Method for high-temperature continuous acylation in sucralose production
A sucralose, medium and high temperature technology, applied in the chemical industry, can solve the problems of energy consumption, low reaction yield, low reaction temperature, etc., and achieve the effects of improving operating temperature, product purity, and high reaction yield
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[0013] Example 1
[0014] Pump the esterification liquid containing sucrose organotin intermediate (including intermediate: 65wt%, DMF: 35wt%) and acetic anhydride into the acylation reactor at the same time, the temperature of the reactor is about 30℃, the esterification liquid and acetic anhydride The mass ratio is 10:1, while adjusting the flow rate of acetic anhydride to make the pH value of the mixture after the reaction reach 4.5, the acylation reaction can be completed in 0.2s. The material at the outlet of the acylation reactor enters the acylation freezer to cool down at 10-15°C, keep it warm with chilled water, and keep it for 1 hour.
[0015] The acylation reaction solution is then subjected to a hydrolysis reaction, and then cyclohexane is added for extraction to recover the organotin acetate produced after the reaction. The content of sucrose-6-ethyl ester in the acylation reaction solution is detected, and the reaction yield is ≥98%.
[0016] The organotin acetate extr...
Example Embodiment
[0017] Example 2
[0018] The esterification liquid containing sucrose organotin intermediate: intermediate: 65wt%, DMF: 35wt% esterified liquid is pumped into the acylation reactor, and acetic anhydride is pumped to adjust the flow rate to make the pH value of the mixture after the reaction to 5, esterification The liquid and acetic anhydride are pumped into the acylation reactor at the same time, the mass ratio of esterification liquid to acetic anhydride is 13:1, the temperature of the reactor is controlled at 10-15℃, and the reaction time is controlled at 0.2s. The material at the outlet of the reactor enters the acylation. In the freezing kettle, use circulating water for heat preservation.
[0019] The acylation reaction solution is then subjected to a hydrolysis reaction, and then cyclohexane is added for extraction to recover the organotin acetate produced after the reaction. The content of sucrose-6-ethyl ester in the acylation reaction solution is detected, and the reacti...
Example Embodiment
[0021] Example 3
[0022] The esterification liquid containing sucrose organotin intermediate: intermediate: 65wt%, DMF: 35wt% esterified liquid is pumped into the acylation reactor, and acetic anhydride is pumped to adjust the flow rate to make the pH value of the mixture after the reaction to 5, esterification The liquid and acetic anhydride are pumped into the acylation reactor at the same time, the mass ratio of esterification liquid to acetic anhydride is 15:1, the temperature of the reactor is controlled at 10-15℃, and the reaction time is controlled at 0.2s. The material at the outlet of the reactor enters the acylation. In the freezing kettle, use circulating water for heat preservation.
[0023] The acylation reaction solution is then subjected to a hydrolysis reaction, and then cyclohexane is added for extraction to recover the organotin acetate produced after the reaction. The content of sucrose-6-ethyl ester in the acylation reaction solution is detected, and the reacti...
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