Organic solvent-free hydrogenation of diene-based polymers
A polymer and conjugated diene technology, applied in the field of hydrogenation of carbon-carbon double bonds, can solve the problems of no research on hydrogenation of diene-based polymers, slow reaction rate, etc.
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Embodiment 1
[0046] A 300 ml glass lined stainless steel autoclave with temperature control, stirrer and hydrogen addition point was used. 0.6 g of butadiene-acrylonitrile polymer with a limited acrylonitrile content of about 38% by weight and a Mooney viscosity (ML1+4 @ 100°C) of about 50 was used in the form of loose pellets 1-2 mm in diameter. Use 0.003g of catalyst RhCl (PPh 3 ) 3 and 0.03 g of triphenylphosphine. A temperature of 145°C and a hydrogen pressure of 500 psi (3.4 MPa) were applied for 6 hours. The system was then cooled, depressurized, and all polymer particles were removed from the reactor, dissolved in methyl ethyl ketone, and the degree of hydrogenation determined by infrared analysis of the hydrogenated polymer and further confirmed by NMR. A degree of hydrogenation of 97.9% was obtained and no gels were produced in the hydrogenated polymer.
Embodiment 2
[0048] The same procedure as described in Example 1 was used, but with a reaction time of 3 hours. The degree of hydrogenation was 89%, and no gel was produced in the hydrogenated polymer.
Embodiment 3
[0050] The same procedure as described in Example 1 was used, but the reaction time was 1 hour and the reaction temperature was 160°C. A degree of hydrogenation of 77.6% was obtained, and no gel was produced in the hydrogenated polymer.
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Abstract
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