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Method for polymerization of alpha, beta-unsaturated carbonyl and nitrile monomer

A polymerization method and unsaturated technology, which is applied in the field of anionic polymerization, can solve the problems of low polymerization temperature and low initiation efficiency, and achieve the effects of less polymerization side reactions, short polymerization time, and reduced side reactions

Inactive Publication Date: 2005-04-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem that the present invention solves: In order to overcome organic alkali metal or alkaline earth metal compound to α, the attack of carbonyl and nitrile group in β-unsaturated carbonyl and nitrile compound, and the polymerization temperature that existing initiation system exists is relatively low, and initiation efficiency The present invention proposes a kind of anionic solution polymerization method, when the initiator reacts with α, β-unsaturated carbonyl and nitrile compounds, there are few polymerization side reactions, so that the polymerization can be carried out at room temperature, and has higher initiation efficiency

Method used

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Examples

Experimental program
Comparison scheme
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Embodiment approach

[0011] The preparation of the monovalent copper salt and the organolithium initiator system is to add the monovalent copper salt below 50% of the organolithium moles in the solvent system, and then stir and add the organolithium compound below 0°C;

[0012] The monovalent copper salt complex and the organic lithium initiator first react with the monovalent copper salt and the complexing agent to form a monovalent copper salt organic complex, and then add the organic lithium compound with stirring below 0°C, wherein the moles of copper Less than the number of moles of organic lithium;

[0013] The preparation of organic copper and organic lithium initiator is firstly to prepare organic copper by organic lithium and cuprous chloride, cuprous bromide or cuprous iodide, and then add the equimolar or excess organic lithium with copper.

[0014] The following examples are provided to further illustrate the method of the present invention.

Embodiment 1

[0016] The 100ml three-necked bottle was vacuum-baked and filled with nitrogen. Add 50ml of tetrahydrofuran with a syringe, accurately weigh 0.0495g of cuprous chloride, then add 1.0ml of n-butyllithium at a concentration of 1.0mol / L, and react at 0°C for 2 to 30 minutes. 5 g of methyl methacrylate was added at 20° C., and the polymerization time was 20 minutes. After removing the solvent, the polymerization was characterized by gel liquid chromatography (GPC), nuclear magnetic resonance (NMR) and other testing means. The molecular weight of the polymer was 13000 with a distribution of 1.1 to 1.6.

Embodiment 2

[0018] The 100ml three-necked bottle was vacuum baked and filled with nitrogen gas, added 50ml dimethylformamide with a syringe, accurately weighed 0.0495g cuprous chloride, then added 1.0ml phenyllithium with a concentration of 1.0mol / L, and reacted at -20°C 2min to 30min. 5 g of methyl methacrylate was added at -20°C, and the polymerization time was 40 minutes. After removing the solvent, the polymerization was characterized by GPC, NMR and other testing means. The molecular weight of the polymer was 13000 with a distribution of 1.1 to 1.6.

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Abstract

This invention puts forward a polymerization method of alpha,beta-unsaturation carbonyl and nitrile grouping monomer. Initiator system is consisted by organic lithium and monovalence cupric salt and monovalence organic copper compound or monovalence cupric salt and monovalence copper organic complex, then polymerization reaction is initiated proceeded byalpha,beta-unsaturation carbonyl and nitrile grouping monomer. Polymerization side reaction is few when initiator is reacted with alpha,beta-unsaturation carbonyl and nitrile grouping monomer, so the polymerization can proceed under room temperature and can be used conveniently to synthesis of polarity- nonpolarity block copolymer. Quick polymerization reaction and high efficiency of initiation and yield are features.

Description

technical field [0001] The present invention relates to an anionic polymerization method, especially an anionic polymerization method of α, β-unsaturated carbonyl and nitrile monomers initiated by organic metal. Background technique [0002] Representative α, β-unsaturated carbonyl and nitrile monomers mainly include methacrylates, acrylates, acrylonitrile, methacrylonitrile, etc. They can carry out anionic polymerization and free radical polymerization. Through anionic active polymerization, not only can the relative molecular weight, distribution and microstructure of the polymer be controlled, but also can be copolymerized with other non-polar monomers, such as styrene, butadiene, etc. Various amphiphilic block copolymers. Traditionally, the anionic polymerization of polar monomers such as (meth)acrylate generally uses organic alkali metal compounds and Grignard reagents as initiators. The main disadvantage is that organic alkali metal compounds and Grignard reagents ar...

Claims

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Application Information

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IPC IPC(8): C08F4/54C08F120/14
Inventor 韩丙勇严心浩
Owner CHINA PETROLEUM & CHEM CORP
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