Well defined, highly crosslinked nanoparticles and method for making same
a nanoparticle, highly crosslinked technology, applied in the field of nanoparticles, to achieve the effect of improving the physical properties of rubber moldability and tenacity, and beneficial and unexpected improvements in rubber composition
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[0089]A 0.8 liter nitrogen-purged glass bottle sealed with a septum liner and perforated crown cap was used as the reactor vessel for the examples below. Styrene (33 wt % in hexane), hexane, n-butyllithium (1.60 M in hexane), 2,2-bis(2′-tetrahydrofuryl)propane (1.60 M in hexane, stored over calcium hydride), potassium tert-amyloxide (KTA), and BHT solution in hexane were also used. PS-PB diblocks STEREON S730AC and STEREON S721 were obtained from Firestone Polymers. Commercially available reagents were obtained from Aldrich and Gelest Inc. (Morrisville, Pa.) and dried over molecular sieves (3 Å).
examples a-d
[0090]Examples A-D were made by the method below. The only difference between examples A-D is the amount of DVB that was added.
[0091]To a 0.8 liter nitrogen-purged glass bottle was added 140 g of hexane, 60 g of 33 wt % styrene, varying amounts of DVB, 6 ml of 5 wt % STEREON S721, 0.4 ml of 1.6 M 2,2′-di(tetrahydrofuryl)propane (OOPS), and 2 ml of 1.6 M n-butyl lithium. The amount of DVB was added in the amounts shown in FIG. 1. The DVB % shown in FIG. 1 is a weight percent based on the total amount of DVB and monomer. The reaction mixture was stirred for one day at room temperature before terminating with 3 ml isopropanol. After the solvent evaporated, the products were dried in vacuum.
[0092]FIG. 1 graphically shows the yield of nanoparticles obtained compared to the varying amounts of DVB. The DVB was added all at once, and a single solvent system (hexane) was used. This data demonstrates that simply increasing the amount of DVB causes reduced yields.
example 1
[0093]To a 0.8 liter nitrogen-purged glass bottle was added 140 g of hexane, 60 g of 33 wt % styrene, 10 ml of DVB, 6 ml of 5 wt % STEREON S721, 0.4 ml of 1.6 M 2,2′-di(tetrahydrofuryl)propane (OOPS), and 2 ml of 1.6 M n-butyl lithium. The reaction mixture was stirred for one day at room temperature before terminating with 3 ml isopropanol. After the solvent evaporated, the products were dried in vacuum.
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