137/12C10N30/06
CPCB01J27/187C07F9/4075C07F9/4084C10M137/12C10N2030/06
Inventor 董晋湘李旭雷照田成光徐红
Owner TAIYUAN UNIV OF TECH
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