A kind of cationic polymerization system and preparation method of high unsaturated degree isoolefin copolymer
A cationic polymerization and isoolefin technology, which is applied in the field of cationic polymerization system and the preparation of high-unsaturation isoolefin copolymers, can solve the problems of toxic safety of organic nitration reagents, toxic and explosive properties of nitromethane, and achieves unsaturated The effect of improving energy efficiency, efficient utilization and reducing energy consumption
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Embodiment 1
[0022] Under the protection of -40℃ and high-purity nitrogen, CH 2 Cl 2 As the reaction medium, the H 2 O, HCl and AlCl 3 Pre-react for 1 hour, then add butyl chloroacetate, mix well and let stand for 2 hours to obtain a homogeneous solution.
[0023] Under the protection of high-purity nitrogen at -102°C, add 20 mL of a mixed solution containing isobutene (IB), isoprene (IP) and tetrafluoroethane ([IB]=5.0mol / L, IP Feeding amount accounts for 3.0mol% of monomer total amount), then adds above-mentioned homogeneous solution and initiates monomer to carry out polymerization reaction, wherein AlCl 3 The molar ratio to the total amount of monomers is 1.1×10 -3 , H 2 The molar ratio of O to the total amount of monomers is 2.4×10 -5 , the molar ratio of HCl to the total amount of monomers is 2.2×10 -5 , the molar ratio of butyl chloroacetate to monomer (IB+IP) is 1.8×10 -3 . After 0.5 hours of polymerization reaction, 5 mL of ethanol solution containing 1 wt % antioxidant 1...
Embodiment 2
[0025] Under the protection of -50℃ and high-purity nitrogen, CH 2 Cl 2 As the reaction medium, the H 2 O, HCl and AlCl 3 Pre-react for 0.5 hour, then add tert-butyl chloroacetate and isopropyl chloroacetate, mix well and leave for 4 hours to prepare a homogeneous solution.
[0026] The polymerization method is the same as in Example 1, except that the solvent is dichloromethane, [IB] is 3.9mol / L, the IP charging amount is 7.5mol%, AlCl 3 The molar ratio to the total amount of monomers is 6.2×10 -3 , H 2 The molar ratio of O to the total amount of monomers is 6.2×10 -5 , the molar ratio of HCl to the total amount of monomers is 1.0×10 -5 , the molar ratio of tert-butyl chloroacetate to the total amount of monomers is 2.0×10 -3 , the molar ratio of isopropyl chloroacetate to the total amount of monomers is 2.0×10 -4 . The polymerization reaction was terminated after 1 hour, and the termination and aftertreatment methods were the same as in Example 1. The yield of isob...
Embodiment 3
[0028] Under the protection of -90℃ and high-purity nitrogen, CH 2 Cl 2 As the reaction medium, the H 2 O, HCl and AlCl 3 Pre-reacted for 1 hour, then added butyl chloroacetate, mixed evenly and left for 168 hours to obtain a homogeneous solution.
[0029] The polymerization method is the same as in Example 1, [IB] is 3.0mol / L, and the IP charging amount accounts for 2.5mol% of the total amount of monomers, and the AlCl 3 The molar ratio to the total amount of monomers is 1.3×10 -3 , H 2 The molar ratio of O to the total amount of monomers is 6.0×10-5 , the molar ratio of butyl chloroacetate to the total amount of monomers is 1.4×10 -3 . The polymerization reaction was terminated after 2 hours, and the termination and aftertreatment methods were the same as in Example 1. The yield of isobutylene and isoprene copolymer is 28%, M w 3.2×10 5 g / mol, M w / M n It was 2.7, the isoprene content was 2.6%, and the gel content was undetectable.
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