CN113527226A - Method for controlling content of ACH in acid in process of preparing acesulfame potassium - Google Patents
Method for controlling content of ACH in acid in process of preparing acesulfame potassium Download PDFInfo
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- CN113527226A CN113527226A CN202110755635.2A CN202110755635A CN113527226A CN 113527226 A CN113527226 A CN 113527226A CN 202110755635 A CN202110755635 A CN 202110755635A CN 113527226 A CN113527226 A CN 113527226A
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- C07D291/00—Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms
- C07D291/02—Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms not condensed with other rings
- C07D291/06—Six-membered rings
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Abstract
The invention relates to the field of chemical industry, in particular to a method for controlling the content of ACH in acid in a process of preparing acesulfame potassium. According to the invention, by controlling the ACH content in the acid layer in the cyclization hydrolysis section and the retention time of the hydrolysis reaction liquid, the decomposition of the intermediate ACH can be effectively reduced, and the quality of the finished product potassium sulfacetamide is improved.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a method for controlling the content of ACH in acid in a process of preparing acesulfame potassium.
Background
Acesulfame potassium, namely AK sugar (Acesulfame-K), has the Chinese cultural name of 6-Methyl-1,2,3-oxathiazin-4(3H) -ketone-2, 2-potassium dioxide and the English chemical name of 6-Methyl-1,2,3-oxathiazin-4(3H) -one 2,2-dioxide potassium salt, commonly known as Acesulfame potassium. Appearance properties: colorless crystals. Solubility: is easily dissolved in water, and the solubility is 270g/L at 20 ℃. CAS number 55589-62-3. The molecular formula is as follows: c4H4O4KNS. Molecular weight: 201.24. melting Point (. degree. C.): 229-232. Relative density (water ═ 1): 1.81. pH value: the pH value is 5.5-7.5. The acesulfame potassium has the advantages of safety, no toxicity, stable property, sweet taste, no bad aftertaste, proper price, etcThe sweetener has the advantages of being one of the sweeteners with the best stability in the world at present and being used as a sweetener in the aspects of food, medicine and the like.
At present, the sulfamic acid-sulfur trioxide method is a mainstream process for producing acesulfame potassium due to easily available raw materials, mild reaction conditions, high product yield and high purity. In the cyclization/hydrolysis section reaction, the generated intermediate 6-methyl-3, 4-dihydro-1, 2,3-oxathiazin-4(3H) -ketone-2, 2-dioxide (ACH) is easy to decompose under acidic conditions. If the content of ACH in the reaction is too high, the ACH is finally decomposed to generate acetone, carbon dioxide, sulfuric acid and ammonium sulfate, so that the yield is reduced, and the quality of the finished product potassium acetylsulfanilate is influenced; if the ACH content in the reaction is too low, the production and treatment costs are greatly increased.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention aims to provide a method for controlling the content of ACH in the acid in the process of preparing acesulfame potassium.
In order to achieve the above objects and other related objects, the present invention adopts the following technical solutions:
the invention provides a method for controlling the content of ACH in acid in a process of preparing acesulfame potassium, which comprises the following steps:
SO3the solution and acetyl sulfacetamide triethylamine salt solution are subjected to cyclization reaction, and the material after cyclization reaction and water are subjected to hydrolysis reaction to obtain hydrolysate, wherein an acid layer of the hydrolysate contains sulfuric acid and ACH.
In a preferred embodiment, the sulfuric acid content of the acid layer is 30% to 70%. Further, the content range of the sulfuric acid in the acid layer is 40-60%.
In a preferred embodiment, the ACH content in the acid layer is 1% to 5%. Further, the ACH content in the acid layer ranges from 2% to 4%.
In a preferred embodiment, the hydrolysate stays in the hydrolysis reaction kettle for 5-80 min. Further, the hydrolysate stays in the hydrolysis reaction kettle for 10-70 min. Furthermore, the hydrolysate stays in the hydrolysis reaction kettle for 10-50 min.
In a preferred embodiment, SO3The solution is made of SO3Dissolving in dichloromethane. SO (SO)3The concentration of the solution is 20-40%.
In a preferred embodiment, dichloromethane is used as a solvent, sulfamic acid and triethylamine are subjected to neutralization reaction, and the prepared solution is subjected to acylation reaction with diketene to prepare the acetyl sulfanilic acid triethylamine salt solution.
In a preferred embodiment, the concentration of the acetoacetamidotriethylamine salt solution is 25% to 40%.
The invention also provides the application of the method in the production of acesulfame potassium.
The invention also provides a process for producing the acesulfame potassium, which comprises the method.
The method for controlling the content of ACH in the acid in the process of preparing the acesulfame potassium has the following beneficial effects:
according to the invention, by controlling the ACH content in the acid layer in the cyclization hydrolysis section and the retention time of the hydrolysis reaction liquid, the decomposition of the intermediate ACH can be effectively reduced, and the quality of the finished product potassium sulfacetamide is improved.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It is to be understood that the processing equipment or apparatus not specifically identified in the following examples is conventional in the art. Furthermore, it is to be understood that one or more method steps mentioned in the present invention does not exclude that other method steps may also be present before or after the combined steps or that other method steps may also be inserted between these explicitly mentioned steps, unless otherwise indicated; it is also to be understood that a combined connection between one or more devices/apparatus as referred to in the present application does not exclude that further devices/apparatus may be present before or after the combined device/apparatus or that further devices/apparatus may be interposed between two devices/apparatus explicitly referred to, unless otherwise indicated. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
Example 1
Taking dichloromethane as a solvent, carrying out neutralization reaction on sulfamic acid and triethylamine, and carrying out acylation reaction on the prepared solution and diketene to prepare 35% (mass percentage content) acetoacetyl sulfanilic acid triethylamine salt solution, which is marked as DKA solution. SO (SO)3Dissolving in dichloromethane to obtain SO with a concentration of 20% (mass percentage content)3And (3) solution.
Adding 20% SO3The solution and 35% DKA solution were introduced into the input end of the cyclization reactor for the cyclization reaction. The outlet of the reactor directly sprays the materials after the cyclization reaction into a hydrolysis reaction kettle to perform hydrolysis reaction with water in a proportional amount; after the hydrolysis reaction is finished, the sulfuric acid content in the acid layer is 30% (mass percentage content), and the ACH content in the acid layer is 1.0% (mass percentage content); the hydrolysate stays in the hydrolysis reaction kettle for 80min, and the ACH content in the acid is not changed.
Example 2
Taking dichloromethane as a solvent, carrying out neutralization reaction on sulfamic acid and triethylamine, and carrying out acylation reaction on the prepared solution and diketene to prepare 25% (mass percentage content) acetoacetyl sulfanilic acid triethylamine salt solution, which is marked as DKA solution. SO (SO)3Dissolving in dichloromethane to obtain SO with concentration of 30% (mass percentage content)3And (3) solution.
Mixing with 30% SO3The solution and 25% DKA solution are introduced into the input of the cyclization reactorThe outlet directly sprays the materials after the cyclization reaction into a hydrolysis reaction kettle to perform hydrolysis reaction with water in a proportional amount; after the hydrolysis reaction is finished, the sulfuric acid content in the acid layer is 70% (mass percentage content), and the ACH content in the acid layer is 2.0% (mass percentage content); the hydrolysate stays in the hydrolysis reaction kettle for 5min, and the ACH content in the acid is not changed.
Example 3
Taking dichloromethane as a solvent, carrying out neutralization reaction on sulfamic acid and triethylamine, and carrying out acylation reaction on the prepared solution and diketene to prepare a 30% (mass percentage content) acetoacetyl sulfanilic acid triethylamine salt solution which is marked as a DKA solution. SO (SO)3Dissolving in dichloromethane to obtain SO with concentration of 40% (mass percentage content)3And (3) solution.
Adding 40% SO3Introducing the solution and 30% DKA solution into the input end of a cyclization reactor, and directly injecting materials subjected to cyclization reaction into a hydrolysis reaction kettle from the reactor outlet for hydrolysis reaction with water in a proportional amount; after the hydrolysis reaction is finished, the sulfuric acid content in the acid layer is 50% (mass percentage content), and the ACH content in the acid layer is 5% (mass percentage content); the hydrolysate stays in the hydrolysis reaction kettle for 30min, and the ACH content in the acid is not changed.
Example 4
Taking dichloromethane as a solvent, carrying out neutralization reaction on sulfamic acid and triethylamine, and carrying out acylation reaction on the prepared solution and diketene to prepare a 40% (mass percentage content) acetoacetyl sulfanilic acid triethylamine salt solution, which is marked as a DKA solution. SO (SO)3Dissolving in dichloromethane to obtain 35% (mass percentage) SO3And (3) solution.
Adding 35% SO3Introducing the solution and 40% DKA solution into the input end of a cyclization reactor, and directly injecting materials subjected to cyclization reaction into a hydrolysis reaction kettle from the reactor outlet for hydrolysis reaction with water in a proportional amount; after the hydrolysis reaction is finished, the sulfuric acid content in the acid layer is 55% (mass percentage content), and the ACH content in the acid layer is 4% (mass percentage content); the hydrolysate stays in the hydrolysis reaction kettle for 25min, and the ACH content in the acid is not changed.
Example 5
Taking dichloromethane as a solvent, carrying out neutralization reaction on sulfamic acid and triethylamine, and carrying out acylation reaction on the prepared solution and diketene to prepare an acetoacetyl sulfanilic acid triethylamine salt solution with the concentration of 20% (mass percentage content), which is marked as a DKA solution. SO (SO)3Dissolving in dichloromethane to obtain SO with concentration of 25% (mass percentage)3And (3) solution.
Adding 25% SO3Introducing the solution and 20% DKA solution into the input end of a cyclization reactor, and directly injecting materials subjected to cyclization reaction into a hydrolysis reaction kettle from the reactor outlet for hydrolysis reaction with water in a proportional amount; after the hydrolysis reaction is finished, the sulfuric acid content in the acid layer is 45% (mass percentage content), and the ACH content in the acid layer is 2.2% (mass percentage content); the hydrolysate stays in the hydrolysis reaction kettle for 70min, and the ACH content in the acid is not changed.
Comparative example 1
Taking dichloromethane as a solvent, carrying out neutralization reaction on sulfamic acid and triethylamine, and carrying out acylation reaction on the prepared solution and diketene to prepare 35% (mass percentage content) acetoacetyl sulfanilic acid triethylamine salt solution, which is marked as DKA solution. SO (SO)3Dissolving in dichloromethane to obtain SO with a concentration of 20% (mass percentage content)3And (3) solution.
Adding 20% SO3Introducing the solution and 35% DKA solution into the input end of a cyclization reactor, and directly injecting materials subjected to cyclization reaction into a hydrolysis reaction kettle from the reactor outlet for hydrolysis reaction with water in a proportional amount; after the hydrolysis reaction is finished, the sulfuric acid content in the acid layer is 45% (mass percentage content), and the ACH content in the acid layer is 5.5% (mass percentage content); after the hydrolysate stays in the hydrolysis reaction kettle for 2min, the ACH content in the acid is obviously reduced.
Comparative example 2
Taking dichloromethane as a solvent, carrying out neutralization reaction on sulfamic acid and triethylamine, and carrying out acylation reaction on the prepared solution and diketene to prepare a 30% (mass percentage content) acetoacetyl sulfanilic acid triethylamine salt solution which is marked as a DKA solution. SO (SO)3Dissolving in dichloromethane to obtain 35% (mass percentage) SO3And (3) solution.
Adding 35% SO3Introducing the solution and 30% DKA solution into the input end of a cyclization reactor, and directly injecting materials subjected to cyclization reaction into a hydrolysis reaction kettle from the reactor outlet for hydrolysis reaction with water in a proportional amount; after the hydrolysis reaction is finished, the sulfuric acid content in the acid layer is 65% (mass percentage content), and the ACH content in the acid layer is 0.8% (mass percentage content); the hydrolysate stays in the hydrolysis reaction kettle for 85min, and the ACH content in the acid is obviously reduced.
In conclusion, the present invention effectively overcomes various disadvantages of the prior art and has high industrial utilization value.
The above examples are intended to illustrate the disclosed embodiments of the invention and are not to be construed as limiting the invention. In addition, various modifications of the methods and compositions set forth herein, as well as variations of the methods and compositions of the present invention, will be apparent to those skilled in the art without departing from the scope and spirit of the invention. While the invention has been specifically described in connection with various specific preferred embodiments thereof, it should be understood that the invention should not be unduly limited to such specific embodiments. Indeed, various modifications of the above-described embodiments which are obvious to those skilled in the art to which the invention pertains are intended to be covered by the scope of the present invention.
Claims (10)
1. A method for controlling the content of ACH in acid in the process of preparing acesulfame potassium comprises the following steps: SO (SO)3The solution and acetyl sulfacetamide triethylamine salt solution are subjected to cyclization reaction, and the material after cyclization reaction and water are subjected to hydrolysis reaction to obtain hydrolysate, wherein an acid layer of the hydrolysate contains sulfuric acid and ACH.
2. The method according to claim 1, characterized in that the sulfuric acid content in the acid layer is 30-70%, preferably 40-60%.
3. The method of claim 1, wherein the acid layer has an ACH content of 1% to 5%.
4. The method of claim 1, wherein the ACH content of the acid layer is in the range of 2% to 4%.
5. The method of claim 1, wherein the hydrolysate stays in the hydrolysis reaction kettle for 5-80 min, preferably 10-70 min.
6. The method of claim 1, wherein the hydrolysate stays in the hydrolysis reaction kettle for 10-50 min.
7. The method of claim 1, wherein SO is3The solution is made of SO3Prepared by dissolving in dichloromethane, SO3The concentration of the solution is 20-40%.
8. The method as claimed in claim 1, wherein dichloromethane is used as solvent, sulfamic acid and triethylamine are subjected to neutralization reaction, the prepared solution is subjected to acylation reaction with diketene to obtain the acetoacetamidosulfuric triethylamine salt solution, and the concentration of the acetoacetamidosulfuric triethylamine salt solution is 25-40%.
9. Use of the method according to any one of claims 1 to 8 for the production of acesulfame potassium.
10. A process for the production of acesulfame potassium comprising the method of any one of claims 1 to 8.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86105339A (en) * | 1985-09-03 | 1987-04-08 | 赫彻斯特股份公司 | 6-methyl-3,4-dihydro-1,2,3-oxygen thia azine hexamethylene-4-ketone 2, the preparation of 2-dioxide and method of purification |
| CN104411693A (en) * | 2012-06-08 | 2015-03-11 | 鹿特诺瓦营养品和食品有限公司 | Process for producing acesulfame potassium |
| CN107868064A (en) * | 2016-09-23 | 2018-04-03 | 中国科学院大连化学物理研究所 | A kind of method that 3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt precursor ASH is synthesized in micro passage reaction |
| CN111377886A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Micro-channel reaction method and reaction system for cyclization and hydrolysis section in preparation of acesulfame potassium |
| CN112142688A (en) * | 2019-06-27 | 2020-12-29 | 南通醋酸化工股份有限公司 | Stepwise neutralization reaction method in preparation of acesulfame potassium |
| CN112142687A (en) * | 2019-06-27 | 2020-12-29 | 南通醋酸化工股份有限公司 | Continuous acylation synthesis method in synthesis of acesulfame potassium |
-
2021
- 2021-07-05 CN CN202110755635.2A patent/CN113527226A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86105339A (en) * | 1985-09-03 | 1987-04-08 | 赫彻斯特股份公司 | 6-methyl-3,4-dihydro-1,2,3-oxygen thia azine hexamethylene-4-ketone 2, the preparation of 2-dioxide and method of purification |
| CN104411693A (en) * | 2012-06-08 | 2015-03-11 | 鹿特诺瓦营养品和食品有限公司 | Process for producing acesulfame potassium |
| CN107868064A (en) * | 2016-09-23 | 2018-04-03 | 中国科学院大连化学物理研究所 | A kind of method that 3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt precursor ASH is synthesized in micro passage reaction |
| CN111377886A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Micro-channel reaction method and reaction system for cyclization and hydrolysis section in preparation of acesulfame potassium |
| CN112142688A (en) * | 2019-06-27 | 2020-12-29 | 南通醋酸化工股份有限公司 | Stepwise neutralization reaction method in preparation of acesulfame potassium |
| CN112142687A (en) * | 2019-06-27 | 2020-12-29 | 南通醋酸化工股份有限公司 | Continuous acylation synthesis method in synthesis of acesulfame potassium |
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