CN111377885B - Method for cyclization and hydrolysis in continuous production of acesulfame potassium - Google Patents
Method for cyclization and hydrolysis in continuous production of acesulfame potassium Download PDFInfo
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Abstract
The invention discloses a cyclization and hydrolysis method in continuous production of acesulfame potassium, which comprises cyclization and hydrolysis, wherein a microreactor is adopted for reaction, and the microreactor comprises a cyclization section and a hydrolysis section; the cyclization section comprises a cyclization mixing section and a cyclization reaction section; the hydrolysis section comprises a hydrolysis mixing section and a hydrolysis reaction section; the peripheries of the cyclization mixing section, the cyclization reaction section, the hydrolysis mixing section and the hydrolysis reaction section are heat exchange areas; the DKA solution and the cyclizing agent continuously enter a cyclization section of the microreactor through an A, B interface of the microreactor, and after full reaction of a cyclization mixing section and a cyclization reaction section, the DKA solution and the cyclizing agent are subjected to full mixing reaction with water continuously entering from a C interface in the same reactor through a hydrolysis mixing section and a hydrolysis reaction section, and then the acetyl sulfanilic acid reaction liquid is obtained from an outlet D and enters a post-treatment process. According to the invention, ASH is continuously prepared through the microchannel reactor, continuous preparation of AK sugar is realized, the yield of the intermediate is stable and high, and the energy consumption is reduced by 60% compared with that of an intermittent kettle type reaction.
Description
Technical Field
The invention relates to the field of synthesis of acesulfame potassium, and particularly relates to a method for continuously producing acesulfame potassium.
Background
Acetyl sulfanilic acid
The name of English: acesufame
Appearance properties: colorless or white needle-like crystals
Solubility: is easily soluble in water and slightly soluble in ethanol
The molecular formula is as follows: C4H5NO4S
Molecular weight: 163
Action and use: acesulfame is a precursor for the preparation of acesulfame which has a very wide range of uses 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/l 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 preparation method for synthesizing potassium acetylsulfonate is mainly a ketene dimer-sulfur trioxide method, the main step of the method influencing yield is cyclization-hydrolysis, and because the heat release amount 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, the hydrolysis operation condition is not easy to control, the yield is only 69% [1], and the kettle type intermittent process has the biggest defects of low yield, high energy consumption and generation of a large amount of three wastes. The synthesis mode of the process directly results in no space for further improvement of the yield, and the process 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 method solves the problems that the cyclization intermediate is unstable before hydrolysis and the acetylsulfanilic Acid (ASH) intermediate is easy to decompose at high temperature after hydrolysis, and the yield of cyclization and hydrolysis reaction reaches 90-95 percent.
Principle of ASH decomposition:
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) Chenguanghong, coke phoenix army, a method for synthesizing AK sugar precursor ASH in a microchannel reactor [ P ]. Liaoning: CN107868064A, 2016-09-23.
The method discloses a method for continuously preparing an ASH precursor through a microchannel reactor, wherein cyclization and hydrolysis are carried out in two microchannel reactors until the total yield of AK sugar is 50-70%.
The cyclization hydrolysis of the process is carried out separately, and the cyclization intermediate has long retention time and is unstable, so that the overall yield is reduced.
Disclosure of Invention
Therefore, 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 the cyclization and hydrolysis method in the continuous production of the acesulfame potassium, which has simple process, less side reaction and stable process.
The technical scheme of the invention is that the cyclization and hydrolysis method in the continuous production of acesulfame potassium comprises the steps of:
adopting a microreactor for reaction, wherein the microreactor comprises a cyclization section and a hydrolysis section; the cyclization section comprises a cyclization mixing section and a cyclization reaction section; the hydrolysis section comprises a hydrolysis mixing section and a hydrolysis reaction section; the peripheries of the cyclization mixing section, the cyclization reaction section, the hydrolysis mixing section and the hydrolysis reaction section are heat exchange areas;
the DKA solution and the cyclizing agent continuously enter a cyclization section of the microreactor through an A, B interface of the microreactor, and after full reaction of a cyclization mixing section and a cyclization reaction section, the DKA solution and the cyclizing agent are subjected to full mixing reaction with water continuously entering from a C interface in the same reactor through a hydrolysis mixing section and a hydrolysis reaction section, and then the acetyl sulfanilic acid reaction liquid is obtained from an outlet D and enters a post-treatment process;
the feeding ratio of the DKA reaction liquid to the cyclizing agent to water is 1: 0.2-3: 0.3-3;
the specific gravity of the DKA reaction liquid is 1.19-1.32 g/cm3, and the specific gravity of the cyclizing agent is 1.4-1.9 g/cm 3; the viscosity of the DKA reaction liquid is 5-30 cp, and the viscosity of the cyclizing agent is 5-25 cp;
the cyclization reaction temperature is 25-100 ℃, and the reaction pressure is 0-10 MPa;
the hydrolysis reaction temperature is 25-100 ℃, and the reaction pressure is 0-10 MPa;
the cyclization residence time is 0.01S-30 min, and the hydrolysis residence time is 0.01S-30 min.
The specific gravity of the reaction liquid in the process is in a linear relation with the concentration, and the specific gravity corresponds to a corresponding concentration range.
According to the method for continuously producing the acesulfame potassium, which is disclosed by the invention, in the method for continuously producing the acesulfame potassium, the cyclization and hydrolysis reaction yield is preferably 90-95% in terms of DKA.
According to the method for cyclization and hydrolysis in continuous production of acesulfame potassium, the post-treatment process is preferably continuous extraction, continuous neutralization, continuous concentration and continuous drying separation.
According to the method for cyclization and hydrolysis in continuous production of potassium acetylsulfanilate, the feeding ratio of the DKA reaction liquid, the cyclizing agent and water is preferably 1: 0.8-1.5: 0.5-1.8;
preferably, the specific gravity of the DKA reaction liquid is 1.24-1.30 g/cm3, and the specific gravity of the cyclizing agent is 1.45-1.6 g/cm 3;
preferably, the cyclization reaction temperature is 25-40 ℃; the reaction pressure is 0.5-5 MPa;
preferably, the hydrolysis reaction temperature is 25-40 ℃; the reaction pressure is 0.5-5 MPa;
preferably, the cyclization residence time is 0.01S-10 min; the hydrolysis retention time is 0.01S-15 min.
In the microreactor, the ratio of the cyclization I area to the hydrolysis II area of the microreactor is preferably 1: 0.5-10, and more preferably the ratio of the cyclization I area to the hydrolysis II area is 1: 1-5.
Preferably, the proportion of the mixing section in the cyclization I area in 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%. More preferably, the proportion of the reaction zone in the internal channels of the zone is between 1% and 99%.
According to the method for cyclization and hydrolysis in continuous production of acesulfame potassium, the structure of the cyclization mixed section is preferably selected from one or more of heart type, Y type, U type and T type; the hydrolysis mixing section structure is selected from one or more of a heart type, a Y type, a U type and a T type.
Furthermore, the heart-shaped channel is a heart-shaped channel with the upper end and the lower end of the heart-shaped channel communicated with each other through pipelines, and the heart-shaped part is provided with a blocking component; for example, the heart-shaped part is provided with a blocking part such as a crescent. The degree of mixing uniformity of the fluid within the channel can be increased. Furthermore, the heart shape is formed by connecting a plurality of heart shapes in series in the figure. The blocking component is shown in the central type of fig. 2, and the arc-shaped and dot-shaded parts play a blocking role, so that the uniform mixing degree of the fluid in the channel can be increased.
Further, in the Y-shaped channel, the opening of Y is 10-170 degrees; further, the lower Y is in communication with a channel of other shape. The other shape may be one of a parallelogram, a circle, a rectangle, or a triangle. Preferably a parallelogram channel connection (see figure 2Y). The connection of Y to other shaped channels is to increase the degree of mixing of the fluid within the channels.
Further, the U-shaped channel is communicated with the channels with other shapes through a U shape; the U-shaped channel is communicated with the channels with other shapes through a U-shaped channel. Still further, the other shape may be one of a circle, a parallelogram, a rectangle, or a triangle. From a hydrodynamic point of view, the connection of U to the next approximately circular channel is to increase the degree of mixing of the fluid inside the channel (see figure 2U). Other shapes may be used.
Further, the lower part of the T-shaped channel is communicated with a channel with other shape. The lower part of the T-shaped channel is communicated with a channel with other shapes. Still further, the other shape may be one of a circle, a parallelogram, a rectangle, or a triangle. From a hydrodynamic perspective, T is connected to the lower rectangular channel to increase the mixing uniformity of the fluid within the channel (see figure 2T). Other shapes may be used.
According to the method for cyclization and hydrolysis in continuous production of acesulfame potassium, the structure of the cyclization reaction section is preferably selected from one or more of snake-shaped, zoom-type, M-type and straight-type; the structure of the hydrolysis reaction section is selected from one or more of serpentine, scaled, M-shaped and straight. See fig. 3.
Scaled refers to alternating channel sizes.
According to the method for cyclization and hydrolysis in continuous production of acesulfame potassium, the size of a reaction channel of the microreactor is preferably 10-1000 μm.
Furthermore, the size of the reaction channel of the microreactor is 100-500 mu m.
According to the method for cyclization and hydrolysis in continuous production of acesulfame potassium, the microreactor is preferably made of a material selected from the group consisting of: one or more of silicon carbide, hastelloy, zirconium, tantalum, stainless steel and glass.
The invention has the beneficial effects that:
by adopting the technology, ASH is continuously prepared through the microchannel reactor, AK sugar is continuously prepared, the yield of the intermediate is stable, the yield is higher than that of the conventional batch kettle type process and reaches 90-95% (the yield of the conventional batch kettle type process is about 71%), and compared with the production energy consumption, the energy consumption of the process is reduced by 60% compared with that of the batch kettle type process, so that the energy-saving and consumption-reducing environmental protection requirements are met.
Drawings
FIG. 1 is a schematic diagram of a microreactor configuration.
FIG. 2 is a schematic diagram of several configurations of a mixing section of a microreactor.
FIG. 3 is a schematic diagram of several structures of a micro-reaction section.
FIG. 4 is a schematic diagram of a cyclized hydrolysis process.
In fig. 1, a: DKA reaction solution, B: cyclizing agent, C: process water, D: acetyl sulfanilic acid reaction solution, E: cyclizing mixed section, F: cyclization reaction section, G: hydrolysis mixing section, H: hydrolysis reaction section, zone I: ring-closing section, zone II: the hydrolysis section and the shaded area in the figure are heat exchange areas.
Detailed Description
Example 1:
the basic process flow is shown in FIG. 4. Taking 5000g (DKA3.26mol) of acetoacetamidosulfonic acid triethylamine salt (DKA) solution, preparing the solution into DKA solution with the specific gravity of 1.24g/cm3, and cyclizing agent with the specific gravity of 1.52g/cm3, wherein the volume ratio of the solution V (DKA solution) to the solution V (cyclizing agent) to the solution V (water) is 1: 0.5, continuously entering the solution into a microreactor (shown in figure 1) through a A, B, C interface of the microreactor respectively, in a cyclization section of the microreactor, fully mixing and reacting a mixing section with a Y-type structure (material: Hastelloy) and a reaction section with a snake-type structure (material: Hastelloy) at the reaction temperature of 25 ℃, the pressure of 5MPA and the residence time of 10min, in a hydrolysis section of the microreactor, fully mixing and reacting a mixing section with a heart-type structure (material: zirconium) and a M-type structure (material: zirconium), the reaction temperature was 35 ℃, the pressure was 6MPA, and the residence time was 1min, whereby 491.5g of acesulfame was obtained by analysis, and the yield was 92.5%.
Example 2:
taking 5000g (DKA3.26mol) of acetoacetamidosulfonic acid triethylamine salt (DKA) solution, preparing the solution into DKA solution with the specific gravity of 1.28g/cm3, mixing the solution with cyclizing agent with the specific gravity of 1.6g/cm3 according to the volume ratio of V (DKA solution) to V (cyclizing agent) to V (water) of 1: 0.8: 0.9, continuously entering the solution into a microreactor through a A, B, C interface of the microreactor respectively, fully mixing and reacting a mixing section with a T-shaped (material: glass) structure and a reaction section with a straight (material: glass) structure in the cyclizing section of the microreactor, wherein the reaction temperature is 30 ℃, the pressure is 1.5MPA, the residence time is 20S, the cyclizing reaction liquid and the water continuously entering a C interface are fully mixed and reacted through a mixing section with a U-shaped (material: zirconium) structure and a scaled (material: silicon carbide) structure in the hydrolyzing section of the microreactor, the reaction temperature is 30 ℃, the pressure was 2.0MPA, the residence time was 2min, and the reaction mixture was analyzed to obtain 486.7g of acesulfame, with a yield of 91.6%.
Example 3:
taking 5000g (DKA3.26mol) of acetoacetamidosulfonic acid triethylamine salt (DKA) solution, preparing the solution into DKA solution with the specific gravity of 1.30g/cm3, and cyclizing agent with the specific gravity of 1.45g/cm3, then continuously feeding the prepared raw materials into a microreactor through A, B, C interfaces of the microreactor according to the volume ratio of V (DKA solution) to V (cyclizing agent) to V (water) of 1: 1.5: 1.2, fully mixing and reacting in a cyclization section of the microreactor through a mixing section with a heart-shaped structure (material: stainless steel) and a reaction section with a scaling-shaped structure (material: stainless steel), wherein the reaction temperature is 28 ℃, the pressure is 1.2MPA, the residence time is 10S, the cyclization reaction liquid and the water continuously fed in a C interface are subjected to full mixing reaction in a hydrolysis section of the microreactor through a mixing section with a Y-shaped structure (material: silicon carbide) and a reaction section with a straight-shaped structure (material: silicon carbide), the reaction temperature was 25 ℃, the pressure was 1.4MPA, and the residence time was 5min, to obtain the reaction solution of acesulfame, which was analyzed to obtain 495.2g of acesulfame with a yield of 93.2%.
Example 4:
taking 5000g (DKA3.26mol) of acetoacetamidosulfonic acid triethylamine salt (DKA) solution, preparing the solution into DKA solution with the specific gravity of 1.26g/cm3 and cyclizing agent with the specific gravity of 1.48g/cm3, and mixing the solution according to the volume ratio of V (DKA solution): v (cyclizing agent) and V (water) are 1: 1.3: 1.8, respectively, continuously enter the microreactor through A, B, C interfaces of the microreactor, and are subjected to a sufficient mixing reaction through a mixing section with a U-shaped structure (material: silicon carbide) and a reaction section with an M-shaped structure (material: silicon carbide) in a cyclization section of the microreactor, wherein the reaction temperature is 35 ℃, the pressure is 2.2MPA, the residence time is 0.02S, and the cyclization reaction liquid and the water continuously enter the C interface, and are subjected to a sufficient mixing reaction through a mixing section with a T-shaped structure (material: stainless steel) and a reaction section with a snake shape (material: stainless steel) in a hydrolysis section of the microreactor, wherein the reaction temperature is 40 ℃, the pressure is 2.5MPA, and the residence time is 15min, so that the reaction liquid of the acetyl sulfanilic acid is obtained, and the analysis shows that the acetyl sulfanilic acid is 503.2g, and the yield is 94.7%.
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.
The invention discloses a method for cyclization and hydrolysis in continuous production of acesulfame potassium, which comprises the steps of completing continuous cyclization and hydrolysis processes by a DKA solution, a cyclizing agent and water in the same microreactor, regulating the ratio 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, reducing side reactions by utilizing internal strong heat exchange, and ensuring that the yield of cyclization and hydrolysis reaction reaches 90-95%.
Claims (10)
1. A method for cyclization and hydrolysis in continuous production of acesulfame potassium, comprising cyclization and hydrolysis, characterized in that: the method comprises the following steps:
adopting a microreactor for reaction, wherein the microreactor comprises a cyclization section and a hydrolysis section; the cyclization section comprises a cyclization mixing section and a cyclization reaction section; the hydrolysis section comprises a hydrolysis mixing section and a hydrolysis reaction section; the peripheries of the cyclization mixing section, the cyclization reaction section, the hydrolysis mixing section and the hydrolysis reaction section are heat exchange areas;
the DKA solution and the cyclizing agent continuously enter a cyclization section of the microreactor through an A, B interface of the microreactor, and after full reaction of a cyclization mixing section and a cyclization reaction section, the DKA solution and the cyclizing agent are subjected to full mixing reaction with water continuously entering from a C interface in the same reactor through a hydrolysis mixing section and a hydrolysis reaction section, and then the acetyl sulfanilic acid reaction liquid is obtained from an outlet D and enters a post-treatment process;
the feeding ratio of the DKA reaction liquid to the cyclizing agent to water is 1: 0.2-3: 0.3-3;
the specific gravity of the DKA reaction liquid is 1.19-1.32 g/cm3, and the specific gravity of the cyclizing agent is 1.4-1.9 g/cm 3; the viscosity of the DKA reaction liquid is 5-30 cp, and the viscosity of the cyclizing agent is 5-25 cp;
the cyclization reaction temperature is 25-100 ℃, and the reaction pressure is 0-10 MPa;
the hydrolysis reaction temperature is 25-100 ℃, and the reaction pressure is 0-10 MPa;
the cyclization residence time is 0.01S-30 min, and the hydrolysis residence time is 0.01S-30 min.
2. The process of claim 1 for the cyclization and hydrolysis in the continuous production of acesulfame potassium, characterized in that: the reaction yield of cyclization and hydrolysis is 90-95% in terms of DKA.
3. The process of claim 1 for the cyclization and hydrolysis in the continuous production of acesulfame potassium, characterized in that: the post-treatment process comprises continuous extraction, continuous neutralization, continuous concentration and continuous drying and separation.
4. The process of claim 1 for the cyclization and hydrolysis in the continuous production of acesulfame potassium, characterized in that: the feeding ratio of the DKA reaction liquid to the cyclizing agent to water is 1: 0.8-1.5: 0.5-1.8;
the specific gravity of the DKA reaction liquid is 1.24-1.30 g/cm3, and the specific gravity of the cyclizing agent is 1.45-1.6 g/cm 3;
the cyclization reaction temperature is 25-40 ℃; the reaction pressure is 0.5-5 MPa;
the hydrolysis reaction temperature is 25-40 ℃; the reaction pressure is 0.5-5 MPa;
the cyclization residence time is 0.01S-10 min; the hydrolysis retention time is 0.01S-15 min.
5. The process of claim 1 for the cyclization and hydrolysis in the continuous production of acesulfame potassium, characterized in that: the ring-closure mixed section structure is selected from one or more of heart type, Y type, U type and T type; the hydrolysis mixing section structure is selected from one or more of a heart type, a Y type, a U type and a T type.
6. The process of claim 5 for the cyclization and hydrolysis in the continuous production of acesulfame potassium, wherein: the heart-shaped channel is a heart-shaped channel with the upper end and the lower end of the heart-shaped channel communicated with each other through pipelines, and the heart-shaped part is provided with a blocking component;
in the Y-shaped channel, the opening of the Y is 10-170 degrees;
the U-shaped channel is communicated with the channels with other shapes through a U-shaped channel;
the lower part of the T-shaped channel is communicated with a channel with other shapes.
7. The process of claim 1 for the cyclization and hydrolysis in the continuous production of acesulfame potassium, characterized in that: the structure of the cyclization reaction section is selected from one or more of snake shape, zoom type, M type and straight type; the structure of the hydrolysis reaction section is selected from one or more of serpentine, scaled, M-shaped and straight.
8. The process of claim 1 for the cyclization and hydrolysis in the continuous production of acesulfame potassium, characterized in that: the size of a reaction channel of the microreactor is 10-1000 mu m.
9. The process of claim 1 for the cyclization and hydrolysis in the continuous production of acesulfame potassium, characterized in that: the size of the reaction channel of the microreactor is 100-500 mu m.
10. The process of claim 1 for the cyclization and hydrolysis in the continuous production of acesulfame potassium, characterized in that: the material of the micro-reactor is selected from: one or more of silicon carbide, hastelloy, zirconium, tantalum, stainless steel and glass.
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| CN107868064A (en) * | 2016-09-23 | 2018-04-03 | 中国科学院大连化学物理研究所 | A kind of method that 3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt precursor ASH is synthesized in micro passage reaction |
| CN108191790A (en) * | 2018-01-13 | 2018-06-22 | 安徽金禾实业股份有限公司 | Sulfonation microchannel plate induction method and device in a kind of acesulfame potassium production |
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| CN107868064A (en) * | 2016-09-23 | 2018-04-03 | 中国科学院大连化学物理研究所 | A kind of method that 3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt precursor ASH is synthesized in micro passage reaction |
| CN108191790A (en) * | 2018-01-13 | 2018-06-22 | 安徽金禾实业股份有限公司 | Sulfonation microchannel plate induction method and device in a kind of acesulfame potassium production |
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