Method of producing cis-rich butadiene-styrene block copolymer
A technology of styrene-butadiene block and copolymer is applied in the field of preparation of high-cis styrene-butadiene block copolymer, can solve the problems of low p-styrene polymerization activity, high cost, reduced polymerization activity and the like, and achieves easy preparation and low cost. Low, high active effect
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Embodiment 1
[0025] Embodiment 1: Preparation of SB two-block high cis-butadiene benzene block copolymer
[0026] Add 0.055 mmol of ethyl trichloroacetate and 0.9 mmol of Al(i-Bu) to a 10 mL catalyst preparation bottle under nitrogen protection 3 With 0.2mmol of AlH(i-Bu) 2, after mixing evenly, add 0.07mmol neodymium octanoate and 2.1mmol chloroform, mix evenly and age at 50°C for 2 hours to form a light blue homogeneous transparent solution.
[0027] Add 9.5mL styrene (St) / cyclohexane solution ([St]=2.7mol / L) to the 100mL dry polymerization bottle under the protection of nitrogen, then add the catalyst solution prepared above, catalyst component A and butane The molar ratio of diene monomer is 9.0×10 -4 . After mixing evenly, polymerize at 65°C for 18 hours, then add 55mL of butadiene (Bd) and raffinate (ie C 6 ~C 8 alkane mixed solution) and cyclohexane mixed solution ([Bd]=2.5mol / L, raffinate / cyclohexane=1 / 1(v / v)), after continuing polymerization at 45°C for 27 hours, The reactio...
Embodiment 2
[0028] Embodiment 2: the preparation of SBS triblock high cis-butadiene benzene block copolymer
[0029] Add 0.055 mmol of ethyl trichloroacetate, 0.002 mmol of ethyl monochloroacetate, 1.1 mmol of Al(i-Bu) to a 10 mL catalyst preparation bottle under nitrogen protection 3 After mixing evenly, 0.07 mmol of neodymium octanoate and 2.1 mmol of chloroform were added, and after mixing evenly, it was aged at 50° C. for 2 hours to form a light blue homogeneous transparent solution.
[0030] The polymerization method of the first two steps is the same as in Example 1. After the SB diblock copolymer is synthesized in the first two steps, 9.5 mL of styrene / cyclohexane solution ([St]=2.7 mol / L) is added in the third step, at 65 The polymerization was continued for 32 hours at °C to prepare the SBS tri-block copolymer. Block efficiency was 67%. M of the obtained triblock copolymer w 5.84×10 5 g / mol, M w / M n is 5.71, St% is 28.2% (wt), and the cis content of butadiene chain unit in...
Embodiment 3
[0031] Embodiment 3: the preparation of SB diblock high cis-butadiene benzene block copolymer
[0032] Add 0.09mmol of neodymium octanoate and 2.7mmol of chloroform to a 10mL catalyst preparation bottle under nitrogen protection, mix well and then add 1.4mmol of Al(i-Bu) 3 and 0.07 mmol of ethyl trichloroacetate were aged at 15°C for 3 hours to form a light blue homogeneous transparent solution.
[0033] The polymerization method and conditions are the same as in Example 1, except that the styrene / butadiene molar ratio is increased to 0.77, and the added styrene / cyclohexane solution is 30mL ([St]=4.0mol / L), the second step The polymerization temperature and polymerization time were 50° C. and 27 hours, respectively. The block efficiency was 53.0%. M of the obtained diblock copolymer w 2.85×10 5 g / mol, M w / M n is 6.60, St% is 47.3% (Wt), and the cis content of butadiene chain unit in the copolymer is 96.9% (mol).
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