CN111377884A - Method for continuously preparing acesulfame potassium through microchannel reactor - Google Patents
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Abstract
The invention belongs to the field of chemical production, and provides a method for continuously preparing acesulfame potassium by a microchannel reactor, which comprises the following steps: the method comprises the steps of enabling the acetoacetamidosulfonic triethylamine salt solution and a cyclizing agent to continuously enter a microreactor through an A, B interface of the microreactor, enabling the solution and the cyclizing agent to be subjected to full reaction in a mixing section and a reaction section, enabling the solution and water continuously entering from an interface C to be subjected to full mixing reaction in the mixing section and the reaction section in the same reactor, obtaining a reaction solution of the acesulfame from an outlet D, and performing separation processes such as continuous extraction, continuous neutralization, continuous concentration and continuous drying to obtain the acesulfame potassium. The DKA solution, the cyclizing agent and the water complete the continuous cyclization and hydrolysis process in the same microreactor, the mixture ratio of raw materials for cyclization and hydrolysis is adjusted by changing and combining the mixing section and the reaction section of the microreactor, the temperature of reaction materials in the microreactor and the residence time of the mixing and reaction section are controlled, and the side reaction is reduced by utilizing the internal strong heat exchange.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a method for continuously preparing acesulfame potassium through a microchannel reactor.
Background
Acesulfame potassium, chinese name: acesulfame potassium, a-K sugar, english name: acesufame lotus, appearance properties: a crystalline powder which is colorless or white, odorless and strongly sweet; solubility: easily soluble in water and slightly soluble in ethanol, CAS No. 55589-62-3, molecular formula C4H4KNO4S
Structural formula (xvi):
molecular weight 201.2, melting point (. degree. C.): 225, density: 1.81 (g/cm)3)，
Acid-base (1% w/v aqueous solution): the pH value is 5.5-7.5.
Action and use: the acesulfame potassium has wide application, and can be used as a sweet source for all foods and beverages. Because it is stable to acid heat, it is more suitable for acidic beverages and foods requiring high-temperature sterilization and baking. The acesulfame potassium is used in combination with sorbitol, has better sweet taste, and is particularly suitable for being used as an incapability candy and a food requiring a filler.
When 800-1000 mg/1 or less of acesulfame potassium is added into the low-energy beverage, satisfactory sweet taste can be obtained. The food or beverage using acesulfame potassium as sweet source has no calorie, and is especially suitable for patients with obesity, diabetes and phenylketonuria.
In oral, cosmetic and pharmaceutical preparations, bitter taste is often imparted by the addition of surfactants or other reasons and can be masked by the sweet taste of acesulfame potassium.
Granular materials such as medicines, etc., or a compound of acesulfame potassium and dextrin as a sweet coating layer. In addition, the acesulfame potassium is added into the animal beverage, so that the palatability of the animal beverage can be improved, the animal is facilitated to eat, and the animal growth is promoted.
At present, the conventional synthesis method for preparing potassium acetylsulfonate mainly comprisesThe main steps of the method for influencing the yield are cyclization-hydrolysis, and because the heat release of local reaction in the reaction step is large, a cyclization intermediate is subjected to high temperature and can be rapidly decomposed within a certain time, and the yield is greatly reduced. Therefore, the domestic main synthesis process is a low-temperature kettle type intermittent process, the process needs to carry out cyclization-hydrolysis reaction at low temperature, the retention time of a cyclization intermediate is long, and the hydrolysis operation condition is not easy to control, so that the yield is only 69 percent[1]The kettle type intermittent process has the biggest defects of low yield, high energy consumption and large amount of three wastes. The synthesis mode of the process directly leads to no further improvement of yield, and is gradually replaced by other synthesis modes[2]。
The potassium acetylsulfonate product has more and more fierce market competition at home and abroad and more strict environmental protection requirements, and a method for continuously preparing the potassium acetylsulfonate through a microchannel reactor is researched from the consideration of how to improve the yield of the potassium acetylsulfonate. The cyclization and hydrolysis are carried out in the same microchannel reactor, the cyclization intermediate rapidly enters a hydrolysis process, and rapidly enters a reaction section after being fully mixed, so as to complete hydrolysis reaction, and a reaction system is rapidly removed for subsequent treatment. The difficult problems that the cyclized intermediate is unstable before hydrolysis and the hydrolyzed acetylsulfanilic Acid (ASH) intermediate is easy to decompose at high temperature are solved, and the yield of the acesulfame potassium reaches 80-85 percent after cyclization, hydrolysis and subsequent continuous separation.
The prior art treatment process comprises the following steps:
(1) tantong, fourth generation synthetic sweetener acesulfame preparation method [ J ] Guangxi chemical industry: 1992,[1],40-43.
The sulfamic acid-diketene-sulfur trioxide process is a low-temperature intermittent process, and the acesulfame potassium is obtained through a series of post-treatments, and the yield is 69%.
The low-temperature batch process has the defects of complex process control, high energy consumption, low yield and unstable yield among batches.
(2) Yangxiangjian, Qifei, Wangkang, a sulfonated microchannel reaction method and device in acesulfame K production [ P ]. Anhui: CN108191790A,2018-01-13.
The method discloses a method for continuously preparing acesulfame potassium by a microchannel reactor, wherein cyclization and hydrolysis are carried out by connecting a plurality of microchannel reactors in series, so that continuous operation is realized, and waste acid is reduced.
The cyclization hydrolysis of the process is carried out separately and is carried out in cascade step-by-step cyclization hydrolysis, which is not favorable for the stability of a cyclization intermediate and leads to the decomposition of the intermediate and the reduction of the yield.
Disclosure of Invention
The invention aims to develop a method for continuously preparing acesulfame potassium by a microchannel reactor, which comprises the steps of continuously preparing a triethylamine acetylacetamidosulfonate (DKA) solution, metering the DKA solution, a cyclizing agent and water by a flowmeter, then completing continuous cyclization and hydrolysis processes in a same microreactor according to a certain proportion, adjusting the proportion of raw materials for cyclization and hydrolysis by changing and combining a mixing section and a reaction section of the microreactor, controlling the temperature of reaction materials in the microreactor and the retention time of the mixing and reaction section, and reducing side reactions by utilizing internal strong heat exchange. And (3) continuously layering, continuously extracting, continuously neutralizing, continuously concentrating, continuously crystallizing and continuously drying the hydrolysate (the flow is shown in figure 4) to obtain the acesulfame potassium, wherein the yield of the acesulfame potassium reaches 80-85%.
The technical scheme provided by the invention is as follows:
a method for continuously preparing acesulfame potassium through a microchannel reactor is characterized by comprising the following steps:
after the acetoacetamidosulfonic triethylamine salt solution and the cyclizing agent are measured by a flow meter, the solution continuously enters the microreactor through an A, B interface of the microreactor according to a certain proportion, after the solution is fully reacted in a mixing section and a reaction section, the solution is fully reacted in the same reactor with water continuously entering from a C interface after being measured by the flow meter, after the solution is fully mixed and reacted in the mixing section and the reaction section, the acetylsulfanilic acid reaction solution is obtained from an outlet D, and separation processes such as continuous extraction, continuous neutralization, continuous concentration, continuous drying and the like are performed to obtain the acetylsulfanilic acid.
The preparation of the acetoacetamidosulfonic acid triethylamine salt (DKA) solution can be a continuous process, sulfamic acid and dichloromethane are continuously mixed and dissolved, then are continuously neutralized with triethylamine solution, a neutralization reaction liquid and diketene enter a continuous reactor, and a DKA reaction liquid is obtained through addition acylation reaction.
Further, the continuous mixing and dissolving are carried out according to the following proportion: n (sulfamic acid): n (dichloromethane) 1: 1-20, preferably 1: 8-12; the temperature is 0-40 ℃; preferably 15 to 25 ℃. The continuous neutralization is carried out, wherein the pH value of the neutralization is 7-9; the triethylamine solution is a mixed solution of triethylamine and dichloromethane, and the proportion is n (triethylamine): n (dichloromethane) ═ 1:0 to 5, preferably 1:0 to 2; the neutralization temperature is 10 ℃ to 40 ℃, preferably 20 ℃ to 30 ℃. The addition acylation reaction, the proportion n (sulfamic acid): n (diketene) is 1:0.5 to 1.5, preferably 1:1 to 1.2; n (diketene): n (dichloromethane) ═ 1:0 to 1.5, preferably 1:0 to 1; the acylation reaction temperature is 0-30 ℃, and is optimally controlled at 20-25 ℃; the acylation retention time is 0.01 s-30 min, preferably 30 s-10 min; the continuous reactor is one or more of kettle type continuous, channel continuous and micro reactor. The DKA reaction yield is 95-98% by weight of sulfamic acid.
According to the method for continuously preparing the acesulfame potassium by the microchannel reactor, the cyclizing agent is SO3The cyclizing agent is prepared by mixing with dichloromethane, and the specific gravity of the cyclizing agent is 1.4-1.9 g/cm3Preferably, the specific gravity of the cyclizing agent is 1.45-1.6 g/cm3。
According to the method for continuously preparing the potassium sulfacetamide by the microchannel reactor, the feeding volume ratio of the DKA reaction liquid, the cyclizing agent and the water, vDKA reaction liquid：vCyclizing reagent：vWater (W)0.3 to 3, preferably 1:0.8 to 1.5:0.5 to 1.8;
further, the specific gravity of the DKA reaction liquid is 1.19-1.32 g/cm3The specific gravity of the cyclizing agent is 1.4-1.9 g/cm3Preferably, the specific gravity of the DKA reaction liquid is 1.24-1.30 g/cm3The specific gravity of the cyclizing agent is 1.45-1.6 g/cm3(ii) a The viscosity of the DKA reaction liquid is 5-30 cp, and the viscosity of the cyclizing agent is 5-25 cp;
further, the cyclization reaction temperature is 25-100 ℃, and preferably 25-40 ℃; the reaction pressure is 0-10 MPa, preferably 0.5-5 MPa;
further, the hydrolysis reaction temperature is 25-100 ℃, and preferably 25-40 ℃; the reaction pressure is 0-10 MPa, preferably 0.5-5 MPa;
further, the cyclization residence time is 0.01S-30 min, preferably 0.01S-10 min; the hydrolysis retention time is 0.01S-30 min, preferably 0.01S-15 min;
further, neutralizing the extracted organic phase with a KOH solution, wherein the neutralization reaction 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%.
According to the method for continuously preparing the acesulfame potassium through the microchannel reactor, the microreactor comprises a cyclization I area, a hydrolysis II area and a heat exchange area; the cyclization I area consists of a mixing section and a reaction section, and the hydrolysis II area consists of a mixing section and a reaction section; the structure of the mixed section of the cyclization I area or the mixed section of the hydrolysis II area is composed of one or more of a heart type, a Y type, a U type and a T type, and the structure of the reaction section of the cyclization I area or the reaction section of the hydrolysis II area is composed of one or more of a snake shape, a zoom type, an M type and a straight type.
Furthermore, the ratio of the cyclization I area to the hydrolysis II area of the microreactor is 1: 0.5-10, preferably 1: 1-5.
Furthermore, the proportion of the mixing section in the cyclization I area to the internal channel of the area is 1-100%; the proportion of the reaction section occupying the internal channel of the zone is 0-99%. The proportion of the mixing section in the hydrolysis II area in the internal channel of the area is 1 to 100 percent; the proportion of the reaction section occupying the internal channel of the zone is 0-99%.
Further, the size of the reaction channel of the microreactor is 10-1000 μm, and preferably 100-500 μm. The sizes of the reaction channels are the sizes of the pipelines of the mixing section and the reaction section in the cyclization reaction section and the hydrolysis reaction section, and are the parameter ranges.
Further, the material of the microreactor is as follows: one or more of silicon carbide, hastelloy, zirconium, tantalum, stainless steel and glass.
The invention also provides a system for continuously preparing the acesulfame potassium through the microchannel reactor, which comprises an acylation reactor, a microreactor, an extraction tower, a neutralization tower, a concentration device and a dryer, wherein the acylation reactor, the microreactor, the extraction tower, the neutralization tower, the concentration device and the dryer are sequentially connected through pipelines; the microreactor comprises a cyclization I area, a hydrolysis II area and a heat exchange area; the cyclization I area consists of a mixing section and a reaction section, and the hydrolysis II area consists of a mixing section and a reaction section;
further, the structure of the mixed section of the cyclization I area or the mixed section of the hydrolysis II area is composed of one or more of a heart type, a Y type, a U type and a T type.
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. The opening angle of Y is 10-170 degrees, and Y is connected with the channel of the parallelogram to increase the uniform mixing degree of the fluid in the channel.
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 of the cyclization I zone or the reaction section of the hydrolysis II zone is composed of one or more of a snake shape, a zoom type, an M type and a straight type.
Further, the size of the reaction channel of the microreactor is 10-1000 μm, and preferably 100-500 μm.
Further, the material of the microreactor is as follows: one or more of silicon carbide, hastelloy, zirconium, tantalum, stainless steel and glass.
Detailed description of the invention:
the invention mainly aims at the intermittent synthesis mode of the acesulfame potassium and the problems of low yield, high energy consumption, high production cost and the like in the cyclization and hydrolysis processes, and develops a method for continuously preparing the acesulfame potassium by a microchannel reactor.
The main process comprises the following steps:
1. the preparation of the acetoacetamidosulfonic acid triethylamine salt (DKA) solution is a continuous process preparation.
2. The DKA solution and the cyclizing agent continuously enter the microreactor through an A, B interface of the microreactor, and after the full reaction of the mixing section and the reaction section, the DKA solution and the cyclizing agent continuously enter the microreactor in the same reactor through the C interface, and the water continuously enters the microreactor through the mixing section and the reaction section, and the reaction solution of the acesulfame acid is obtained from an outlet D for continuous extraction.
3. The feed ratio of the DKA reaction liquid, cyclizing agent and water, v (DKA reaction liquid): v (cyclizing agent): v (water) ═ 1:0.2 to 3:0.3 to 3, and preferably 1:0.8 to 1.5:0.5 to 1.8.
4. The specific gravity of the DKA reaction liquid is 1.19-1.32 g/cm3The specific gravity of the cyclizing agent is 1.4-1.9 g/cm3Preferably, the specific gravity of the DKA reaction liquid is 1.24-1.30 g/cm3The specific gravity of the cyclizing agent is 1.45-1.6 g/cm3(ii) a The viscosity of the DKA reaction liquid is 5-30 cp, and the viscosity of the cyclizing agent is 5-25 cp.
5. The cyclization reaction temperature is 25-100 ℃, and preferably 25-40 ℃; the reaction pressure is 0-10 MPa, preferably 0.5-5 MPa.
6. The hydrolysis reaction temperature is 25-100 ℃, and preferably 25-40 ℃; the reaction pressure is 0-10 MPa, preferably 0.5-5 MPa.
7. The cyclization residence time is 0.01S-30 min, preferably 0.01S-10 min; the hydrolysis retention time is 0.01S-30 min, preferably 0.01S-15 min.
8. The reaction yield of cyclization and hydrolysis is 90-95% in terms of DKA.
9. The post-treatment process comprises separation processes such as continuous extraction, continuous neutralization, continuous concentration and continuous drying.
10. The yield of the acesulfame potassium is 80-85% in terms of sulfamic acid.
11. The microreactor structure comprises a cyclization reaction section and a hydrolysis reaction section which are both arranged in the same microreactor, wherein the cyclization section consists of a mixing section and a reaction section, and the hydrolysis section consists of a mixing section and a reaction section; the mixed section structure is composed of one or more of a heart type, a Y type, a U type and a T type, and the reaction section structure is composed of one or more of a snake shape, a zoom type, an M type and a straight type.
12. The size of the reaction channel of the micro-reactor is 10-1000 μm, and preferably 100-500 μm.
13. The micro-reactor is made of the following materials: one or more of silicon carbide, hastelloy, zirconium, tantalum, stainless steel and glass.
Advantageous technical effects
The invention provides a method for continuously preparing acesulfame potassium by a microchannel reactor, which realizes the continuous preparation of acesulfame potassium by the microchannel reactor, realizes the continuous preparation of AK sugar, has stable product quality, has finished product content of more than 99 percent, has higher yield than the prior batch kettle process and reaches 80 to 85 percent, and has reduced energy consumption by 60 percent compared with the batch kettle process from the production energy consumption, thereby meeting the environmental protection requirements of energy saving and consumption reduction.
Drawings
FIG. 1 is a schematic diagram of a microreactor structure,
wherein: a: DKA reaction liquid, B is cyclizing agent, C: process water, D: acetyl sulfanilic acid reaction solution, E: cyclizing mixed-phase, F: cyclization reaction section, G: hydrolysis mixing section, H: hydrolysis reaction section, zone i: cyclized region I, region II: and in the hydrolysis II area, the shaded area in the figure is heat exchange.
FIG. 2 is a schematic diagram of several configurations of a mixing section of a microreactor, wherein: 1-Y type, 2-U type, 3-T type and 4-heart type.
FIG. 3 is a schematic diagram of several structures of a micro-reaction section, wherein: 5-straight type, 6-M type, 7-zoom type, 8-snake type.
FIG. 4 is a schematic diagram of a process for preparing acesulfame potassium.
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.
The preparation of the acetoacetamidosulfonic acid triethylamine salt (DKA) solution can be a continuous process, sulfamic acid and dichloromethane are continuously mixed and dissolved, then are continuously neutralized with triethylamine solution, a neutralization reaction liquid and diketene enter a continuous reactor, and a DKA reaction liquid is obtained through addition acylation reaction. The continuous mixing and dissolving are carried out according to the following proportion: n (sulfamic acid): n (dichloromethane) 1: 8; the temperature was 15 ℃. The continuous neutralization is carried out, wherein the pH value of the neutralization is 7-9; the triethylamine solution is a mixed solution of triethylamine and dichloromethane, and the proportion is n (triethylamine): n (dichloromethane) ═ 1: 2; the neutralization temperature was 20 ℃. The addition acylation reaction, the proportion n (sulfamic acid): n (diketene) ═ 1: 1; n (diketene): n (dichloromethane) ═ 1:1, acylation reaction temperature 25 ℃; acylation residence time 30 s; the continuous reactor is one or more of kettle type continuous, channel continuous and micro reactor. The DKA reaction yield is 95-98% by weight of sulfamic acid.
Example 1:
5000g (DKA 3.26mol) of acetoacetamidosulfonic acid triethylamine salt (DKA) solution prepared continuously is added to prepare a DKA solution with a specific gravity of 1.24g/cm3The specific gravity of the cyclizing agent is 1.52g/cm3Then, the prepared raw materials are mixed according to the volume ratio of V (DKA solution): v (cyclizing agent): v (water) ═ 1: 1:0.5, respectively continuously entering the microreactor through an A, B, C interface of the microreactor with the ratio of the cyclization I area to the hydrolysis II area being 1:1, wherein in the cyclization I area of the microreactor, a mixing section accounts for 20 percent of the cyclization I area, and the microreactor is subjected to full mixing reaction through a mixing section with a Y-shaped structure (material: Hastelloy) and a reaction section with a snake-shaped structure (material: Hastelloy), wherein the reaction temperature is 25 ℃, the pressure is 5MPA, and the retention time is 10min, the cyclization reaction liquid and water continuously entering a C interface are in a hydrolysis II area of a micro reactor, the mixing section accounts for 50% of the hydrolysis II area, the reaction temperature is 35 ℃, the pressure is 6MPA, the residence time is 1min after the full mixing reaction of the mixing section with a core type (material: zirconium) structure and the reaction section with an M type (material: zirconium) structure, the reaction liquid of the acesulfame is obtained, the reaction liquid is subjected to continuous extraction, continuous neutralization, continuous concentration and continuous drying to obtain 527.3g of acesulfame potassium, the yield is 80.4%, and the content is 99.2%.
Example 2:
5000g (DKA 3.26mol) of acetoacetamidosulfonic acid triethylamine salt (DKA) solution prepared continuously was added to prepare a DKA solution having a specific gravity of 1.28g/cm3The specific gravity of the cyclizing agent is 1.6g/cm3Then, the prepared raw materials are mixed according to the volume ratio of V (DKA solution): v (cyclizing agent): v (water) ═ 1: 0.8: 0.9, respectively continuously entering the microreactor through an A, B, C interface of the microreactor with the ratio of a cyclization I area to a hydrolysis II area being 1:1.2, wherein a mixing section of the microreactor in the cyclization I area accounts for 50% of the cyclization I area, the microreactor is subjected to a sufficient mixing reaction through a mixing section with a T-shaped structure (material: glass) and a reaction section with a straight structure (material: glass) at a reaction temperature of 30 ℃, a pressure of 1.5MPA and a residence time of 20S, a cyclization reaction liquid and water continuously entering a C interface are subjected to a sufficient mixing reaction through a mixing section with a U-shaped structure (material: zirconium) and a reaction section with a scaled structure (material: silicon carbide) in the hydrolysis II area of the microreactor at a reaction temperature of 30 ℃, a pressure of 2.0MPA and a residence time of 2min to obtain an acetyl sulfanilic acid reaction liquid, and the acetyl sulfanilic acid reaction liquid is subjected to a continuous extraction, Continuous neutralization, continuous concentration and continuous drying are carried out to obtain 547.6g of acesulfame potassium, the yield is 83.5 percent, and the content is 99.1 percent.
Example 3:
5000g (DKA 3.26mol) of acetoacetamidosulfonic acid triethylamine salt (DKA) solution prepared continuously is added to prepare a DKA solution with a specific gravity of 1.30g/cm3The specific gravity of the cyclizing agent is 1.45g/cm3Then, the prepared raw materials are mixed according to the volume ratio of V (DKA solution): v (cyclizing agent): v (water) ═ 1: 1.5: 1.2 by cyclizing the I-zone with water, respectivelyThe A, B, C interface of the micro-reactor with the proportion of the solution II zone being 1:2 continuously enters the micro-reactor, the mixing section of the micro-reactor accounts for 70 percent of the cyclization I zone in the cyclization I zone of the micro-reactor, the solution is subjected to the full mixing reaction of the mixing section with the structure of a heart type (material: stainless steel) and the reaction section with the structure of a zoom type (material: stainless steel), the reaction temperature is 28 ℃, the pressure is 1.2MPA, the residence time is 10S, the cyclization reaction solution and the water continuously entering the interface C, the mixing section of the hydrolysis II zone of the micro-reactor accounts for 60 percent of the hydrolysis II zone, the solution is subjected to the full mixing reaction of the mixing section with the structure of a Y type (material: silicon carbide) and the reaction section with the structure of a straight type (material: silicon carbide), the reaction temperature is 25 ℃, the pressure is 1.4MPA, the residence time is 5min, the acetyl sulfanilic acid reaction solution is obtained, and the reaction solution is subjected to, The continuous drying is carried out to obtain 543.1g of acesulfame potassium, the yield is 82.8 percent, and the content is 99.4 percent.
Example 4:
5000g (DKA 3.26mol) of acetoacetamidosulfonic acid triethylamine salt (DKA) solution prepared continuously was added to prepare a DKA solution having a specific gravity of 1.26g/cm3The specific gravity of the cyclizing agent is 1.48g/cm3Then, the prepared raw materials are mixed according to the volume ratio of V (DKA solution): v (cyclizing agent): v (water) ═ 1: 1.3: 1.8, continuously feeding the mixture into a microreactor through an A, B, C interface of the microreactor with the ratio of a cyclization I area to a hydrolysis II area being 1:2.5, wherein the mixing section accounts for 5% of the cyclization I area in the cyclization I area of the microreactor, the mixture is subjected to a sufficient mixing reaction of a mixing section with a U-shaped structure (material: silicon carbide) and a reaction section with an M-shaped structure (material: silicon carbide) at a reaction temperature of 35 ℃, a pressure of 2.2MPA and a residence time of 0.02S, the cyclization reaction liquid is continuously fed with water through a C interface, the mixture is subjected to a sufficient mixing reaction of a mixing section with a T-shaped structure (material: stainless steel) and a reaction section with a snake-shaped structure (material: stainless steel) at a reaction temperature of 40 ℃, a pressure of 2.5MPA and a residence time of 15min in the hydrolysis II area of the microreactor to obtain an acetyl sulfanilic acid reaction liquid, and the acetyl sulfanilic acid reaction liquid is continuously extracted and hydrolyzed, Continuous neutralization, continuous concentration and continuous drying are carried out to obtain 558.8g of acesulfame potassium, the yield is 85.2 percent, and the content is 99.3 percent.
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 method for continuously preparing acesulfame potassium through a microchannel reactor is characterized by comprising the following steps:
the method comprises the steps of enabling the acetoacetamidosulfonic triethylamine salt solution and a cyclizing agent to continuously enter a microreactor through an A, B interface of the microreactor, enabling the solution and the cyclizing agent to be subjected to full reaction in a mixing section and a reaction section, enabling the solution and water continuously entering from an interface C to be subjected to full mixing reaction in the mixing section and the reaction section in the same reactor, obtaining a reaction solution of the acesulfame from an outlet D, and performing separation processes such as continuous extraction, continuous neutralization, continuous concentration and continuous drying to obtain the acesulfame potassium.
2. The method for continuously preparing acesulfame potassium through the microchannel reactor as claimed in claim 1, wherein the cyclizing agent is SO3Mixing with dichloromethane, and preparing; the DKA reaction liquid, the cyclizing agent and water are fed in a volume ratio vDKA reaction liquid：vCyclizing reagent：vWater (W)＝1:0.2～3:0.3～3。
3. The method for continuously preparing acesulfame potassium through the microchannel reactor as claimed in claim 1, wherein the specific gravity of the DKA reaction solution is 1.19-1.32 g/cm3The specific gravity of the cyclizing agent is 1.4-1.9 g/cm3(ii) a The viscosity of the DKA reaction liquid is 5-30 cp, and the viscosity of the cyclizing agent is 5-25 cp.
4. The method for continuously preparing the acesulfame potassium through the microchannel reactor according to claim 1, wherein the cyclization reaction temperature is 25-100 ℃; the reaction pressure is 0-10 MPa; the hydrolysis reaction temperature is 25-100 ℃, and the reaction pressure is 0-10 MPa.
5. The method for continuously preparing the acesulfame potassium through the microchannel reactor according to claim 1, wherein the cyclization residence time is 0.01S-30 min; the hydrolysis retention time is 0.01S-30 min.
6. The method for continuously preparing the acesulfame potassium through the microchannel reactor according to claim 1, wherein the microreactor comprises a cyclization I zone, a hydrolysis II zone and a heat exchange zone; the cyclization I area consists of a mixing section and a reaction section, and the hydrolysis II area consists of a mixing section and a reaction section; the structure of the mixed section of the cyclization I area or the mixed section of the hydrolysis II area is composed of one or more of a heart type, a Y type, a U type and a T type, and the structure of the reaction section of the cyclization I area or the reaction section of the hydrolysis II area is composed of one or more of a snake shape, a zoom type, an M type and a straight type.
7. The method for continuously preparing the acesulfame potassium through the microchannel reactor as claimed in claim 6, wherein the ratio of the cyclization I area and the hydrolysis II area of the microreactor is 1: 0.5-10; the proportion of the mixing section in the cyclization I area to the internal channel of the area is 1-100%; the proportion of the reaction section occupying the internal channel of the zone is 0-99 percent; the proportion of the mixing section in the hydrolysis II area in the internal channel of the area is 1 to 100 percent; the proportion of the reaction section occupying the internal channel of the zone is 0-99%.
8. The method for continuously preparing acesulfame potassium through the microchannel reactor according to claim 1, wherein the size of the reaction channel of the microreactor is 10-1000 μm.
9. The method for continuously preparing acesulfame potassium through the microchannel reactor according to claim 1, wherein the microreactor is made of: one or more of silicon carbide, hastelloy, zirconium, tantalum, stainless steel and glass.
10. A system for continuously preparing acesulfame potassium through a microchannel reactor is characterized by comprising an acylation reactor, a microreactor, an extraction tower, a neutralization tower, a concentration device and a dryer which are sequentially connected through pipelines; the microreactor comprises a cyclization I area, a hydrolysis II area and a heat exchange area; the cyclization I area consists of a mixing section and a reaction section, and the hydrolysis II area consists of a mixing section and a reaction section;
the structure of the mixed section of the cyclization I area or the mixed section of the hydrolysis II area is composed of one or more of a heart type, a Y type, a U type and a T type, and the structure of the reaction section of the cyclization I area or the reaction section of the hydrolysis II area is composed of one or more of a snake shape, a zoom type, an M type and a straight type.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN113454056A (en) * | 2021-05-28 | 2021-09-28 | 安徽金禾实业股份有限公司 | Preparation method of acetoacetamide-N-sulfonic acid triethylamine salt |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN113454056A (en) * | 2021-05-28 | 2021-09-28 | 安徽金禾实业股份有限公司 | Preparation method of acetoacetamide-N-sulfonic acid triethylamine salt |
| CN113454056B (en) * | 2021-05-28 | 2022-11-04 | 安徽金禾实业股份有限公司 | Preparation method of acetoacetamide-N-sulfonic acid triethylamine salt |
| 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 |
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