A kind of liquid polyconjugated diene rubber and preparation method thereof
A technology of polyconjugated diene and conjugated diene, which is applied in the field of liquid polyconjugated diene rubber and its preparation, can solve the problems of poor molecular chain linearity, fast anionic polymerization rate, and reduced reaction rate, and achieve saving Desolvent removal link, good industrial application value, and the effect of improving production efficiency
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[0016] The invention provides a preparation method of liquid polyconjugated diene rubber, the method comprising:
[0017] (1) in the presence of an organolithium compound and a non-polar solvent, the conjugated diene is subjected to an initiation reaction, and the initiation reaction time is 1-8min;
[0018] (2) In the presence of a retarder, the first polymerization reaction of the product initiated by the reaction is carried out until the conversion rate of the conjugated diene is more than 70% by weight; wherein, the retarder is selected from a metal alkyl compound. one or more;
[0019] (3) In the presence of an accelerator, the product of the first polymerization reaction is subjected to a second polymerization reaction; wherein, the accelerator is one or more of saturated ether compounds.
[0020] According to the present invention, the conjugated diene can be a variety of conjugated dienes known in the art that can prepare liquid polyconjugated diene rubber, preferably...
Embodiment 1
[0057] This example is used to illustrate the liquid polybutadiene rubber of the present invention and its preparation method.
[0058] Under nitrogen protection, 1650 g of n-heptane and 720 g of butadiene were added to the reaction vessel, and 130 mL of a hexane solution (1 mol.L of n-butyllithium) was added under stirring at 150 rpm at 40 °C -1 , the same below) react for 2min; then add 120mL triisobutylaluminum hexane solution (1mol.L -1 , the same below), heated to 70°C for polymerization for 100min (conversion rate of butadiene was 84% by weight, and the highest temperature of the polymerization system was 131°C); then 85mL of THF (about 1mol) was added, and the reaction was carried out at 80°C for 1.5h; In the reaction system, continue to feed carbon dioxide gas at 70 ° C, the pressure is 0.5MPa, and the time is 20min; stop feeding carbon dioxide gas, after 10min, add 1520 antioxidant (purchased from Ciba Chemistry, Switzerland) with a weight ratio of 1:1. (China) Co....
Embodiment 2
[0060] This example is used to illustrate the liquid polybutadiene rubber of the present invention and its preparation method.
[0061] Under nitrogen protection, 1200 g of isooctane and 1200 g of butadiene were added to the reaction vessel, and under stirring at 150 rpm and at 30 °C, 120 mL of a hexane solution of sec-butyllithium (1 mol.L -1, the same below) react for 4min; then add the hexane solution of 108mL triisobutylaluminum, be heated to 60 ℃ to carry out polymerization reaction 120min (the conversion rate of butadiene is 88% by weight, and the maximum temperature of the polymerization system is 129 ℃); then add 50mL THF (about 0.6mol), react at 70°C for 1.5h; continue to feed carbon dioxide gas into the reaction system at 70°C, the pressure is 0.6MPa, and the time is 15min; stop feeding carbon dioxide gas, and add weight after 10min After mixing 2.4g of 1520 antioxidant and 1076 antioxidant in a ratio of 1:1 and stirring for 10min; obtain liquid polybutadiene rubber ...
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