Nanostructured block copolymer film comprising a biodegradable polyester block
A technology of block copolymers and nanostructures, which is applied in the direction of photolithography, instruments, and optomechanical equipment on the patterned surface, and can solve the problems of unmentioned morphology of nano domains and too long period.
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Embodiment 1
[0077] Embodiment 1 (comparison): Poly(ε-caprolactone) 43 -block- LBH-P3000-block-poly(ε-hexyl ester) 43 Preparation of triblock copolymers
[0078] Weigh the macroinitiator ( LBH-P3000, 2eq. (equivalent), 1.5g) and ε-CL (80eq., 4.11g) were introduced into a dry Schlenk flask. Place the Schlenk flask under a controlled argon atmosphere, and then add solvents (9ml of toluene, [ε-CL] 0 =4 mol / l) and methanesulfonic acid (1 eq., 78 μl). The reaction medium is stirred at 30° C. for 2 h 30 under argon. Once the monomer is fully consumed (by 1 H NMR monitoring to determine), just add excess diisopropylethylamine (DIEA) to neutralize the acid catalyst. The solvent was then evaporated under vacuum. The obtained polymer was then dissolved in a minimum amount of dichloromethane, then precipitated by adding to cold methanol, filtered and dried under vacuum.
[0079] The polymerization reaction of ε-CL monomer and macroinitiator is as follows:
[0080]
[0081] The r...
Embodiment 2
[0086] Embodiment 2 (comparative): Poly(ε-caprolactone) 80 -block-Krasol LBH-P3000-block-poly(ε-caprolactone) 80 Preparation of triblock copolymers
[0087] Macroinitiator (Krasol LBH-P3000, 2 eq., 1.5 g) and ε-CL (160 eq., 8.22 g) were weighed in a glove box and introduced into a dry Schlenk flask. Place the Schlenk flask under a controlled argon atmosphere, and then add solvents (18 ml of toluene, [ε-CL] 0 =4 mol / l) and methanesulfonic acid (1 eq., 156 µl). The reaction medium is stirred at 30° C. for 2 h 30 under argon. Once the monomer is fully consumed (by 1 H NMR monitoring to determine), just add excess diisopropylethylamine (DIEA) to neutralize the acid catalyst. The solvent was then evaporated under vacuum. The obtained polymer was then dissolved in a minimum amount of dichloromethane, then precipitated by adding to cold methanol, filtered and dried under vacuum.
[0088] The results obtained are as follows:
[0089] Get PCL 80 -b-Krasol-b-PCL 80 Trib...
Embodiment 3
[0093] Example 3: Poly(β-butyrolactone) 75 -block-Krasol LBH-P3000-block-poly(β-butyrolactone) 75 Triblock Copolymer Preparation
[0094] Macroinitiator (Krasol LBH-P3000, 2 eq., 1.27 g) and β-BL (160 eq., 5.25 g) were weighed in a glove box and introduced into a dry Schlenk flask. The Schlenk flask was placed under a controlled argon atmosphere, and the solvents (4.6 ml of toluene, [β-BL] 0 =7 mol / l) and trifluoromethanesulfonic acid (2eq., 91μl). The reaction medium is stirred at 30° C. for 3 h 30 under argon. Once the β-BL monomer is completely consumed (by 1 H NMR monitoring to determine), just add excess diisopropylethylamine (DIEA) to neutralize the acid catalyst. The solvent was then evaporated under vacuum. The obtained polymer was then dissolved in a minimum amount of dichloromethane, then precipitated by adding to cold methanol, filtered and dried under vacuum.
[0095] The polymerization reaction of β-BL monomer and macroinitiator is as follows:
[0096...
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