Solvent composition for recrystallization of 2-acrylamido-2-methylpropanesulfonic acid and application thereof
A methylpropanesulfonic acid and acrylamide-based technology, which is applied in the preparation of sulfonic acid, the preparation of organic compounds, organic chemistry, etc., can solve the problem of low recrystallization yield, achieve huge commercial value, controllable raw material cost, Effects in simple steps
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Embodiment 1
[0042] In a four-neck flask equipped with a temperature control device, a stirrer, a thermometer and a gas feed device, add 330 g of analytically pure acrylonitrile (wherein the content of acrylonitrile is 99.7 wt % of the total amount, and the balance is water). Cool to -10°C, slowly add 2wt% SO 3 61g of fuming sulfuric acid (that is, the sulfuric acid meter concentration is 100wt%), constant temperature 120 minutes. The temperature was raised to 40° C., and 35 g of gaseous isobutene was slowly introduced for reaction. After the introduction of isobutene is completed, the reaction is terminated after 1 hour of heat preservation, and a slurry product is obtained. The slurry product is vacuum filtered to obtain a filter cake and a filtrate. The filter cake is vacuum-dried at a drying temperature of 100° C. and a drying pressure of 10 KPa to obtain a dried filter cake that is crude 2-acrylamido-2-methylpropanesulfonic acid. After analysis, the yield was 91.5%, and the purity ...
Embodiment 2
[0045] The difference from Example 1 is that during the recrystallization process, 210 g of solvent composition (including 30 g of water and 180 g of ethylene glycol) was used, cooled to 65° C., and then about 135 g of solvent was extracted using a rotary evaporator. Through analysis, the yield of the recrystallization process is 91.7%, and the purity is 99.3wt%.
Embodiment 3
[0047] The difference from Example 1 is that during the recrystallization process, 220g of solvent composition (including 40g of N,N-dimethylformamide and 180g of heptane) was used and heated to 85°C (the heating rate was 3°C / min ), and then use a rotary evaporator to extract about 140 g of solvent. Through analysis, the yield of the recrystallization process is 94.0%, and the purity is 99.3wt%.
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