Method for synthesizing stereo-regular polymethylacrylamide
A technology of polymethacrylamide and methacrylamide, which is applied in the field of synthesis of polymethacrylamide, can solve problems such as being difficult to realize, and achieve the effects of simple operation, mature technology, and clear and feasible synthesis route.
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Embodiment 1
[0023] (1) Using microcrystalline cellulose as the matrix material and 3,5-dimethylphenylisocyanate as the derivatization reagent, the helical polymer cellulose-tris(3,5-dimethylbenzene) was synthesized by the traditional esterification method base carbamate) (CDMPC).
[0024] (2) Add the synthesized cellulose derivatives as chiral additives to the radical polymerization of methacrylamide, use its regular helical structure to induce the radical polymerization of methacrylamide, and finally prepare a Polymethacrylamide with high syndiotacticity.
Embodiment 2
[0026] (1) Take microcrystalline cellulose and vacuum-dry it at high temperature for 4 hours, then stir and reflux in anhydrous N,N-dimethylacetamide for 12 hours; add an appropriate amount of lithium chloride after cooling to room temperature; continue to stir for 2 hours, then heat up again , add anhydrous pyridine, reflux for 6 hours, add excess 3,5-dimethylphenylisocyanate, react for 13 hours, stop the reaction; cool to room temperature, add methanol to settle, filter and wash, vacuum dry at 60°C to constant weight, and produce The rate is 92%.
[0027] (2) Weigh 32.84 mg of azobisisobutyronitrile and dissolve it in 1 mL of n-heptanol solution to make a 0.2 mmol / L solution. Weigh 426mg of methacrylamide monomer again, and according to the molar ratio of methacrylamide and cellulose-tris(3,5-dimethylphenylcarbamate) is 30 / 70 to 20 / 80 Weigh the corresponding mass of cellulose derivative CDMPC. Take the methacrylamide monomer and dry it in vacuum at room temperature for 4 h...
Embodiment 3
[0029] (1) Take 1g of microcrystalline cellulose and vacuum-dry at high temperature for 4h, then stir and reflux in 30mL of anhydrous N,N-dimethylacetamide for 12h; add 1.5g of lithium chloride after cooling to room temperature; continue stirring for 2h , reheated to 80°C, added 15 mL of anhydrous pyridine, refluxed for 6 hours, added excess 3,5-dimethylphenyl isocyanate, continued to stir and refluxed for 12 hours, then stopped the reaction; cooled to room temperature, added methanol to settle, filter and wash, 60 °C and vacuum-dried to constant weight with a yield of 92%.
[0030] (2) Weigh 32.84 mg of azobisisobutyronitrile and dissolve it in 1 mL of n-heptanol solution to make a 0.2 mmol / L solution. Weigh 426 mg of methacrylamide monomer and dry it in vacuum at room temperature for 4 hours; then raise the temperature to 60°C and add the reaction solvent n-heptanol under the protection of nitrogen; after the monomer is completely dissolved, add the corresponding mass of ( ...
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