Improved solventless sulfonation of exchange resins
A sulfonation and resin technology, applied in the field of improved solvent-free sulfonation of exchange resins, can solve the problems of increasing the time of the total production cycle, increasing expenditure, etc.
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Embodiment 1-10
[0047] The laboratory sulfonator is a glass vessel with a capacity of 1.7 liters. It has a fill port, a fluoropolymer paddle agitator, and a foot valve. The stirrer was driven by a variable speed motor at 200 rpm. The temperature gradient is controlled by an automatic process control computer. The acid concentration is determined by first taking a small sample and titrating it with caustic. Microscopic observation was used to determine when sulfonation was complete, ie, there was no visible polymer core surrounded by a shell of sulfonated polymer.
Embodiment 1
[0049] Experiments were performed at low hydration rates using high initial sulfuric acid concentrations. The copolymers were seeded in situ (semi-batch, Harris, in U.S. Patent 4,564,644 and U.S. Patent 5,068,255) and used 5 wt% active divinylbenzene from 55% DVB and 45% A monomer mixture of ethylvinylbenzene is polymerized. The measured toluene swell crosslinking corresponds to 8% DVB. The copolymer beads were 20 / 45 US mesh in size (that is, the beads were between 354 and 841 microns in size). The copolymer itself has a gel structure. T of copolymer / monomer mixture g Estimated to be 117°C. The copolymer was sulfonated by adding 97% sulfuric acid and heating at 1.0°C / minute to 140°C and maintaining at this temperature for two hours. The resin was hydrated as follows: Acid was pumped into the top of the resin bed so that the acid concentration was reduced and the resin was hydrated at a rate of 1.2 to 1.75% per minute. Acid was removed from the bottom of the column at the...
Embodiment 2
[0051] Experiments were performed on a second polymer to show the effect of reducing the acid concentration at a given temperature. Copolymerization of 8% active divinylbenzene with a particle size of 20 / 45 US mesh (that is, the particle size of the beads is between 354 and 381 microns) at three different starting acid concentrations For sulfonation, the copolymer and acid slurry was heated to 140°C at 1°C / min and maintained at 140°C for the time listed in the table to achieve complete sulfonation. T of copolymer / monomer mixture g Estimated to be 113°C. figure 1 Results are shown for WUBs at each concentration after hydration at a rate of 12% / min. Higher concentrations have shorter sulfonation times, but a lower percentage of intact, unbroken beads.
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