CN113896692A - Preparation method of acesulfame potassium composition - Google Patents
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- CN113896692A CN113896692A CN202111011051.0A CN202111011051A CN113896692A CN 113896692 A CN113896692 A CN 113896692A CN 202111011051 A CN202111011051 A CN 202111011051A CN 113896692 A CN113896692 A CN 113896692A
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Abstract
The invention relates to a preparation method of a potassium sulfacetamide composition, which reduces organic by-products generated by sulfur trioxide and dichloromethane and reduces the content of volatile components in products by controlling the reaction conditions of a cyclizing agent composition, thereby preventing the occurrence of the caking phenomenon of the potassium sulfacetamide composition and improving the product quality.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a preparation method of a potassium acetylsulfanilate composition.
Background
Acesulfame potassium, chemical name is 6-methyl-1, 2, 3-thiazine-4 (3) -ketone-2, 2-potassium dioxide, commonly known as Acesulfame potassium, AK sugar (Acesulfame-K). Because the acesulfame potassium has the advantages of safety, no toxicity, stable property, sweet taste, no bad aftertaste, proper price and the like, the acesulfame potassium is one of the sweeteners with the best stability in the world at present and is used as a sweetener in the aspects of food, medicine and the like.
In a conventional acesulfame potassium production process, sulfamic acid is reacted with an amine (e.g., triethylamine) to form an ammonium sulfamate. The ammonium sulfamate is then reacted with diketene to form acetoacetamidotriethylamine salt. The acetoacetanilide triethylamine salt is cyclized, hydrolyzed and neutralized to form acesulfame potassium. The patent with application number 201780001641.0 specifically discloses a method for producing acesulfame potassium.
Typically, the acetoacetamidotriethylamine salt is cyclized intermediately by reaction with sulfur trioxide in an inorganic or organic solvent to form a sulfur trioxide adduct of acesulfame, the solvent used for the reaction being an organic solvent. The adduct formed by this reaction is then hydrolyzed and then neutralized with potassium hydroxide to form acesulfame potassium.
The agglomeration is a phenomenon commonly existing in the process of storing the acesulfame potassium, and the length of the agglomeration period directly influences the production process and the subsequent use of the acesulfame potassium. At present, most manufacturers reduce the caking degree of the potassium acetylsulfanilate in a short period by controlling the drying weight loss of the finished potassium acetylsulfanilate and the external environment (packaging temperature and air humidity), but the caking phenomenon still occurs in the later period. The previous experimental research finds that the volatile components in the finished product of the acesulfame potassium have certain influence on the caking: under the condition that other conditions (product particle size distribution, drying weight loss, packaging temperature and air humidity) are the same, the more volatile components in the product are, the more difficult the volatile components are to be discharged from the product, and the more easy the volatile components are to agglomerate; on the contrary, the cake is not formed after long-time storage.
Through a large number of researches, the preparation process of sulfur trioxide and dichloromethane in the cyclization section has a remarkable influence on the generation of volatile components. The traditional preparation process of sulfur trioxide and dichloromethane comprises the following steps: the sulfur trioxide and the dichloromethane are carried out in a preparation kettle, and then a circulating pump is utilized for circulation so as to fully mix the sulfur trioxide and the dichloromethane. Because the intermittent preparation time is long and the proportion cannot be accurately controlled, the sulfur trioxide and the dichloromethane generate side reaction to generate organic byproducts which are difficult to remove in the refining process, and volatile components in the product are increased and are easy to agglomerate. Therefore, there is a need for a process for further improving the content of volatile components in the product for producing a non-caking potassium sulfacetamide composition.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of the acesulfame potassium composition, which reduces organic by-products generated by sulfur trioxide and dichloromethane and reduces the content of volatile components in products by controlling the reaction conditions of a cyclizing agent composition, thereby preventing the occurrence of caking phenomenon of the acesulfame potassium composition and improving the product quality.
In order to solve the technical problems, the invention adopts a technical scheme that:
a preparation method of acesulfame potassium composition comprises the following steps:
(1) mixing a solvent and a cyclizing agent to form a cyclizing agent composition;
(2) reacting the acetoacetyl sulfanilic triethylamine salt with a cyclizing agent in a cyclizing agent composition to form a sulfur trioxide adduct of acetyl sulfanilic acid;
(3) forming a refined acesulfame potassium composition from a sulfur trioxide adduct of acesulfame acid, the refined acesulfame potassium composition comprising acesulfame potassium and less than 10ppm of a volatile component;
wherein the mixing time in the step (1) is less than 2min, and the mass ratio of the cyclizing agent to the solvent is 1: 3-6.
Preferably, step (3) is specifically:
hydrolyzing the sulfur trioxide adduct of the acetyl sulfanilic acid to form an acetyl sulfanilic acid H composition;
neutralizing the acesulfame H in the acesulfame H composition to form a crude acesulfame-k composition, the crude acesulfame-k composition comprising acesulfame-k and less than 10ppm of volatile components;
a refined acesulfame potassium composition is formed from the crude acesulfame potassium composition.
Preferably, the mixing temperature in the step (1) is-15 to 50 ℃.
Preferably, the mixing pressure in the step (1) is 0-10 MPa.
Preferably, the specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition is 1.38-1.44 g/mL.
Preferably, the volatile component comprises acetone.
Preferably, the method comprises the following steps:
(1) reacting sulfamic acid and triethylamine in a solvent to form an ammonium sulfamate solution;
(2) reacting an ammonium sulfamate solution with diketene to form an acetoacetamidotriethylamine salt solution;
(3) mixing dichloromethane and sulfur trioxide to form a cyclizing agent composition;
(4) reacting the acetoacetyl sulfanilic triethylamine salt with sulfur trioxide in a cyclizing agent composition to form a sulfur trioxide adduct of acetyl sulfanilic acid;
(5) hydrolyzing the sulfur trioxide adduct of the acetyl sulfanilic acid to form an acetyl sulfanilic acid H composition;
(6) neutralizing the acesulfame H in the acesulfame H composition to form a crude acesulfame potassium composition, the crude acesulfame potassium composition comprising acesulfame potassium and less than 10ppm of volatile components;
(7) concentrating and separating from the crude acesulfame potassium composition to form a refined acesulfame potassium composition, the refined acesulfame potassium composition comprising acesulfame potassium and less than 10ppm of volatile components;
wherein the mixing time in the step (3) is less than 2min, and the mass ratio of the cyclizing agent to the solvent is 1: 3-6.
Preferably, the mixing temperature in the step (3) is-15 to 50 ℃.
Preferably, the mixing pressure in the step (3) is 0-10 MPa.
Preferably, the specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition is 1.38-1.44 g/mL.
Preferably, the mixing time in step (3) is 0.01s to 1 min.
Preferably, the volatile component comprises acetone.
Preferably, the specific operation of step (3) is: sulfur trioxide sequentially passes through a charging pump a and a mass flow meter a from a sulfur trioxide storage tank and is connected with a micro mixer; the dichloromethane sequentially passes through a feeding pump b and a mass flow meter b from a dichloromethane storage tank and is connected with a micro mixer.
Further preferably, the micro mixer includes one or more of a heart-type micro mixer, a Y-type micro mixer, a U-type micro mixer, and a T-type micro mixer.
The invention also provides a refined acesulfame potassium composition prepared by the method.
Preferably, it contains acesulfame potassium and less than 10ppm of volatile components.
Preferably, the volatile component comprises acetone.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages:
the invention realizes continuous production, shortens the retention time of the cyclizing agent by controlling the reaction condition of the cyclizing agent composition, reduces the organic by-products generated by sulfur trioxide and dichloromethane, and reduces the content of volatile components in the product, thereby preventing the occurrence of agglomeration of the acesulfame potassium composition and improving the product quality.
Drawings
FIG. 1 is a flow diagram of the dosing of sulfur trioxide with dichloromethane;
FIG. 2 is a schematic structural diagram of a core-type microreactor;
FIG. 3 is a schematic structural diagram of a Y-type microreactor;
FIG. 4 is a schematic structural diagram of a U-shaped microreactor;
FIG. 5 is a schematic structural diagram of a T-type microreactor.
Detailed Description
The invention is described in further detail below with reference to the figures and the specific embodiments.
A process for producing a potassium sulfacetamide composition comprising the steps of:
ammonium sulfamate formation reaction
In a first reaction step, sulfamic acid is reacted with an amine to form an ammonium sulfamate. An exemplary reaction mechanism using triethylamine as the amine and producing triethylammonium sulfamate is shown in reaction (1) below.
The amine may also be selected from the group consisting of trimethylamine, tri-n-butylamine, triisobutylamine, triisopropylamine and mixtures thereof.
Acetosulfacetamide triethylamine salt formation reaction
The ammonium sulfamate is reacted with an acetoacetylating agent to form acetoacetamidotriethylamine salt, preferably acetoacetamide-N-sulfonic acid triethylammonium salt. The acetoacetylating agent comprises diketene.
An exemplary reaction mechanism for forming acetoacetamidotriacetyl triethylamine salt uses acetoacetamide-N-sulfonic acid triethylammonium salt and diketene as reactants and produces acetoacetamide triethylammonium salt, which is shown in reaction (2) below.
The ammonium sulfamate-forming reaction and the acetoacetamidotriethylamine salt-forming reaction may use an organic solvent, preferably dichloromethane, chloroform, trichloroethylene, acetone, glacial acetic acid, and a mixture thereof.
Cyclization and hydrolysis
Under the action of cyclizing agent in cyclizing agent composition, the acetyl sulfanilic triethylamine salt is made to form sulfur trioxide adduct composition of acetyl sulfanilic acid.
An exemplary cyclization reaction using sulfur trioxide as a cyclizing agent is shown in reaction (3) below.
The solvent used for the cyclization reaction is preferably dichloromethane, acetone, glacial acetic acid, trichloroethylene and mixtures thereof.
The research of the invention finds that the mixing time of the solvent and the cyclizing agent is shortened, the organic by-product generated by sulfur trioxide adduct of the acesulfame is reduced, and the content of volatile components in the product is reduced, so that the occurrence of the caking phenomenon of the acesulfame potassium is prevented. Similarly, the mass ratio of the solvent to the cyclizing agent, the specific gravity of the cyclizing agent in the cyclizing agent composition, and the temperature and pressure at which the solvent and the cyclizing agent are mixed are all found to affect the organic by-product generated from the sulfur trioxide adduct of acesulfame, thereby reducing the content of volatile components in the product. Therefore, the mixing time of sulfur trioxide and dichloromethane is limited to be less than 2min, preferably 0.01 s-1 min, the mixing pressure is 0-10 Mpa, the mixing temperature is-15-50 ℃, the mass ratio of the sulfur trioxide to the dichloromethane is 1: 3-6, and the specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition is 1.38-1.44 g/mL. The organic by-products produced from sulfur trioxide adducts of acetyl sulfanilic acids are shown in the following diagram:
the specific operation process is as follows:
as shown in the attached fig. 1 to 5, one end of a feed pump a is connected with a sulfur trioxide storage tank, the other end of the feed pump a is connected with a mass flow meter a, and the other end of the mass flow meter a is connected with one end of a micro mixer;
one end of a feeding pump b is connected with the dichloromethane storage tank, the other end of the feeding pump b is connected with a mass flow meter b, and the other end of the mass flow meter b is connected with the other end of the micro mixer;
in a micromixer, mixing sulfur trioxide and dichloromethane according to a mass ratio of 1: 3-6, and simultaneously entering a micro mixer, wherein the mixing temperature is-15-50 ℃, and the mixing pressure is 0-10 MPa. The specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition is 1.38-1.44 g/mL, the cyclizing agent and the solvent stay in the micro mixer for 0.01 s-1 min, and finally the cyclizing agent flows out from the tail end of the micro mixer and enters a cyclization section.
The micro mixer comprises one or more of a heart-shaped micro mixer, a Y-shaped micro mixer, a U-shaped micro mixer and a T-shaped micro mixer.
The sulfur trioxide adduct of the acetyl sulfanilic acid can be hydrolyzed via conventional means (e.g., using water). Hydrolyzing the sulfur trioxide adduct of the acetyl sulfanilic acid to form an acetyl sulfanilic acid H composition. An exemplary hydrolysis reaction mechanism is shown in reaction (4) below.
The addition of water results in phase separation. The majority of the sweetener acid is present in the organic phase.
Neutralization
Neutralization of the acesulfame H with a base in the acesulfame H composition produces a crude acesulfame potassium composition. The base is preferably KOH, KHCO3，K2CO3And potassium alkoxides. An exemplary reaction mechanism using potassium hydroxide as a neutralizing agent is shown in the following reaction (5).
The crude acesulfame potassium composition contains acesulfame potassium and less than 10ppm of volatile components including acetone.
Concentrating and separating
The crude acesulfame potassium composition is concentrated, decolorized, and recrystallized via evaporation to form a refined acesulfame potassium composition that includes acesulfame potassium and less than 10ppm of volatile components including acetone.
Example 1:
in a heart-shaped micromixer, mixing sulfur trioxide and dichloromethane in a mass ratio of 1:3 simultaneously entering a heart-shaped micro mixer, wherein the mixing temperature is-15 ℃, and the mixing pressure is 1 MPa. The specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition was 1.44g/mL, and the residence time in the heart-type micromixer was 0.01 s. The cyclizing agent composition and acetyl sulfanilamide acid triethylamine salt solution prepared by sulfamic acid, triethylamine and diketene in a solvent are subjected to continuous cyclization, hydrolysis, extraction, neutralization, evaporation concentration, decolorization and recrystallization to form a refined potassium sulfacetamide composition, the refined potassium sulfacetamide composition contains volatile components including potassium sulfacetamide and 8ppm of acetone, and no obvious caking phenomenon is generated after the product is stored for 3 years.
Example 2:
in a T-shaped micromixer, mixing sulfur trioxide and dichloromethane according to a mass ratio of 1: 6 simultaneously entering a T-shaped micro mixer, wherein the mixing temperature is 50 ℃, and the mixing pressure is 9 MPa. The specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition is 1.38g/mL, and the residence time in a T-shaped micromixer is 1 min. The cyclizing agent composition and acetyl sulfanilamide acid triethylamine salt solution prepared by sulfamic acid, triethylamine and diketene in a solvent are subjected to continuous cyclization, hydrolysis, extraction, neutralization, evaporation concentration, decolorization and recrystallization to form a refined potassium sulfacetamide composition, the refined potassium sulfacetamide composition contains volatile components including potassium sulfacetamide and 6ppm of acetone, and no obvious caking phenomenon is generated after the product is stored for 3 years.
Example 3:
in a U-shaped micromixer, mixing sulfur trioxide and dichloromethane according to a mass ratio of 1: 5 simultaneously entering a U-shaped micro mixer, wherein the mixing temperature is 20 ℃, and the mixing pressure is 5 MPa. The specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition was 1.40g/mL, and the residence time in the U-shaped micromixer was 0.5 s. The cyclizing agent composition and acetyl sulfanilamide acid triethylamine salt solution prepared by sulfamic acid, triethylamine and diketene in a solvent are subjected to continuous cyclization, hydrolysis, extraction, neutralization, evaporation concentration, decolorization and recrystallization to form a refined potassium sulfacetamide composition, the refined potassium sulfacetamide composition contains volatile components including potassium sulfacetamide and 8ppm of acetone, and no obvious caking phenomenon is generated after the product is stored for 3 years.
Example 4:
in a Y-shaped mixer, mixing sulfur trioxide and dichloromethane according to a mass ratio of 1: 4 simultaneously entering a Y-shaped mixer, wherein the mixing temperature is 35 ℃, and the mixing pressure is 6 MPa. The specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition was 1.41g/mL, and the residence time in the Y-type micromixer was 0.75 s. The cyclizing agent composition and acetyl sulfanilamide acid triethylamine salt solution prepared by sulfamic acid, triethylamine and diketene in a solvent are subjected to continuous cyclization, hydrolysis, extraction, neutralization, evaporation concentration, decolorization and recrystallization to form a refined potassium sulfacetamide composition, the refined potassium sulfacetamide composition contains volatile components including potassium sulfacetamide and 7ppm of acetone, and no obvious caking phenomenon is generated after the product is stored for 3 years.
Comparative example 1:
in a Y-shaped micromixer, mixing sulfur trioxide and dichloromethane according to a mass ratio of 1: 4 simultaneously entering a Y-shaped micro mixer, wherein the mixing temperature is 35 ℃, and the mixing pressure is 6 MPa. The specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition is 1.41g/mL, and the residence time in the Y-shaped micro-mixer is 20 min. The cyclizing agent composition and acetyl sulfanilamide acid triethylamine salt solution prepared by sulfamic acid, triethylamine and diketene in a solvent are subjected to continuous cyclization, hydrolysis, extraction, neutralization, evaporation concentration, decolorization and recrystallization to form a refined potassium sulfacetamide composition, the refined potassium sulfacetamide composition contains the potassium sulfacetamide and 30ppm of volatile components containing acetone, and the product is stored for 1 year and has a caking phenomenon.
Comparative example 2:
in a T-shaped micromixer, mixing sulfur trioxide and dichloromethane according to a mass ratio of 1: 6 simultaneously entering a T-shaped micro mixer, wherein the mixing temperature is 50 ℃, and the mixing pressure is 9 MPa. The specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition is 1.38g/mL, and the residence time in a T-shaped micromixer is 40 min. The cyclizing agent composition and acetyl sulfanilamide acid triethylamine salt solution prepared by sulfamic acid, triethylamine and diketene in a solvent are subjected to continuous cyclization, hydrolysis, extraction, neutralization, evaporation concentration, decolorization and recrystallization to form a refined potassium sulfacetamide composition, the refined potassium sulfacetamide composition contains volatile components including potassium sulfacetamide and 60ppm of acetone, and the product is stored for 6 months and has a caking phenomenon.
Comparative example 3:
in a T-shaped micromixer, mixing sulfur trioxide and dichloromethane according to a mass ratio of 1: 10 simultaneously enters a T-shaped micro mixer, the mixing temperature is 50 ℃, and the mixing pressure is 9 MPa. The specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition is 1.36g/mL, and the residence time in a T-shaped micromixer is 1 min. The cyclizing agent composition and acetyl sulfanilamide acid triethylamine salt solution prepared by sulfamic acid, triethylamine and diketene in a solvent are subjected to continuous cyclization, hydrolysis, extraction, neutralization, evaporation concentration, decolorization and recrystallization to form a refined potassium sulfacetamide composition, the refined potassium sulfacetamide composition contains volatile components including potassium sulfacetamide and 31ppm of acetone, and the product is stored for 9 months and has a caking phenomenon.
Comparative example 4:
in a T-shaped micromixer, mixing sulfur trioxide and dichloromethane according to a mass ratio of 1: 2 simultaneously entering a T-shaped micro mixer, wherein the mixing temperature is 50 ℃, and the mixing pressure is 9 MPa. The specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition is 1.48g/mL, and the residence time in a T-shaped micromixer is 1 min. The cyclizing agent composition and acetyl sulfanilamide acid triethylamine salt solution prepared by sulfamic acid, triethylamine and diketene in a solvent are subjected to continuous cyclization, hydrolysis, extraction, neutralization, evaporation concentration, decolorization and recrystallization to form a refined potassium sulfacetamide composition, the refined potassium sulfacetamide composition contains volatile components including potassium sulfacetamide and 55ppm of acetone, and the product is stored for 8 months and has a caking phenomenon.
The present invention has been described in detail, and the embodiments are only used for understanding the method and the core idea of the present invention, and the purpose of the present invention is to enable those skilled in the art to understand the content of the present invention and to implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (17)
1. A preparation method of acesulfame potassium composition is characterized in that: the method comprises the following steps:
(1) mixing a solvent and a cyclizing agent to form a cyclizing agent composition;
(2) reacting acetoacetamidotriethylamine salt with a cyclizing agent in said cyclizing agent composition to form a sulfur trioxide adduct of acesulfame;
(3) forming a refined acesulfame potassium composition from the sulfur trioxide adduct of acesulfame acid, the refined acesulfame potassium composition comprising acesulfame potassium and less than 10ppm of a volatile component;
wherein the mixing time in the step (1) is less than 2min, and the mass ratio of the cyclizing agent to the solvent is 1: 3-6.
2. The method for preparing acesulfame potassium composition according to claim 1, characterized in that: the step (3) is specifically as follows:
hydrolyzing the sulfur trioxide adduct of the acetyl sulfanilic acid to form an acetyl sulfanilic acid H composition;
neutralizing acesulfame H in the acesulfame H composition to form a crude acesulfame potassium composition comprising acesulfame potassium and less than 10ppm of volatile components;
forming a refined acesulfame potassium composition from the crude acesulfame potassium composition.
3. The method for preparing acesulfame potassium composition according to claim 2, characterized in that: the mixing temperature in the step (1) is-15-50 ℃.
4. The method for preparing acesulfame potassium composition according to claim 2, characterized in that: and (2) the mixing pressure in the step (1) is 0-10 Mpa.
5. The method for preparing acesulfame potassium composition according to claim 2, characterized in that: the specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition is 1.38-1.44 g/mL.
6. The method for preparing acesulfame potassium composition according to claim 2, characterized in that: the volatile component comprises acetone.
7. The method for preparing acesulfame potassium composition according to claim 1, characterized in that: the method comprises the following steps:
(1) reacting sulfamic acid and triethylamine in a solvent to form an ammonium sulfamate solution;
(2) reacting the ammonium sulfamate solution with diketene to form an acetoacetamidotriethylamine salt solution;
(3) mixing dichloromethane and sulfur trioxide to form a cyclizing agent composition;
(4) reacting the acetoacetamidoacetic triethylamine salt with sulfur trioxide in a cyclizing agent composition to form a sulfur trioxide adduct of the acetyl sulfanilic acid;
(5) hydrolyzing the sulfur trioxide adduct of the acetyl sulfanilic acid to form an acetyl sulfanilic acid H composition;
(6) neutralizing acesulfame H in the acesulfame H composition to form a crude acesulfame potassium composition, the crude acesulfame potassium composition comprising acesulfame potassium and less than 10ppm of volatile components;
(7) concentrating and separating from the crude acesulfame potassium composition to form a refined acesulfame potassium composition comprising acesulfame potassium and less than 10ppm of volatile components;
wherein the mixing time in the step (3) is less than 2min, and the mass ratio of the cyclizing agent to the solvent is 1: 3-6.
8. The method of preparing acesulfame potassium composition of claim 7, wherein: the mixing temperature in the step (3) is-15-50 ℃.
9. The method of preparing acesulfame potassium composition of claim 7, wherein: and (4) the mixing pressure in the step (3) is 0-10 Mpa.
10. The method of preparing acesulfame potassium composition of claim 7, wherein: the specific gravity of the cyclizing agent and the solvent in the cyclizing agent composition is 1.38-1.44 g/mL.
11. The method of preparing acesulfame potassium composition of claim 7, wherein: the mixing time in the step (3) is 0.01 s-1 min.
12. The method of preparing acesulfame potassium composition of claim 7, wherein: the volatile component comprises acetone.
13. The method of preparing acesulfame potassium composition of claim 7, wherein: the specific operation of the step (3) is as follows: the sulfur trioxide sequentially passes through a charging pump a and a mass flow meter a from a sulfur trioxide storage tank and is connected with a micro mixer; the dichloromethane sequentially passes through a feeding pump b and a mass flow meter b from a dichloromethane storage tank and is connected with a micro mixer.
14. The method of preparing acesulfame potassium composition of claim 13, wherein: the micro mixer comprises one or more of a heart-shaped micro mixer, a Y-shaped micro mixer, a U-shaped micro mixer and a T-shaped micro mixer.
15. A acesulfame potassium composition prepared by the process according to any one of claims 1 to 14.
16. The acesulfame potassium composition of claim 15, wherein: contains acesulfame potassium and less than 10ppm of volatile components.
17. The acesulfame potassium composition of claim 16, wherein: the volatile component comprises acetone.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180079736A1 (en) * | 2016-09-21 | 2018-03-22 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| CN107835807A (en) * | 2016-09-21 | 2018-03-23 | 国际人造丝公司 | Acesulfame-K composition and its production method |
| CN111377882A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Method for continuously producing acesulfame |
| CN112110876A (en) * | 2020-09-26 | 2020-12-22 | 安徽金禾实业股份有限公司 | Method for continuous sulfonation cyclization in acesulfame potassium production |
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- 2021-08-31 CN CN202111011051.0A patent/CN113896692A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180079736A1 (en) * | 2016-09-21 | 2018-03-22 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| CN107835807A (en) * | 2016-09-21 | 2018-03-23 | 国际人造丝公司 | Acesulfame-K composition and its production method |
| CN111377882A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Method for continuously producing acesulfame |
| CN112110876A (en) * | 2020-09-26 | 2020-12-22 | 安徽金禾实业股份有限公司 | Method for continuous sulfonation cyclization in acesulfame potassium production |
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