CN212595732U - A multistage pipeline reactor for synthesizing triethyl citrate - Google Patents
A multistage pipeline reactor for synthesizing triethyl citrate Download PDFInfo
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Abstract
The utility model discloses a multistage pipeline reactor for synthesizing triethyl citrate, including the pipeline reactor of establishing ties more than the two-stage that dissolves the cauldron, connect with the cauldron discharge gate, the ethanol evaporator and the blender that are located between the adjacent two-stage pipeline reactor, the ethanol concentration tower of being connected with each ethanol evaporator gas outlet, the condenser of being connected with ethanol concentration tower gas outlet, the ethanol storage tank of being connected with the condenser discharge gate, pan feeding mouth intercommunication No. one of ethanol storage tank discharge gate and each blender. The utility model discloses in utilize the multistage pipeline reactor can realize serialization production, enable the fine mixture of the fluid that gets into the pipeline, and have fine heat transfer characteristic. Not only can realize the continuity of the reaction process, but also can carry out good material mixing and heat exchange processes, and can independently control the mixing ratio and the temperature of the materials in each stage of pipeline reactor.
Description
Technical Field
The utility model relates to a triethyl citrate reactor field especially relates to a multistage pipeline reactor for synthesizing triethyl citrate and a method thereof.
Background
The citrate ester product is a nontoxic green environment-friendly plasticizer which is internationally acknowledged at present, is widely applied to food packaging materials, medical supplies, cosmetics, toys and the like, and has the advantages of good compatibility with resin, no toxicity, easy biodegradation and the like.
Triethyl citrate is an important product, is mainly used as an auxiliary agent of an adhesive and a sealant, and is widely used in medical appliances.
In the prior art (application publication No. CN 105837438A), the most common method for preparing triethyl citrate is to use citric acid and absolute ethyl alcohol as raw materials and concentrated sulfuric acid as a catalyst, during the esterification reaction, the generated water and ethanol are removed by azeotropy, and the absolute ethyl alcohol is continuously added into the system while distilling off the light ethyl alcohol, so as to promote the forward progress of the esterification reaction.
Traditional esterification method adopts reation kettle to operate, because can only single batch reaction, can not realize serialization production, and reation kettle volume generally is 0.5 m to 20m thin year fruit year, and reation kettle's size directly determines output. The investment is greatly increased along with the increase of the volume of the tank reactor.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a multistage pipeline reactor for synthesizing triethyl citrate.
The utility model discloses an innovation point lies in the utility model discloses in utilize synthetic triethyl citrate of multistage pipeline reactor can realize serialization production, the inside structure that adopts many pipeline end to end of every grade pipeline reactor enables the fine mixture of the fluid that gets into the pipeline, and has fine heat transfer characteristic. The method not only can realize the continuity of the reaction process, but also can perform good material mixing and heat exchange processes, and can independently control the mixing ratio and the temperature of the materials in each stage of pipeline reactor, so that compared with the finished products produced by a common reaction kettle, the method has the advantages of good color, high utilization rate of raw materials, short reaction time, low energy consumption and the like. Compared with a kettle type reactor, the pipeline reactor has the advantages of small equipment volume, small occupied area, good safety, small material retention, small equipment investment, and along with the expansion of production scale, the production cost and energy consumption are saved by a lot compared with the traditional kettle type reaction process.
In order to realize the purpose of the utility model, the technical proposal of the utility model is that:
a multi-stage pipeline reactor for synthesizing triethyl citrate comprises a dissolving kettle, more than two stages of pipeline reactors connected in series with a discharge port of the dissolving kettle, an ethanol evaporator and a mixer which are positioned between two adjacent stages of pipeline reactors, an ethanol concentration tower connected with an air outlet of each ethanol evaporator, a condenser connected with an air outlet of the ethanol concentration tower, and an ethanol storage tank connected with a discharge port of the condenser, wherein a discharge port of the ethanol storage tank is communicated with a first feeding port of each mixer; the pipeline reactor comprises a heat exchange tank body and a reaction pipeline positioned in the heat exchange tank body, wherein two ends of the reaction pipeline extend out of the heat exchange tank body, two ends of the reaction pipeline are respectively a material inlet and a material outlet, and a steam inlet and a steam outlet are also formed in the heat exchange tank body; the material outlet of the upper stage pipeline reactor is connected with the material inlet of the ethanol evaporator between two adjacent pipeline reactors, the material outlet of the ethanol evaporator is connected with the material inlet of the mixer II, and the material outlet of the mixer is connected with the material inlet of the lower stage pipeline reactor.
Further, the mixer is a static mixer.
Furthermore, the reaction pipeline comprises a plurality of straight pipes arranged in parallel and bent pipes for communicating the straight pipes end to end, a material inlet and a material outlet of the reaction pipeline are respectively positioned at two ends of the heat exchange tank body, a steam outlet and a steam inlet are respectively positioned at two ends of the heat exchange tank body, the steam inlet is positioned at the material outlet, and the steam outlet is positioned at the material inlet; the material inlet and the steam outlet are located at the lower end of the heat exchange tank body, and the material outlet and the steam inlet are located at the upper end of the heat exchange tank body.
Further, the pipeline reactor has 4-5 grades.
Further, a temperature sensor is arranged in the pipeline reactor. The temperature signal is fed back to the steam heating system by monitoring the change of the temperature of the materials in the pipeline so as to adjust the reaction temperature.
Furthermore, a flow meter is arranged on a pipeline communicated with the discharge port of the ethanol storage tank and the feeding port of each mixer. Used for adjusting the mass ratio of the concentrated ethanol and the ester liquid in each pipeline reactor.
The utility model has the advantages that:
1. the utility model discloses in utilize synthetic triethyl citrate of multistage pipeline reactor can realize serialization production, the inside structure that adopts many pipeline end to end of every grade pipeline reactor enables the fine mixture of the fluid that gets into the pipeline, and has fine heat transfer characteristic. The method not only can realize the continuity of the reaction process, but also can perform good material mixing and heat exchange processes, and can independently control the mixing ratio and the temperature of the materials in each stage of pipeline reactor, so that compared with the finished products produced by a common reaction kettle, the method has the advantages of good color, high utilization rate of raw materials, short reaction time, low energy consumption and the like. Compared with a kettle type reactor, the pipeline reactor has the advantages of small equipment volume, small occupied area, good safety, small material retention, small equipment investment, and along with the expansion of production scale, the production cost and energy consumption are saved by a lot compared with the traditional kettle type reaction process.
Drawings
Fig. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic diagram of a pipeline reactor.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings.
Example 1: as shown in fig. 1 and 2, the multi-stage pipeline reactor for synthesizing triethyl citrate comprises a dissolving kettle 1, more than two stages of pipeline reactors 2 connected with a discharge port 1.1 of the dissolving kettle in series, an ethanol evaporator 3 and a mixer 4 positioned between the adjacent two stages of pipeline reactors, an ethanol concentration tower 5 connected with an air outlet 3.3 of each ethanol evaporator, a condenser 6 connected with an air outlet 5.1 of the ethanol concentration tower, and an ethanol storage tank 7 connected with a discharge port 6.1 of the condenser, wherein the mixer 4 is a static mixer. A discharge port 7.1 of the ethanol storage tank is communicated with a feeding port 4.1 of each mixer, and a flow meter 8 is arranged on a pipeline communicated with the discharge port 7.1 of the ethanol storage tank and the feeding port 4.1 of each mixer; the pipeline reactor 2 has 4-5 grades, and a temperature sensor is arranged in the pipeline reactor 2; the pipeline reactor 2 comprises a heat exchange tank body 2.1 and a reaction pipeline 2.2 positioned in the heat exchange tank body 2.1, two ends of the reaction pipeline 2.2 extend out of the heat exchange tank body 2.1, two ends are respectively a material inlet 2.3 and a material outlet 2.4, and the heat exchange tank body 2.1 is also provided with a steam inlet 2.5 and a steam outlet 2.6; the reaction pipeline 2.2 comprises a plurality of straight pipes 2.2.1 arranged in parallel and bent pipes 2.2.2 for communicating the straight pipes 2.2.1 end to end, a material inlet 2.3 and a material outlet 2.4 of the reaction pipeline 2.2 are respectively positioned at two ends of the heat exchange tank body 2.1, a steam outlet 2.5 and a steam inlet 2.6 are also respectively positioned at two ends of the heat exchange tank body 2.1, the steam inlet 2.6 is positioned at the material outlet 2.4, and the steam outlet 2.5 is positioned at the material inlet 2.3; the material inlet 2.3 and the steam outlet 2.5 are positioned at the lower end of the heat exchange tank body 2.1, and the material outlet 2.4 and the steam inlet 2.6 are positioned at the upper end of the heat exchange tank body 2.1. The material outlet 2.4 of the upper stage pipeline reactor 2 between the two adjacent pipeline reactors 2 is connected with the material inlet 3.1 of the ethanol evaporator, the material outlet 3.2 of the ethanol evaporator is connected with the material inlet 4.2 of the mixer II, and the material outlet 4.3 of the mixer is connected with the material inlet 2.3 of the lower stage pipeline reactor 2.
Example 2: a method for synthesizing triethyl citrate by using a multistage pipeline reactor comprises the following steps: taking materials, wherein the materials comprise ethanol, citric acid and a catalyst, the mass ratio of the ethanol to the citric acid is 1.3:1, the catalyst is toluenesulfonic acid, and the mass of the catalyst is 0.2% of the mass of the materials; preheating the material in a dissolving kettle 1 to 65 ℃, pumping the material into a first-stage pipeline reactor 2, wherein the flow rate during pumping is 1.5L/min, and controlling the temperature of the first-stage pipeline reactor 2 to be 95 ℃; the material of the first stage pipeline reactor 2 sequentially passes through a second stage pipeline reactor 2, a third stage pipeline reactor 2, a fourth stage pipeline reactor 2 and a fifth stage pipeline reactor 2, the material discharged from each stage pipeline reactor 2 firstly enters an ethanol evaporator 3, the ethanol obtained at the upper part of the ethanol evaporator 3 enters an ethanol concentration tower 5 for concentration and evaporation, then enters an ethanol storage tank 7 after being condensed by a condenser 6, the concentrated ethanol sent from the ethanol storage tank 7 and the material obtained at the lower part of the ethanol evaporator 3 enter a mixer 4 for mixing and then enter the next stage pipeline reactor 2, the mass ratio of the concentrated ethanol and the ester liquid entering the second stage pipeline reactor 2 is controlled to be 0.8: 1 by a flowmeter 8, the mass ratio of the concentrated ethanol and the ester liquid entering the third stage pipeline reactor 2 is 0.75: 1, the mass ratio of the concentrated ethanol and the ester liquid entering the fourth stage pipeline reactor 2 is 0.7: 1, the mass ratio of the concentrated ethanol entering the fifth-stage pipeline reactor 2 to the ester liquid is 0.6: 1; controlling the temperature of the second-stage pipeline reactor 2 to be 105 ℃, the temperature of the third-stage pipeline reactor 2 to be 115 ℃, the temperature of the fourth-stage pipeline reactor 2 to be 125 ℃ and the temperature of the fifth-stage pipeline reactor 2 to be 133 ℃; discharging the materials from the first-stage pipeline reactor 2 to the fifth-stage pipeline reactor 2, wherein the total retention time is 4 h; and (3) performing post-treatment on the discharged material of the fifth-stage pipeline reactor 2 to obtain a finished product, wherein the post-treatment comprises dealcoholization, alkali washing, water washing, decoloration and dehydration. Discharging the material from the fifth-stage pipeline reactor 2 into a dealcoholization kettle, wherein the vacuum degree of the dealcoholization kettle is 5-10 kPa, the dealcoholization temperature is 100-110 ℃, and the dealcoholized ethanol can be used as a material of the dissolving kettle 1; the alkali washing adopts 6 percent sodium carbonate aqueous solution, the consumption is 400 kg/t product, the alkali washing temperature is 60 ℃, and the alkali washing time is 30 min; washing with 350-400 kg/t product at 60 ℃ for 30 min; and (3) feeding the material into a refining kettle, decoloring by adopting 0.1% of active carbon, performing dehydration at 120 ℃ and under the vacuum degree of 5-6 kPa, and finally filtering to obtain triethyl citrate with the finished product yield of 97%.
Parameters of the finished product are as follows:
| color and luster (platinum cobalt) | Content (%) | Moisture (%) | Acid value (mgKOH/g) | Relative density (25 ℃ C.) |
| 15# | 99.5 | 0.056 | 0.033 | 1.136 |
Example 3: a method for synthesizing triethyl citrate by using a multistage pipeline reactor comprises the following steps: taking materials, wherein the materials comprise ethanol, citric acid and a catalyst, the mass ratio of the ethanol to the citric acid is 1.4:1, the catalyst is sodium bisulfate, and the mass of the catalyst is 0.35% of the mass of the materials; preheating the material in a dissolving kettle 1 to 70 ℃, pumping the material into a first-stage pipeline reactor 2, wherein the flow rate during pumping is 1.8L/min, and controlling the temperature of the first-stage pipeline reactor 2 to be 96 ℃; the material of the first stage pipeline reactor 2 sequentially passes through a second stage pipeline reactor 2, a third stage pipeline reactor 2, a fourth stage pipeline reactor 2 and a fifth stage pipeline reactor 2, the material discharged from each stage pipeline reactor 2 firstly enters an ethanol evaporator 3, the ethanol obtained at the upper part of the ethanol evaporator 3 enters an ethanol concentration tower 5 for concentration and evaporation, then enters an ethanol storage tank 7 after being condensed by a condenser 6, the concentrated ethanol sent from the ethanol storage tank 7 and the material obtained at the lower part of the ethanol evaporator 3 enter a mixer 4 for mixing and then enter the next stage pipeline reactor 2, the mass ratio of the concentrated ethanol and the ester liquid entering the second stage pipeline reactor 2 is controlled to be 0.85: 1 by a flowmeter 8, the mass ratio of the concentrated ethanol and the ester liquid entering the third stage pipeline reactor 2 is 0.77: 1, the mass ratio of the concentrated ethanol and the ester liquid entering the fourth stage pipeline reactor 2 is 0.72: 1, the mass ratio of the concentrated ethanol entering the fifth-stage pipeline reactor 2 to the ester liquid is 0.65: 1; controlling the temperature of the second-stage pipeline reactor 2 to be 107 ℃, the temperature of the third-stage pipeline reactor 2 to be 116 ℃, the temperature of the fourth-stage pipeline reactor 2 to be 126 ℃ and the temperature of the fifth-stage pipeline reactor 2 to be 134 ℃; discharging the materials from the first-stage pipeline reactor 2 to the fifth-stage pipeline reactor 2, wherein the total retention time is 4.3 h; and (3) performing post-treatment on the discharged material of the fifth-stage pipeline reactor 2 to obtain a finished product, wherein the post-treatment comprises dealcoholization, alkali washing, water washing, decoloration and dehydration. The discharge flow of the fifth-stage pipeline reactor 2 is 90-110 kg/h, and the acid value of the esterification liquid is less than 1.0% (calculated by citric acid%).
Example 4: a method for synthesizing triethyl citrate by using a multistage pipeline reactor comprises the following steps: taking materials, wherein the materials comprise ethanol, citric acid and a catalyst, the mass ratio of the ethanol to the citric acid is 1.5:1, the catalyst is toluenesulfonic acid, and the mass of the catalyst is 0.5% of the mass of the materials; preheating the material in a dissolving kettle 1 to 75 ℃, pumping the material into a first-stage pipeline reactor 2, wherein the flow rate during pumping is 2L/min, and controlling the temperature of the first-stage pipeline reactor 2 to be 98 ℃; the material of the first stage pipeline reactor 2 sequentially passes through a second stage pipeline reactor 2, a third stage pipeline reactor 2, a fourth stage pipeline reactor 2 and a fifth stage pipeline reactor 2, the material discharged from each stage pipeline reactor 2 firstly enters an ethanol evaporator 3, the ethanol obtained at the upper part of the ethanol evaporator 3 enters an ethanol concentration tower 5 for concentration and evaporation, then enters an ethanol storage tank 7 after being condensed by a condenser 6, the concentrated ethanol sent from the ethanol storage tank 7 and the material obtained at the lower part of the ethanol evaporator 3 enter a mixer 4 for mixing and then enter the next stage pipeline reactor 2, the mass ratio of the concentrated ethanol and the ester liquid entering the second stage pipeline reactor 2 is controlled to be 0.9: 1 by a flowmeter 8, the mass ratio of the concentrated ethanol and the ester liquid entering the third stage pipeline reactor 2 is 0.8: 1, the mass ratio of the concentrated ethanol and the ester liquid entering the fourth stage pipeline reactor 2 is 0.75: 1, the mass ratio of the concentrated ethanol entering the fifth-stage pipeline reactor 2 to the ester liquid is 0.7: 1; controlling the temperature of the second-stage pipeline reactor 2 to be 108 ℃, the temperature of the third-stage pipeline reactor 2 to be 118 ℃, the temperature of the fourth-stage pipeline reactor 2 to be 128 ℃ and the temperature of the fifth-stage pipeline reactor 2 to be 135 ℃; discharging the materials from the first-stage pipeline reactor 2 to the fifth-stage pipeline reactor 2, wherein the total retention time is 4.5 h; and (3) performing post-treatment on the discharged material of the fifth-stage pipeline reactor 2 to obtain a finished product, wherein the post-treatment comprises dealcoholization, alkali washing, water washing, decoloration and dehydration.
The described embodiments are only some, but not all embodiments of the invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
Claims (6)
1. A multi-stage pipeline reactor for synthesizing triethyl citrate is characterized by comprising a dissolving kettle, more than two stages of pipeline reactors connected in series with a discharge port of the dissolving kettle, an ethanol evaporator and a mixer which are positioned between two adjacent stages of pipeline reactors, an ethanol concentration tower connected with an air outlet of each ethanol evaporator, a condenser connected with an air outlet of the ethanol concentration tower, and an ethanol storage tank connected with a discharge port of the condenser, wherein a discharge port of the ethanol storage tank is communicated with a feeding port I of each mixer; the pipeline reactor comprises a heat exchange tank body and a reaction pipeline positioned in the heat exchange tank body, wherein two ends of the reaction pipeline extend out of the heat exchange tank body, two ends of the reaction pipeline are respectively a material inlet and a material outlet, and a steam inlet and a steam outlet are also formed in the heat exchange tank body; the material outlet of the upper stage pipeline reactor is connected with the material inlet of the ethanol evaporator between two adjacent pipeline reactors, the material outlet of the ethanol evaporator is connected with the material inlet of the mixer II, and the material outlet of the mixer is connected with the material inlet of the lower stage pipeline reactor.
2. A multi-stage pipeline reactor for the synthesis of triethyl citrate according to claim 1 wherein the mixer is a static mixer.
3. The multi-stage pipeline reactor for synthesizing triethyl citrate according to claim 1, wherein the reaction pipeline comprises a plurality of straight pipes arranged in parallel and bent pipes for connecting the straight pipes end to end, a material inlet and a material outlet of the reaction pipeline are respectively positioned at two ends of the heat exchange tank body, a steam outlet and a steam inlet are respectively positioned at two ends of the heat exchange tank body, the steam inlet is positioned at the material outlet, and the steam outlet is positioned at the material inlet; the material inlet and the steam outlet are located at the lower end of the heat exchange tank body, and the material outlet and the steam inlet are located at the upper end of the heat exchange tank body.
4. The multi-stage pipeline reactor for synthesizing triethyl citrate according to claim 1 wherein the pipeline reactor has 4-5 stages.
5. The multi-stage pipeline reactor for synthesizing triethyl citrate of claim 1 wherein a temperature sensor is disposed within the pipeline reactor.
6. The multi-stage pipeline reactor for synthesizing triethyl citrate according to claim 1, wherein a flow meter is arranged on the pipeline communicating the outlet of the ethanol storage tank and the inlet of each mixer.
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| CN116393048A (en) * | 2023-06-07 | 2023-07-07 | 山东金城医药化工有限公司 | Continuous production system and production method of ethyl 4-chloro-2-methoxyiminoacetoacetate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116393048A (en) * | 2023-06-07 | 2023-07-07 | 山东金城医药化工有限公司 | Continuous production system and production method of ethyl 4-chloro-2-methoxyiminoacetoacetate |
| CN116393048B (en) * | 2023-06-07 | 2023-09-12 | 山东金城医药化工有限公司 | Continuous production system and production method of ethyl 4-chloro-2-methoxyiminoacetoacetate |
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