Process for the preparation of isoolefin copolymers
A polymer and isoprene technology, applied in the field of preparation of isomeric olefin copolymers, can solve problems such as difficulties
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[0038] Experiment Details
[0039]The gel content is determined in toluene: a concentration of 12.5 g / l is dissolved in toluene at 30° C. for a period of 24 h. Then, the insoluble components were separated by ultracentrifugation (20,000 rpm, 25° C., 1 h). The samples with high gelling content were examined in o-dichlorobenzene at 140°C.
[0040] The solution viscosity η of the soluble component was measured in toluene at 30° C. with an Ubbelohde (capillary) viscometer.
[0041] The molecular weight Mv calculated from the intrinsic viscosity is determined by the following formula: 1n(Mv)(Mooney)=12.48+1.565.1nη.
[0042] Mooney values are determined after a measurement time of 8 min at 125°C.
[0043] Argon 4.8 (supplied by Linde) was used as the shielding gas.
[0044] Monomer incorporation rates and "branch points" (J.L. White, T.D. Shaffer, C.J. Ruff, J.P. Cross: Macromolecules (1995) 28, 3290) were determined using high-field proton resonance.
[0045] The isobutylen...
example 1
[0053] Example 1 (preparation of initiator)
[0054] 0.233 g of zirconium tetrachloride was weighed into a Schlenk-type vessel under argon protection, and then 60 μl of acetyl chloride were added. Subsequently, 100 g of methyl chloride was condensed-in at -40° C., and stirred at this temperature for 4 h. The initiator solution was slightly cloudy. The initiator can be used as such directly or in diluted form.
example 2
[0055] Example 2 (polymerization, metering of initiator solution)
[0056] 2a
[0057] 700 g of dry methyl chloride and 300 g of isobutene were condensed at -90°C and charged into a Schlenk-type four-necked flask. 24.5 g of isoprene was added in liquid form. Then, the monomer feed temperature was controlled at -80°C. The initiator described in Example 1 was transferred to a dropping funnel cooled to -40°C. The polymerization reaction was carried out by slowly adding the initiator solution dropwise so that the temperature was kept at -80°C. 22mL initiator solution was added dropwise within 17min. After 16 min, the initially milky suspension had agglomerated so violently that the internal temperature could no longer be maintained and rose to -75.2°C. The reaction was terminated. As a result 54.6 g of dry polymer were obtained with a Staudinger index of 1.7 dl / g and a gel content of 0.9%. The 1,4-bound isoprene content was 2.4 mol%.
[0058] 2b
[0059] 700 g of dry meth...
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