Star-shaped polymyrcene-polylactic acid block copolymer and preparation method thereof
A technology of block copolymer and myrcene is applied in the field of star-shaped polymyrcene-polylactic acid block copolymer and its preparation. Low cost, excellent elastic deformation recovery performance, and the effect of improving physical and mechanical properties
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Embodiment 1
[0025] Synthesis of star-shaped hydroxyl-terminated polymyrcene macroinitiators: Add 10 g of myrcene monomer, 100 mL of cyclohexane and 0.72 g of anhydrous tetrahydrofuran into a 250 mL single-necked round-bottom flask, and then add 3.0×10 -3 mol tert-butyldimethylsiloxypropyllithium ((CH 3 ) 3 C-Si(CH 3 ) 2 -O-(CH 2 ) 3 -Li) initiates polymerization, reacts at 50°C for 3 hours, then lowers the temperature to room temperature, and adds 3.0×10 -3 mol divinylbenzene (DVB) coupling (measured according to the molar ratio of DVB to tert-butyldimethylsilyloxybutyllithium as 1), react at 0°C for 1 hour, and then add excess isopropanol to terminate. The product was washed with water until neutral, dried in vacuum at room temperature, and finally hydrolyzed with concentrated hydrochloric acid to obtain a hydroxyl-terminated star polymyrcene macromolecular initiator, which was dried in vacuum at room temperature. The product was tested by GPC, and its number average molecular weig...
Embodiment 2
[0027]Synthesis of star-shaped hydroxyl-terminated polymyrcene macroinitiators: 10 g of myrcene monomer, 100 mL of toluene and 0.72 g of anhydrous tetrahydrofuran were added to a 250 mL single-necked round-bottom flask, and then 2.1×10 -3 mol tert-butyldimethylsiloxybutyllithium ((CH 3 ) 3 C-Si(CH 3 ) 2 -O-(CH 2 ) 4 -Li) initiates polymerization, reacts at 40°C for 4h, then lowers the temperature to room temperature, and adds 2.1×10 -2 mol divinylbenzene (DVB) coupling (measured according to the molar ratio of DVB to lithium initiator is 10), reacted at 15°C for 30 minutes and then terminated by adding excess isopropanol. The product was washed with water until neutral, dried in vacuum at room temperature, and finally hydrolyzed with concentrated hydrochloric acid to obtain a hydroxyl-terminated star polymyrcene macromolecular initiator, which was dried in vacuum at room temperature. The product was tested by GPC, and its number average molecular weight before coupling w...
Embodiment 3
[0029] Synthesis of star-shaped hydroxyl-terminated polymyrcene macroinitiators: 10 g of myrcene monomer, 100 mL of cyclohexane and 0.72 g of tetramethylethylenediamine were added to a 250 mL single-necked round-bottom flask, and then 2.0×10 -3 mol tert-butyldimethylsiloxybutyllithium ((CH 3 ) 3 C-Si(CH 3 ) 2 -O-(CH 2 ) 4 -Li) initiates polymerization, after 5 hours of reaction at 30 ° C, the temperature is lowered to room temperature, and 0.04 mol of divinylbenzene (DVB) is added for coupling (measured according to the molar ratio of DVB to lithium initiator of 20), and after 6 minutes of reaction at 30 ° C Add excess isopropanol to terminate. The product was washed with water until neutral, dried in vacuum at room temperature, then hydrolyzed with concentrated hydrochloric acid to obtain a hydroxyl-terminated star polymyrcene macromolecular initiator, and dried in vacuum at room temperature. The product was tested by GPC, and its number average molecular weight before ...
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