Method for modifying cellulose nanocrystals by using photoresponsive fluorine-containing amphiphilic block copolymer
An amphiphilic block and copolymer modification technology, which is applied in the field of graft modification on the surface of nanoparticles, can solve the problems of strong hydrophilicity and easy agglomeration of cellulose nanocrystals, and overcome the problems of strong hydrophilicity and Easy to agglomerate and improve application performance
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Embodiment 1
[0075] Step 1. At room temperature, S-1-dodecyl-S′-(α,α″-dimethyl-α″-acetic acid) trithio with a mass ratio of 20:4:350:1050 Carbonic acid ester, azobisisobutyronitrile, N,N-dimethylaminoethyl methacrylate, 1,4-dioxane, add in the four-neck flask equipped with reflux condenser, air guide tube and thermometer; Argon for 20 minutes, heated up to 65°C, and stirred for 6 hours to obtain N,N-dimethylaminoethyl methacrylate;
[0076] Step 2, adding azobisisobutyronitrile, glycidyl methacrylate, and 1,4-dioxane with a mass ratio of 1:100:300 to the polymethacrylic acid N obtained in step 1, In a four-necked flask of N-dimethylaminoethyl ester; pass argon for 20 minutes, heat up to 70°C, and stir for 6 hours to obtain N, N-dimethylaminoethyl methacrylate-b-polyglycidyl methacrylate ester;
[0077] Step 3. Add azobisisobutyronitrile, hexafluorobutyl acrylate, and 1,4-dioxane with a mass ratio of 1:450:1350 to the polymethacrylic acid N, N -Dimethylaminoethyl ester-b-polyglycidyl met...
Embodiment 2
[0082] Step 1. At room temperature, S-1-dodecyl-S′-(α,α″-dimethyl-α″-acetic acid) trithiocarbonic acid with a mass ratio of 50:15:1250:3750 Ester, azobisisobutyronitrile, N,N-dimethylaminoethyl methacrylate, put into a four-necked flask equipped with a reflux condenser, air guide tube, and thermometer; argon gas was passed for 25 minutes, the temperature was raised to 70°C, and the mixture was stirred. React for 7h to obtain N, N-dimethylaminoethyl polymethacrylate;
[0083] Step 2. Azobisisobutyronitrile, glycidyl methacrylate, and N,N-dimethylaminoethyl methacrylate with a mass ratio of 5:175:525 are added to the polymethylmethacrylate obtained in step 1. In a four-necked flask of N, N-dimethylaminoethyl methacrylate; argon was passed for 25 minutes, the temperature was raised to 80°C, and the reaction was stirred for 8 hours to obtain N, N-dimethylaminoethyl methacrylate-b-polymethacrylic acid Glycidyl acrylate;
[0084] Step 3. Azobisisobutyronitrile, hexafluorobutyl acr...
Embodiment 3
[0089] Step 1. At room temperature, S-1-dodecyl-S′-(α,α″-dimethyl-α″-acetic acid) trithiocarbonic acid with a mass ratio of 100:25:1600:4800 Esters, azobisisobutyronitrile, and benzene were added to a four-necked flask equipped with a reflux condenser, an air guide tube, and a thermometer; argon was passed for 30 minutes, the temperature was raised to 80°C, and the reaction was stirred for 8 hours to obtain polymethacrylic acid N, N - dimethylaminoethyl ester;
[0090] Step 2, adding azobisisobutyronitrile, glycidyl methacrylate, and benzene with a mass ratio of 14:350:1050 to the poly(N,N-dimethylaminoethyl methacrylate) obtained in step 1 In a four-neck flask; pass argon for 30 minutes, heat up to 85°C, and stir for 8 hours to obtain N,N-dimethylaminoethyl methacrylate-b-polyglycidyl methacrylate;
[0091]Step 3, add azobisisobutyronitrile, hexafluorobutyl acrylate, and benzene with a mass ratio of 14:2250:6750 in turn to the polymethacrylic acid N, N-dimethylaminoethyl est...
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