Isobutylene block copolymer contg. active silicon group and preparing process thereof
A block copolymer and isobutylene technology are applied in the field of preparing isobutylene block copolymers containing reactive silicon groups, and can solve the problems that require strict reaction conditions, the introduction speed of alkenyl groups is not high enough, and the alkenyl functional groups Insufficient responsiveness, etc.
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Embodiment 1
[0072] Add 120 mL of n-hexane (dehydrated with molecular sieves), 80 mL of dichloromethane (dehydrated with molecular sieves), and 0.0876 g (0.38 mmol) of p-dicumyl chloride into the polymerization vessel of a 500 mL separable flask purged with nitrogen. base. The polymerization vessel was cooled in a dry ice / methanol bath at -70°C, and 0.036 g (0.39 mmol) of 2-picoline was added. A Teflon catheter was then connected to a pressure-resistant glass liquefaction tube equipped with a 3-way cock and containing 33.9 mL (419.9 mmol) of isobutylene monomer components, and the isobutylene-based monomer components were added to the polymerization vessel under nitrogen pressure. Next, 1.50 mL (13.7 mmol) of titanium tetrachloride was added to initiate polymerization. After stirring for 1 hour at the same temperature after the start of polymerization, about 1 mL of polymer slurry was sampled. Then, a mixture of 12.15 g (116.7 mmol) of styrene monomer component, 12 mL of n-hexane and 8 m...
Embodiment 2
[0076] Except that the amount of p-dicumyl chloride was 0.35g (1.52mmol) and that of 2-picoline was 0.072g (0.78mmol), the procedure of Example 1 was repeated.
[0077] The GPC analysis of gained block copolymer shows, adds the number-average molecular weight of the isobutylene polymer before styrene and molecular weight distribution to be respectively Mn=18000 and Mw / Mn=1.22, and the block copolymer after styrene polymerization The corresponding values are Mn=26000 and Mw / Mn=1.38, respectively.
[0078] in the resulting block copolymer 1 The integrated intensity ratio of isobutylene and allyl groups on the H-NMR spectrum indicated that an average of 1.7 allyl groups had been introduced into each polymer molecule.
Embodiment 3
[0080] In a 200mL four-necked flask equipped with a condenser tube, add 10.0g of the block copolymer obtained in Example 2, 50mL of toluene, 1.8×10 -3 mmol of platinum divinyltetramethyldisiloxane complex (dissolved in xylene) and 0.85 g (0.8 mmol) of dimethoxymethylsilane, the addition was stirred at 80°C for 10 hours to allow block copolymerization undergoes a hydrosilylation reaction. The reaction mixture was then poured into 200 mL of methanol to obtain an isobutylene block copolymer containing reactive silicon groups.
[0081] in the above polymer 1 The integrated intensity ratio of the isobutylene group and the silyl group on the H-NMR spectrum shows that an average of 1.3 dimethoxymethylsilyl groups have been introduced into each polymer molecule.
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