Enzymatic synthesis method of polysiloxane-polyester copolymer
A technology of polysiloxane and oligosiloxane, which is applied in the field of enzyme-catalyzed synthesis of polysiloxane-polyester copolymer, can solve problems such as unreported enzyme-catalyzed synthesis, and achieves high product yield and reaction conditions. Mild, no environmental pollution effect
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Embodiment 1
[0026] In a 1000mL three-necked flask, add 340mL allyl alcohol, and drop 635mL hexamethyldisilazane (MM N ), after the dropwise addition was completed and the reaction was continued for 4 hours, the mixture was fractionally distilled, and the fraction at 99-100° C. was collected, and the obtained colorless transparent liquid was allyloxytrimethylsilane (POTMS), with a yield of 81.2%.
[0027] In a 250mL three-necked flask, add 33.67g of 1,3-dihydro-tetramethyldisiloxane (MM H ) and 74.18g octamethylcyclotetrasiloxane (D 4 ), add 2.5mL of concentrated sulfuric acid under stirring, add 10mL of water after stirring at room temperature for 6 hours, continue to stir for 12 hours, wash with water until neutral, dry with anhydrous magnesium sulfate, filter, and decompress the filtrate at 80°C with a water pump for 1.5 Small molecules were removed within hours, and the obtained colorless transparent liquid was α,ω-dihydrooligosiloxane (A1), with a yield of 82.2%.
[0028] In a 250mL...
Embodiment 2
[0040] Obtain B1 by the method of embodiment 1.
[0041] Add 5mmol B1 and 5mmol succinic acid into a 50mL three-necked flask, heat up to the complete melting of the solid, then cool down to 90°C and react for 6 hours, add 0.4g Novozyme-435 (dried at room temperature, 2mmHg for 24 hours), and the system is heated at 90°C The reaction was continued under reduced pressure (2mmHg), and the by-product water was removed by vacuum and reduced pressure. After 48 hours, add 30mL of chloroform, filter after stirring for 20 minutes, and evaporate the filtrate to remove chloroform under reduced pressure. The obtained light yellow viscous liquid is the polysiloxane-polyester copolymer product. The molecular weight is 6016.
[0042] Using suberic acid to react under the same conditions, the yield of the product is 94.2%, and the number average molecular weight is 6882.
Embodiment 3
[0044] Obtain B1 by the method of embodiment 1.
[0045] Add 5mmol B1, 5mmol adipic acid and 8mL phenyl ether into a 50mL three-necked flask, heat up to the complete melting of the solid, then cool down to 90°C and stir for 6 hours, add 0.4g Novozyme-435 (dried at room temperature, 2mmHg for 24 hours), The system continued to react at 90° C. under reduced pressure (10 mmHg), and the by-product water was removed by vacuum and reduced pressure. After 48 hours, add 30mL of chloroform, filter after stirring for 20 minutes, the filtrate is evaporated under reduced pressure to remove solvent and chloroform, the light yellow viscous liquid obtained is polysiloxane-polyester copolymer product, the productive rate is 91.4%, the number of products The average molecular weight was 3029.
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