CN210279110U - Micro-reaction equipment - Google Patents
Micro-reaction equipment Download PDFInfo
- Publication number
- CN210279110U CN210279110U CN201920809324.8U CN201920809324U CN210279110U CN 210279110 U CN210279110 U CN 210279110U CN 201920809324 U CN201920809324 U CN 201920809324U CN 210279110 U CN210279110 U CN 210279110U
- Authority
- CN
- China
- Prior art keywords
- tank
- reaction
- micro
- fixed bed
- bed catalytic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses a micro-reaction device, which at least comprises a device unit, wherein the device unit comprises a feeding tank I, a feeding tank II, a fixed bed catalytic micro-reaction tank I, a fixed bed catalytic micro-reaction tank II, a constant flow pump I, a constant flow pump II, a cooling tank, a receiving tank and a gas heating tank; an inlet of the constant flow pump I is connected with the feeding tank I, and an outlet of the constant flow pump I is connected with an inlet of the fixed bed catalytic micro-reaction tank I, so that the constant flow pump I pumps the materials in the feeding tank I into the fixed bed catalytic micro-reaction tank I; and a product outlet of the fixed bed catalytic micro-reaction tank I is connected with an inlet of the feeding tank II. It the utility model has the advantages of simple structure, no amplification effect, operating condition easily control and inherent safety, the little chemical industry process that uses little response device to go on has and replaces intermittent type process with continuous process, and the process is reinforceed, and the security improves, and product property changes, advantages such as distributed production.
Description
Technical Field
The utility model relates to a little response device belongs to chemical industry technical field.
Background
Currently, benzocaine, known by the chemical name ethyl p-aminobenzoate, has the structural formula:
ethyl p-aminobenzoate is known As Benzocaine (ABEE). Colorless rhombohedral crystal, odorless and tasteless. Molecular weight 165.19. The melting point is 91-92 ℃. Is easily soluble in alcohol, ether and chloroform. Can be dissolved in oleum Armeniacae amarum, oleum Olivarum, and dilute acid. Is poorly soluble in water. It is clinically used for relieving pain and itching of wound surfaces, ulcer surfaces, burns, skin chapping and hemorrhoids. Benzocaine is a fat-soluble surface anesthetic, and is less potent than other local anesthetics such as lidocaine and dibucaine, and therefore does not cause discomfort due to anesthetic action when applied to the mucosa. It is a drug with strong fat solubility, so it is easy to combine with the lipid layer of mucosa or skin, but not easy to permeate and generate toxicity in human body. The benzocaine can be used as a precursor raw material of the oxpocaine, the oxvacaine, the procaine and the like; meanwhile, the ointment is also used as a local anesthetic in medicine, has the effects of relieving pain and itching, is mainly used for anesthesia, pain and itching of wound surfaces, ulcer surfaces, mucosal surfaces and hemorrhoids, and can also be used for lubricating and relieving pain of nasopharynx catheters, endoscope and the like. Temporary relief of painful and itchy skin discomfort, minor burns, sunburn, wounds and insect bites. Otic preparations are used to relieve pain and itching associated with acute congestive, otitis externa, swimming, and for external application to the ear. It is also effective on toothache, sore throat, oral ulcer, various hemorrhoids, anal fissure, and pudendum itch, and can be used as male genital desensitizer to relieve ejaculation. Or as anesthetic lubricants for catheters and endoscopes. The topical application of benzocaine can block nerve impulse transmission, temporarily lose various senses, and paralyze sensory nerve endings to relieve pain and itching. The local anesthetic action of benzocaine is weaker than that of procaine, and the benzocaine can be slowly absorbed by external application, has lasting effect and has the effects of relieving pain and itching. The toxicity of benzocaine is only 1/20-1/160 of cocaine.
The ethyl p-nitrobenzoate is used as a raw material to produce benzocaine, has higher economic added value, and is a better way for deeply processing the benzocaine. Currently, the mainstream production method in industry is palladium-carbon hydrogenation catalytic reduction. Due to the characteristics of the batch type reaction kettle, the reaction speed is low, the yield is low, the danger is high, hydrogen is not easy to recover, and the cost is increased.
Disclosure of Invention
The utility model aims to solve the technical problem that overcome prior art's defect, provide a little response unit, it has simple structure, does not have advantages such as enlarged effect, operating condition easily control and inherent safety, and the little chemical process that uses little response unit to go on has and replaces intermittent type process with continuous process, and the process is reinforceed, and the security improves, and product property changes, advantages such as distributed production.
In order to solve the technical problem, the technical scheme of the utility model is that: a micro-reaction device at least comprises a device unit, wherein the device unit comprises a feeding tank I, a feeding tank II, a fixed bed catalytic micro-reaction tank I, a fixed bed catalytic micro-reaction tank II, a constant flow pump I, a constant flow pump II, a cooling tank, a receiving tank and a gas heating tank; wherein the content of the first and second substances,
an inlet of the constant flow pump I is connected with the feeding tank I, and an outlet of the constant flow pump I is connected with an inlet of the fixed bed catalytic micro-reaction tank I, so that the constant flow pump I pumps the materials in the feeding tank I into the fixed bed catalytic micro-reaction tank I;
a product outlet of the fixed bed catalytic micro-reaction tank I is connected with an inlet of the feeding tank II so that a product generated by the fixed bed catalytic micro-reaction tank I enters the feeding tank II;
an inlet of the constant flow pump II is connected with an outlet of the feeding tank II, and an outlet of the constant flow pump II is connected with a first inlet of the fixed bed catalytic micro-reaction tank II, so that the constant flow pump II pumps the material in the feeding tank II into the fixed bed catalytic micro-reaction tank II;
the inlet of the gas heating tank is used for supplying hydrogen and nitrogen or hydrogen, and the outlet of the gas heating tank is connected with the second inlet of the fixed bed catalytic micro-reaction tank II so as to at least introduce hydrogen into the fixed bed catalytic micro-reaction tank II;
an atomization nozzle which is connected with a first inlet and is used for atomizing the pumped materials and mixing the atomized materials with the introduced hydrogen is arranged in the fixed bed catalytic micro-reaction tank II;
and the inlet of the cooling tank is connected with the product outlet of the fixed bed catalytic micro-reaction tank II, and the outlet of the cooling tank is connected with the receiving tank.
The micro-reaction equipment also comprises a constant temperature heater, and the constant temperature heater is respectively connected with the jackets of the feeding tank I, the feeding tank II, the fixed bed catalytic micro-reaction tank I, the fixed bed catalytic micro-reaction tank II and the cooling tank.
Further, the aperture of the atomizing nozzle is 0.5 mm.
Further, the receiving tank is a feeding tank I of the next equipment unit.
Further, the outlet of the constant flow pump I is also connected with the inlet of the feeding tank I, so that the materials in the feeding tank I can be circulated through the constant flow pump I.
Further, the outlet of the constant flow pump II is connected with the inlet of the feeding tank II so as to circulate the materials in the feeding tank II through the constant flow pump II.
Furthermore, the inlet of the gas heating tank is connected with the hydrogen steel cylinder and the nitrogen steel cylinder or the hydrogen steel cylinder through the gas inlet valve group.
The utility model also provides a method for synthesizing benzocaine, which is carried out in the micro-reaction equipment.
Further, the method comprises the following steps:
putting a p-nitrobenzoic acid solution with ethanol as a solvent into a feeding tank I, pumping the p-nitrobenzoic acid solution in the feeding tank I into a fixed bed catalytic micro-reaction tank I through a constant flow pump I, and carrying out esterification reaction under the action of a catalyst in the fixed bed catalytic micro-reaction tank I to obtain a p-nitrobenzoic acid ethyl ester solution;
and (2) putting the ethyl p-nitrobenzoate solution into a feeding tank II, pumping the ethyl p-nitrobenzoate solution in the feeding tank II into a fixed bed catalytic micro-reaction tank II through a constant flow pump II, atomizing the ethyl p-nitrobenzoate solution through an atomizing nozzle, mixing the atomized ethyl p-nitrobenzoate solution with introduced hydrogen, carrying out hydrogenation reaction under the action of a catalyst in the fixed bed catalytic micro-reaction tank II, and then treating to obtain benzocaine.
Further, the temperature of a feeding tank I is 70 ℃, the temperature of a fixed bed catalytic micro-reaction tank I is 80-85 ℃, the reaction pressure is 0.4MPa, and the feeding flow is 5 ml/min;
further, the temperature of the feeding tank II is 70-80 ℃, the temperature of the fixed bed catalytic micro-reaction tank II is 140 ℃, the reaction pressure is 17-35 kg, and the feeding flow is 80-120 ml/min.
Further, the catalyst in the fixed bed catalytic micro-reaction tank I is a sulfonic acid resin catalyst;
and/or the catalyst in the fixed bed catalytic micro reaction tank II is a palladium carbon catalyst or a platinum aluminum catalyst.
Further, before the benzocaine is synthesized by using the micro-reaction equipment, the constant flow pump I and the constant flow pump II are calibrated by using absolute ethyl alcohol.
After the technical scheme is adopted, the utility model discloses the raw materials that use in the method are liquid or for the solid matter that can dissolve in the raw materials, and the result of formation also is liquid, is fit for being used for the utility model discloses a little response device.
The utility model discloses a little response device has the advantage that the process is reinforceed, and in the esterification reaction's that goes on in fixed bed catalysis micro-reaction jar I in-process, it is fully mixed in the very short time with sulfonic acid type resin catalyst to be to nitrobenzoic acid, and guaranteed the timely transmission of reaction heat, prevented that traditional technology from because of the emergence of the polymerization side reaction that reaction time overlength, mixed effect are limited and heat transfer rate slow to lead to, reduced product impurity content, improved the conversion rate of product; in the hydrogenation reaction carried out in the fixed bed catalytic micro-reaction tank II, because of the three-phase reaction, the atomizing nozzle can quickly and uniformly mix hydrogen and liquid, thereby greatly improving the mixing effect, completing the reaction in a short time, and avoiding the side reactions such as hydrolysis, polymerization and the like of the product caused by prolonging the reaction time of the product in a conventional reaction system due to nonuniform stirring. The advantages of stirring and mixing and system heat transfer in the conventional reaction are avoided, so that the synthesis efficiency is greatly improved, and the method is suitable for continuous synthesis.
Therefore, the utility model has the following advantages;
the micro-reaction equipment of the utility model, materials are pumped in through the constant flow pump, which ensures the accuracy of material measurement and convenient and safe operation; the transportation and transfer of the materials in the reaction system are in a closed state, so that the reaction operation is safe and environment-friendly; and related process parameters can be adjusted on line in real time, and can be visually displayed, so that the control of the synthesis process is facilitated.
The micro-reaction equipment of the utility model is applied to the synthesis of benzocaine, and the conversion rate of raw materials and the purity of the product benzocaine in the two-step reaction are higher than those of the traditional process; the synthesis process is continuously operated, the reaction time and energy consumption are saved, and the reaction process is simple and convenient to amplify; conventional chemical reaction equipment such as a reaction kettle, a condenser and the like is not needed, and the equipment investment and maintenance cost is low; the raw materials are directly pumped by the constant flow pump, so that the feeding link is facilitated, and the operation safety is enhanced; the process conditions are easy to control, and can be adjusted on line at any time according to needs.
Drawings
Fig. 1 is a schematic structural diagram of a micro-reaction device of the present invention.
Detailed Description
The utility model provides a little reaction equipment and use its synthetic benzocaine's method, and the technical staff in the field can refer to this text content, suitably improves the technological parameter and realizes. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the scope of the invention. While the methods and applications of the present invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the art that variations and modifications may be made in the methods and applications described herein without departing from the spirit and scope of the invention.
As shown in fig. 1, a micro-reaction apparatus is composed of at least one apparatus unit including a feed tank I1, a feed tank II2, a fixed-bed catalytic micro-reaction tank I3, a fixed-bed catalytic micro-reaction tank II4, a constant flow pump I5, a constant flow pump II6, a cooling tank 7, a receiving tank 8, and the gas heating tank 9; wherein the content of the first and second substances,
the inlet of the constant flow pump I5 is connected with the feed tank I1, and the outlet of the constant flow pump I5 is connected with the inlet of the fixed bed catalytic micro-reaction tank I3, so that the constant flow pump I5 pumps the material in the feed tank I1 into the fixed bed catalytic micro-reaction tank I3;
the product outlet of the fixed bed catalytic micro reaction tank I3 is connected with the inlet of the feed tank II2, so that the product generated by the fixed bed catalytic micro reaction tank I3 enters the feed tank II 2;
an inlet of the constant flow pump II6 is connected with an outlet of the feeding tank II2, and an outlet of the constant flow pump II6 is connected with a first inlet of the fixed bed catalytic micro-reaction tank II4, so that the constant flow pump II6 pumps the materials in the feeding tank II2 into the fixed bed catalytic micro-reaction tank II 4;
the inlet of the gas heating tank 9 is used for supplying hydrogen and nitrogen or hydrogen, and the outlet of the gas heating tank 9 is connected with the second inlet of the fixed bed catalytic micro-reaction tank II4 so as to at least introduce hydrogen into the fixed bed catalytic micro-reaction tank II 4;
an atomization nozzle which is connected with a first inlet and is used for atomizing the pumped materials and mixing the atomized materials with the introduced hydrogen is arranged in the fixed bed catalytic micro-reaction tank II 4;
the inlet of the cooling tank 7 is connected with the product outlet of the fixed bed catalytic micro-reaction tank II4, and the outlet of the cooling tank 7 is connected with the receiving tank 8.
Specifically, the fixed bed catalytic micro-reaction tank I3 and the fixed bed catalytic micro-reaction tank II4 are both fixed bed catalytic reactors.
Specifically, the micro-reaction equipment further comprises a constant temperature heater which is respectively connected with the jackets of the feeding tank I1, the feeding tank II2, the fixed bed catalytic micro-reaction tank I3, the fixed bed catalytic micro-reaction tank II4 and the cooling tank 7.
The fixed-bed catalytic micro-reaction tank II4 had a channel diameter of 5cm and a length of 30cm to 50cm, but is not limited thereto.
The aperture of the atomizing nozzle may be 0.5mm, but is not limited thereto.
The receiving tank 8 is the feed tank I1 of the next said equipment unit.
As shown in fig. 1, the outlet of the constant flow pump I5 is also connected to the inlet of the feed tank I1 to circulate the material in the feed tank I1 through the constant flow pump I5.
As shown in fig. 1, the outlet of the constant flow pump II6 is also connected to the inlet of the feed tank II2 to circulate the material in the feed tank II2 via the constant flow pump II 6.
As shown in fig. 1, the inlet of the gas heating tank 9 is connected with a hydrogen cylinder and a nitrogen cylinder or connected with a hydrogen cylinder through a gas inlet valve group. Wherein, whether the inlet of the gas heating tank 9 is filled with hydrogen, nitrogen or hydrogen and nitrogen can be selected by operating the gas inlet valve group.
The utility model also provides a method for synthesizing benzocaine, which is carried out in the micro-reaction equipment.
The reaction formula for the synthesis of benzocaine is as follows:
specifically, the steps of the method include:
putting a p-nitrobenzoic acid solution with ethanol as a solvent into a feeding tank I1, pumping the p-nitrobenzoic acid solution in a feeding tank I1 into a fixed bed catalytic micro-reaction tank I3 through a constant flow pump I5, and carrying out esterification reaction under the action of a catalyst in a fixed bed catalytic micro-reaction tank I3 to obtain a p-nitrobenzoic acid ethyl ester solution;
putting the ethyl p-nitrobenzoate solution into a feeding tank II2, pumping the ethyl p-nitrobenzoate solution in the feeding tank II2 into a fixed bed catalytic micro-reaction tank II4 through a constant flow pump II6, atomizing the ethyl p-nitrobenzoate solution through an atomizing nozzle, mixing the atomized ethyl p-nitrobenzoate solution with introduced hydrogen, carrying out hydrogenation reaction under the action of a catalyst in the fixed bed catalytic micro-reaction tank II4, and then treating to obtain benzocaine.
The utility model discloses in, the back is specifically do through handling: cleaning, decoloring, crystallizing and drying.
The temperature of the feeding tank I1 is 70 ℃, the temperature of the fixed bed catalytic micro reaction tank I3 is 80-85 ℃, the reaction pressure is 0.4MPa, and the feeding flow is 5 ml/min; these parameters are defined primarily to allow better completion of the esterification reaction and to increase the conversion.
The temperature of the feeding tank II2 is 70-80 ℃, the temperature of the fixed bed catalytic micro-reaction tank II4 is 140 ℃, the reaction pressure is 17-35 kg, and the feeding flow is 80-120 ml/min; these parameters are defined primarily to allow better completion of the hydrogenation reaction and to increase its conversion.
Specifically, the catalyst in the fixed bed catalytic micro-reaction tank I3 is a sulfonic acid resin catalyst;
and the catalyst in the fixed bed catalytic micro reaction tank II4 is a palladium carbon catalyst or a platinum aluminum catalyst.
Before the synthesis of benzocaine using the microreaction device, the constant flow pump I5 and the constant flow pump II6 were calibrated using absolute ethanol.
The utility model discloses a little response device has the advantage that the process is reinforceed, in the esterification reaction's that goes on in fixed bed catalysis micro-reaction jar I3 in-process, is that p-nitrobenzoic acid fully mixes with sulfonic acid type resin catalyst in the very short time to guaranteed the timely transmission of reaction heat, prevented that traditional technology from because of the emergence of the polymerization side reaction that reaction time overlength, mixed effect are limited and heat transfer rate slow to lead to, reduced product impurity content, improved the conversion rate of product; in the hydrogenation reaction carried out in the fixed bed catalytic micro-reaction tank II4, because of the three-phase reaction, the atomizing nozzle can quickly and uniformly mix hydrogen and liquid, thereby greatly improving the mixing effect, completing the reaction in a short time, and avoiding the side reactions such as hydrolysis, polymerization and the like of the product caused by prolonging the reaction time of the product in a conventional reaction system due to nonuniform stirring. The advantages of stirring and mixing and system heat transfer in the conventional reaction are avoided, so that the synthesis efficiency is greatly improved, and the method is suitable for continuous synthesis.
The micro-reaction equipment of the utility model, materials are pumped in through the constant flow pump, which ensures the accuracy of material measurement and convenient and safe operation; the transportation and transfer of the materials in the reaction system are in a closed state, so that the reaction operation is safe and environment-friendly; and related process parameters can be adjusted on line in real time, and can be visually displayed, so that the control of the synthesis process is facilitated.
The micro-reaction equipment of the utility model is applied to the synthesis of benzocaine, and the conversion rate of raw materials and the purity of the product benzocaine in the two-step reaction are higher than those of the traditional process; the synthesis process is continuously operated, the reaction time and energy consumption are saved, and the reaction process is simple and convenient to amplify; conventional chemical reaction equipment such as a reaction kettle, a condenser and the like is not needed, and the equipment investment and maintenance cost is low; the raw materials are directly pumped by the constant flow pump, so that the feeding link is facilitated, and the operation safety is enhanced; the process conditions are easy to control, and can be adjusted on line at any time according to needs.
In order that the present invention may be more readily and clearly understood, the following detailed description of the present invention is provided in connection with the accompanying drawings.
Example 1:
22.4g of p-nitrobenzoic acid is dissolved in an ethanol solution (the mass percent of ethanol is 99.9 percent) to prepare a 4 percent p-nitrobenzoic acid solution, and the p-nitrobenzoic acid solution is put into a feeding tank I1 of a micro-reaction device for circulation. Sulfonic acid resin catalyst is filled in a fixed bed catalytic micro reaction tank I3, palladium carbon catalyst or platinum aluminum catalyst is filled in a fixed bed catalytic micro reaction tank II4, the temperature of a feeding tank I1 of micro reaction equipment is set to be 70 ℃, the temperature of a fixed bed catalytic micro reaction tank I3 is set to be 80 ℃, the reaction pressure is 0.4MPa, and the flow is 5 ml/min. And opening a constant flow pump I5, pumping the solution into a fixed bed catalytic micro-reaction tank I3, then carrying out esterification reaction, and receiving the reaction product in a feeding tank II. Then replacing the fixed bed catalytic micro-reaction tank II4 with nitrogen and hydrogen for three times, setting the temperature of the feeding tank II to be 70 ℃, the temperature of the fixed bed catalytic micro-reaction tank II to be 140 ℃, the reaction pressure to be 35 kg and the flow to be 80 ml/min; and the cooling tank is at-5 ℃, pumping the liquid received in the feeding tank II into a fixed bed catalytic micro-reaction tank II through a constant flow pump II6, introducing hydrogen for reaction, and receiving. In the continuous reaction, three product samples and one mixed sample are taken and detected by high performance liquid chromatography, and the conversion rate of the reaction is 97.46 percent.
Example 2:
22.4g of p-nitrobenzoic acid is dissolved in an ethanol solution (the mass percent of ethanol is 99.9 percent) to prepare a 4 percent p-nitrobenzoic acid solution, and the p-nitrobenzoic acid solution is put into a feeding tank I1 of a micro-reaction device for circulation. Sulfonic acid resin catalyst is filled in a fixed bed catalytic micro reaction tank I3, palladium carbon catalyst or platinum aluminum catalyst is filled in a fixed bed catalytic micro reaction tank II, the temperature of a feeding tank I1 of micro reaction equipment is set to be 70 ℃, the temperature of a fixed bed catalytic micro reaction tank I3 is set to be 80 ℃, the reaction pressure is 0.4MPa, and the flow is 5 ml/min. And opening a constant flow pump I5, pumping the solution into a fixed bed catalytic micro-reaction tank I3, then carrying out esterification reaction, and receiving the reaction product in a feeding tank II. Then replacing the fixed bed catalytic micro-reaction tank II4 with nitrogen and hydrogen for three times, setting the temperature of the feeding tank II to be 70 ℃, the temperature of the fixed bed catalytic micro-reaction tank II to be 140 ℃, the reaction pressure to be 17 kg and the flow to be 80 ml/min; and the cooling tank is at-5 ℃, liquid received in the feeding tank II is pumped into a fixed bed catalytic micro reaction tank II4 through a constant flow pump II6, and hydrogen is introduced for reaction and receiving. In the continuous reaction, three product samples and one mixed sample are taken and detected by high performance liquid chromatography, and the conversion rate of the reaction is 96.53 percent.
Example 3:
22.4g of p-nitrobenzoic acid is dissolved in an ethanol solution (the mass percent of ethanol is 99.9 percent) to prepare a 4 percent p-nitrobenzoic acid solution, and the p-nitrobenzoic acid solution is put into a feeding tank I1 of a micro-reaction device for circulation. Sulfonic acid resin catalyst is filled in a fixed bed catalytic micro reaction tank I3, palladium carbon catalyst or platinum aluminum catalyst is filled in a fixed bed catalytic micro reaction tank II4, the temperature of a feeding tank I of the micro reaction equipment is set to be 70 ℃, the temperature of the fixed bed catalytic micro reaction tank I is set to be 80 ℃, the reaction pressure is set to be 0.4MPa, and the flow is 5 ml/min. And opening a constant flow pump I5, pumping the solution into a fixed bed catalytic micro-reaction tank I3, then carrying out esterification reaction, and receiving the reaction product in a feeding tank II. Then replacing the fixed bed catalytic micro-reaction tank II4 with nitrogen and hydrogen for three times, setting the temperature of the feeding tank II to be 70 ℃, the temperature of the fixed bed catalytic micro-reaction tank II to be 140 ℃, the reaction pressure to be 35 kg and the flow to be 120 ml/min; and the cooling tank is at-5 ℃, the liquid received in the feeding tank II is pumped into a fixed bed catalytic micro reaction tank II4, and hydrogen is introduced for reaction and receiving. In the continuous reaction, three product samples and one mixed sample are taken and detected by high performance liquid chromatography, and the conversion rate of the reaction is 91.86%.
The micro-reaction apparatus used in the above examples was purchased from Rixi Ribes Biotech Co., Ltd, and the analytical grade of ethanol was purchased from Yongfeng Chemicals Co., Ltd, Jiangsu.
The above-mentioned embodiments further explain in detail the technical problems, technical solutions and advantages solved by the present invention, and it should be understood that the above only is a specific embodiment of the present invention, and is not intended to limit the present invention, and any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
In the description of the present invention, it is to be understood that the terms indicating orientation or positional relationship are based on the orientation or positional relationship shown in the drawings, and are only for convenience of description and simplification of description, and do not indicate or imply that the equipment or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," and "fixed" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate the position or positional relationship based on the position or positional relationship shown in the drawings, or the position or positional relationship which is usually placed when the product of the present invention is used, and are only for convenience of description and simplification of the description, but do not indicate or imply that the device or element referred to must have a specific position, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
Furthermore, the terms "horizontal", "vertical", "overhang" and the like do not imply that the components are required to be absolutely horizontal or overhang, but may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the present disclosure, unless otherwise expressly stated or limited, the first feature may comprise both the first and second features directly contacting each other, and also may comprise the first and second features not being directly contacting each other but being in contact with each other by means of further features between them. Also, the first feature being above, on or above the second feature includes the first feature being directly above and obliquely above the second feature, or merely means that the first feature is at a higher level than the second feature. A first feature that underlies, and underlies a second feature includes a first feature that is directly under and obliquely under a second feature, or simply means that the first feature is at a lesser level than the second feature.
Claims (7)
1. A micro-reaction device at least comprises a device unit, and is characterized in that the device unit comprises a feeding tank I (1), a feeding tank II (2), a fixed bed catalytic micro-reaction tank I (3), a fixed bed catalytic micro-reaction tank II (4), a constant flow pump I (5), a constant flow pump II (6), a cooling tank (7), a receiving tank (8) and a gas heating tank (9); wherein the content of the first and second substances,
an inlet of the constant flow pump I (5) is connected with the feeding tank I (1), and an outlet of the constant flow pump I (5) is connected with an inlet of the fixed bed catalytic micro-reaction tank I (3), so that the constant flow pump I (5) pumps the materials in the feeding tank I (1) into the fixed bed catalytic micro-reaction tank I (3);
the product outlet of the fixed bed catalytic micro-reaction tank I (3) is connected with the inlet of the feeding tank II (2) so that the product generated by the fixed bed catalytic micro-reaction tank I (3) enters the feeding tank II (2);
an inlet of the constant flow pump II (6) is connected with an outlet of the feeding tank II (2), and an outlet of the constant flow pump II (6) is connected with a first inlet of the fixed bed catalytic micro-reaction tank II (4), so that the constant flow pump II (6) pumps the material in the feeding tank II (2) into the fixed bed catalytic micro-reaction tank II (4);
the inlet of the gas heating tank (9) is used for supplying hydrogen and nitrogen or hydrogen, and the outlet of the gas heating tank (9) is connected with the second inlet of the fixed bed catalytic micro-reaction tank II (4) so as to at least introduce hydrogen into the fixed bed catalytic micro-reaction tank II (4);
an atomization nozzle which is connected with a first inlet and is used for atomizing the pumped materials and mixing the atomized materials with the introduced hydrogen is arranged in the fixed bed catalytic micro-reaction tank II (4);
the inlet of the cooling tank (7) is connected with the product outlet of the fixed bed catalytic micro-reaction tank II (4), and the outlet of the cooling tank (7) is connected with the receiving tank (8).
2. The micro-reaction device according to claim 1,
the device is characterized by further comprising a constant temperature heater, wherein the constant temperature heater is respectively connected with the jackets of the feeding tank I (1), the feeding tank II (2), the fixed bed catalytic micro-reaction tank I (3), the fixed bed catalytic micro-reaction tank II (4) and the cooling tank (7).
3. The micro-reaction device according to claim 1,
the aperture of the atomizing nozzle is 0.5 mm.
4. The micro-reaction device according to claim 1,
the receiving tank (8) is the feed tank I (1) of the next plant unit.
5. The micro-reaction device according to claim 1,
the outlet of the constant flow pump I (5) is also connected with the inlet of the feeding tank I (1) so as to circulate the materials in the feeding tank I (1) through the constant flow pump I (5).
6. The micro-reaction device according to claim 1,
and the outlet of the constant flow pump II (6) is also connected with the inlet of the feeding tank II (2) so as to circulate the materials in the feeding tank II (2) through the constant flow pump II (6).
7. The micro-reaction device according to claim 1,
and the inlet of the gas heating tank (9) is connected with the hydrogen steel cylinder and the nitrogen steel cylinder or the hydrogen steel cylinder through a gas inlet valve group.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920809324.8U CN210279110U (en) | 2019-05-31 | 2019-05-31 | Micro-reaction equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920809324.8U CN210279110U (en) | 2019-05-31 | 2019-05-31 | Micro-reaction equipment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN210279110U true CN210279110U (en) | 2020-04-10 |
Family
ID=70071769
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201920809324.8U Active CN210279110U (en) | 2019-05-31 | 2019-05-31 | Micro-reaction equipment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN210279110U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075773A (en) * | 2019-05-31 | 2019-08-02 | 常州瑞曦生物科技有限公司 | The method of its synthesis benzocainum of micro-reactor apparatus and application |
-
2019
- 2019-05-31 CN CN201920809324.8U patent/CN210279110U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075773A (en) * | 2019-05-31 | 2019-08-02 | 常州瑞曦生物科技有限公司 | The method of its synthesis benzocainum of micro-reactor apparatus and application |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN210279110U (en) | Micro-reaction equipment | |
| CN108017575B (en) | Method for synthesizing crizotinib intermediate by using microchannel reactor | |
| US8653296B2 (en) | Method for preparing ester of cyclohexane polycarboxylic acid from ester of benzene polycarboxylic acid | |
| CN102617744B (en) | Preparation method of narrow-distribution medium-molecular-weight hydroxyethyl starch | |
| CN109125252A (en) | A kind of preparation method of alkannin liposome gel | |
| CN102558267A (en) | Preparation method of testosterone enanthate | |
| CN111732522A (en) | Preparation method of doxycycline | |
| CN101693694B (en) | Preparation method of glyoxaline formic ether and derivative thereof | |
| CN103159599A (en) | Synthesis process of gingerol derivative | |
| CN110075773A (en) | The method of its synthesis benzocainum of micro-reactor apparatus and application | |
| CN107501108B (en) | 4-aminobenzoic acid ethyl ester raw powder's production technology | |
| CN110511117B (en) | Method for synthesizing 4-n-butylresorcinol by microchannel reaction | |
| CN104478972B (en) | Method for preparing troxerutin by adopting self-suction type stirred autoclave | |
| CN104231272A (en) | Industrialized preparation method of medicinal dimethyl silicone oil | |
| CN1434026A (en) | Process for prepraring p-acetpamidophenol | |
| CN107115831A (en) | A kind of preparation method of microreactor and dihydrostreptomycin sulfate based on microreactor | |
| CN107573385B (en) | Oxaliplatin impurity C and preparation method and application thereof | |
| CN113042040B (en) | Method for preparing tranexamic acid by using platinum-carbon catalyst | |
| CN109280015A (en) | A kind of synthesis of D-VB5 sodium and chiral separation method | |
| CN110698333B (en) | Method for continuously synthesizing o-phthalaldehyde by using microchannel reaction device | |
| CN110156618A (en) | A kind of preparation process of ethylaminobenzoate | |
| CN103772241B (en) | A kind of preparation method of sulfonated dehydro sylvate | |
| CN106167465B (en) | A kind of Edaravone dimer impurity compound and preparation method thereof | |
| CN105949127B (en) | A kind of method of purification of imidazophenylurea | |
| CN1076725C (en) | Process for preparing sodium lactate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |