Preparation method of ethylene-tetrafluoroethylene copolymer resin
A tetrafluoroethylene copolymer resin and tetrafluoroethylene technology are applied in the field of fluorine-containing plastics and their preparation, which can solve the problems of high initiation temperature of inorganic peroxides, harsh storage and use conditions, and high initiator costs, and avoid high costs. And the problem of harsh use conditions, high shear mechanical strength, and the effect of solving high initiating temperature
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Embodiment 1
[0017] A preparation method of ethylene-tetrafluoroethylene copolymer resin, characterized in that the steps are:
[0018] ⑴ Evacuate and replace the gas mixing tank with a volume of 20L and its related pipelines, add tetrafluoroethylene gas to a gauge pressure of 0.7MPa (that is, an absolute pressure of 0.8MPa), and then add ethylene gas to a gauge pressure of 1.5MPa (absolute pressure of 1.6MPa) , the absolute pressure and partial pressure of tetrafluoroethylene and ethylene are both equal to 0.8MPa, that is, the number of moles is equal), and the gas in the tank is passed through an external circulating return line / pressurized buffer line by a compression pump to generate a circulating flow;
[0019] (2) Add 5 L of 1‰ ammonium persulfate solution to a 10L reaction kettle, use a circulating constant temperature tank to lower the temperature in the kettle to 10°C, add tetrafluoroethylene gas to a gauge pressure of 1.37MPa (absolute pressure 1.47MPa), and then Add ethylene gas...
Embodiment 2
[0023] Change the gas mixing tank volume into 10L among the embodiment 1, change the reactor volume into 2L, change the ammonium persulfate solution volume into 1 liter, change the ferrous sulfate solution volume into 150ml, change the metering pump flow into 75ml / h, other same Example 1 operation. The test results of this example are: fluorine content 58.99%; melting point 277.94°C, melting peak width 21°C; X-ray diffraction angle 18.620° single peak.
Embodiment 3
[0025] Change the gas mixing tank volume into 1000L among the embodiment 1, change the reactor volume into 500L, change the ammonium persulfate solution volume into 250 liters, change the ferrous sulfate solution volume into 3.75L, and change the metering pump flow into 1.875L / h, Others operate with embodiment 1. The test results of this example are: the fluorine content is 59.34%, the melting point is 275.66°C, the melting peak width is 30.3°C, and the X-ray diffraction angle is 18.780° single peak.
[0026] Elemental analysis characterizes the content of fluorine in the polymer. Through calculation, the corresponding fluorine content should be 59.375% when the molecular numbers of the two monomer components are equal (that is, the molar ratio is equal); XRD represents the X-ray diffraction angle, -CH 2 -CF 2 - 18.6° is the eigenvalue of the alternating structure, other structures - CF 2 -CF 2 -Diffraction angle is 25°, -CH 2 -CH 2 - According to different crystal forms,...
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