Suspending solid phase polymerization method for preparing polymer
A solid-phase polymerization and polymer technology, which is applied in the field of suspension solid-phase polymerization for producing polymers, can solve the problems of difficult continuous production, easy agglomeration, affecting polymer properties, etc., and achieves good polymerization effect and prevents agglomeration. Effect
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[0038] Example 1:
[0039] Starter: Nylon 6 prepolymer powder (containing 0.03wt% sodium hypophosphite), powder particle size D≈200um, molecular weight (determined by end group analysis method, the same below) Mn=7k, enthalpy of fusion ΔHm=58J / g, melting point Tm=204℃, glass transition temperature Tg=45℃
[0040] Liquid inert medium: phenyl silicone oil
[0041] Put 250ml of phenyl silicone oil into a 500ml three-necked flask with a magnet. The three-necked flask is connected to nitrogen at one end, vacuum system at the other, and thermocouple thermometer at the other. Put the three-necked flask in the oil bath and start stirring, turn on the vacuum, and replace the nitrogen three times. Under a nitrogen atmosphere, 25 g of nylon 6 prepolymer powder was slowly added to the three-necked flask. After opening the vacuum to lower the pressure to 200 Pa, the temperature was raised to 180°C and the polymerization temperature Ts was 180°C and the polymerization temperature pressure P wa...
Example Embodiment
[0042] Example 2:
[0043] Starting material: nylon 6 prepolymer powder (containing 0.03wt% sodium hypophosphite), powder particle size D≈500um, molecular weight (determined by end group analysis method, the same below) Mn=7k, melting enthalpy ΔHm=58J / g, melting point Tm=204℃, glass transition temperature Tg=45℃
[0044] Liquid inert medium: phenyl silicone oil
[0045] Put 250ml of phenyl silicone oil into a 500ml three-necked flask with a magnet. The three-necked flask is connected to nitrogen at one end, vacuum system at the other, and thermocouple thermometer at the other. Put the three-necked flask in the oil bath and start stirring, turn on the vacuum, and replace the nitrogen three times. Under a nitrogen atmosphere, 25 g of nylon 6 prepolymer powder was slowly added to the three-necked flask. After opening the vacuum to lower the pressure to 200 Pa, the temperature was raised to 180°C and the polymerization temperature Ts was 180°C and the polymerization temperature press...
Example Embodiment
[0046] Example 3:
[0047] Starter: Nylon 6 prepolymer powder (containing 0.03wt% sodium hypophosphite), powder particle size D≈200um, molecular weight (determined by end group analysis method, the same below) Mn=8k, enthalpy of fusion ΔHm=60J / g, melting point Tm=206℃, glass transition temperature Tg=45℃
[0048] Liquid inert medium: phenyl silicone oil
[0049] Put 250ml of phenyl silicone oil into a 500ml three-necked flask with a magnet. The three-necked flask is connected to nitrogen at one end, vacuum system at the other, and thermocouple thermometer at the other. Put the three-necked flask in the oil bath and start stirring, turn on the vacuum, and replace the nitrogen three times. Under a nitrogen atmosphere, 25 g of nylon 6 prepolymer powder was slowly added to the three-necked flask. After opening the vacuum to reduce the pressure to 200 Pa, the temperature was raised to 190°C and the polymerization temperature Ts was 190°C and the polymerization temperature pressure P w...
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