Sulfonated polyolefin-based flame retardant material
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example 1
Preparation of Sulfonated Polyolefin (LLDPE) Fiber
[0078]An as-spun tow of neat LLDPE of 1560 filaments (18 micrometer filament diameter) was continuously processed through a two-part reactor containing (1) concentrated sulfuric acid, and (2) oleum with 20% SO3. The speed of the fiber was adjusted to attain proper residence time. A tensile stress of 5 MPa was applied to the fiber during semi-continuous processing. For the concentrated sulfuric acid bath, the temperature was maintained at 115° C. A temperature below 100° C. in the concentrated sulfuric acid bath did not result in an infusible fiber even after 12 hours of treatment. For the oleum bath (which is a concentrated sulfuric acid bath containing dissolved SO3 gas), the temperature was maintained at 90° C. A residence time of 4 hours and 40 minutes was used for the concentrated sulfuric acid and oleum baths, respectively, which resulted in infusible fibers that were found to be hygroscopic under ambient conditions.
[0079]The ol...
example 2
Preparation of Sulfonated Polyolefin (LLDPE) Fiber Using E-beam Irradiation
[0083]The LLDPE fiber tow discussed in Example 1 was e-beam irradiated at 10-1000 kGy to reduce the melting temperature, which in turn accelerated the sulfonation kinetics during subsequent sulfonation reaction. As shown in FIG. 4, increasing radiation dosage results in a reduction in melting temperature of polyethylene fibers with overall heat of fusion, i.e., crystallinity, of the fibers remaining unchanged, even when they were irradiated at 1000 kGy dosage. However, when polyethylene fiber was irradiated in the presence of a SO2 gas and at 500 kGy dose, a significant reduction in crystallinity was observed, as also shown in FIG. 4. This indicates crosslinking of the polymer by the SO2 gas and e-beam. The highly irradiated fibers were dissolved in the sulfonation bath due to vigorous reaction. However, unlike the neat PE fiber sample described in Example 1, the 10 kGy irradiated fiber, when treated with con...
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