A method for free radical polymerization of electron-deficient olefins
An electron-deficient and free radical technology, applied in the field of polymer synthesis, can solve the problems of uncontrollable polymer molecular weight, wide molecular weight distribution, complex preparation process, etc., to achieve clear and controllable polymer structure, less reaction components, and excellent preparation process simple effect
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Embodiment 1
[0031] Example 1: Continuous precipitation polymerization of acrylonitrile in water.
[0032] In a 500ml three-necked flask, add acrylonitrile (26.50g, 0.500mol), FeCl 3 ·6H 2 O (0.54g, 0.002mol) and 75mlH 2 O, stir and heat up to 60°C; add hydrogen peroxide-water solution 25g (wt.%=3.4%, 0.025mol) dropwise at a rate of d / 1s until the addition is complete, and react for 1h; Suspended solids appeared; the reaction solution was filtered to obtain a crude product, washed three times with deionized water, and dried to obtain 24.94 g of white powder, with a yield of 94.1%. That 1 H-NMR (400MHz, DMSO) spectrum as figure 1 shown.
Embodiment 2
[0033] Example 2: Living / Controlled Free Radical Polymerization of Acrylonitrile in DMF.
[0034] In a 500ml three-necked flask, add acrylonitrile (26.50g, 0.500mol), FeCl 3 ·6H 2 O (0.54g, 0.002mol) and 75ml of DMF, stirred and heated to 60°C; dropwise added 25g of hydrogen peroxide-DMF solution (wt.% = 3.4%, 0.025mol) at a rate of d / 1s, until the dropwise addition was completed, reflux reaction 2h; the reaction liquid was precipitated by adding water, and the crude product was obtained by filtration, washed three times with deionized water, and dried to obtain 25.76 g of white powder, with a yield of 97.2%.
Embodiment 3
[0035] Example 3: Living / Controlled Free Radical Polymerization of Acrylonitrile in DMSO.
[0036] In a 500ml three-necked flask, add acrylonitrile (26.50g, 0.500mol), 0.27gFeCl 3 ·6H 2 O (0.27g, 0.001mol) and 75ml of DMSO, stirred and heated to 60°C; added dropwise 25g of hydrogen peroxide-DMSO solution (wt.%=4.1%, 0.030mol) at a speed of d / 1s, until the addition was completed, and reacted for 2h Add water to the reaction solution to precipitate, filter to obtain the crude product, wash with deionized water 3 times, and dry to obtain 25.20 g of white powder with a yield of 95.1%.
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