4-Morpholineethanesulfonic acid synthesis

Yield:4432-31-9 85%

Reaction Conditions:

in water at 60; for 6 h;Large scale;

Steps:

1.2; 1.3; 1.4

2> Add 130kg of 25% sodium vinyl sulfonate (SVS) solution to the synthetic tank.105 kg of morpholine was added, and the reaction was carried out at 60 ° C for 2 hours, and then refluxed for 4 hours.Concentrate under reduced pressure, remove unreacted morpholine, to a thick form, add deionized water 600L to dissolve,It was diluted with deionized water to a volume of 3000 L and subjected to column chromatography.3> 42,000 dilutions of 12000 L were applied to the column at a rate of 2000 L/h.The column is filled with strong acidic ion exchange resin, and the exchange capacity is 10kmol. After the completion, the ionized water is 2000L/h.The effluent with neutral pH and pH 4 or higher was discarded, the effluent with pH 4 was finally discarded.After each use of the resin (12000L), it needs to be activated by acid activation before it can be used.4> The pH <4 collection solution is concentrated under reduced pressure, controlled vacuum 0.09 ~ 0.095MPa, temperature <80 ° C, concentrated to a thick,The temperature was lowered to 0 ° C, suction filtration, and the filtrate was accumulated to 3000 L. The product was concentrated by crystallization, and the filter cake was washed twice with 20 L of absolute ethanol.Dry, control the vacuum in the rotary vacuum dryer to 0.09MPa or more, dry at 80 °C,The temperature was lowered to 40 ° C, and the vacuum was discharged with nitrogen, sampled, bagged, and sealed.The product was obtained in 664 kg, and the yield was 85% (in terms of SVS).

References:

CN109836399,2019,A Location in patent:Paragraph 0029; 0031-0033