Method for preparing polythene derivative in supercritical fluid
A technology of supercritical fluid and polyethylene, which is applied in the production of bulk chemicals to achieve the effects of reducing loss, reducing molecular weight distribution, and reducing production costs
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Embodiment 1
[0030] Taking the raw material trifluoroethyl methacrylate 10.214g (0.0608 mole) used for preparing polytrifluoroethyl methacrylate as an example, other raw materials used and the preparation process steps are as follows:
[0031] 1. Vacuumize the reactor
[0032] Charge CO into the reaction kettle 8 with a syringe pump 5 at room temperature 2 The pressure of the gas to the reactor 8 is 0.5MPa, release the charged gas, vacuumize the reactor 8 with a vacuum pump 1 to make the vacuum degree in the reactor 8 0.09MPa, repeat the above steps 2 times. It is also possible to fill the reactor with N 2 gas, Ar gas can also be filled, and N in the reactor can be filled 2 Or the pressure of Ar gas and the vacuum degree after the reactor is evacuated and filled with CO 2 Same for gas.
[0033] 2. Polymerization reaction
[0034] In this embodiment, the monomer is trifluoroethyl methacrylate, the free radical initiator is azobisisobutyronitrile, and the fluid is CO 2 . 10.214 g of t...
Embodiment 2
[0044] Taking the raw material trifluoroethyl methacrylate 10.214g (0.0608 mole) used for preparing polytrifluoroethyl methacrylate as an example, other raw materials used and the preparation process steps are as follows:
[0045] In polymerization step 2, trifluoroethyl methacrylate is selected as the monomer in this embodiment, azobisisobutyronitrile is selected as the free radical initiator, and CO is selected as the fluid. 2 . 10.214 g of trifluoroethyl methacrylate is added to the reaction kettle 8 with the metering pump 6, and the CO is charged into the reaction kettle 8 with the syringe pump 5 2 To the pressure in the reactor 8 is 6.9MPa, trifluoroethyl methacrylate and CO in the reactor 8 2 The volume of the fluid is 20%~30% of the volume of the reactor 8, and the reactor 8 is warmed up to 47.5°C with the heater 7, and 0.0099 g of azobisisobutyronitrile is added to the reactor 8 through the sample tube 4 and the syringe pump 5, The molar ratio of trifluoroethyl metha...
Embodiment 3
[0051] Taking the raw material trifluoroethyl methacrylate 10.214g (0.0608 mole) used for preparing polytrifluoroethyl methacrylate as an example, other raw materials used and the preparation process steps are as follows:
[0052] In polymerization step 2, trifluoroethyl methacrylate is selected as the monomer in this embodiment, azobisisobutyronitrile is selected as the free radical initiator, and CO is selected as the fluid. 2 . 10.214 g of trifluoroethyl methacrylate is added to the reactor 8 with the metering pump 6, and CO is charged into the reactor 8 with the syringe pump 5 until the pressure in the reactor 8 is 6.7 MPa, and the methacrylic acid in the reactor 8 is Trifluoroethyl ester and CO 2 The volume of the fluid is 20%~30% of the volume of the reactor 8, and the reactor 8 is warmed up to 70° C. with the heater 7, and 0.223 g of azobisisobutyronitrile is added to the reactor 8 through the sample tube 4 with the syringe pump 5, The molar ratio of trifluoroethyl me...
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