Method for polymerization of alpha, beta-unsaturated carbonyl and nitrile monomer
A polymerization method and unsaturated technology, 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, shorter polymerization time and higher polymerization temperature
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[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 organo-copper and organo-lithium initiator is firstly to prepare organo-copper through organo-lithium and cuprous chloride, cuprous bromide or cuprous iodide, and then add an equimolar or excessive amount of 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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