Liquid poly conjugated 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 time of the initiation reaction is 1-8 minutes;
[0018] (2) In the presence of a retarder, the product of the initiating reaction is subjected to the first polymerization reaction to a conversion rate of more than 70% by weight of the conjugated diene; wherein, the retarder is selected from one of the metal alkyl compounds one or more kinds;
[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 capable of producing liquid polyconjugated...
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 of n-butyllithium (1mol.L -1 , the same below) to react for 2min; then add 120mL of triisobutylaluminum in hexane (1mol.L -1 , the same below), heated to 70°C for 100 minutes of polymerization reaction (the conversion rate of butadiene was 84% by weight, and the highest temperature of the polymerization system was 131°C); then 85mL THF (about 1mol) was added, and the reaction was carried out at 80°C for 1.5h; Continuously feed carbon dioxide gas into the reaction system at 70° C., the pressure is 0.5 MPa, and the time is 20 min; stop feeding carbon dioxide gas, and add 1520 antioxidant (purchased from Ciba Chemicals, Switzerland) with a weight ratio of 1:1 after 10 min. (China) Co., Ltd., hereinafter the s...
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, 1200g of isooctane and 1200g of butadiene were added to the reaction vessel, and 120mL of a hexane solution of sec-butyllithium (1mol.L -1, the same below) to react for 4min; then add 108mL triisobutylaluminum hexane solution, heat to 60°C to carry out polymerization reaction for 120min (butadiene conversion rate is 88% by weight, and the highest temperature of the polymerization system is 129°C); then add 50mL THF (about 0.6mol), react at 70°C for 1.5h; continuously 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 2.4g of the mixture of 1520 antioxidant and 1076 antioxidant at a ratio of 1:1 and stirred for 10 minutes, a liquid polybutadiene rubber LCBR-2 was obtained with a number average molecu...
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