反应详情

温度

40 °C

To a pressure-resistant reactor, 23.3 kg of cyclohexane, 2.5 millimoles of N,N,N′,N′-tetramethyl ethylene diamine (herein below, referred to as TMEDA) and 1.55 kg of styrene were added and stirred at 40° C. Added thereto was 164.7 millimoles of n-butyl lithium, and while the temperature was increased to 50° C., the mixture was polymerized for 1 hour. The degree of polymerization conversion of styrene in this stage was 100%. Subsequently, 5.20 kg of isoprene was added to the reactor continuously over 1 hour while the temperature was controlled to maintain 50 to 60° C. After the addition of isoprene was finished, the mixture was polymerized for additional 1 hour. The degree of polymerization conversion of isoprene was 100%. Subsequently, 60.1 millimoles of dimethyl dimethoxysilane was added thereto as a coupling agent and the coupling reaction was performed for 2 hours to produce a styrene-isoprene-styrene block copolymer, which would be the block copolymer B. Next, 23.1 millimoles of methanol was added to the reactor to deactivate the active terminal of part of the styrene-isoprene block copolymer. After that, while the temperature was controlled such that it was kept at 50 to 60° C., 3.25 kg of styrene was continuously added over 1 hour. After the addition of styrene was completed, the polymerization was performed for additional 1 hour to produce a styrene-isoprene-styrene block copolymer, which would be the block copolymer A. The degree of polymerization conversion of styrene was 100%. After that, 329.4 millimoles of methanol was added as a polymerization terminator and mixed well to terminate the reaction. The amount of each reagent used for the reaction is shown in Table 1. Part of the reaction solution obtained was extracted and the weight average molecular weight of each block copolymer and block copolymer composition, the weight average molecular weight of each styrene polymer block, the weight average molecular weight of each isoprene polymer block, the content of the styrene unit in each block copolymer, the content of the styrene unit in the block copolymer composition, the vinyl bond content in the isoprene polymer block, and the weight ratio of each block copolymer were measured. The results are shown in Table 2. To 100 parts of the reaction solution obtained (containing 30 parts of polymer components), 0.3 part of 2,6-di-tert-butyl-p-cresol was added as an anti-oxidant and mixed well. The mixture solution was added dropwise in small portions to hot water heated to 85 to 95° C. to evaporate the solvent. Accordingly, the precipitates were obtained, pulverized, and dried with hot air (85° C.) to recover the block copolymer composition of Preparation example 1.

1. additionAdded
2. temperaturewhile the temperature was increased to 50° C.
3. customthe mixture was polymerized for 1 hour
4. temperatureto maintain 50 to 60° C
5. customthe mixture was polymerized for additional 1 hour
6. customas a coupling agent and the coupling reaction