Chemical reaction equipment capable of realizing continuous production

Abstract

The utility model relates to chemical reaction equipment capable of realizing continuous production. The chemical reaction equipment comprises a double-layer kettle body, a kettle body upper cover, a filter component, a middle kettle body, a heating jacket and a vacuum pump, wherein the upper end and the lower end of the double-layer kettle body are open; an upper connecting disc is arranged at the lower end of the double-layer kettle body; the filtering assembly is installed on the lower connecting disc, a sealing ring is arranged on the face, making contact with the double-layer kettle body, of the filtering assembly, the lower connecting disc is fixedly connected with the upper connecting disc through a connecting piece and used for fixing the filtering assembly to the lower end of the double-layer kettle body, and a discharging opening is formed in the bottom of the filtering assembly; the middle kettle body is arranged in the heating sleeve, is connected with the discharge port through a first connecting pipe and is connected with the vacuum pump through a second connecting pipe, a second reflux condensation assembly is arranged on the middle kettle body, a discharge port is formed in the bottom of the middle kettle body, and valves are arranged on the first connecting pipe and the second connecting pipe. According to the equipment, the operations of chemical reaction, filtration, extraction and solvent recovery can be continuously completed in one device, the whole process is simple to operate, and the continuous production of daphnetin is realized.

Description

TECHNICAL FIELD

[0001] The utility model belongs to the field of chemical reaction equipment relates to a chemical reaction equipment that can realize the continuous production. BACKGROUND

[0002] Daphnetin as an important medicinal active ingredient, has extensive application value in the fields of anticancer, antibacterial, anti-inflammatory, etc. The traditional daphnetin synthesis process mainly relies on round bottom flask or general reaction kettle for production. These devices can meet the basic needs in small-scale laboratory synthesis. However, with the innovation of daphnetin production process, its synthesis process becomes more complex, involving multi-step reactions, including intermediate filtration, extraction and solvent recovery operations. In the existing production equipment, these operations usually need to transfer the reaction materials between different devices, not only the operation is complicated, but also it is easy to cause material loss and pollution, seriously affecting the production efficiency and product quality. For example, the synthesis process of daphnetin contains filtering, extraction, activated carbon decolorization and other steps, and the traditional equipment cannot realize the continuous and automation of these operations. In addition, the solvent recovery process is also relatively complex, which needs additional equipment support, further increasing the production cost and operation difficulty. Therefore, developing an integrated daphnetin production equipment, which can organically combine the reaction, filtration, extraction and solvent recovery operations, to realize continuous production, has important significance for improving the production efficiency of daphnetin, reducing the cost and improving the product quality.

[0003] Chinese patent CN 201470374 U discloses a "multifunctional reaction kettle device", which integrates reaction kettle, liquid separator, filter and distillation recovery device, can make chemical reaction, liquid separation, filtration and solvent distillation recovery operation in one device to complete continuously, reduce the factors affecting reaction quality in production process and the probability of environmental pollution. However, the device needs to rotate the reaction kettle during use, which has the defects of inconvenient operation, and is not suitable for continuous production of daphnetin. SUMMARY

[0004] In view of the above technical problems and shortcomings, the purpose of the utility model is to provide a chemical reaction equipment that can realize continuous production. The reaction equipment integrates self-designed double-layer kettle body, filter assembly, spherical glass kettle body and vacuum pump, which can make chemical reaction, filtration, extraction and solvent recovery operation in one device to complete continuously, the whole process is simple to operate, realizes the continuous production of daphnetin, reduces the intermediate material transfer, and reduces the loss and pollution risk.

[0005] To achieve the above purpose, the utility model adopts the following technical scheme:

[0006] The utility model provides a chemical reaction equipment of realizing continuous production, including the double -deck cauldron body of both ends being open, cauldron body upper cover, filter assembly, intermediate cauldron body, heating jacket, vacuum pump, wherein, the double -deck cauldron body's side wall is equipped with interlayer import in the position near the lower end, is equipped with interlayer export in the position near the upper end, and interlayer import, interlayer export communicate with the interlayer of double -deck cauldron body side wall, and the lower end of double -deck cauldron body is equipped with upper connecting disc;

[0007] Cauldron body upper cover is fixed on the upper end of double -deck cauldron body, and is equipped with solid feeding port, constant pressure hopper, stirring mechanism on cauldron body upper cover;

[0008] Filter assembly is installed on lower connecting disc, and the periphery of the surface of filter assembly and double -deck cauldron body is equipped with sealing ring, and lower connecting disc is fixedly connected with upper connecting disc through connecting piece, is used for fixing filter assembly on the lower end of double -deck cauldron body, and the bottom of filter assembly is equipped with discharge port, and is equipped with lower discharge valve on discharge port;

[0009] Intermediate cauldron body is arranged in heating jacket, and the first connector of intermediate cauldron body is connected with discharge port through first connecting pipe, and the second connector is connected with vacuum pump through second connecting pipe, and intermediate cauldron body is equipped with second reflux condensing assembly on, and is equipped with discharge port on the bottom, and is equipped with discharge valve on discharge port, and is equipped with valve on first connecting pipe, second connecting pipe.

[0010] As the preferred of the utility model, the filter assembly is PTFE filter assembly, including filter disc, PTFE filter core, pressure ring, wherein, the filter disc is installed on lower connecting disc, and the surface of filter disc and double -deck cauldron body is equipped with sealing ring installation groove along the periphery, the sealing ring is arranged in sealing ring installation groove, and the filter disc is equipped with filter core installation groove, the filter core installation groove is communicated with the discharge port of filter disc bottom, the PTFE filter core is arranged in filter core installation groove, and the pressure ring is arranged in filter core installation groove and is pressed on PTFE filter core.

[0011] As the preferred of the utility model, the stirring mechanism includes stirring motor, and the stirring paddle is connected with stirring motor, and the stirring motor is controlled by frequency conversion controller to rotate, and the stirring paddle extends into the inside of double -deck cauldron body and is used for stirring during reaction.

[0012] As the preferred of the utility model, the cauldron body upper cover is also equipped with thermometer sleeve, cock, first reflux condensing assembly, wherein, the thermometer sleeve is equipped with thermometer, and the thermometer extends into the inside of double -deck cauldron body and is used for monitoring reaction temperature.

[0013] As the preferred of the utility model, the intermediate cauldron body is spherical glass cauldron body, the vacuum pump is circulating water type vacuum pump, and the heating jacket is electric heating jacket.

[0014] As the preferred of the utility model, the chemical reaction equipment further includes a support, the double-layer kettle body, the heating jacket, the stirring mechanism, the first reflux condensing component and the second reflux condensing component are fixed on the support, and the bottom of the support is provided with universal wheels.

[0015] As the preferred of the utility model, the first reflux condensing component includes a first reflux head, a first condenser and a first air suction head, the first reflux head is connected to the kettle body upper cover through a first elbow pipe and communicates with the inside of the double-layer kettle body, the first condenser is arranged on the first reflux head, and the first air suction head is arranged on the first condenser.

[0016] As the preferred of the utility model, the chemical reaction equipment is used for continuous production of daphnetin.

[0017] The utility model has the advantages and beneficial effects that:

[0018] (1) the chemical reaction equipment provided by the utility model can realize continuous completion of chemical reaction, filtration, extraction and solvent recovery operation in one device through the integrated double-layer kettle body, the filter assembly, the spherical glass kettle body and the vacuum pump, the whole process operation is simple, the continuous production of daphnetin is realized, the intermediate material transfer is reduced, and the loss and pollution risk are reduced.

[0019] (2) the chemical reaction equipment provided by the utility model can realize solvent recovery and recycling, and the solvent recovery and recycling function reduces the production cost and meets the environmental protection requirements.

[0020] (3) the chemical reaction equipment provided by the utility model is simple to operate, has low labor intensity, high safety, is suitable for large-scale production, has remarkable economic benefits and environmental friendliness, provides an efficient solution for the industrialized production of daphnetin.

[0021] (4) the first reflux condensing component is arranged on the kettle body upper cover, the first reflux condensing component is used for reflux condensation, and plays a role when the activated carbon is decolorized. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1 It is the whole structure schematic view of the chemical reaction equipment that the utility model can realize continuous production.

[0023] Figure 2 It is the schematic view of the filter assembly.

[0024] : double-layer kettle body 1, kettle body upper cover 2, filter assembly 3, middle kettle body 4, heating jacket 5, vacuum pump 6, upper connecting disc 7, lower connecting disc 8, sealing ring 9, long bolt 10, lower discharge valve 11, first connecting pipe 12, second connecting pipe 13, first reflux head 14, first condenser 15, first air suction head 16, second reflux head 17, second condenser 18, second air suction head 19, stirring motor 20, stirring paddle 21, frequency conversion controller 22, interlayer inlet 101, interlayer outlet 102, interlayer 103, solid feeding port 201, constant pressure funnel 202, filter disc 301, PTFE filter core 302, pressing ring 303, feeding port 401. DETAILED DESCRIPTION

[0025] The technical solutions in the embodiments of the present application will be clearly and completely described in combination with the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the scope of protection of the present application.

[0026] In the description of the present application, it should be further explained that, unless otherwise explicitly specified and limited, the terms "arranged", "connected" should be understood in a broad sense, for example, can be fixedly connected, can be detachably connected, or integrally connected; can be mechanically connected, can be directly connected, or indirectly connected through an intermediate medium, can be the communication inside two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0027] As shown in Figure 1 , Figure 2 , the chemical reaction equipment capable of realizing continuous production provided by the embodiment comprises a double-layer kettle body 1 with both upper and lower ends being open, a kettle body upper cover 2, a filter assembly 3, a middle kettle body 4, a heating jacket 5, and a vacuum pump 6; wherein the double-layer kettle body 1 is provided with an interlayer inlet 101 near the lower end and an interlayer outlet 102 near the upper end on the side wall, the interlayer inlet 101 and the interlayer outlet 102 are in communication with an interlayer 103 of the side wall of the double-layer kettle body, and the lower end of the double-layer kettle body 1 is provided with an upper connecting disc 7;

[0028] The kettle body upper cover 2 is fixed at the upper end of the double-layer kettle body 1, and the kettle body upper cover 2 is provided with a solid feeding port 201, a constant pressure funnel 202, and a stirring mechanism;

[0029] The filter assembly 3 is installed on the lower connecting disc 8, and the periphery of the surface of the filter assembly 3 in contact with the double-layer kettle body 1 is provided with a sealing ring 9. The lower connecting disc 8 is fixedly connected with the upper connecting disc 7 through connecting members (long bolts 10), which are used to fix the filter assembly 3 at the lower end of the double-layer kettle body 1. The bottom of the filter assembly 3 is provided with a discharge port (not marked), and the discharge port is provided with a lower discharge valve 11.

[0030] The intermediate kettle body 4 is arranged in the heating jacket 5. The first joint of the intermediate kettle body 4 is connected with the discharge port through the first connecting pipe 12, and the second joint is connected with the vacuum pump 6 through the second connecting pipe 13. The intermediate kettle body 4 is provided with a second reflux condensing assembly, and the bottom is provided with a discharge port (not marked), and the discharge port is provided with a discharge valve (not marked). The first connecting pipe 12 and the second connecting pipe 13 are provided with valves (not shown).

[0031] Further, as shown in Figure 1 , Figure 2 , in the embodiment, the kettle body upper cover 2 is further provided with a thermometer sleeve 203, a cock 204, and a first reflux condensing assembly. The thermometer sleeve 203 is provided with a thermometer (not marked), and the thermometer extends into the interior of the double-layer kettle body 1 to monitor the reaction temperature. The intermediate kettle body 4 is provided with a feed port 401.

[0032] Further, as shown in Figure 1 , Figure 2 , in the embodiment, the chemical reaction equipment further comprises a support (not marked), and the double-layer kettle body 1, the heating jacket 5, the stirring mechanism, the first reflux condensing assembly, and the second reflux condensing assembly are fixed on the support. The bottom of the support is provided with universal wheels (not marked) to facilitate the movement of the entire reaction equipment.

[0033] Further, as shown in Figure 1 , Figure 2 , in the embodiment, the first reflux condensing assembly comprises a first reflux head 14, a first condenser 15, and a first air suction head 16. The first reflux head 14 is connected to the kettle body upper cover 2 through a first elbow pipe (not marked) and communicates with the interior of the double-layer kettle body 1. The first condenser 15 is arranged on the first reflux head 14, and the first air suction head 16 is arranged on the first condenser 15. The second reflux condensing assembly comprises a second reflux head 17, a second condenser 18, and a second air suction head 19. The second reflux head 17 is connected to the intermediate kettle body 4 through a second elbow pipe (not marked) and communicates with the interior of the intermediate kettle body 4. The second condenser 18 is arranged on the second reflux head 17, and the second air suction head 19 is arranged on the second condenser 18.

[0034] Further, in the embodiment, the stirring mechanism comprises a stirring motor 20, and a stirring paddle 21 connected to the stirring motor; the stirring motor 20 is controlled by a frequency converter 22 to control the rotating speed of the stirring motor; the stirring paddle 21 extends into the double-layered kettle body 1 to stir the reaction; and the frequency converter 22 is fixed on the support.

[0035] Further, as shown in Figure 1 , Figure 2 In the embodiment, the filter assembly is a PTFE filter assembly, which comprises a filter disc 301, a PTFE filter cake 302, and a pressing ring 303; the filter disc 301 is installed on the lower connecting disc 8, and a sealing ring installation groove is arranged around the side of the filter disc 301 which is connected to the double-layered kettle body 1; the sealing ring 9 is arranged in the sealing ring installation groove; a filter core installation groove is arranged on the filter disc 301, and the filter core installation groove is in communication with the discharge port at the bottom of the filter disc; the PTFE filter core 302 is arranged in the filter core installation groove; and the pressing ring 303 is arranged in the filter core installation groove and is pressed on the PTFE filter core 302.

[0036] In the embodiment, the intermediate kettle body is a spherical glass kettle body, the vacuum pump is a circulating water type vacuum pump, and the heating jacket is an electric heating jacket; and the provided chemical reaction equipment can realize continuous production of daphnetin; and the specific operation steps are as follows:

[0037] Step 1. In the double-layered kettle body 1, 2, 3, 4-trihydroxybenzaldehyde (61.6 g, 400 mmol), Mille acid (57.6 g, 400 mmol), and water (2.0 L) are added, and 1-ethyl-3-methylimidazole acetate (34.0 g, 200 mmol) is slowly added under stirring; the rotating speed is adjusted to 500 rpm, and the temperature is gradually increased to 50℃; and the reaction is carried out for 30 h.

[0038] When the reaction is carried out, the lower discharge valve 11 and the valve on the first connecting pipe 12 are in the closed state; at this time, the double-layered kettle body 1 is used as an independent chemical reaction device, the chemical reaction is carried out by using the double-layered kettle body, and the reaction heating process is mainly carried out by the way of introducing hot water or hot oil into the interlayer inlet 101 to control the temperature.

[0039] Step 2. After the above reaction is completed, the temperature is cooled to room temperature, and then the valves of the lower discharge valve 11, the first connecting pipe 12, and the second connecting pipe 13 are opened, so that the double-layered kettle body 1, the intermediate kettle body 4, and the vacuum pump 6 are in communication; under the action of the vacuum pump 6, the reaction liquid is removed by pressure reduction filtration; the filter cake is the first product 7, 8-dihydroxycoumarin-3-carboxylic acid; and the filtrate is left in the spherical glass kettle body and is discharged through the discharge port at the bottom of the spherical glass kettle body.

[0040] When this step is performed, the double-layered kettle-ball-type glass kettle-vacuum pump combination is used as an extraction device to complete the extraction of the product obtained in Step 3 and collect the organic phase.

[0041] Step 3. Glycerol (2.0 L) is added to the double-layered kettle to dissolve 7,8-dihydroxycoumarin-3-carboxylic acid, and then 1-(2-pyrimidinyl)piperazine (65.6 g, 400 mmol) is slowly added under stirring at a speed of 500 rpm, and the temperature is gradually increased to 150°C. The reaction is carried out for 10 h.

[0042] When this step is performed, the double-layered kettle 1 is still used as an independent chemical reaction device.

[0043] Step 4. After the reaction is completed, the reaction solution is cooled to room temperature, and then water (3.6 L) and 2N HCl aqueous solution (0.4 L) are added, followed by the addition of dichloromethane (2.0 L). The stirring is started at a speed of 500 rpm, and after 5 min, the stirring is stopped, and the layers are separated. Then, the valves on the bottom discharge valve 11, the first connecting pipe 12, and the second connecting pipe 13 are opened, and the double-layered kettle 1, the intermediate kettle 4, and the vacuum pump 6 are connected. Under the action of the vacuum pump 6, the dichloromethane layer is transferred to the ball-type glass kettle. Then, dichloromethane (2.0 L) is added to the double-layered kettle, and the above operation is repeated twice. The organic phase extracted three times is discharged through the discharge port of the ball-type glass kettle, collected in a conical flask, dried with anhydrous sodium sulfate (60.0 g), and the aqueous phase in the double-layered kettle 1 is discharged through the discharge port at the bottom of the filter assembly 3.

[0044] When this step is performed, the double-layered kettle-ball-type glass kettle-vacuum pump combination is used as an extraction device to complete the extraction of the product obtained in Step 3 and collect the organic phase.

[0045] Step 5. The organic phase containing the drying agent is transferred to the double-layered kettle, and the organic phase is transferred to the ball-type glass kettle by vacuum filtration using the vacuum pump. Then, the long bolt 10 connecting the lower connecting disc 8 and the upper connecting disc 7 is opened, the filter assembly 3 is removed, and after the drying agent is cleaned, it is installed on the double-layered kettle.

[0046] When this step is performed, the double-layered kettle-ball-type glass kettle-vacuum pump combination is used as a filter device to complete the filtration and collect the organic phase.

[0047] Step 6. The heating jacket 5 is opened to heat the ball-type glass kettle, concentrate the organic phase, and recover the organic phase using the second reflux head 17 at the lower part of the second condenser, which is recycled for subsequent extraction.

[0048] When this step is performed, the spherical glass kettle body is used as a separate device to recover the organic solvent.

[0049] Step 7. The product concentrated in the spherical glass kettle body in the previous step is dissolved with ethanol (2.0 L), and the ethanol solution is manually transferred to the double-layer kettle body, activated carbon (14.0 g) is added, and decolorization is performed at 80°C for 0.5 h.

[0050] When this step is performed, the double-layer kettle body is used as a decolorization device.

[0051] Step 8. After cooling slightly, activated carbon is removed by vacuum filtration, and ethanol is transferred to the spherical glass kettle body; activated carbon is cleaned by removing the filter assembly 3.

[0052] When this step is performed, the double-layer kettle body-spherical glass kettle body-vacuum pump combination is used as a filtration device.

[0053] Step 9. The spherical glass kettle body is opened for heating, and the organic phase is concentrated, and the second reflux head at the lower part of the second condenser is used to recover the organic phase, which is recycled for subsequent decolorization. After most of the organic phase is removed, the product is discharged through the discharge port of the spherical glass kettle body, and further concentrated using a rotary evaporator to obtain a milky yellow solid 59.3 g, with a yield of 83.20% and an HPLC purity of 99.48%.

[0054] When this step is performed, the spherical glass kettle body is used as a concentration device.

[0055] The above is a specific embodiment of the present application, but the protection scope of the present application is not limited thereto, any person skilled in the art can easily think of changes or replacements within the technical range disclosed by the present application, which should be covered within the protection scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.

Claims

1. A chemical reaction apparatus capable of continuous production, characterized in that, The utility model provides a chemical reaction equipment, including double -deck cauldron body that both ends are open, cauldron body upper cover, filter assembly, intermediate cauldron body, heating jacket, vacuum pump, wherein, the double -deck cauldron body's side wall is equipped with interlayer import in the position near the lower end, is equipped with interlayer export in the position near the upper end, and interlayer import, interlayer export communicate with the interlayer of double -deck cauldron body side wall, and the lower end of double -deck cauldron body is equipped with upper connecting disc, The cauldron body upper cover is fixed on the upper end of the double -deck cauldron body, and the cauldron body upper cover is provided with a solid feeding port, a constant pressure funnel and a stirring mechanism. The filter assembly is installed on the lower connecting disc, and a sealing ring is arranged on the periphery of the surface of the filter assembly in contact with the double -deck cauldron body, the lower connecting disc is fixedly connected to the upper connecting disc through a connecting piece, and the filter assembly is fixed on the lower end of the double -deck cauldron body, the bottom of the filter assembly is provided with a discharge port, and a lower discharge valve is arranged on the discharge port. The intermediate cauldron body is arranged in the heating jacket, a first connector of the intermediate cauldron body is connected to the discharge port through a first connecting pipe, a second connector is connected to the vacuum pump through a second connecting pipe, a second reflux condensing assembly is arranged on the intermediate cauldron body, a discharge port is arranged at the bottom of the intermediate cauldron body, and a discharge valve is arranged on the discharge port.

2. The chemical reaction apparatus capable of continuous production according to claim 1, wherein The filter assembly is a PTFE filter assembly, which comprises a filter disc, a PTFE filter core and a pressing ring, wherein the filter disc is installed on the lower connecting disc, a sealing ring mounting groove is arranged on the periphery of the surface of the filter disc in abutment with the double -deck cauldron body, the sealing ring is arranged in the sealing ring mounting groove, a filter core mounting groove is arranged on the filter disc, the filter core mounting groove is in communication with the discharge port at the bottom of the filter disc, the PTFE filter core is arranged in the filter core mounting groove, and the pressing ring is arranged in the filter core mounting groove and is pressed on the PTFE filter core.

3. The chemical reaction apparatus capable of realizing continuous production according to claim 1, wherein The stirring mechanism comprises a stirring motor and a stirring paddle connected to the stirring motor, the stirring motor is controlled by a frequency conversion controller to control the rotating speed, and the stirring paddle extends into the double -deck cauldron body to stir during the reaction.

4. The chemical reaction apparatus capable of continuous production according to claim 1, wherein A thermometer sleeve, a cock and a first reflux condensing assembly are further arranged on the cauldron body upper cover, wherein a thermometer is arranged in the thermometer sleeve, the thermometer extends into the double -deck cauldron body to monitor the reaction temperature.

5. The chemical reaction apparatus capable of realizing continuous production according to claim 1, wherein The intermediate cauldron body is a spherical glass cauldron body, the vacuum pump is a circulating water type vacuum pump, and the heating jacket is an electric heating jacket.

6. The chemical reaction apparatus capable of realizing continuous production according to claim 4, wherein The chemical reaction equipment further comprises a support, and the double -deck cauldron body, the heating jacket, the stirring mechanism, the first reflux condensing assembly and the second reflux condensing assembly are fixed on the support, and universal wheels are arranged at the bottom of the support.

7. The chemical reaction apparatus capable of realizing continuous production according to claim 6, wherein The first reflux condensing assembly comprises a first reflux head, a first condenser and a first air suction head, the first reflux head is connected to the cauldron body upper cover through a first elbow pipe and is in communication with the inside of the double -deck cauldron body, the first condenser is arranged on the first reflux head, and the first air suction head is arranged on the first condenser; the second reflux condensing assembly comprises a second reflux head, a second condenser and a second air suction head, the second reflux head is connected to the intermediate cauldron body through a second elbow pipe and is in communication with the inside of the intermediate cauldron body, the second condenser is arranged on the second reflux head, and the second air suction head is arranged on the second condenser.

8. The chemical reaction apparatus capable of realizing continuous production according to any one of claims 1 to 7, characterized by The chemical reaction equipment is a continuous production equipment for daphnetin.

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