Synthetic method of AMPS (2-Acrylamide-2-methylpropanesulfonic acid)
A methylpropanesulfonic acid and acrylamide-based technology, which is applied in the preparation of sulfonic acid and organic chemistry, can solve the problems of energy consumption and achieve the effects of reducing energy consumption and inhibiting side reactions
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reference example 1
[0023] In the four-necked flask that is provided with temperature control device, stirrer, thermometer and gas feeding device, add 135g commercially available analytical pure acrylonitrile (wherein the content of acrylonitrile is 99.7% by weight, the balance is water), the acrylonitrile Cool to 0°C, slowly add 1 mass% SO 3 31g of fuming sulfuric acid, and then adjust the temperature of the reaction system to 40°C, and slowly introduce 17g of isobutene to react. After the introduction of isobutene is completed, the reaction is terminated after keeping the temperature for one hour, and the reaction solution is vacuum filtered. After filtering, the filter cake and filtrate are obtained, the filtrate is recovered, and 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.
[0024] The dried filter cake is the crude AMPS product, the LC purity is 95% by weight, and the calculated yield of AMPS is 90%.
Embodiment 1
[0026] In the four-necked flask that is provided with temperature control device, stirrer, thermometer and gas feeding device, add the acrylonitrile (wherein the content of acrylonitrile is 99.2% by weight) that reclaims in the reference example 1 of 135g, acrylonitrile is cooled to 0 °C, slowly add 1 wt% SO 331g of fuming sulfuric acid, and then adjust the temperature of the reaction system to 40°C, and pass 17g of isobutene to react. After the isobutene is passed through, the reaction is completed after 1 hour of heat preservation, and the reaction solution is vacuum filtered. After filtering, the filter cake and filtrate are obtained, the filtrate is recovered, and 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.
[0027] The dried filter cake is the crude AMPS product, the LC purity is 95.4% by weight, and the calculated yield of AMPS is 93.5%.
Embodiment 2
[0029] In a four-necked flask provided with a temperature control device, a stirrer, a thermometer and a gas feed device, add 90 g of the acrylonitrile waste liquid recovered in Reference Example 1 (the content of acrylonitrile in the acrylonitrile waste liquid is 99.2% by weight) and 45g of commercially available analytically pure acrylonitrile, the acrylonitrile was cooled to 4°C, and slowly added 3 11.5g of oleum, and then adjust the temperature of the reaction system to 30°C, and slowly introduce 5.3g of isobutene to react. After the introduction of isobutene is completed, the reaction is terminated after 1 hour of heat preservation, and the reaction solution is filtered. The filtrate and filter cake were obtained after filtration, the filtrate was recovered, and the filter cake was vacuum-dried at a drying temperature of 80° C. and a drying pressure of 10 KPa to obtain a dried filter cake.
[0030] The dried filter cake is the crude AMPS product, the LC purity is 95.4% by...
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