- A new method for the preparation of 6-Methyl-1,2,3-oxathiazine-4(3H)-one 2,2-dioxide, Potassium salt (acesulfame K)
-
A simple two-step synthesis of the title compound, an artificial sweetener, starting from amidosulfonic acid and diketene is described.
- Linkies,Reuschling
-
-
Read Online
- Preparation method of potassium acetylsulfamate
-
The preparation method comprises the following steps: dissolving an acetoacetamide - N - sulfonic acid triethylamine salt solution as a working fluid, dissolving sulfur trioxide in a solvent to form a cyclization agent solution as an injection fluid. The working fluid enters from the nozzle of the Venturi reactor, the injection fluid enters from the suction chamber of the Venturi reactor, and the pressure of the control working fluid is higher than the pressure of the injection fluid. A working fluid is mixed with the injection fluid in a mixing section and a diffusion section of the Venturi reactor to undergo a sulfonation loop reaction, and a sulfonated cyclization product is injected into the flow reactor. The sulfonated loop product is subjected to hydrolysis reaction with a hydrolysis agent preset in the flow reactor to obtain a hydrolysis product solution. Addition of potassium hydroxide to the organic phase of the hydrolyzate solution gives potassium acetylate. The method reduces the probability that organic impurities remain in the final product acesulfame, improves the purity of the acesulfame, and is suitable for large-scale industrial production.
- -
-
Paragraph 0081-0088
(2021/10/16)
-
- Potassium acetylsulfamate composition
-
The invention discloses an acesulfame potassium composition, comprising potassium acetylsulfamate and potassium acetylsulfamate, wherein the content of chloride of potassium acetylsulfamate is less 300 ppm. The composition is prepared by adding triethylamine in an amino sulfonic acid solution to carry out amination reaction, and generating an amino sulfonic acid ammonium salt solution. A diketene is added to an ammonium sulfamate solution, acylation reaction is carried out under the action of a solid acid catalyst, and an intermediate solution is obtained. The intermediate solution and the cyclization agent solution are subjected to sulphonation cyclization reaction under the action of a supported solid alkali heterogeneous catalyst to obtain a sulfonated cyclization product, and Hydrolysis step and salt formation step, the potassium acetylsulfamate composition with extremely low impurity content can be prepared through combination of the two catalysts, so that the process of post-treatment of the potassium acetylsulfanilamide is reduced to a great extent, and the production cost of potassium acetylsulfanilate is reduced.
- -
-
Paragraph 0076; 0083-0088
(2021/09/29)
-
- Preparation method of acesulfame potassium composition
-
The invention relates to a preparation method of an acesulfame potassium composition. According to the preparation method, a proper amount of organic acid is added to adjust the pH value of a neutralization reaction solution so as to change the pH value of an acetoacesulfame triethylamine salt solution generated by acylation reaction, so that the subsequent cyclization hydrolysis yield is increased to 95% or above, and therefore, the content of organic impurities in the acesulfame potassium composition finished product is reduced, and the product quality is improved.
- -
-
Paragraph 0062; 0067; 0070; 0074; 0077-0086
(2021/10/30)
-
- Preparation method of acesulfame potassium composition
-
The invention relates to a preparation method of an acesulfame potassium composition. According to the preparation method, a proper amount of organic acid is added to adjust the pH value of a neutralization reaction solution so as to change the pH value of an acetoacesulfame triethylamine salt solution generated by acylation reaction, so that the subsequent cyclization hydrolysis yield is increased to 95% or above, and therefore, the chromatic value of the acesulfame potassium composition finished product is influenced, and the product quality is improved.
- -
-
Paragraph 0072; 0075-0084
(2021/10/30)
-
- Preparation method of acesulfame potassium
-
The invention relates to a preparation method of acesulfame potassium. The preparation method comprises the following steps: (1) preparation of acetoacetamido-N-sulfonyl methyl ester: dissolving methyl sulfamate in a chlorinated hydrocarbon solvent, and reacting with diketene under the catalysis of strongly alkaline macroporous resin to generate an intermediate acetoacetamido-N-sulfonyl methyl ester; and (2) preparation of acesulfame potassium: carrying out cyclization reaction on acetoacetamido-N-sulfonyl methyl ester under the action of a copper pyridine complex catalyst, removing byproduct methanol through reactive distillation, and then performing KOH treatment to obtain acesulfame potassium. Compared with the existing production process, the copper pyridine complex is used for replacing a strong acid catalyst in the cyclization process, so that the polymerization side reaction of the intermediate is obviously reduced, and the product yield is increased. Meanwhile, triethylamine and SO3 are prevented from being used, and generation of waste acid and waste water is greatly reduced.
- -
-
Paragraph 0024; 0034; 0037-0039; 0042-0044; 0047; 0048; 0050
(2021/06/02)
-
- Continuous preparation method of acesulfame potassium
-
The invention belongs to the field of chemical production, and provides a continuous preparation method of acesulfame potassium. The method comprises the following steps: firstly, mixing SO3 and dichloromethane to prepare a cyclizing agent; adding a certain amount of stabilizer into the cyclizing agent; then, enabling the cyclizing agent added with the stabilizer and a DKA solution to enter a cyclization reaction module through a metering pump; enabling the generated cyclization reaction liquid and water to enter a hydrolysis reaction module, enabling the generated acesulfamic acid to pass through a continuous extraction tower, enabling a separated water phase to enter a waste acid treatment process, enabling an organic phase and a KOH solution to enter a neutralization reaction module, and concentrating, crystallizing, separating and drying the generated acesulfamic acid potassium reaction liquid to obtain an acesulfame potassium finished product. According to the invention, the overall continuity of the preparation process is realized, and meanwhile, the mixing section and reaction section proportion control and the optimal selection of the mixing module are carried out on the micro-channel reactor, so that the product yield of acesulfame potassium is greatly improved, the product quality is more stable, and the process operation is more controllable.
- -
-
Paragraph 0054-0080
(2020/07/24)
-
- Method for continuously producing acesulfame potassium
-
The invention belongs to the field of chemical production, and provides a method for continuously producing acesulfame potassium, which comprises the following steps: continuously mixing and dissolving sulfamic acid and dichloromethane, continuously neutralizing with a triethylamine solution, introducing the neutralized reaction solution and ketene dimer into a continuous reactor, and carrying outaddition acylation reaction to obtain a DKA reaction solution; sulfur trioxide and solvent micro-mixing: S03, enabling dichloromethane to enter a micro-mixer, so as to prepare a cyclizing agent; cyclization and hydrolysis: continuously feeding the DKA reaction solution and a cyclizing agent into a cyclization microreactor to generate a cyclization reaction solution, and continuously feeding the cyclization reaction solution into a hydrolysis microreactor to obtain an acesulfamic acid reaction solution; enabling the acesulfame acid reaction liquid and dichloromethane to enter continuous extraction equipment, enabling an extracted organic phase and a potassium hydroxide aqueous solution to enter a continuous neutralization reactor to obtain acesulfame acid potassium reaction liquid, and subjecting the acesulfame acid potassium reaction liquid to continuous concentration, continuous crystallization, continuous separation and continuous drying to obtain the acesulfame acid potassium finished product. The process has the characteristics of simple process, low cost, good product quality, continuous whole process and the like.
- -
-
Paragraph 0089-0120
(2020/07/24)
-
- Technology for synthesizing acesulfame-K precursor ASH in microchannel reactor
-
The invention provides a technology for synthesizing acesulfame (acesulfame-K) in a microchannel reactor and specifically relates to a key reaction for precursor ASH cyclization synthesis in the technology. The technology comprises feeding a reaction intermediate triethylamine acetoacetamidosulfonate as a raw material having a concentration of 20-60% and a SO3 cyclizing agent with a mass concentration of 25-100% into a microchannel reactor 1, carrying out cyclization, continuously feeding the cyclization liquid into a microchannel reactor 2, and carrying out hydrolysis in water to obtain a precursor ASH. In the cyclization and hydrolysis processes, an integrated microchannel heat exchanger fast removes heat produced by the cyclization and hydrolysis and the cyclization temperature is controlled in a range of -30 to 10 DEG C. Compared with the existing kettle process, the technology has short reaction time, a high cyclization reaction temperature, a small SO3 cyclizing agent use amountand an ASK total yield of 45 to 60% and can be continuously operated.
- -
-
Paragraph 0027-0028; 0029-0030; 0031-0032; 0033-0036
(2018/04/21)
-
- ACESULFAME POTASSIUM COMPOSITIONS AND PROCESSES FOR PRODUCING SAME
-
Improved processes for producing high purity acesulfame potassium. In one embodiment, the process comprises the steps of contacting a solvent, e.g., dichloromethane, and a cyclizing agent, e.g., sulfur trioxide, to form a cyclizing agent composition and reacting an acetoacetamide salt with the cyclizing agent in the composition to form a cyclic sulfur trioxide adduct. The contact time is less than 60 minutes. The process also comprises forming from the cyclic sulfur trioxide adduct composition a finished acesulfame potassium composition comprising non-chlorinated, e.g., non-chlorinated, acesulfame potassium and less than 35 wppm 5-halo acesulfame potassium, preferably less than 5 wppm.
- -
-
Paragraph 0164-0169
(2018/04/13)
-
- ACESULFAME POTASSIUM COMPOSITIONS AND PROCESSES FOR PRODUCING SAME
-
A process for producing acesulfame potassium, the process comprising the steps of providing a cyclizing agent composition comprising a cyclizing agent and a solvent and having an initial temperature, cooling the cyclizing agent composition to form a cooled cyclizing agent composition having a cooled temperature less than 35° C., reacting an acetoacetamide salt with the cyclizing agent in the cooled cyclizing agent composition to form a cyclic sulfur trioxide adduct composition comprising cyclic sulfur trioxide adduct; and, forming from the cyclic sulfur trioxide adduct in the cyclic sulfur trioxide adduct composition the finished acesulfame potassium composition comprising non-chlorinated acesulfame potassium and less than 39 wppm 5-chloro-acesulfame potassium. The cooled temperature is at least 2° C. less than the initial temperature.
- -
-
Paragraph 0179
(2018/04/13)
-
- ACESULFAME POTASSIUM COMPOSITIONS AND PROCESSES FOR PRODUCING SAME
-
Compositions and processes for producing high purity acesulfame potassium are described. One process comprises the steps of providing a crude acesulfame potassium composition comprising acesulfame potassium and acetoacetamide, concentrating the crude acesulfame potassium composition to form a water stream and an intermediate acesulfame potassium composition comprising acesulfame potassium and less than 33 wppm acetoacetamide, and separating the intermediate acesulfame potassium composition to form the finished acesulfame potassium composition comprising acesulfame potassium and less than 33 wppm acetoacetamide. The concentrating step is conducted at a temperature below 90° C. and the separating step is conducted at a temperature at or below 35° C.
- -
-
Page/Page column 0186-0191
(2018/04/13)
-
- METHOD FOR PRODUCING POTASSIUM SALT OF 3,4-DIHYDRO-1,2,3-OXATHIAZIN-4-ONE-2,2-DIOXIDE COMPOUND
-
A method for producing a high quality potassium salt of 3,4-dihydro-1,2,3-oxathiazin-4-one-2,2-dioxide compound easily and efficiently is provided. The producing method of the invention includes the steps of neutralizing 3,4-dihydro-1,2,3-oxathiazin-4-one-2, 2-dioxide compound represented by the following formula (1) (wherein R1 and R2 are the same as or different from each other and are hydrogen atom or an organic group inert to the reaction) with potassium hydroxide in a mixed solvent of water and a water soluble organic solvent to form a potassium salt of 3,4-dihydro-1,2,3-oxathiazin-4-one-2,2-dioxide compound represented by the following formula (2) and, during the neutralization, precipitating potassium sulfate derived from sulfuric acid contained in the compound represented by Formula (1) as an impurity.
- -
-
Page/Page column 6-7
(2009/12/28)
-
- Process for the preparation of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide and its non-toxic salts
-
6-Methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide and its non-toxic salts are prepared by reacting acetoacetamide with an S-O compound of the formula I wherein Y=F, Cl, --OSO2 F or --OSO2 Cl, preferably only F, in the presence of bases. The non-toxic salts--especially the potassium salt--are valuable synthetic sweeteners.
- -
-
-
