55589-62-3

Basic information

• Product Name: 6-Methyl-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide potassium salt
• Synonyms: 6-METHYL-1,2,3-OXATHIAZIN-4(3H)-ONE 2,2-DIOXIDE POTASSIUM SALT;ACESULFAME K;ACESULFAME POTASSIUM SALT;ACESULFAME POTASSIUM;1,2,3-oxathiazin-4(3h)-one,6-methyl-,2,2-dioxide,potassiumsalt;6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one2,2-dioxidepotassiumsalt;potassiumacesulfame;Potassiumsaltof6-methyl-1,2,3-oxathiazin-4(3H)-one-2,2-dioxide
• CAS NO: 55589-62-3
• Molecular Formula: C₄H₄NO₄S*K
• Molecular Weight: 202.25
• EINECS: 259-715-3
• Product Categories: Food & Feed ADDITIVES;K (Potassium) Compounds (excluding simple potassium salts);Classes of Metal Compounds;Typical Metal Compounds;Sweeteners;Food & Flavor Additives;Heterocycles;Sulfur & Selenium Compounds;SUNETT
• Mol File: 55589-62-3.mol

Chemical Properties

• Melting Point: 229-232°C (dec.)
• Boiling Point: 332.7oC at 760 mmHg
• Flash Point: 155oC
• Appearance: /
• Density: (solid) 1.81 g/cm3; d (bulk) 1.1-1.3 kg/dm3
• Vapor Pressure: 1.03E-05mmHg at 25°C
• Storage Temp.: 0-6°C
• Solubility: Soluble in water, very slightly soluble in acetone and in ethanol (96 per cent).
• Water Solubility: almost transparency
• Merck: 14,37
• BRN: 3637857
• CAS DataBase Reference: 6-Methyl-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide potassium salt(CAS DataBase Reference)
• NIST Chemistry Reference: 6-Methyl-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide potassium salt(55589-62-3)
• EPA Substance Registry System: 6-Methyl-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide potassium salt(55589-62-3)

Safety Data

• Statements: 36/37/38
• Safety Statements: 26-36/37/39
• WGK Germany: 1
• RTECS: RP4489165
• Hazardous Substances Data: 55589-62-3(Hazardous Substances Data)

Usage

Chemical Properties

Different sources of media describe the Chemical Properties of 55589-62-3 differently. You can refer to the following data:
1. White to Off-White Solid
2. Acesulfame potassium occurs as a colorless to white-colored, odorless, crystalline powder with an intensely sweet taste.

Originator

Acesulfame Potassium ,Hoechst

History

Acesulfame-K, the potassium salt of acesulfame, is a sweetener that resembles saccharin in structure and taste profile. 5,6-Dimethyl-1,2,3-oxathiazine-4(3H)-one 2,2-dioxide, the first of many sweet compounds belonging to the dihydrooxathiazinone dioxide class, was discovered accidentally in 1967. From these many sweet compounds, acesulfame was chosen for commercialization. To improve water solubility, the potassium salt was made. Acesulfame-K (Sunett) was approved for dry product use in the United States in 1988 and in Canada in October, 1994. In 2003, acesulfame-K was approved as a general purposes sweetener by the FDA.

Uses

Different sources of media describe the Uses of 55589-62-3 differently. You can refer to the following data:
1. 'New generation', heat-stable sweetener that has not been suspected to cause cancer nor be genotoxic. Allelic variation of the Tas1r3 gene affects behavioral taste responses to this molecule, suggesting that it is a T1R3 receptor ligand.
2. Potassium salt as sweetener for foods, cosmetics.
3. Acesulfame-K is the potassium salt of 6-methyl-l,2,3-oxathiazin-4(3H)- one-2,2-dioxide. This sweetener was discovered in Germany and was first approved by the FDA in 1988 for use as a nonnutritive sweetener. The complex chemical name of this substance led to the creation of the trademark common name, acesulfame-K, which is based on its following relationships to acetocetic acid and sulfanic acid, and to its potassium salt nature. Acesulfame-K is 200 times as sweet as sugar and is not metabolized and is thus noncaloric. It is exceptionally stable at elevated temperatures encountered in baking, and it is also stable in acidic products, such as carbonated soft drinks. It has a synergistic effect when mixed with other low-calorie sweetners, such as aspartame. Common applications of acesulfame-K are table uses, chewing gums, beverages, foods, bakery products, confectionary, oral hygiene products, and pharmaceuticals.

Production Methods

Different sources of media describe the Production Methods of 55589-62-3 differently. You can refer to the following data:
1. Acesulfame potassium is synthesized from acetoacetic acid tertbutyl ester and fluorosulfonyl isocyanate. The resulting compound is transformed to fluorosulfonyl acetoacetic acid amide, which is then cyclized in the presence of potassium hydroxide to form the oxathiazinone dioxide ring system. Because of the strong acidity of this compound, the potassium salt is produced directly. An alternative synthesis route for acesulfame potassium starts with the reaction between diketene and amidosulfonic acid. In the presence of dehydrating agents, and after neutralization with potassium hydroxide, acesulfame potassium is formed.
2. The principal commercial process for acesulfame-K is depicted below:

Manufacturing Process

80 g (1.096 mol) of dimethylethylamine were added drop-wise, with cooling, to 80 g (0.825 mol) of sulfamic acid suspended in 500 ml of glacial acetic acid. When dissolution was complete, 80 ml (1.038 mol) of diketene were added, while cooling at 25°-35°C. After 16 hours, the mixture was evaporated and the residue was stirred with acetone, whereupon crystallization of dimethylethylammonium acetoacetamide-N-sulfonate took place. Yield: 110 g (43%), melting point 73°-75°C. 12.7 g (50 mmol) of dimethylethylammonium acetoacetamide-N-sulfonate in 110 ml of methylene chloride were added drop-wise to 8 ml (200 mmol) of liquid SO3 in 100 ml of CH2Cl2 at -30°C, stirring vigorously, within 60 minutes. 30 minutes later, 50 ml of ethyl acetate and 50 g of ice were added to the solution. The organic phase was separated off, and the aqueous phase was extracted twice more with ethyl acetate. The combined organic phases were dried over sodium sulfate, evaporated and the residue was dissolved in methanol. On neutralization of the solution with methanolic KOH, the potassium salt of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide precipitated out. Yield: 7.3 g (73%). The product was detected by thinlayer chromatography; the structure of it was confirmed with IR spectrum.

Pharmaceutical Applications

Acesulfame potassium is used as an intense sweetening agent in cosmetics, foods, beverage products, table-top sweeteners, vitamin and pharmaceutical preparations, including powder mixes, tablets, and liquid products. It is widely used as a sugar substitute in compounded formulations,and as a toothpaste sweetener. The approximate sweetening power is 180–200 times that of sucrose, similar to aspartame, about one-third as sweet as sucralose, one-half as sweet as sodium saccharin, and about 4-5 times sweeter than sodium cyclamate.It enhances flavor systems and can be used to mask some unpleasant taste characteristics.

Safety Profile

When heated to decompositionemits toxic fumes of SOx.

Safety

Acesulfame potassium is widely used in beverages, cosmetics, foods, and pharmaceutical formulations, and is generally regarded as a relatively nontoxic and nonirritant material. Pharmacokinetic studies have shown that acesulfame potassium is not metabolized and is rapidly excreted unchanged in the urine. Long-term feeding studies in rats and dogs showed no evidence to suggest acesulfame potassium is mutagenic or carcinogenic. The WHO has set an acceptable daily intake for acesulfame potassium of up to 15 mg/kg body-weight.The Scientific Committee for Foods of the European Union has set a daily intake value of up to 9 mg/kg of body-weight. LD50 (rat, IP): 2.2 g/kg LD50 (rat, oral): 6.9–8.0 g/kg

storage

Acesulfame potassium possesses good stability. In the bulk form it shows no sign of decomposition at ambient temperature over many years. In aqueous solutions (pH 3.0–3.5 at 208℃) no reduction in sweetness was observed over a period of approximately 2 years. Stability at elevated temperatures is good, although some decomposition was noted following storage at 408℃ for several months. Sterilization and pasteurization do not affect the taste of acesulfame potassium. The bulk material should be stored in a well-closed container in a cool, dry place and protected from light.

Regulatory Status

Included in the FDA Inactive Ingredients Database for oral and sublingual preparations. Included in the Canadian List of Acceptable Non-medicinal Ingredients. Accepted for use in Europe as a food additive. It is also accepted for use in certain food products in the USA and several countries in Central and South America, the Middle East, Africa, Asia, and Australia.

InChI:InChI=1/C4H5NO4S.K/c1-3-2-4(6)5-10(7,8)9-3;/h2H,1H3,(H,5,6);/q;+1/p-1

Synthetic route

Triethylammoniumsalz der Acetoacetamid-N-sulfonsaeure (99911-48-5) → potassium acesulfame (55589-62-3)

Conditions	Yield
Stage #1: Triethylammoniumsalz der Acetoacetamid-N-sulfonsaeure With sulfur trioxide In dichloromethane; water at 100℃; under 75007.5 Torr; for 2.77778E-06h; Stage #2: With potassium hydroxide In water at 50℃; for 0.1h; Pressure; Temperature;	85%
Stage #1: Triethylammoniumsalz der Acetoacetamid-N-sulfonsaeure With sulfur trioxide In dichloromethane at 1.5 - 4.5℃; Stage #2: With potassium hydroxide In water Temperature;	56.7%
Yield given. Multistep reaction;
Stage #1: Triethylammoniumsalz der Acetoacetamid-N-sulfonsaeure With sulfur trioxide In dichloromethane at -35 - -25℃; for 0.0833333h; Stage #2: With water In dichloromethane at -22 - 20℃; Stage #3: With potassium hydroxide In dichloromethane; water at 24 - 26℃; Time; Temperature; Reagent/catalyst;
With sulfur trioxide In dichloromethane at 11℃;

4-methyleneoxetan-2-one (674-82-8) → potassium acesulfame (55589-62-3)

Conditions	Yield
Stage #1: 4-methyleneoxetan-2-one With aminosulfonic acid; triethylamine In dichloromethane at 20 - 25℃; for 0.00833333h; Stage #2: With sulfur trioxide In dichloromethane at 20 - 40℃; under 0 - 7500.75 Torr; Stage #3: With potassium hydroxide In dichloromethane; water Temperature;	85%

acetoacetamido (5977-14-0) → potassium acesulfame (55589-62-3)

Conditions	Yield
Yield given. Multistep reaction;

fluorosulfonyl fluoride (640723-20-2, 2699-79-8, 12769-73-2) + methanolic KOH + acetoacetamido (5977-14-0) → potassium acesulfame (55589-62-3)

Conditions	Yield
With triethylamine In acetonitrile

methanolic KOH + acetoacetamido (5977-14-0) → potassium acesulfame (55589-62-3)

Conditions	Yield
With triethylamine In acetonitrile

acetosulfam (33665-90-6) → potassium acesulfame (55589-62-3)

Conditions	Yield
With potassium hydroxide In methanol; water at 35℃; Product distribution / selectivity;

C4H5NO4S*4O3S → potassium acesulfame (55589-62-3)

Conditions	Yield
Stage #1: C4H5NO4S*4O3S With water In dichloromethane at -22 - -5℃; for 0.166667h; Stage #2: With potassium hydroxide In dichloromethane; water at 24 - 26℃; for 0.333333h;

acetosulfam (33665-90-6) → 5-chloroacesulfame potassium + potassium acesulfame (55589-62-3)

Conditions	Yield
With potassium hydroxide at 25℃; for 0.333333h;

potassium acesulfame (55589-62-3) + oxybuprocaine hydrochloride (5987-82-6) → oxybuprocaine acesulfamate

Conditions	Yield
In ethanol at 20℃;	100%

N,N-diethyl-N',N'-di-n-propyl-N''-n-hexyl-N''-n-octylguanidinium chloride (1260486-47-2) + potassium acesulfame (55589-62-3) → N,N-diethyl-N',N'-di-n-propyl-N''-n-hexyl-N''-n-octylguanidinium acesulfamate (1260486-62-1)

Conditions	Yield
In water at 60℃;	99%

potassium acesulfame (55589-62-3) + epinephrine hydrochloride (55-31-2) → epinephrine acesulfamate

Conditions	Yield
In acetonitrile at 50℃; for 4h; Sonication;	99%

potassium acesulfame (55589-62-3) + lidocaine hydrochloride (73-78-9) → 2-((2,6-dimethylphenyl)amino)-N,N-diethyl-2-oxoethan-1-aminium 6-methyl-1,2,3-oxathiazin-4-olate 2,2-dioxide

Conditions	Yield
In acetonitrile at 50℃; for 4h; Sonication;	98%

N,N-diethyl-N',N'-di-n-propyl-N''-n-hexyl-N''-n-decylguanidinium chloride (1260486-48-3) + potassium acesulfame (55589-62-3) → N,N-diethyl-N',N'-di-n-propyl-N''-n-hexyl-N''-n-decylguanidinium acesulfamate (1260486-63-2)

Conditions	Yield
In water at 60℃;	97%

potassium acesulfame (55589-62-3) + mepivacaine hydrochloride (1722-62-9) → mepivacaine acesulfamate

Conditions	Yield
In acetonitrile at 50℃; for 4h; Sonication;	97%

pyridin-3-ylamine (462-08-8) + water (7732-18-5) + potassium acesulfame (55589-62-3) + cobalt(II) perchlorate hexahydrate → C10H20CoN4O4(2+)*2C4H4NO4S(1-)*2H2O

Conditions	Yield
In ethanol at 65 - 75℃; for 6h; High pressure;	92%

Dodecyl-((1R,2S,5R)-2-isopropyl-5-methyl-cyclohexyloxymethyl)-dimethyl-ammonium; chloride + potassium acesulfame (55589-62-3) → butyldimethyl[(1R,2S,5R)-(-)menthoxymethyl]ammonium acesulfamate

Conditions	Yield
In water at 20℃; for 2h;	91.5%

3-hydroxy-1-pentyloxymethylpyridinium chloride (454234-72-1) + potassium acesulfame (55589-62-3) → 3-hydroxy-1-pentyloxymethylpyridinium acesulfamate (1127350-75-7)

Conditions	Yield
In water for 26h;	91%

1-butoxymethyl-3-hydroxypyridinium chloride (454234-71-0) + potassium acesulfame (55589-62-3) → 1-butoxymethyl-3-hydroxypyridinium acesulfamate (1127350-74-6)

Conditions	Yield
In water for 26h;	91%

3-hydroxy-1-propoxymethylpyridinium chloride (454234-70-9) + potassium acesulfame (55589-62-3) → 3-hydroxy-1-propoxymethylpyridinium acesulfamate (1127350-73-5)

Conditions	Yield
In water for 26h;	90%

3-hydroxy-1-undecyloxymethylpyridinium chloride (454234-78-7) + potassium acesulfame (55589-62-3) → 3-hydroxy-1-undecyloxymethylpyridinium acesulfamate (1127350-78-0)

Conditions	Yield
In water for 26h;	90%

zinc perchlorate + potassium acesulfame (55589-62-3) → acesulfame zinc

Conditions	Yield
In water Cooling with ice;	90%

sodium tetrachloropalladate + potassium acesulfame (55589-62-3) → dipotassium-tetrakis[6-methyl-1,2,3-oxathiazine-4(3H)-one-3-ato-2,2-dioxide]palladate(II)

Conditions	Yield
In water soln. of Na2PdCl4 and the oxathiazine-dioxide in 3 ml H2O stirred (12 h, room temp.); ppt. sucked off, washed with H2O and EtOH, dried (vac.); elem. anal.;	89%

N,N-diethyl-N',N'-di-n-propyl-N'',N''-di-n-hexylguanidinium chloride (1260486-46-1) + potassium acesulfame (55589-62-3) → N,N-diethyl-N',N'-di-n-propyl-N'',N''-di-n-hexyl-guanidinium acesulfamate (1260486-61-0)

Conditions	Yield
In water at 60℃;	88%

potassium acesulfame (55589-62-3) + dimethyl dodecyl 3-hydroxypropyl ammonium bromide → C17H38NO(1+)*C4H4NO4S(1-)

Conditions	Yield
In ethanol at 60℃; for 24h;	88%

potassium acesulfame (55589-62-3) + N-(3-(diethoxyphosphoryl)propyl)-N,N-dimethyloctadecan-1-ammonium bromide → N-(3-(diethoxyphosphoryl) propyl)-N,N-dimethyloctadecan-1-aminium-6-methyl-4-oxo-4H-1,2,3-oxathiazin-3-ide-2,2-dioxide

Conditions	Yield
In ethanol at 60℃; for 24h;	88%

potassium acesulfame (55589-62-3) + 3'-nitro-2-bromoacetophenone (2227-64-7) → 6-methyl-3-[2-(3-nitrophenyl)-2-oxoethyl]-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide (1621619-40-6)

Conditions	Yield
In N,N-dimethyl-formamide at 80℃; for 24h; Inert atmosphere;	87%

C16H36NO2(1+)*Br(1-) + potassium acesulfame (55589-62-3) → dodecyl(2-(2-hydroxyethoxy)ethyl)dimethylammonium acesulfame

Conditions	Yield
In methanol at 40℃; for 24h;	87%

C20H44NO2(1+)*Br(1-) + potassium acesulfame (55589-62-3) → hexadecyl(2-(2-hydroxyethoxy)ethyl)dimethylammonium acesulfame

Conditions	Yield
In methanol at 40℃; for 24h;	86%

Upstream product

• 5977-14-0 acetoacetamido 
• 99911-48-5 Triethylammoniumsalz der Acetoacetamid-N-sulfonsaeure 
• 640723-20-2 fluorosulfonyl fluoride 
• 33665-90-6 acetosulfam 
• 674-82-8 4-methyleneoxetan-2-one 
• 761-02-4 Triethylammoniumsalz der Amidosulfonsaeure 

Downstream Products

• 33665-90-6 acetosulfam 
• 1621619-31-5 4-[(2-bromobenzyl)oxy]-6-methyl-1,2,3-oxathiazine 2,2-dioxide 
• 1621619-32-6 3-(3-bromobenzyl)-6-methyl-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide 
• 1621619-33-7 3-(2-fluorobenzyl)-6-methyl-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide 
• 1621619-36-0 3-(2,6-difluorobenzyl)-6-methyl-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide 
• 1621619-37-1 4-[(6-methyl-2,2-dioxido-4-oxo-1,2,3-oxathiazin-3(4H)-yl)methyl]benzonitrile 
• 1621619-40-6 6-methyl-3-[2-(3-nitrophenyl)-2-oxoethyl]-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide 
• 1621619-27-9 6-methyl-3-(2-nitrobenzyl)-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide 
• 1621619-28-0 6-methyl-4-[(2-nitrobenzyl)oxy]-1,2,3-oxathiazine 2,2-dioxide 
• 1621619-29-1 6-methyl-3-(3-nitrobenzyl)-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide 
• 1621619-30-4 6-methyl-4-[(3-nitrobenzyl)oxy]-1,2,3-oxathiazine 2,2-dioxide 
• 1621619-34-8 3-(3-fluorobenzyl)-6-methyl-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide 
• 1621619-35-9 4-[(3-fluorobenzyl)oxy]-6-methyl-1,2,3-oxathiazine 2,2-dioxide 
• 1621619-38-2 6-methyl-3-(2-oxo-2-phenylethyl)-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide 

Relevant articles and documents

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.