Hydroxyl-terminated polyisoprene polyurethane synthesized by biological method as well as preparation method and application of hydroxyl-terminated polyisoprene polyurethane
A technology of hydroxyl-terminated polyisoprene and hydroxyl-terminated polyisoprene is applied in the field of hydroxyl-terminated polyisoprene type polyurethane and its preparation, and achieves the effects of narrow molecular weight distribution, excellent heat resistance and easy molecular weight control
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Embodiment 1
[0029] Embodiment 1. The preparation of biological method isoprene
[0030] The single clones of engineering strain G02 were inoculated in 5ml of seed culture medium respectively, and cultivated at 37°C and 220rpm for 12-18 hours to obtain the first-grade seed liquid. Transfer 1ml of first-grade seeds to 100ml of seed culture medium, culture at 37°C and 220rpm for 12-18h, and obtain second-grade seed liquid. Inoculate the secondary seeds in a 5L small fermenter with 2L fermentation medium at a ratio of 1:100, add ampicillin to a final concentration of 100 μg / mL, chloramphenicol to a final concentration of 34 μg / mL, and base sugar to 20- 30g / L glucose. By adding ammonia water, the pH is maintained at 7.0, the initial rotation speed is 400 rpm, and the dissolved oxygen is controlled at 5% to 10%. The culture temperature is 37°C, and when the OD600 is in the range of 15-20, add the inducer IPTG and VB12 to the final concentration of 0.5mM and 5μM respectively, ferment at 30°C f...
Embodiment 2
[0032] Example 2. Preparation of bio-based hydroxyl-terminated polyisoprene
[0033] In the 0.5L autoclave, add biological process isoprene monomer 100g, methyl alcohol 100g, H 2 o 2 (50%) 30g, mix evenly; keep the reaction system at (110±2)°C by temperature control, stop the reaction after 7 hours of reaction time; when the temperature in the kettle drops to 50°C, press the mixture out of the kettle. Put the crude product in a 500mL three-necked flask, use a rotary evaporator to evaporate residual monomers and methanol / ethanol, then transfer the organic layer into a separatory funnel, wash it three times with distilled water at 100°C, and take the organic layer after standing for layers. The layer was distilled under reduced pressure at 80°C and 100.6kPa for 2h to obtain transparent hydroxyl-terminated liquid polyisoprene.
[0034] The relative molecular weight was tested by a 150C GPC gel permeation chromatograph, tetrahydrofuran was used as the mobile phase, and polystyre...
Embodiment 3
[0035] Example 3. Preparation of bio-based hydroxyl-terminated polyisoprene
[0036] In the 0.5L autoclave, add biological process isoprene monomer 100g, methyl alcohol 100g, H 2 o 2 (50%) 20g, mix evenly; keep the reaction system at (120±2)°C by temperature control, stop the reaction after 5 hours of reaction time; when the temperature in the kettle drops to 50°C, press the mixture out of the kettle. Put the crude product in a 500mL three-necked flask, use a rotary evaporator to evaporate residual monomers and methanol / ethanol, then transfer the organic layer into a separatory funnel, wash it three times with distilled water at 100°C, and take the organic layer after standing for layers. The layer was distilled under reduced pressure at 80°C and 100.6kPa for 2h to obtain transparent hydroxyl-terminated liquid polyisoprene.
[0037] After testing, the initiator H 2 o 2 Accounting for 20% of the content of monomer biological isoprene, the reaction temperature is controlled ...
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