METHOD FOR PREPARING ACESULFAME POTASSIUM

20240083862

18/518796

November 24, 2023

Described herein is a method for preparing acesulfame potassium, comprising: adding triethylamine to a sulfamic acid solution, and carrying out an amination reaction to produce a sulfamic acid ammonium salt solution; adding diketene to the obtained sulfamic acid ammonium salt solution, and under the action of a solid superacid catalyst, carrying out an acylation reaction to obtain an intermediate solution; dissolving sulfur trioxide in a solvent to form a cyclizing agent solution; adding the cyclizing agent solution to the intermediate solution, and carrying out a sulfonation cyclization reaction to obtain a cyclized product solution; adding a hydrolysis agent to the cyclized product solution, and carrying out a hydrolysis reaction to obtain a hydrolysis product solution; and adding a potassium hydroxide solution to the organic phase of the hydrolysis product solution to obtain acesulfame potassium.

1. A method for preparing acesulfame potassium, wherein comprising: an intermediate preparation step: adding triethylamine to a sulfamic acid solution, carrying out an amination reaction to produce an ammonium sulfamate solution, adding diketene to the obtained ammonium sulfamate solution, and carrying out an acylation reaction under the action of a solid superacid catalyst to obtain an intermediate solution; a sulfonation cyclization step: dissolving sulfur trioxide in a solvent to form a cyclizing agent solution, adding the cyclizing agent solution to the intermediate solution, and carrying out a sulfonation cyclization reaction to obtain a cyclized product solution; a hydrolysis step: adding a hydrolysis agent into the cyclized product solution, and carrying out a hydrolysis reaction to obtain a hydrolysate solution; and a salt forming step: adding potassium hydroxide to the organic phase of the hydrolysate solution to obtain acesulfame potassium.

2. The method of claim 1, wherein the solid superacid catalyst is a SO42−/MxOy type catalyst, wherein M represents a metal atom.

3. The method of claim 2, wherein the solid superacid catalyst is a SO42−/Fe2O3 type catalyst.

4. The method of claim 1, wherein the hydrolysis agent is deionized water or an aqueous ethanol solution.

5. The method of claim 4, wherein the hydrolysis agent is the ethanol aqueous solution, wherein the mass concentration of ethanol in the ethanol aqueous solution is 30-65%.

6. The method of claim 1, wherein the reaction temperature of the hydrolysis reaction is 0 to 20° C., more preferably 10 to 20° C.; and the reaction time of the hydrolysis reaction is 30-400 s.

7. The method of claim 1, wherein the molar ratio of the amount of the sulfamic acid to the amount of the sulfur trioxide is 4-8:1, preferably 6:1; and the solvent is dichloromethane.

8. The method of claim 1, wherein the molar ratio of the amount of sulfur trioxide to the content of water in the hydrolysis agent is 1: 1-4, preferably 1: 1-1.5.

9. The method of claim 1, wherein the specific steps of the intermediate preparation step comprise: dissolving sulfamic acid in a first solvent to prepare a first reaction solution; dissolving triethylamine in a second solvent to prepare a second reaction solution, adding the second reaction solution into the first reaction solution, and carrying out an amination reaction to form an ammonium sulfamate solution; dissolving diketene in a third solvent to prepare a third reaction solution; and filling the reactor with a solid superacid catalyst, sequentially adding the ammonium sulfamate solution and the third reaction solution to the reactor, and reacting under a preset condition to form an acetylacetamide-N-sulfonic acid triethylamine salt solution as an intermediate solution.

10. The method of claim 1, wherein the method is carried out in a continuous reactor, and the continuous reactor is a fixed bed reactor, a continuous stirred tank reactor or a microchannel reactor.

07; 01; 01

edspap.20240083862