Preparation method and application of polyvinylpyrrolidone
A polyvinylpyrrolidone and a polymerization reaction technology, which is applied in the field of preparation of polyvinylpyrrolidone, can solve the problems of wide molecular weight distribution, narrow molecular weight distribution of polyvinylpyrrolidone, and difficulty in controlling the molecular weight of polymers.
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[0023] According to one aspect of the present invention, the present invention provides a method for preparing polyvinylpyrrolidone, including the following steps: dissolving N-vinylpyrrolidone in an organic solvent, using transition metal salt as a catalyst, and cross-linked povidone as a catalyst Ligand, halogen-containing organic substance as initiator, polymerization reaction, polymerization to obtain polyvinylpyrrolidone with a weight average molecular weight of 20,000 to 120,000 and a molecular weight distribution index of 1.2-1.7.
[0024] The typical but non-limiting weight average molecular weight of the polyvinylpyrrolidone prepared by the preparation method of polyvinylpyrrolidone provided by the present invention is 20,000, 25,000, 30,000, 35,000, 40,000, 45,000, 50,000, 55,000 , 60,000, 65,000, 70,000, 75,000, 80,000, 85,000, 90,000, 95,000, 100,000, 105,000, 110,000, 115,000 or 120,000.
[0025] The preparation method of polyvinylpyrrolidone provided by the present in...
Embodiment 1
[0049] This embodiment provides a method for preparing polyvinylpyrrolidone, which is prepared according to the following steps:
[0050] (a) Add 0.51mmol ferrous chloride and 0.2g crospovidone into the flask, add 40mL ethanol, and stir evenly under the protection of nitrogen;
[0051] (b) Add 160mmol of N-vinylpyrrolidone into the flask and stir evenly;
[0052] (c) Add 0.8 mmol of methyl 2-bromopropionate to the flask, stir at 40°C for polymerization reaction, react for 7 hours, and filter to obtain crude polyvinylpyrrolidone;
[0053] (d) Add 1g of cross-linked povidone to the crude polyvinylpyrrolidone and mix, stir evenly, filter, and distill under reduced pressure to remove the solvent, and then wash with anhydrous ether to obtain polyvinylpyrrolidone;
[0054] Among them, the particle size of the cross-linked povidone used is 5 μm, and the bulk density is 0.4 g / mL.
Embodiment 2
[0056] This embodiment provides a method for preparing polyvinylpyrrolidone, which is prepared according to the following steps:
[0057] (a) Put 0.85mmol ferrous bromide, 0.18mmol ferric chloride and 0.2g crospovidone into the flask, add 40mL N,N-dimethylformamide, and stir evenly under nitrogen protection;
[0058] (b) Add 160mmol of N-vinylpyrrolidone into the flask and stir evenly;
[0059] (c) Add 1.2 mmol of ethyl 2-bromopropionate into the flask, stir at 40°C for polymerization reaction, react for 7 hours, and filter to obtain crude polyvinylpyrrolidone;
[0060] (d) Add 1g of cross-linked povidone to the crude polyvinylpyrrolidone and mix, stir evenly, filter, and distill under reduced pressure to remove the solvent, and then wash with anhydrous ether to obtain polyvinylpyrrolidone;
[0061] Among them, the particle size of the cross-linked povidone used is 10 μm, and the bulk density is 0.35 g / mL.
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