CN111377880A - Continuous preparation method of acesulfame potassium - Google Patents
Continuous preparation method of acesulfame potassium Download PDFInfo
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Abstract
The invention belongs to the field of chemical production, and provides a continuous preparation method of acesulfame potassium, which comprises the following steps: first SO3Mixing the obtained product with dichloromethane to prepare a cyclizing agent, adding a certain amount of stabilizer into the cyclizing agent, adding the cyclizing agent added with the stabilizer and a DKA solution into a cyclization reaction module through a metering pump, adding the generated cyclization reaction liquid and water into a hydrolysis reaction module, allowing the generated acesulfame to pass through a continuous extraction tower, allowing a separated water phase to enter a waste acid treatment process, allowing an organic phase and a KOH solution to enter a neutralization reaction module, and concentrating, crystallizing, separating and drying the generated acesulfame potassium reaction liquid to obtain an acesulfame potassium finished product. The invention realizes the whole continuity of the preparation process, and simultaneously carries out the proportional control of the mixing section and the reaction section and the optimized selection of the mixing module on the microchannel reactor, thereby greatly improving the product yield of the potassium acetylsulfanilate, ensuring more stable product quality and more controllable process operation.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a continuous preparation method of acesulfame potassium.
Background
Acesulfame potassium (acesulfame potassium), 6-methyl-1,2, 3-oxooxazine-4- (3H) -one-2, 2-dioxide; 6-methyl-1,2, 3-oxaxine-4- (3H) -one-2, 2-dioxypotassium salt; 6-methyl-1,2, 3-oxooxazine-4- (3H) -one-2, 2-dioxypotassium salt; 6-methyl-2, 2-dioxo-1, 2, 3-oxathiazepine; acesulfame potassium; 6-methyl-1,2, 3-oxazin-4- (3H) -one-2, 2-dioxysylvite; AK sugar english name: RARECHEM AM UC 0205; SWEET ONE; SUNETTE; POTASSIUM 6-METHYL-1,2,3-OXATHIAZIN-4(3H) -ONE 2, 2-DIOXIDE; 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2, 2-dioxide; acesulfame; ACE surfame K; ACESULFAME POTASSIUM. Appearance properties: white crystalline powder, readily soluble in water, slightly soluble in ethanol; CAS number 55589-62-3;
the molecular formula is C4H4KNO 4S; the molecular weight is 201.2; melting point: 225 °; water solubility: 270g/L at 20 ℃;
density: 1.81; structural formula (xvi):
action and use: the product has strong sweet taste, sweetness about 130 times of sucrose, and taste similar to saccharin. It has bitter taste at high concentration. It has no moisture absorption, is stable at room temperature, and has good mixing property with sugar alcohol, sucrose, etc. As a non-nutritive sweetener, it can be widely used in various foods. According to the regulation of GB 2760-90 in China, the product can be used for liquid, solid beverage, ice cream, cake, jam, pickles, sweetmeat, chewing gum and table sweetener, and the maximum using amount is 0.3 g/kg.
The synthesis process in the prior art comprises the following steps:
in the traditional preparation process of the acesulfame potassium, the cyclization, hydrolysis and neutralization all adopt batch reactor type reaction, a certain amount of solvent is paved in a reaction kettle, and the reaction raw materials are all subjected to batch reaction in a dropwise manner. Recently, many research institutes have conducted the preparation of acesulfame potassium in a continuous manner, but generally in lower yields.
(1) A method for synthesizing AK sugar precursor ASH in a microchannel reactor is CN107868064A.2016-09-23.
The invention and the technical scheme mainly carry out cyclization and hydrolysis reaction on a reaction intermediate acylating agent and a cyclizing agent with certain concentration through a microchannel reactor, the total yield of the product is only 45-60%, and the process has the defects that sulfur trioxide is unstable under reaction conditions, the cyclization reaction speed is not controlled, and side reactions are easy to occur.
(2) A sulfonated microchannel reaction method and device in Anhui Jinhe actual industry Co., Ltd in Ansai honey production is CN108191790A.2018-01-13 in China.
The invention leads the intermediate raw material and the cyclizing agent raw material to be respectively carried out in the first and the second microreactors and then to exchange heat by the heat exchanger, and has the defect that the cyclization is divided into two modules for reaction, and the cyclized intermediate in the first group is easy to be decomposed by the reaction zone in the second group due to the over-high cyclization speed under the condition.
Disclosure of Invention
The invention aims to provide a continuous preparation method of acesulfame potassium, which solves the problem that a cyclized intermediate is easy to decompose in the process of preparing acesulfame potassium by adding a certain amount of stabilizing agent into a cyclizing agent, and adopts a microchannel reactor to carry out three groups of reaction modules for cyclization, hydrolysis and neutralization reaction in series, thereby realizing the integral continuity of the preparation process, simultaneously carrying out the proportion control of a mixing section and a reaction section and the optimized selection of the mixing module on the microchannel reactor, enhancing the mixing and heat exchange in the continuous preparation process, greatly improving the product yield of acesulfame potassium, ensuring the product quality to be more stable and controlling the process operation.
The technical scheme of the invention is as follows:
a continuous preparation method of acesulfame potassium is characterized by comprising the following steps:
first SO3Mixing the obtained product with dichloromethane to prepare a cyclizing agent, adding a certain amount of stabilizer into the cyclizing agent, adding the cyclizing agent added with the stabilizer and a DKA solution into a cyclization reaction module through a metering pump, adding the generated cyclization reaction liquid and water into a hydrolysis reaction module, allowing the generated acesulfame to pass through a continuous extraction tower, allowing a separated water phase to enter a waste acid treatment process, allowing an organic phase and a KOH solution to enter a neutralization reaction module, and concentrating, crystallizing, separating and drying the generated acesulfame potassium reaction liquid to obtain an acesulfame potassium finished product.
Further, the stabilizer is selected from one of ethylene glycol, boric acid, thionyl chloride, carbon tetrachloride and the like; the addition amount of the stabilizer accounts for 0.001-0.1% of the mass ratio of the cyclizing agent.
Further, the volume ratio of the DKA reaction liquid to the cyclizing agent to the water is 1: 0.2-3: 0.3-3.
Further, the specific gravity of the DKA reaction liquid is 1.19-1.32, the specific gravity of the cyclizing agent is 1.4-1.9, the viscosity of the DKA reaction liquid is 5-30, and the viscosity of the cyclizing agent is 5-25.
Further, the cyclization reaction temperature is 25-100 ℃, the reaction pressure is 0.1-10 MPa, the retention time is 0.01 s-30 min, and the optimal time is 0.01 s-5 min; the hydrolysis reaction temperature is 25-100 ℃, the reaction pressure is 0.1-10 MPa, the retention time is 0.01 s-30 min, and the optimal time is 0.01 s-5 min.
Further, in the continuous extraction, m (acesulfame reaction solution): m (CH2Cl2) is 1: 0.5-15.
Further, the neutralization reaction temperature is 10-50 ℃, the reaction pressure is 0.1-10 MPa, the retention time is 0.01 s-30 min, and 5 s-6 min is preferred; DKA to KOH mol ratio nDKA:nKOHThe ratio of KOH to KOH is 1: 0.8-2, and the concentration of KOH aqueous solution is 1% -48%.
According to the continuous preparation method of the acesulfame potassium, the continuous preparation of the acesulfame potassium is realized by a microchannel reaction module; the microchannel reaction module is a cyclization, hydrolysis and neutralization reaction module, the structures of the cyclization, hydrolysis and neutralization reaction modules are consistent, and the pipe diameter is 10-1000 mu m; the reaction and heat exchange of the cyclization, hydrolysis and neutralization reaction modules are integrated in the same module, the reaction module is internally divided into a mixing section and a reaction section, and the mixing section accounts for 1-100%, preferably 10-60% of the whole internal channel; the proportion of the reaction section in the whole internal channel is 0-99%, preferably 40-90%.
Further, the structure of the mixing section is one or the combination of two of Y-shaped, T-shaped, U-shaped and heart-shaped, wherein the angle range of the Y-shaped is 10-170 degrees, and preferably 30-100 degrees.
The heart-shaped channel is a cross-sectional view, and the arc-shaped and dot-shaped shaded parts play a role of blocking in order to increase the uniform mixing degree of the fluid in the channel. Opening angle of Y is 10-170oY is connected to the parallelogram channels to increase the degree of mixing of the fluid within the channels.
From a hydrodynamic point of view, the connection of U to the next, near circular channel is to increase the degree of mixing of the fluid inside the channel. Other shapes may be used.
From a hydrodynamic perspective, T is connected to the lower rectangular channel to increase the degree of mixing of the fluid within the channel. Other shapes may be used.
Further, the structure of the reaction section is one or the combination of two of a straight type, a snake type, an M type and a zoom type.
Further, the material of the reactor in the reaction module is one of glass, stainless steel, silicon carbide or hastelloy.
The invention also provides a continuous preparation system of the acesulfame potassium, which comprises a cyclization reaction module, a hydrolysis reaction module, a continuous extraction tower and a neutralization reaction module which are connected in sequence, wherein the cyclization reaction module, the hydrolysis reaction module and the neutralization reaction module are all connected with a metering pump; the cyclization reaction module, the hydrolysis reaction module and the neutralization reaction module are consistent in structure, and the pipe diameter is 10-1000 mu m; the reaction and heat exchange of the cyclization, hydrolysis and neutralization reaction modules are integrated in the same module, the reaction module is internally divided into a mixing section and a reaction section, and the mixing section accounts for 1-100%, preferably 10-60% of the whole internal channel; the proportion of the reaction section in the whole internal channel is 0-99%, preferably 40-90%.
The pipe diameter is the pipe diameter of internal channel, including mixing section and reaction section, and the concrete structure sees the attached drawing.
Further, the structure of the mixing section is one or the combination of two of Y-shaped, T-shaped, U-shaped and heart-shaped, wherein the angle range of the Y-shaped is 10-170 degrees, and preferably 30-100 degrees.
Further, the structure of the reaction section is one or the combination of two of a straight type, a snake type, an M type and a zoom type.
Further, the material of the reactor in the reaction module is one of glass, stainless steel, silicon carbide or hastelloy.
Detailed description of the invention:
the invention provides a continuous preparation method of acesulfame potassium, which comprises the following specific operation steps:
first SO3Mixing the obtained mixture with dichloromethane to prepare a cyclizing agent, adding a certain amount of a stabilizer into the cyclizing agent, adding the cyclizing agent of the stabilizer and a DKA (full name: triethylamine acetylacetamidosulfonate) solution into a cyclization reaction module according to a certain proportion through a metering pump, adding the generated cyclization reaction liquid and water into a hydrolysis reaction module according to a certain proportion, allowing the generated acesulfame to pass through a continuous extraction tower, allowing a separated water phase to enter a waste acid treatment process, allowing an organic phase and a KOH solution to enter a neutralization reaction module according to a certain proportion, concentrating, crystallizing, separating and drying the generated acesulfame potassium reaction liquid to obtain the acesulfame potassium finished product, wherein the product yield is 80-85%, the content of the finished product is 99.0-99.3%, the preparation process flow is shown in figure 1, and the equipment in the reaction process is shown in figure 2.
1) The specific gravity of the cyclizing agent is 1.4-1.9, the added stabilizer is one of ethylene glycol, boric acid, thionyl chloride, carbon tetrachloride and the like, and the addition amount of the stabilizer accounts for 0.001-0.1% of the mass ratio of the cyclizing agent;
2) the volume ratio of the DKA reaction liquid to the cyclizing agent to the water is 1: 0.2-3: 0.3-3;
3) the specific gravity of the DKA reaction liquid is 1.19-1.32, the specific gravity of the cyclizing agent is 1.4-1.9, the viscosity of the DKA reaction liquid is 5-30, and the viscosity of the cyclizing agent is 5-25;
4) the cyclization reaction temperature is 25-100 ℃, the reaction pressure is 0.1-10 MPa, the residence time is 0.01 s-30 min, and the optimal time is 0.01 s-5 min; the hydrolysis reaction temperature is 25-100 ℃, the reaction pressure is 0.1-10 MPa, the retention time is 0.01 s-30 min, and the optimal time is 0.01 s-5 min;
5) the continuous extraction step, m (acesulfame reaction solution): m (CH2Cl2) is 1: 0.5-15;
6) the neutralization reaction temperature is 10-50 ℃, the reaction pressure is 0.1-10 MPa, the retention time is 0.01 s-30 min, and the preferred time is 5 s-6 min; n (DKA) 1: 0.8-2, concentration of KOH aqueous solution is 1% -48%;
7) the microchannel reaction module is shown in the figure, wherein the structures of the cyclization reaction module, the hydrolysis reaction module and the neutralization reaction module are consistent, the pipe diameter is 10-1000 mu m, and the material of the reactor is one of glass, stainless steel, silicon carbide or Hastelloy; the reaction module integrates reaction and heat exchange in the same module, the interior of the reaction module is divided into a mixing section and a reaction section (see figure 3 specifically), the mixing section accounts for 1% -100%, preferably 10% -60% of the whole internal channel, the structure of the mixing section is one or a combination of two of Y-shaped, T-shaped, U-shaped and heart-shaped (see figure 4 specifically), wherein the angle range of the Y-shaped is 10-170 degrees, preferably 30-100 degrees; the proportion of the reaction section in the whole internal channel is 0-99%, preferably 40-90%, and the structure of the reaction section is one or two of straight type, snake type, M type and zoom type (see figure 5 in detail).
Advantageous technical effects
1) According to the invention, a certain amount of stabilizer is added into the cyclizing agent, so that the cyclization reaction becomes more mild and controllable, the decomposition of a cyclization reaction intermediate is inhibited, and the reaction yield of the potassium acetylsulfanilate is improved;
2) according to the invention, through accurate control of the proportion of the mixing section to the reaction section in the reaction module, a more effective mixing section structure and reaction section structure are screened, the mass transfer and heat transfer of the microchannel reactor are enhanced, the reaction conversion is more complete, and the reaction efficiency is further improved;
3) the invention adopts the microchannel reactor, integrates the cyclization, hydrolysis and neutralization reaction processes into a whole in a continuous flow mode, realizes the continuity of the whole reaction, ensures that the process operation becomes more stable, further improves the production safety and ensures that the product quality is more stable.
Drawings
FIG. 1 is a process flow diagram of a continuous preparation method of acesulfame potassium.
FIG. 2 is a reaction process equipment diagram of a continuous preparation method of acesulfame potassium.
FIG. 3 is a diagram of a microchannel reaction block.
FIG. 4 is a schematic diagram of the structure of the mixing section, wherein the mixing section is 1-Y-shaped, 2-U-shaped, 3-T-shaped, and 4-heart-shaped.
FIG. 5 is a schematic diagram of the reaction section, wherein the reaction section is a 5-straight type, a 6-M type, a 7-scaled type, and an 8-serpentine type.
Detailed Description
The present invention is further illustrated below with reference to examples, which are understood by those skilled in the art to be illustrative only and not to constitute any limitation to the present invention.
Example 1:
first SO3Mixing with dichloromethane to prepare a cyclizing agent, adding a certain amount of stabilizer into the cyclizing agent, adding the cyclizing agent of the stabilizer and DKA (full name: triethylamine acetylacetamidosulfonate) solution into a cyclization reaction module according to a certain proportion by a metering pump, adding the generated cyclization reaction liquid and water into a hydrolysis reaction module according to a certain proportion, allowing the generated acesulfame to pass through a continuous extraction tower, allowing the separated water phase to enter a waste acid treatment process, allowing the organic phase and KOH solution to enter a neutralization reaction module according to a certain proportion, concentrating, crystallizing, separating and drying the generated acesulfame potassium reaction liquid to obtain the acesulfame potassium finished product, wherein the product yield is 80%, the finished product content is 99.0%, the preparation process flow is shown in figure 1, and the equipment of the reaction process is shown in figure 2.
1) The specific gravity of the cyclizing agent is 1.4, the added stabilizer is ethylene glycol, and the addition amount of the stabilizer accounts for 0.001% of the mass ratio of the cyclizing agent;
2) the volume ratio of the DKA reaction liquid to the cyclizing agent to the water is 1:0.2: 0.3;
3) the specific gravity of the DKA reaction liquid is 1.19, the specific gravity of the cyclizing agent is 1.4, the viscosity of the DKA reaction liquid is 5, and the viscosity of the cyclizing agent is 5;
4) the cyclization reaction temperature is 25 ℃, the reaction pressure is 0.1MPa, the residence time is 5min, the hydrolysis reaction temperature is 25 ℃, the reaction pressure is 0.1MPa, and the residence time is 5 min;
5) the continuous extraction step, m (acesulfame reaction solution): m (CH2Cl2) 1: 0.5;
6) the neutralization reaction temperature is 10 ℃, the reaction pressure is 0.1MPa, and the retention time is 6 min; n (DKA) 1:0.8, concentration of KOH aqueous solution is 1%;
7) the microchannel reaction module is shown in the figure, wherein the structures of the cyclization reaction module, the hydrolysis reaction module and the neutralization reaction module are all consistent, the pipe diameter is 10 mu m, and the reactor is made of glass; the reaction module integrates reaction and heat exchange in the same module, the interior of the reaction module is divided into a mixing section and a reaction section (see figure 3 specifically), the mixing section accounts for 10% of the whole internal channel, the structure of the mixing section is Y-shaped (see figure 4 specifically), and the angle range of the Y-shaped is 30 degrees; the proportion of the reaction section in the whole internal channel is 90%, and the structure of the reaction section is straight (see figure 5 in particular).
Example 2:
first SO3Mixing with dichloromethane to prepare cyclizing agent, adding a certain amount of stabilizer, adding cyclizing agent of stabilizer and DKA (full name: triethylamine acetylacetamido sulfonate) solution into cyclization reaction module by metering pump according to a certain proportion, adding generated cyclization reaction liquid and water into hydrolysis reaction module according to a certain proportion, making the generated acesulfame acid pass through continuous extraction tower, making separated water phase enter waste acid treatment procedure, making organic phase and KOH solution enter neutralization reaction module according to a certain proportion, concentrating, crystallizing, separating and drying the generated acesulfame potassium reaction liquid to obtain acesulfame potassium finished product, its product yield is 82%, and its finished product can be made into the invented productThe product content is 99.2%, the preparation process flow is shown in figure 1, and the equipment in the reaction process is shown in figure 2.
1) The specific gravity of the cyclizing agent is 1.6, the added stabilizer is boric acid, and the addition amount of the stabilizer accounts for 0.05 percent of the mass ratio of the cyclizing agent;
2) the volume ratio of the DKA reaction liquid to the cyclizing agent to the water is 1:1.5: 1.2;
3) the specific gravity of the DKA reaction liquid is 1.20, the specific gravity of the cyclizing agent is 1.6, the viscosity of the DKA reaction liquid is 18, and the viscosity of the cyclizing agent is 12;
4) the cyclization reaction temperature is 35 ℃, the reaction pressure is 3MPa, and the retention time is 1 min; the hydrolysis reaction temperature is 40 ℃, the reaction pressure is 5MPa, and the retention time is 2 min;
5) the continuous extraction step, m (acesulfame reaction solution): m (CH2Cl2) ═ 1: 5;
6) the neutralization reaction temperature is 30 ℃, the reaction pressure is 5MPa, and the retention time is 4 min; n (DKA) n (KOH) 1:1.2, concentration of KOH aqueous solution 15%;
7) the microchannel reaction module is shown in the figure, wherein the structures of the cyclization reaction module, the hydrolysis reaction module and the neutralization reaction module are all consistent, the pipe diameter is 200 mu m, and the reactor is made of silicon carbide; the reaction module integrates reaction and heat exchange in the same module, the interior of the reaction module is divided into a mixing section and a reaction section (see figure 3 specifically), the mixing section accounts for 30% of the whole internal channel, and the mixing section is in a T-shaped and heart-shaped combination structure; the proportion of the reaction section occupying the whole internal channel was 70% of the structure of the reaction section being a combination of M-type and scaled-type (see FIG. 5 in particular).
Example 3
First SO3Mixing with dichloromethane to prepare cyclizing agent, adding a certain amount of stabilizer, adding cyclizing agent of stabilizer and DKA (full name: acetyl acetamido sulfonic acid triethylamine) solution into cyclization reaction module by metering pump, adding generated cyclization reaction solution and water into hydrolysis reaction module by a certain proportion, passing generated acetyl sulfanilic acid through continuous extraction tower, separating out water phase, treating waste acid, and neutralizing organic phase and KOH solution by a certain proportionAnd (3) performing concentration, crystallization, separation and drying on the generated acesulfame potassium reaction solution to obtain an acesulfame potassium finished product, wherein the product yield is 85 percent, the finished product content is 99.3 percent, the preparation process flow is shown in figure 1, and the equipment in the reaction process is shown in figure 2.
1) The specific gravity of the cyclizing agent is 1.9, the added stabilizer is one of ethylene glycol, boric acid, thionyl chloride, carbon tetrachloride and the like, and the addition amount of the stabilizer accounts for 0.1% of the mass ratio of the cyclizing agent;
2) the volume ratio of the DKA reaction liquid to the cyclizing agent to the water is 1:3: 3;
3) the specific gravity of the DKA reaction liquid is 1.32, the specific gravity of the cyclizing agent is 1.9, the viscosity of the DKA reaction liquid is 30, and the viscosity of the cyclizing agent is 25;
4) the cyclization reaction temperature is 100 ℃, the reaction pressure is 10MPa, and the retention time is 0.01 s; the hydrolysis reaction temperature is 100 ℃, the reaction pressure is 10MPa, and the retention time is 0.01 s;
5) the continuous extraction step, m (acesulfame reaction solution): m (CH2Cl2) 1: 15;
6) the neutralization reaction temperature is 50 ℃, the reaction pressure is 10MPa, and the retention time is 6 min; n (DKA) n (KOH) 1:2, 48% aqueous KOH solution;
7) the microchannel reaction module is shown in the figure, wherein the structures of the cyclization reaction module, the hydrolysis reaction module and the neutralization reaction module are all consistent, the pipe diameter is 1000 mu m, and the material of the reactor is hastelloy; the reaction module integrates reaction and heat exchange in the same module, the interior of the reaction module is divided into a mixing section and a reaction section (see figure 3 specifically), the mixing section accounts for 60% of the whole internal channel, and the mixing core type (see figure 4 specifically); the proportion of the reaction section occupying the whole internal passage is 40%, and the structure of the reaction section is of a scaled type (see fig. 5 in particular).
The present invention has been disclosed in terms of the preferred embodiment, but it is not intended to be limited to the embodiment, and all technical solutions obtained by substituting or converting the equivalent embodiments fall within the scope of the present invention.
Claims (10)
1. A continuous preparation method of acesulfame potassium is characterized by comprising the following steps:
first SO3Mixing the obtained product with dichloromethane to prepare a cyclizing agent, adding a certain amount of stabilizer into the cyclizing agent, adding the cyclizing agent added with the stabilizer and a DKA solution into a cyclization reaction module through a metering pump, adding the generated cyclization reaction liquid and water into a hydrolysis reaction module, allowing the generated acesulfame to pass through a continuous extraction tower, allowing a separated water phase to enter a waste acid treatment process, allowing an organic phase and a KOH solution to enter a neutralization reaction module, and concentrating, crystallizing, separating and drying the generated acesulfame potassium reaction liquid to obtain an acesulfame potassium finished product.
2. The continuous preparation method of acesulfame potassium according to claim 1, wherein the stabilizer is selected from one of ethylene glycol, boric acid, thionyl chloride and carbon tetrachloride; the addition amount of the stabilizer accounts for 0.001-0.1% of the mass ratio of the cyclizing agent.
3. The continuous preparation method of acesulfame potassium according to claim 1, wherein the volume ratio of the DKA reaction liquid to the cyclizing agent to the water is 1: 0.2-3: 0.3-3.
4. The continuous preparation method of acesulfame potassium according to claim 1, wherein the DKA reaction liquid has a specific gravity of 1.19 to 1.32, the cyclizing agent has a specific gravity of 1.4 to 1.9, the DKA reaction liquid has a viscosity of 5 to 30cp, and the cyclizing agent has a viscosity of 5 to 25 cp.
5. The continuous preparation method of acesulfame potassium according to claim 1, wherein the cyclization reaction temperature is 25-100 ℃, the reaction pressure is 0-10 MPa, and the retention time is 0.01 s-30 min; the hydrolysis reaction temperature is 25-100 ℃, the reaction pressure is 0-10 MPa, and the retention time is 0.01 s-30 min.
6. The continuous process for preparing acesulfame potassium according to claim 1, wherein the neutralization temperature is set toThe temperature is 10-50 ℃, the reaction pressure is 0-10 MPa, and the retention time is 0.01 s-30 min; DKA to KOH mol ratio nDKA:nKOHThe ratio of KOH to KOH is 1: 0.8-2, and the concentration of KOH aqueous solution is 1% -48%.
7. The continuous preparation method of acesulfame potassium according to claim 1, wherein the continuous preparation of acesulfame potassium is realized by a microchannel reaction module; the microchannel reaction module is a cyclization, hydrolysis and neutralization reaction module, the structures of the cyclization, hydrolysis and neutralization reaction modules are consistent, and the pipe diameter is 10-1000 mu m; the reaction and heat exchange of the cyclization, hydrolysis and neutralization reaction modules are integrated in the same module, the reaction module is internally divided into a mixing section and a reaction section, and the mixing section accounts for 1-100% of the whole internal channel; the proportion of the reaction section in the whole internal channel is 0-99%.
8. The continuous preparation method of acesulfame potassium according to claim 7, wherein the structure of the mixing section is one or a combination of two of Y-type, T-type, U-type and heart-type, wherein the angle of Y-type is 10-170 °; the structure of the reaction section is one or the combination of two of a straight type, a snake type, an M type and a zoom type.
9. The continuous preparation method of acesulfame potassium according to claim 7, wherein the material of the reactor in the reaction module is one of glass, stainless steel, silicon carbide or hastelloy.
10. The continuous preparation system of the acesulfame potassium is characterized by comprising a cyclization reaction module, a hydrolysis reaction module, a continuous extraction tower and a neutralization reaction module which are sequentially connected, wherein the cyclization reaction module, the hydrolysis reaction module and the neutralization reaction module are all connected with a metering pump; the cyclization reaction module, the hydrolysis reaction module and the neutralization reaction module are consistent in structure, and the pipe diameter is 10-1000 mu m; the reaction and heat exchange of the cyclization, hydrolysis and neutralization reaction modules are integrated in the same module, the reaction module is internally divided into a mixing section and a reaction section, and the mixing section accounts for 1-100% of the whole internal channel; the proportion of the reaction section in the whole internal channel is 0-99%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113454072A (en) * | 2021-05-28 | 2021-09-28 | 安徽金禾实业股份有限公司 | Preparation method of acesulfame potassium |
| WO2023123405A1 (en) * | 2021-12-31 | 2023-07-06 | 安徽金禾实业股份有限公司 | Method and apparatus for processing hydrolysis reaction product containing acesulfame |
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| CN113454072B (en) * | 2021-05-28 | 2022-11-25 | 安徽金禾实业股份有限公司 | Preparation method of acesulfame potassium |
| WO2023123405A1 (en) * | 2021-12-31 | 2023-07-06 | 安徽金禾实业股份有限公司 | Method and apparatus for processing hydrolysis reaction product containing acesulfame |
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