Process for selective hydrogenation of conjugated diolefine polymer
A technology of conjugated diene and polymer, applied in the field of selective hydrogenation of conjugated diene polymer
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reference example 1
[0081] Add 2700 grams of cyclohexane and 90 grams of styrene in the polymerization reactor (inner volume is 5 liters), stir and heat rapidly after adding 0.69 grams of n-butyllithium and THF with 40 times the molar number of n-butyllithium React at 60°C for 3 hours, then add 210 grams of 1,3-butadiene, and then polymerize at 60°C for 2 hours, add 0.9 grams of benzene to the block styrene-butadiene active copolymer solution Phenyl acid coupling, then 29.5% of bound styrene, 43% of 1,2-vinyl content, number average molecular weight of 9.5×10 4 of polymers.
reference example 2
[0083] Add 2600 grams of hexanaphthene, 45 grams of styrene in the polymerization reactor (inner volume is 5 liters), stir rapidly after adding 0.35 grams of n-butyllithium and THF of n-butyl molarity 30 times and heat to React at 60°C for 2 hours, then add 220 grams of 1,3-butadiene and react at 60°C for 2 hours, then add 45 grams of styrene and react at 60°C for 2 hours, and finally add n-butyl Deactivation of methanol with 4 times the number of moles of base lithium yields 29.0% bound styrene, 35% 1,2-vinyl content, and a number-average molecular weight of 9.0×10 4 of polymers.
Embodiment 1
[0099] In the glove box, 0.189 g of biscyclopentadienyl cobalt (II) was dissolved in 100 ml of cyclohexane, and 1.1 ml of n-butyllithium was added as a reducing agent, and the solution was fully stirred for more than 5 hours. The solution of Reference Example 2 was diluted with cyclohexane until the weight percentage of the polymer was 7.3%. 330 grams of the diluted polymer solution was injected into an autoclave with an inner volume of 1 liter. Use nitrogen to remove internal gas impurities, and inject 24ml of prepared hydrogenation catalyst solution, and finally inject hydrogen, and keep 251kg / cm 2 The pressure and the hydrogenation at 80 ° C, the reaction is roughly as follows:
[0100] Reaction time 60min 120min 180min 240min 300min
[0101] Residual amount of trans double bonds (%) 7.2 2.2 0 0 0
[0102] 1,2-vinyl double bond residue (%) 0.2 0 0 0 0
[0103] Hydrogenation rate (%) 95.7 99.2 100 100 100
[0104] Hydrogenation rate of benzene ring (%) <1 <1 <1 <1 <1
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