Synthesis of molecular weight controllable polylactic acid without metal residual
A synthesis method and molecular weight technology, applied in the field of synthesis of organic polymer materials, can solve the problems of complex production process, large equipment investment, high technical requirements, etc., and achieve the effect of simple process, high product yield and narrow molecular weight distribution
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Embodiment 1
[0026] (1) Under normal temperature, normal pressure, and argon protection, in a reaction device equipped with a stirrer, add 10 g of L-lactide, add 69.4 mL of dichloromethane, stir well, and prepare L-lactide with a molar concentration of 1M. lactide solution. With 2-propyn-1 alcohol as the initiator, according to the molar ratio of L-lactide, 2-propyn-1 alcohol, 1,8-diazabicyclo[5.4.0]undec-7-ene The ratio is 8:1:0.08. Add 2-propyn-1 alcohol and 1,8-diazabicyclo[5.4.0]undec-7-ene sequentially under stirring, and react for 0.25h.
[0027] (2) According to the molar ratio of 2-propyn-1 alcohol to benzoic acid is 1:2, add benzoic acid under stirring and react for 20 minutes.
[0028] (3) Prepare methanol according to the volume ratio of the reaction solution to methanol at 1:20, drop the reaction solution into methanol, polylactic acid forms a precipitate, filter, and wash with methanol twice. Vacuum dry at 30°C for 24h.
[0029] (4) The product is poly-L-lactic acid whose e...
Embodiment 2
[0031] (1) The experimental device and experimental conditions were the same as in Example 1. Add 10 g of D-lactide and 100 mL of dichloromethane, and stir evenly to prepare a D-lactide solution with a molar concentration of 0.7 M. With 4-ethynyl benzyl alcohol as initiator, according to the molar ratio of D-lactide, 4-ethynyl benzyl alcohol, 1,8-diazabicyclo[5.4.0]undec-7-ene is 28 : 1: 0.28, add 4-ethynyl benzyl alcohol and 1,8-diazabicyclo[5.4.0]undec-7-ene sequentially under stirring, and react for 0.5h.
[0032] (2) According to the molar ratio of 4-ethynyl benzyl alcohol and benzoic acid as 1:3, add benzoic acid under stirring and react for 18 minutes.
[0033] (3) Prepare methanol according to the volume ratio of the reaction solution to methanol at 1:15, drop the reaction solution into methanol, polylactic acid forms a precipitate, filters, and washes twice with methanol. Dry in vacuum at 20°C for 48h.
[0034] (4) The product is poly-D-lactic acid whose end group is...
Embodiment 3
[0036] (1) The experimental device and experimental conditions were the same as in Example 1. Add 15 g of L-lactide and 150 mL of dichloromethane, stir evenly, and prepare an L-lactide solution with a molar concentration of 0.7 M. With 6-azido-1-hexanol as the initiator, according to L-lactide, 6-azido-1-hexanol, 1,8-diazabicyclo[5.4.0]undeca-7- The molar ratio of alkenes is 200:1:2, and 6-azido-1-hexanol and 1,8-diazabicyclo[5.4.0]undec-7-ene are added sequentially under stirring and reacted for 1.5h.
[0037] (2) According to the molar ratio of 6-azido-1-hexanol to benzoic acid of 1:2, add benzoic acid under stirring and react for 20 minutes.
[0038] (3) Prepare methanol according to the volume ratio of the reaction solution to methanol at 1:15, drop the reaction solution into methanol, polylactic acid forms a precipitate, filter, and wash with methanol three times. Vacuum dry at 25°C for 48h.
[0039](4) The product is poly-L-lactic acid whose end group is an azido group...
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