A kind of preparation method of high cis diene polymer
A diene polymer and diene technology, applied in the field of polymer preparation, can solve the problems of increasing volatile content, needing to reach a certain temperature, solvent residue, etc.
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[0018] The invention provides a kind of preparation method of high cis-diene polymer, comprising:
[0019] In an anhydrous and oxygen-free airtight container, the reaction solution including diene monomer, liquid propane and rare earth composite catalyst is polymerized to obtain a high cis diene polymer; the diene monomer is liquid butadiene and / or isoprene; the filling degree of the reaction solution in the airtight container is 30-70%.
[0020] In the present invention, the diene monomer is liquid butadiene and / or isoprene. In the present invention, when the diene monomer is liquid butadiene, the diene polymer is polybutadiene; when the diene monomer is isoprene, the diene polymer The compound is polyisoprene; when the diene monomer is liquid butadiene and isoprene, the diene polymer is a butadiene-isoprene copolymer. The present invention has no special limitation on the molar ratio of the liquid butadiene and isoprene, it can be adjusted according to the desired product....
Embodiment 1
[0037] Under vacuum, add 7mL of isoprene monomer and 6mL of butadiene monomer to a clean and dry 100ml polymerization bottle in sequence, and put 20mL of propane into the polymerization bottle under liquid nitrogen freezing conditions to form a monomer solution , the molar ratio of butadiene to isoprene is 1:1, then add about 6mL of the prepared catalyst solution, the catalyst molar ratio [Nd] / [Al] / [Cl] / =1 / 15 / 2, the catalyst The molar ratio of medium rare earth compound to monomer [Nd] / [M]=10.5×10 -4 : 1; the catalyst and the solvent hexane are configured into a solution, the rare earth compound is configured into a 0.1mol / L solution, the alkylaluminum 1.0mol / L solution, and the halogen-containing compound 0.1mol / L solution is configured into a solution for convenient metering and addition.
[0038] The rare earth compound in the catalyst is neodymium neodecanoate, the alkylaluminum is triisobutylaluminum, and the halogen-containing compound is diisobutylaluminum chloride.
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Embodiment 2
[0042] Under vacuum, add 17.5ml of isoprene monomer and 15mL of butadiene monomer to a clean and dry 100ml polymerization bottle in sequence, and add 25mL of propane into the polymerization bottle under liquid nitrogen freezing conditions to form a monomer solution, the molar ratio of butadiene to isoprene is 1:1, then add about 6ml of prepared catalyst solution, catalyst molar ratio [Nd] / [Al] / [Cl]=1 / 15 / 2, catalyst The molar ratio of medium rare earth compound to monomer [Nd] / [M]=4.2×10 -4 :1;
[0043] The rare earth compound in the catalyst is neodymium neodecanoate, the alkylaluminum is triisobutylaluminum, and the halogen-containing compound is diisobutylaluminum chloride.
[0044] Put the polymerization bottle in a constant temperature water bath, and react at a constant temperature of 30° C. for 5 hours, then add an anhydrous ethanol solution containing 1% antiaging agent 264 to terminate the reaction.
[0045] After repeated washing with absolute ethanol three times, t...
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