Amphipathic starlike three-arm polyvinylidene fluoride block copolymer
A polyvinylidene fluoride and block copolymer technology, which is applied in the field of amphiphilic star-shaped three-arm polyvinylidene fluoride block copolymer and its preparation, can solve the problems of uncontrollable graft length, low graft rate, and poor grafting. The problem of uneven distribution of branch segments, etc., achieves a good three-dimensional hydrophilic structure, avoids unstable groups, and improves the effect of hydrophilicity
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Embodiment 1
[0039] A preparation method of an amphiphilic star-shaped three-arm polyvinylidene fluoride block copolymer, comprising the steps of:
[0040] In a 1L reactor, add 500 g of N,N-dimethylformamide, (CF 3 CF 2 (CF 2 OCF (CF 3 )) 2 COO) 2 Initiator 2.03g, HOCH 2 C(CH 2 CH 2 SC(=S)OCH 2 CF 3 ) 3 2.08 g of chain transfer agent, lower the temperature to 0°C, slowly pass through nitrogen for 30 minutes, remove the oxygen in the system, and fill with 96.0 g of vinylidene fluoride and 165.0 g of CO 2; The temperature was raised to 35°C to start polymerization, the polymerization pressure was 16 MPa, the reaction time was 12 h and cooled to room temperature to complete the polymerization, and the unreacted VDF monomer was recovered to obtain polyvinylidene fluoride active macromolecules. Continue to add 15.8 g of vinyl acetate and 0.65 g of azobisisobutyronitrile into the kettle, start stirring and raise the temperature to 70°C to continue the reaction for 12 h, then stop, add...
Embodiment 2
[0046] In a 1L reactor, add 500 g of N,N-dimethylformamide, (CF 3 CF 2 (CF 2 OCF (CF 3 )) 2 COO) 2 Initiator 2.03g, HOCH 2 C(CH 2 CH 2 SC(=S)OCH 2 CF 3 ) 3 2.08 g of chain transfer agent, lower the temperature to 0°C, slowly pass through nitrogen for 30 minutes, remove the oxygen in the system, and fill in 128.0 g of vinylidene fluoride and 163.5 g of CO 2 ; The temperature was raised to 35°C, the polymerization pressure was 17MPa, the polymerization was started, the reaction time was 12 h, the polymerization was completed after cooling to room temperature, and the unreacted VDF monomer was recovered to obtain polyvinylidene fluoride active macromolecules. Add 15.8 g of vinyl acetate and 0.65 g of azobisisobutyronitrile into the kettle, start stirring and raise the temperature to 70°C to continue the reaction for 12 h, then stop, add methanol / water (volume ratio 1:1) to obtain a white precipitate, filter in a vacuum Dry to obtain PVDF-PVAc block copolymer.
[0047]...
Embodiment 3
[0052] In a 1L reactor, add N,N-dimethylformamide 500g, (CF 3 CF 2 (CF 2 OCF (CF 3 )) 2 COO) 2 Initiator 1.95 g, HOCH 2 C(CH 2 CH 2 SC(=S)OCH 2 CF 3 ) 3 Chain transfer agent 1.63 g, cool down to 0 °C, slowly pass through nitrogen for 30 minutes, remove the oxygen in the system, fill with 128.0 g of vinylidene fluoride and 174.0 g of CO 2 ; The temperature was raised to 35°C, the polymerization pressure was 28MPa, the polymerization was started, the reaction time was 12 h, the polymerization was completed after cooling to room temperature, and the unreacted VDF monomer was recovered to obtain polyvinylidene fluoride active macromolecules. Add 18.5 g of vinyl acetate and 0.65 g of azobisisobutyronitrile into the kettle, start stirring and raise the temperature to 70°C to continue the reaction for 12 hours, then stop, add methanol / water (volume ratio 1:1) to obtain a white precipitate, filter and dry in vacuo A PVDF-b-PVAc block copolymer is obtained.
[0053] Take 2...
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