WO2022246867A1 - Procédé de préparation d'acésulfame de potassium - Google Patents

Procédé de préparation d'acésulfame de potassium Download PDF

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WO2022246867A1
WO2022246867A1 PCT/CN2021/097015 CN2021097015W WO2022246867A1 WO 2022246867 A1 WO2022246867 A1 WO 2022246867A1 CN 2021097015 W CN2021097015 W CN 2021097015W WO 2022246867 A1 WO2022246867 A1 WO 2022246867A1
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reaction
reactor
solution
working fluid
fluid
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PCT/CN2021/097015
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Chinese (zh)
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周睿
丁震
陈永旭
杨峰宝
刘刚
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安徽金禾实业股份有限公司
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Priority to PCT/CN2021/097015 priority Critical patent/WO2022246867A1/fr
Priority to CN202180001421.4A priority patent/CN113508110B/zh
Publication of WO2022246867A1 publication Critical patent/WO2022246867A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts

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  • the invention belongs to the technical field of fine chemical manufacturing, and in particular relates to a preparation method of acesulfame potassium.
  • Acesulfame potassium also known as AK sugar
  • AK sugar is a widely used sugar substitute food additive. Its appearance is white crystalline powder.
  • As an organic synthetic salt its taste is similar to sugarcane, and it is easily soluble in water. , Slightly soluble in alcohol, its chemical properties are stable, and it is not easy to break down and fail; it does not participate in the body's metabolism and does not provide energy; it has high sweetness and low price; it has no cariogenicity; it has good stability to heat and acid.
  • the diketene-sulfur trioxide method is widely used.
  • the specific reaction steps include: reacting sulfamic acid with amine to form amine sulfamic acid salt, and then reacting amine sulfamic acid with diketene , forming acetylacetamide salt; in the presence of sulfur trioxide, acetylacetamide salt undergoes a cyclization reaction to form a cyclic sulfur trioxide adduct; the cyclic compound is hydrolyzed to obtain the hydrolyzate (ASH); subsequent oxidation with hydrogen Potassium treatment of the hydrolyzate yields acesulfame potassium (ASK).
  • the present application is proposed in order to provide a method for preparing acesulfame potassium that overcomes the above problems or at least partially solves the above problems.
  • a kind of preparation method of acesulfame potassium is provided, the method adopts combined reactor to implement, and combined reactor comprises Venturi reactor and flow reactor, the diffuser section of Venturi reactor The outlet is connected to the inlet of the flow reactor; the method comprises:
  • Sulfonated cyclization step use acetoacetamide-N-sulfonic acid triethylamine salt solution as working fluid, dissolve sulfur trioxide in solvent to form cyclizing agent solution as injection fluid; working fluid from Venturi reactor The nozzle enters, and the injection fluid enters from the suction chamber of the Venturi reactor, and the pressure of the working fluid is controlled to be higher than the pressure of the injection fluid; the working fluid and the injection fluid are in the mixing section and the diffuser section of the Venturi reactor mixing and performing a sulfonation ring closure reaction, and spraying the sulfonation ring closure product into the flow reactor;
  • Hydrolysis step the sulfonated cyclization product undergoes a hydrolysis reaction with a hydrolysis agent preset in the flow reactor to obtain a hydrolyzate solution;
  • Salt-forming step adding potassium hydroxide to the organic phase of the hydrolyzate solution to obtain acesulfame potassium.
  • the pressure of the working fluid is 0.4-1.6 MPa
  • the pressure of the injection fluid is 0.2-1.4 MPa
  • the pressure of the working fluid is 0.2-0.4 MPa higher than the pressure of the injection fluid.
  • spraying the sulfonation and cyclization product into the flow reactor includes:
  • the sulfonated cyclization product is sprayed from the outlet of the diffuser section of the Venturi reactor at a pressure of 0.5-1.1 MPa, and sprayed into the flow reactor.
  • the temperature of the working fluid and the injection fluid is maintained at -35°C to 0°C, preferably -15°C to 0°C.
  • the reaction temperature of the hydrolysis reaction is -40°C to 0°C, preferably -20°C to 0°C.
  • the hydrolysis agent is an aqueous ethanol solution, wherein the mass fraction of ethanol in the aqueous ethanol solution is 60-85%.
  • the ratio of the molar mass of sulfur trioxide to the molar mass of water in the hydrolyzing agent is 1:1-1.5.
  • the acetoacetamide-N-sulfonic acid triethylamine salt solution is prepared by the following method:
  • the solid acidic catalyst is a molecular sieve catalyst or a solid superacid catalyst.
  • the molecular sieve catalyst is HZSM-5 molecular sieve and/or Na-ZSM-5 molecular sieve;
  • the solid superacid catalyst is SO 4 2 ⁇ /Fe 2 O 3 type catalyst.
  • the beneficial effects of the present application are that the present application forms a set of combined continuous reactors by using the Venturi reactor in conjunction with the flow reactor, and on the combined reactor, by controlling acetoacetamide-N-sulfonic acid triethyl
  • the relative pressure of the working fluid formed by the amine salt solution and the injection fluid formed by dissolving sulfur trioxide in the solvent into the Venturi reactor makes the cyclization process of acetoacetamide-N-sulfonic acid triethylamine salt and sulfur trioxide It can be completely carried out in the mixing section and diffuser section of the Venturi reactor, which greatly shortens the reaction time of the cyclization reaction, reduces the probability of organic impurities remaining in the final product acesulfame potassium, and improves the acesulfame potassium.
  • the idea of the present application is that, in the process of preparing acesulfame potassium by using diketene-sulfur trioxide method in the prior art, in the step of sulfonation ring closure reaction, due to the low reaction efficiency, the yield of acesulfame potassium is low and there are many impurities.
  • a method for combining the Venturi reaction with a flow reactor is provided, and by controlling the reaction conditions, the above-mentioned technical defects are effectively overcome, and the method can realize continuous reaction and is suitable for large-scale industrial production.
  • the preparation method of acesulfame potassium provided by the application is implemented by a combined reactor, the combined reactor includes a Venturi reactor and a flow reactor, and the outlet of the diffuser section of the Venturi reactor is connected with the inlet of the flow reactor.
  • Fig. 1 is a schematic cross-sectional structure diagram of a Venturi reactor 100 according to an embodiment of the present application, as can be seen from Fig.
  • the mixing effect between the jets has an important influence.
  • the Venturi reactor is mainly composed of nozzle 1, suction chamber 2, mixing section 3, and diffuser section 4.
  • the preparation method of acesulfame potassium provided by the application is carried out using the above-mentioned Venturi reactor, the difference is that the Venturi reactor of the application is connected to a flow reactor, and by controlling the reaction conditions, the sulfonation The ring closure step is completely carried out in the mixing section 3 and the diffuser section 4 of the Venturi reactor 100 .
  • the preparation method of acesulfame potassium provided in this application at least includes step S110 to step S130:
  • Sulfonated cyclization step S110 using acetoacetamide-N-sulfonic acid triethylamine salt solution as the working fluid, dissolving sulfur trioxide in the solvent to form a cyclizing agent solution as the injector fluid; the working fluid reacts from the Venturi
  • the injection fluid enters from the nozzle of the Venturi reactor, and the pressure of the working fluid is controlled to be higher than the pressure of the injection fluid; the working fluid and the injection fluid are mixed and diffused in the Venturi reactor. Section mixing and sulfonation cyclization reaction, and the sulfonation cyclization product is sprayed into the flow reactor.
  • the principle is: the working fluid with higher pressure is compressed and accelerated through the nozzle 1, and the pressure energy is converted into kinetic energy, forming a high-speed and low-pressure area near the outlet of the nozzle 1, and then forming a pressure difference between the inlet and outlet of the suction chamber 2. Under the action of the pressure difference, the injection fluid is sucked into the mixing section through the suction chamber 2.
  • the momentum and energy of the working fluid and the ejection fluid begin to exchange with each other, and due to the shearing effect of the high-speed working fluid, the sucked ejection fluid can be broken, which promotes the mutual mixing between the two phases and increases
  • the two-phase contact area is conducive to the mass transfer of the two phases, thereby speeding up the reaction rate, and then the fully mixed two-phase fluid is decelerated and pressurized through the diffuser section, and the kinetic energy is converted into pressure energy, which can be sprayed into the outlet connected to the diffuser section 4 Inside the reactor.
  • acetoacetamide-N-sulfonic acid triethylamine salt reacts completely with sulfur trioxide to form a sulfonated ring closure product.
  • the Venturi reactor sprays the sulfonated cyclization product onto the surface of the hydrolyzing agent in the flow reactor.
  • Venturi reactor and the setting of working parameters ensure the rapid reaction of acetoacetamide-N-sulfonic acid triethylamine salt and sulfur trioxide, so that the sulfonation ring closure reaction can be completed within 1-15s. It is best to complete the reaction within 1-3s.
  • the short-time reaction reduces the reaction by-products and significantly reduces the impurity content.
  • Hydrolysis step S120 the sulfonated cyclization product undergoes a hydrolysis reaction with a hydrolysis agent preset in the flow reactor to obtain a hydrolyzate solution.
  • the sulfonated cyclization product undergoes hydrolysis reaction with the hydrolysis agent preset in the flow reactor. After the cyclization product is hydrolyzed, it becomes the precursor ASH of acesulfame potassium, which is different from the hydrolysis reaction using acidic solution in the traditional process.
  • This application uses a hydrolysis agent, which can shorten the hydrolysis time. With the reduction of the hydrolysis time, the hydrolysis may produce reduction of impurity content.
  • the hydrolyzing agent is water or an aqueous ethanol solution, which significantly reduces the content of impurities in the cyclization product ASH, reduces the difficulty of subsequent purification of acesulfame potassium, and reduces the cost of purification of acesulfame potassium.
  • the present application adopts a flow reactor, so that the preparation of acesulfame-K realizes continuity, and is suitable for large-scale process production.
  • Salt forming step S130 adding potassium hydroxide to the organic phase of the hydrolyzate solution to obtain acesulfame potassium.
  • potassium hydroxide or aqueous potassium hydroxide solution is usually used to carry out a salt-forming reaction with the hydrolyzed product, thereby obtaining acesulfame potassium (ASK).
  • the so-called salt-forming reaction refers to the process in which the cation of potassium hydroxide is exchanged with the anion of the hydrolyzate to generate the potassium salt of acesulfame.
  • a salt-forming agent can be used instead of traditional potassium hydroxide or potassium hydroxide aqueous solution to carry out a salt-forming reaction
  • inorganic impurities include but are not limited to potassium fluoride, potassium sulfate, etc.
  • the salt-forming agent includes, but is not limited to, an ethanol solution of potassium hydroxide or an ethanol solution of potassium ethoxide.
  • the application forms a set of combined continuous reactors by using the Venturi reactor in combination with the flow reactor, and on the combined reactor, by controlling the acetoacetamide-N-sulfonic acid triethylamine salt
  • the relative pressure of the working fluid formed by the solution and the injection fluid formed by dissolving sulfur trioxide in the solvent into the Venturi reactor makes the cyclization process of acetoacetamide-N-sulfonic acid triethylamine salt and sulfur trioxide possible in
  • the mixing section and the diffuser section of the Venturi reactor are completely carried out, which greatly shortens the reaction time of the cyclization reaction, reduces the probability of organic impurities remaining in the final product acesulfame potassium, and improves the purity of acesulfame potassium.
  • the post-treatment process of acesulfame potassium is simplified, and the production cost of acesulfame potassium is reduced; at the same time, the reaction can be carried out continuously, which is suitable for large-scale industrial production, and the production efficiency of acesulfame potassium is improved.
  • the pressure of the working fluid and the injection fluid and the pressure difference between the two are not limited, and it is sufficient to control the pressure of the working fluid to be higher than the pressure of the injection fluid; in other embodiments , the pressure of the working fluid is 0.4-1.6MPa, the pressure of the injection fluid is 0.2-1.4MPa, and the pressure of the working fluid is 0.2-0.4MPa higher than the pressure of the injection fluid.
  • the purpose of controlling the mixing speed, reaction speed and dosage ratio of the two is achieved, so that the two can be fully and quickly mixed and reacted, and the dosage ratio of the two is controlled at an appropriate level. In the range.
  • the sulfonated ring closure product is sprayed from the outlet of the diffuser section of the Venturi reactor at a pressure of 0.5-1.1 MPa, and sprayed into the flow reactor.
  • the purpose of controlling the dosage ratio of the sulfonated cyclization product and the hydrolyzing agent can be achieved, so that the mixing speed and dosage ratio of the two are in a more reasonable range, and the The reaction is too fast, resulting in insufficient hydrolysis.
  • the reaction temperature of the sulfonation cyclization step is not limited, and prior art may be referred to; in other embodiments of the present application, in the sulfonation cyclization step, the working fluid and the primer
  • the temperature of the injection fluid is between -35°C and 0°C. In some other embodiments, it is preferable to maintain the temperature of the working fluid and the ejection fluid between -15°C and 0°C.
  • the sulfonation ring reaction of acetoacetamide-N-sulfonic acid triethylamine salt and sulfur trioxide is an exothermic reaction, thereby it is more suitable to carry out at low temperature, and the reaction environment of low temperature is conducive to suppressing the generation of side reactions, reducing the content of impurities in the product.
  • the hydrolyzing agent is deionized water or an aqueous ethanol solution, preferably an aqueous ethanol solution, wherein the mass concentration of ethanol in the aqueous ethanol solution is preferably 60-85%.
  • the inventor used a hydrolysis agent, especially an aqueous solution of ethanol, and controlled the water content in the hydrolysis agent, which can significantly reduce the content of impurities in the acesulfame precursor ASH, and reduce the difficulty of subsequent acesulfame potassium purification. The cost of acesulfame purification is reduced.
  • the application is not limited, the consumption of hydrolyzing agent can be determined according to the consumption of sulfur trioxide, specifically, in some embodiments of the application, the consumption of sulfur trioxide and the content of water in the hydrolyzing agent
  • the ratio of the amount of substances is 1:1-4, in some other embodiments, it is 1:1-1.5. That is to say, the amount of water in the hydrolyzing agent is preferably higher than that of sulfur trioxide.
  • the reaction temperature of the hydrolysis reaction is -40°C to 0°C, preferably -20°C to 0°C. That is to say, the hydrolysis reaction step of the present application is preferably carried out at a lower temperature.
  • any one of the prior art can be used for temperature control, such as air condensation technology, circulating water condensation technology and heat exchange plate Wait. After repeated tests, it was found that -40°C to 0°C is the most suitable temperature for the hydrolysis reaction.
  • reaction temperature is lower than -40°C, the hydrolysis may be incomplete, which will result in incomplete hydrolysis, and some cyclization products cannot be converted.
  • the conversion rate of raw materials is low; if the reaction temperature is higher than 0°C, the reaction temperature is too high, and the cyclization product is easy to decompose, which is not conducive to the development of the reaction towards the hydrolysis reaction.
  • the application does not limit the source of the acetoacetamide-N-sulfonic acid triethylamine salt solution, and can refer to the prior art, and can also be prepared by the following method:
  • acetoacetamide-N-sulfonic acid triethylamine salt solution can be more carefully divided into two small steps. First, it is the preparation of ammonium sulfamate, and then the intermediate is prepared by reacting ammonium sulfamate with diketene , That is, acetoacetamide-N-sulfonic acid triethylamine salt.
  • the ammonium salt of sulfamic acid is obtained by adding triethylamine to the sulfamic acid solution for amination reaction.
  • sulfamic acid is dissolved in the first solvent to configure the first reaction solution
  • triethylamine is dissolved in the second solvent to configure the second reaction solution
  • the second The reaction solution is added to the first reaction solution to carry out amination reaction to form a sulfamic acid ammonium salt solution.
  • the first solvent and the second solvent are inert organic solvents that can provide a reaction environment for the amination reaction, such as dichloromethane.
  • Sulfamic acid and triethylamine react exothermicly. During the reaction, the heat generated will vaporize part of the dichloromethane, and the vaporized dichloromethane will leave the reaction system to take away the heat produced. Further, the vaporized dichloromethane Methane can also be recycled.
  • a kind of specific implementation of generating sulfamic acid ammonium salt solution is given below, and this embodiment is only used as an illustration, and the specific production process of sulfamic acid ammonium salt solution can adopt any one in the prior art.
  • the second reaction solution was added dropwise to the first reaction solution.
  • the pH value was 7-9, and the reaction was left to stand for 1 hour.
  • the material after the above reaction was an ammonium sulfamate solution.
  • Solid-state acidic catalysis can provide sufficient acidic sites for the acylation reaction. On the one hand, it can effectively catalyze the acylation reaction of ammonium sulfamate and diketene. On the other hand, solid-state acidic catalysis will not mix into the reaction product. , no special treatment process is required in the follow-up, which saves the post-treatment economy and time cost; and avoids the adverse effect on the product phase of the final product caused by the acetic acid impurities that are not removed in the prior art remaining in the final product.
  • diketene is dissolved in a third solvent to prepare a third reaction solution.
  • the third solvent is an inert organic solvent that can provide a reaction environment for the amination reaction, such as dichloromethane.
  • Fill the reactor with a solid acidic catalyst add the ammonium sulfamate solution and the third reaction solution to the reactor in sequence, and react under preset conditions to form acetoacetamide-N-sulfonic acid triethylamine salt solution as an intermediate solution.
  • a continuous reactor can be selected to realize the present application, such as a fixed bed reactor, a continuous stirred tank reactor or a microchannel reactor, etc.
  • the fixed bed reactor is taken as an example to briefly explain the reaction process.
  • the reaction can be ended after the preset reaction time is reached, and the product acetoacetamide-N-sulfonic acid triethylamine salt solution is obtained. Due to the characteristics of the fixed bed reactor, the reaction can be carried out continuously and is suitable for large-scale industrial production.
  • the solid acid catalysts in this application are molecular sieve catalysts or solid superacid catalysts.
  • the molecular sieve catalyst is HZSM-5 molecular sieve and/or Na-ZSM-5 molecular sieve;
  • the solid superacid catalyst is SO 4 2 ⁇ /Fe 2 O 3 type catalyst.
  • the application does not limit the amount of solid acid catalyst, which can be determined according to the type and specification of the reactor selected.
  • Amination reaction steps Dissolve 98kg of sulfamic acid and the first dichloromethane at a molar ratio of 1:6, and control the dissolution temperature at about 20 to 25°C to obtain a dichloromethane solution of sulfamic acid, that is, the first The reaction solution.
  • Dissolution can be in a continuous mixing device or in a reactor.
  • Acylation reaction step dissolving diketene and third dichloromethane at a molar ratio of 1:1.5, controlling the dissolution temperature at 10 to 20° C. to obtain a third reaction solution.
  • the fixed bed reactor After the solid superacid catalyst is installed in the fixed bed reactor, the fixed bed reactor is started, and the circulating water is adjusted to make the circulating water work normally.
  • the amounts of the ammonium sulfonate salt solution and the third reaction solution are such that the molar ratio of sulfamic acid to diketene is 1:1.1. After the reaction starts, lower the temperature of the cooling water as much as possible, and control the temperature of the reaction system at 20 to 35°C; as the performance of the catalyst declines, the temperature can be slightly increased within the control range.
  • the acetoacetamide-N-sulfonic acid triethylamine salt solution of each embodiment and comparative example is prepared by the above-mentioned method unless otherwise specified, and follow the special instruction if there is any special instruction.
  • Sulfonated cyclization step use acetoacetamide-N-sulfonic acid triethylamine salt solution as working fluid, dissolve sulfur trioxide in solvent to form cyclizing agent solution as injection fluid; working fluid from Venturi reactor The nozzle enters, and the injection fluid enters from the suction chamber of the Venturi reactor.
  • Table 1 for the pressure of the working fluid and the pressure of the injection fluid; make the working fluid and the injection fluid in the Venturi reactor The mixing section and the diffuser section are mixed to carry out the sulfonation ring closure reaction, and the sulfonation ring closure product is sprayed into the flow reactor.
  • Hydrolysis step the sulfonated cyclization product is subjected to a hydrolysis reaction with an aqueous ethanol solution preset in a flow reactor to obtain a hydrolyzate solution;
  • Salt-forming step adding potassium hydroxide to the organic phase of the hydrolyzate solution to carry out a salt-forming reaction to obtain acesulfame potassium.
  • the yield of acesulfame potassium is the ratio of the actual yield of acesulfame potassium to the theoretical yield calculated with diketene.
  • Sulfonated cyclization step use acetoacetamide-N-sulfonic acid triethylamine salt solution as working fluid, dissolve sulfur trioxide in solvent to form cyclizing agent solution as injection fluid; working fluid from Venturi reactor The nozzle enters, and the injection fluid enters from the suction chamber of the Venturi reactor.
  • the pressure of the working fluid is 0.8MPa
  • the pressure of the injection fluid is 0.4MPa
  • the reaction temperature is -10 ° C
  • the reaction time is 3 second
  • the working fluid and the injection fluid are mixed in the mixing section and the diffuser section of the Venturi reactor to carry out the sulfonation ring closure reaction, and the sulfonation ring closure product is sprayed into the flow reactor.
  • Hydrolysis step the sulfonated cyclization product is hydrolyzed with ethanol aqueous solutions of different mass fractions preset in the flow reactor to obtain a hydrolyzate solution; for the specific mass fraction of ethanol, please refer to Table 2, and the hydrolysis reaction temperature is controlled at - 15 ⁇ 0°C.
  • Salt-forming step adding potassium hydroxide to the organic phase of the hydrolyzate solution to carry out a salt-forming reaction to obtain acesulfame potassium.
  • the organic impurity in Table 2 is the organic impurity content of the acesulfame potassium obtained above after one time of impurity removal.
  • Example 1 in implementing comparative example 1D and implementing comparative example 1E, the pressure of working fluid and injection fluid is the same, in this case, the yield of acesulfame potassium is compared with embodiment 1A, Embodiment 1B and embodiment 1C are relatively low, can only reach 59% ⁇ 66%;
  • the difference of embodiment 1A, embodiment 1B and implementing comparative example 1D and implementing comparative example 1E is that the pressure of working fluid is greater than the injection fluid
  • the pressure, and the yield of acesulfame potassium has been significantly improved, reaching 89% to 91%.
  • the factors affecting the yield of acesulfame potassium except pressure control mainly include the sulfonation ring closure reaction time and reaction temperature. 1. Under the reaction conditions of the reaction time of 1-10s, the yield of acesulfame potassium can achieve a more ideal effect.
  • Example 6 the ethanol aqueous solution of different mass fractions was used to hydrolyze the sulfonated cyclization product, and the subsequent salt-forming reaction was carried out.
  • the ethanol content in the ethanol aqueous solution is between 60% and 85% %, the amount of organic impurities in the final product acesulfame potassium has reached below 10ppm.
  • the application forms a set of combined continuous reactors by using the Venturi reactor in combination with the flow reactor, and on the combined reactor, by controlling the acetoacetamide-N-sulfonic acid triethylamine salt
  • the relative pressure of the working fluid formed by the solution and the injection fluid formed by dissolving sulfur trioxide in the solvent into the Venturi reactor makes the cyclization process of acetoacetamide-N-sulfonic acid triethylamine salt and sulfur trioxide possible in
  • the mixing section and the diffuser section of the Venturi reactor are completely carried out, which greatly shortens the reaction time of the cyclization reaction, reduces the probability of organic impurities remaining in the final product acesulfame potassium, and improves the purity of acesulfame potassium.
  • the post-treatment process of acesulfame potassium is simplified, and the production cost of acesulfame potassium is reduced; at the same time, the reaction can be carried out continuously, which is suitable for large-scale industrial production, and the production efficiency of acesulfame potassium is improved.

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Abstract

L'invention concerne un procédé de préparation d'acésulfame de potassium consistant à : utiliser une solution de sel de triéthylamine d'acide acétoacétamide-N-sulfonique en guise de fluide de travail, et dissoudre du trioxyde de soufre dans un solvant pour former une solution d'agent de cyclisation en guise de fluide d'entraînement; introduire le fluide de travail provenant d'une buse d'un réacteur Venturi, introduire le fluide d'entraînement à partir d'une chambre d'aspiration d'air du réacteur Venturi, et réguler la pression du fluide de travail pour qu'elle soit supérieure à celle du fluide d'entraînement; mélanger le fluide de travail et le fluide d'entraînement dans une section de mélange et une section de diffusion du réacteur Venturi, effectuer une réaction de cyclisation par sulfonation, et pulvériser un produit de cyclisation par sulfonation dans un réacteur à écoulement; effectuer une réaction d'hydrolyse sur le produit de cyclisation par sulfonation et un agent d'hydrolyse préintroduit dans le réacteur à écoulement pour obtenir une solution de produit d'hydrolyse; et ajouter de l'hydroxyde de potassium dans la phase organique de la solution de produit d'hydrolyse pour obtenir de l'acésulfame de potassium. Le procédé de préparation réduit la probabilité que des impuretés organiques restent dans le produit final d'acésulfame de potassium, améliore la pureté de l'acésulfame de potassium, et est approprié pour une production industrielle à grande échelle.
PCT/CN2021/097015 2021-05-28 2021-05-28 Procédé de préparation d'acésulfame de potassium WO2022246867A1 (fr)

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WO2023123403A1 (fr) * 2021-12-31 2023-07-06 安徽金禾实业股份有限公司 Procédé de préparation en continu d'intermédiaire d'acésulfame
CN116322984A (zh) * 2021-12-31 2023-06-23 安徽金禾实业股份有限公司 一种用于制备乙酰磺胺酸钾的方法

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