A kind of preparation method of block copolymer and block copolymer
A technology of block copolymers and compounds, which is applied in the preparation of block copolymers and in the field of block copolymers, can solve the problems of complex process, high cost, poor heat resistance, weather resistance and aging resistance, and achieve The process is simple, the generation of styrene homopolymer and double or high-link copolymer is reduced, and the effect of improving block efficiency
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[0025] The invention provides a kind of preparation method of block copolymer, this method comprises the following steps:
[0026] (1) In the presence of a diluent, the isomonoolefin is contacted with each component in the initiator system, and cationic polymerization is carried out to obtain a polymerization system containing polyisomonoolefin with reactive terminals;
[0027] (2) When the conversion rate of the isomonoolefin reaches more than 60%, the polymerization system is mixed with a solution containing styrene to carry out cationic polymerization;
[0028] Wherein, the initiator system contains at least one compound capable of providing carbocations, a Lewis acid and at least one activator,
[0029] The Lewis acid is titanium chloride,
[0030] The activator is selected from compounds shown in formula I-1 and compounds shown in formula I-2,
[0031]
[0032] In formula I-1 and formula I-2, R 1 ~R 8 each independently -H, -X 1 , -NO 2 , and one of -CN, X 1 a...
Embodiment 1
[0078] (1) Configuration of initiator solution: first add 0.246 grams of tetrachloro-p-benzoquinone, 0.084 grams of p-dibenzyl chloride and 5 mL of dichloromethane into a 10 mL volumetric flask, and place them in a cold bath at -80 ° C for subsequent use after dissolving .
[0079] Add 175mL of n-hexane, 175mL of dichloromethane and 30mL of isobutylene into a 1000mL three-necked flask under the protection of nitrogen, place the three-necked flask in a cold bath at -80°C, stir for 20 minutes, add the initiator solution prepared above, and continue stirring After 20 minutes, 1.8 mL of titanium chloride was added for polymerization. After 40 minutes of reaction, 20 mL of isobutene was added to continue the reaction for 20 minutes, and a 1.2 g polyisobutene sample was taken to terminate.
[0080] (2) Add 100mL of styrene solution (which contains 12mL styrene, 44mL n-hexane and 44mL methylene chloride) pre-refrigerated at -80°C to the flask of step (1) and continue the reaction fo...
Embodiment 2
[0091] (1) Configuration of initiator solution: First, add 0.341 grams of 2,3-dichloro-5,6-dicyano-p-benzoquinone, 0.084 grams of p-dibenzyl chloride and 5 mL of dichloromethane into a 10 mL volumetric flask, dissolve Store in a cold bath at -80°C for later use.
[0092] Add 175mL of n-hexane, 175mL of dichloromethane and 30mL of isobutylene into a 1000mL three-necked flask under the protection of nitrogen, place the three-necked flask in a cold bath at -80°C, stir for 20 minutes, add the initiator solution prepared above, and continue stirring After 20 minutes, 1.8 mL of titanium chloride was added for polymerization. After 40 minutes of reaction, 20 mL of isobutene was added to continue the reaction for 20 minutes, and a 1.2 g polyisobutene sample was taken to terminate.
[0093] (2) Cationic polymerization was carried out in the same manner as in step (2) of Example 1.
[0094] Pour the polymer solution obtained after termination into a beaker and inject an equal volume o...
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