CN210545036U

CN210545036U - Photoreaction production equipment

Info

Publication number: CN210545036U
Application number: CN201920947437.4U
Authority: CN
Inventors: 段义杰; 裴佩佩; 陈艳梅; 孟凡生; 吴双俊; 崔茂杰
Original assignee: SHANDONG FANGMING PHARMACEUTICAL GROUP CO Ltd
Current assignee: SHANDONG FANGMING PHARMACEUTICAL GROUP CO Ltd
Priority date: 2019-06-21
Filing date: 2019-06-21
Publication date: 2020-05-19
Anticipated expiration: 2029-06-21

Abstract

The utility model relates to a light reaction production facility, including first reation kettle and second reation kettle, first reation kettle is suitable for adding the mixed material, be equipped with the discharging pipe between first reation kettle's discharge end and the feed end of second reation kettle, the discharging pipe position is equipped with first circulating pump, be equipped with quartz coil pipe in the second reation kettle, quartz coil pipe's one end and discharging pipe link to each other, quartz coil pipe's the other end and feed back pipe link to each other, feed back pipe and first reation kettle's feed end link to each other, make the material in the first reation kettle form circulation flow along discharging pipe, quartz coil pipe and feed back pipe; a light source lamp is arranged in the second reaction kettle. The utility model has the advantages of reasonable design, make the material at first reation kettle and second reation kettle mesocycle flow, continuously carry out the photoreaction, the photoreaction until the material reaches the standard to realize photochemical reaction's scale production, reduce the scale and enlarge the effect, improve the output and the quality that involve the bulk drug of photoreaction, reach reduce cost, energy saving and consumption reduction's effect.

Description

Photoreaction production equipment

Technical Field

The utility model relates to a photoreaction production facility.

Background

At present, the small-scale photochemical reaction of the medicine is easy to realize in a laboratory, and a better reaction effect can be ensured. However, in the large-scale generation process, the photochemical reaction is affected by the energy attenuation in the light propagation process, and after the reaction batch of the materials is enlarged, the corresponding amplification reaction effect of common photoreaction equipment is poor, and the reaction rates are inconsistent, so that the reaction effect after the scale amplification is poor. Compared with the reaction in a laboratory, the method has the problems of long reaction time, incomplete reaction and the like, so that the impurities, yield and the like of the reacted materials have deviation, the capacity of the photoreaction raw material medicine is severely limited, and the production cost is increased.

SUMMERY OF THE UTILITY MODEL

The utility model provides a photoreaction production facility, its structural design is reasonable, makes the material at first reation kettle and second reation kettle mesocycle flow, continuously carries out the photoreaction, and the photoreaction until the material reaches the standard to realize photochemical reaction's scale production, reduce the effect of enlarging scale, improve the output and the quality of the bulk drug that involve the photoreaction, reach reduce cost, energy saving and consumption reduction's effect has solved the problem that exists among the prior art.

The utility model discloses a solve the technical scheme that above-mentioned technical problem adopted and be: a photoreaction production apparatus comprising:

the device comprises a first reaction kettle and a second reaction kettle, wherein the first reaction kettle is suitable for adding mixed materials, a discharge pipe is arranged between the discharge end of the first reaction kettle and the feed end of the second reaction kettle, a first circulating pump is arranged at the position of the discharge pipe, a quartz coil is arranged in the second reaction kettle, one end of the quartz coil is connected with the discharge pipe, the other end of the quartz coil is connected with a material return pipe, and the material return pipe is connected with the feed end of the first reaction kettle so that the materials in the first reaction kettle form circulating flow along the discharge pipe, the quartz coil and the material return pipe; a light source lamp is arranged in the second reaction kettle, and light rays emitted by the light source lamp after being electrified penetrate through the quartz coil pipe to enable the materials to be irradiated for light reaction;

the outer wall of the first reaction kettle is provided with a first interlayer, the outer wall of the second reaction kettle is provided with a second interlayer, the first interlayer and the second interlayer are respectively connected with an external cooling device through pipelines, and the cooling device is used for conveying cooling media to the first interlayer and the second interlayer through the pipelines so as to reduce the temperature of materials.

Further, the light source lamp is arranged in a vertically arranged lamp tube structure, the quartz coil is arranged in a spiral structure along the axial outer side of the light source lamp, and the light source lamp is arranged at the position of the central axis of the quartz coil in the spiral structure.

Furthermore, the second reaction kettle is internally provided with filter liquid covering the quartz coil, and the filter liquid is suitable for filtering the useless wave band of illumination.

Further, the cooling device includes the coolant liquid case, the coolant liquid case links to each other through drain pipe and second intermediate layer, the drain pipe position is equipped with the second circulating pump, is equipped with the connecting pipe between second intermediate layer and the first intermediate layer, links to each other through the liquid return pipe between second intermediate layer and the coolant liquid case.

Further, the drain pipe links to each other with the upper portion import of second intermediate layer, the one end of connecting pipe and the lower part export of second intermediate layer link to each other, and the other end of connecting pipe and the upper portion import of first intermediate layer link to each other, it links to each other with the lower part export of first intermediate layer to return the liquid pipe.

Furthermore, the first circulating pump is connected with a frequency converter and a relay in series through conducting wires, and the frequency converter and the relay are connected with a PLC (programmable logic controller) through conducting wires so as to control the on-off of the first circulating pump and the flow of conveyed materials.

Further, the second circulating pump is connected with a relay through a lead, and the relay is connected with the PLC through a lead; a temperature sensor is arranged in the second reaction kettle and is connected with a PLC (programmable logic controller) through a lead; and after the real-time temperature acquired by the temperature sensor exceeds a preset maximum temperature value, the PLC closes the relay to enable the second circulating pump to work, so that the cooling medium circulates along the pipeline.

Further, be equipped with the level gauge in the second reation kettle, the level gauge links to each other through wire and PLC controller, and the PLC controller links to each other through wire and alarm, and after the position that highly is less than quartz coil pipe of the filter liquid in the second reation kettle, the PLC controller made the alarm send alarm signal.

Further, be equipped with the puddler in the first reation kettle, puddler and servo motor link to each other, servo motor links to each other through wire and PLC controller to the rotational speed of control puddler makes the material in the first reation kettle obtain the stirring.

Furthermore, be equipped with first solenoid valve between first reation kettle and the first circulating pump, drain pipe position between second circulating pump and the coolant liquid case is equipped with the second solenoid valve, and first solenoid valve and second solenoid valve link to each other with the PLC controller through the wire respectively.

The utility model adopts the above structure beneficial effect be, its structural design is reasonable, makes the material at first reation kettle and second reation kettle mesocycle flow, continuously carries out the photoreaction, and the photoreaction until the material reaches the standard to realize the large-scale production of photochemical reaction, reduce the effect of enlarging scale, improve the output and the quality of the bulk drug that involves the photoreaction, reach reduce cost, energy saving and consumption reduction's effect.

Drawings

Fig. 1 is a schematic structural diagram of the present invention.

Fig. 2 is an electrical schematic diagram of the present invention.

In the figure, 1, a first reaction kettle; 101. a first interlayer; 2. a second reaction kettle; 201. a second interlayer; 3. a discharge pipe; 4. a first circulation pump; 5. a quartz coil; 6. a material return pipe; 7. a light source lamp; 8. a coolant tank; 9. a liquid outlet pipe; 10. a second circulation pump; 11. a connecting pipe; 12. a liquid return pipe; 13. a temperature sensor; 14. a liquid level meter; 15. a stirring rod; 16. a servo motor; 17. a first solenoid valve; 18. a second solenoid valve; 19. a three-way joint; 20. a branch pipe; 21. a third valve.

Detailed Description

In order to clearly illustrate the technical features of the present invention, the present invention is explained in detail by the following embodiments in combination with the accompanying drawings.

In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application, however, the present application may be practiced in other ways than those described herein, and therefore the scope of the present application is not limited by the specific embodiments disclosed below.

In addition, in the description of the present application, it is to be understood that the terms "center", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "axial", "radial", "circumferential", and the like, indicate orientations and positional relationships based on those shown in the drawings, are only for convenience of description and simplicity of description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present application.

Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless specifically limited otherwise.

In this application, unless expressly stated or limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can include, for example, fixed connections, removable connections, or integral parts; the connection can be mechanical connection, electrical connection or communication; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.

In this application, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through intervening media. In the description herein, reference to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the application. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

As shown in fig. 1-2, a photoreaction production device comprises a first reaction vessel 1 and a second reaction vessel 1, wherein the first reaction vessel 1 is suitable for adding mixed materials, a discharge pipe 3 is arranged between a discharge end of the first reaction vessel 1 and a feed end of the second reaction vessel 2, a first circulating pump 4 is arranged at the position of the discharge pipe 3, a quartz coil 5 is arranged in the second reaction vessel 2, one end of the quartz coil 5 is connected with the discharge pipe 3, the other end of the quartz coil 5 is connected with a return pipe 6, and the return pipe 6 is connected with the feed end of the first reaction vessel 1, so that the materials in the first reaction vessel 1 form circulating flow along the discharge pipe 3, the quartz coil 5 and the return pipe 6; a light source lamp 7 is arranged in the second reaction kettle 2, and light rays emitted by the light source lamp 7 after being electrified penetrate through the quartz coil 5 to enable the materials to be illuminated for light reaction; the outer wall of first reation kettle 1 is equipped with first intermediate layer 101, and the outer wall of second reation kettle 2 is equipped with second intermediate layer 201, and first intermediate layer 101 and second intermediate layer 201 link to each other with outside cooling device through the pipeline respectively, and cooling medium is carried to the pipeline to first intermediate layer 101 and second intermediate layer 201 in the cooling device to reduce the temperature of material. During the use, at first add the material in first reation kettle 1, after adding the mixture as required with the material, open first circulating pump 4, make the material in first reation kettle 1 follow discharging pipe 3 and get into the quartz coil pipe 5 in second reation kettle 2, the material through quartz coil pipe 5 receives the irradiation of light source lamp 7, carry out the photoreaction, the material of quartz coil pipe 5 gets back to first reation kettle 1 once more along feed back pipe 6, make the material circulate and flow between first reation kettle 1 and second reation kettle 2, continuously carry out the photoreaction, the photoreaction of material reaches the standard, thereby realize the large-scale production of photochemical reaction, reduce the scale amplification effect, improve the output and the quality of the bulk drug who involves the photoreaction, reach reduce cost, energy saving and consumption reduction's effect.

In the preferred embodiment, the light source lamp 7 is provided in a vertically arranged lamp tube structure, the quartz coil 5 is arranged in a spiral structure along the axial outer side of the light source lamp 7, and the light source lamp 7 is arranged at the position of the central axis of the quartz coil 5 in the spiral structure. The distance between the light source lamp 7 and the materials in the quartz coil 5 is kept consistent, the consistency of the reaction rate of the materials is ensured, and the progress of the photoreaction of the materials is kept consistent; and the whole quartz coil 5 adopts a spiral configuration, so that the maximum light source utilization rate is ensured, and the energy consumption is saved.

In the preferred embodiment, the second reactor 2 is provided with a filter liquid covering the quartz coil 5, the filter liquid being adapted to filter the unwanted wavelength band of the illumination. The filter liquid can filter the wave band which is not needed in the reaction process of the materials, thereby ensuring the purity and the yield of the reaction product and avoiding other side reactions; compared with the optical filter (film), the optical filter has the advantages of low cost and convenient replacement, and solves the cooling problem of optical equipment in the reaction process. According to different reaction requirements, corresponding filtering liquid is selected, and the replacement and the use are flexible and convenient. Light filters include, but are not limited to: copper sulfate, potassium dichromate, sodium nitrite, nickel sulfate, copper chloride, calcium chloride and their mixed water solution.

In a preferred embodiment, the cooling device comprises a cooling liquid tank 8, the cooling liquid tank 8 is connected with a second interlayer 201 through a liquid outlet pipe 9, a second circulating pump 10 is arranged at the position of the liquid outlet pipe 9, a connecting pipe 11 is arranged between the second interlayer 201 and the first interlayer 101, and the second interlayer 201 is connected with the cooling liquid tank 8 through a liquid return pipe 12. During the use, carry the coolant in coolant liquid case 8 to second intermediate layer 201 and first intermediate layer 101 in along the pipeline through second circulating pump 10, the coolant in coolant liquid case 8 enters into second intermediate layer 201 at first, because second reation kettle 2 is carrying out the photoreaction, can produce a large amount of heat, the coolant enters into second intermediate layer 201 at first, then enters into first intermediate layer 101 again, can maximize the heat exchange efficiency who utilizes coolant, practices thrift the energy consumption.

In the preferred embodiment, the liquid outlet pipe 9 is connected to the upper inlet of the second interlayer 201, one end of the connecting pipe 11 is connected to the lower outlet of the second interlayer 101, the other end of the connecting pipe 11 is connected to the upper inlet of the first interlayer 101, and the liquid return pipe 12 is connected to the lower outlet of the first interlayer 101. The smooth circulation of the cooling medium is ensured, the cooling medium enters from the upper inlets of the second interlayer 201 and the first interlayer 101, the cooling medium flows out from the lower outlets of the second interlayer 201 and the first interlayer 101 by the aid of the gravity of the cooling medium, and the whole pipeline is reasonably arranged.

In a preferred embodiment, the first circulating pump 4 is connected in series with a frequency converter and a relay through leads, and the frequency converter and the relay are connected with a PLC controller through leads so as to control the on-off of the first circulating pump 4 and the flow rate of conveyed materials. The automatic control of the first circulating pump 4 is realized through a PLC (programmable logic controller), and after the materials in the first reaction kettle 1 are added, the first circulating pump 4 is controlled to be started through the PLC; and the reaction rate is basically kept consistent when the materials are in different batches by controlling the flow rate of the first circulating pump 4. Is not influenced by reaction batch (material charging quantity).

It can be understood that the light source lamp 7 can also be connected with the PLC controller, so that the opening and closing of the light source lamp 7 is controlled by the PLC controller, and the LED lamp is more convenient and intelligent;

in a preferred embodiment, the second circulation pump 10 is connected with a relay through a wire, and the relay is connected with a PLC controller through a wire; a temperature sensor 13 is arranged in the second reaction kettle 2, and the temperature sensor 13 is connected with a PLC controller through a lead; after the real-time temperature acquired by the temperature sensor 13 exceeds the preset maximum temperature value, the PLC controller closes the relay to operate the second circulation pump 2, so that the cooling medium circulates along the pipeline.

In a preferred embodiment, the second reaction kettle 2 is provided with a liquid level meter 14, the liquid level meter 14 is connected with a PLC controller through a lead, the PLC controller is connected with an alarm through a lead, and when the height of the filter liquid in the second reaction kettle 2 is lower than the position of the quartz coil pipe 5, the PLC controller enables the alarm to send out an alarm signal.

In a preferred embodiment, a stirring rod 15 is disposed in the first reaction vessel 1, the stirring rod 15 is connected to a servo motor 16, and the servo motor 16 is connected to a PLC controller via a wire to control the rotation speed of the stirring rod 15, so that the material in the first reaction vessel 1 is stirred.

In a preferred embodiment, a first electromagnetic valve 17 is arranged between the first reaction kettle 1 and the first circulating pump 4, a second electromagnetic valve 18 is arranged at the position of the liquid outlet pipe 9 between the second circulating pump 2 and the cooling liquid tank 8, and the first electromagnetic valve 17 and the second electromagnetic valve 18 are respectively connected with a PLC (programmable logic controller) through leads. The first electromagnetic valve 17 and the second electromagnetic valve 18 are controlled by the PLC controller, so that the on-off of the discharge pipe 3 and the liquid outlet pipe 9 can be controlled, and the automation control degree is high.

It is worth mentioning that a three-way joint 19 is arranged at the position of the discharge pipe 3 and/or the return pipe 6, the three-way joint 19 is externally connected with a branch pipe 20, and a third valve 21 is arranged at the position of the branch pipe 20. After material reaction a period, can take a sample and carry out the thin layer detection reaction to judge the reaction progress of material, specifically can follow branch pipe 20 position sample, only need open third valve 21, make the material in the discharging pipe 3 flow out along branch pipe 20, close third valve 21 after accomplishing the sample, need not like opening 1 lid of first reation kettle among the prior art and take a sample, operate simple and convenient more.

Specific examples of photoreactions using the present apparatus:

1. material proportioning

Lysergol: anhydrous methanol: concentrated sulfuric acid 10Kg, 125(L), 25(L)

2. Procedure of operation

Adding anhydrous methanol into a first reaction kettle of 500L, adding ergosterol, stirring for 30 min, slowly dropwise adding concentrated sulfuric acid, controlling the temperature not to exceed 40 ℃, controlling the temperature to be 25 ℃ and reacting for 8 hours. Monitoring the reaction process by adopting TLC in the reaction process; a GF254 thin-layer silica gel plate is adopted, and the developing agent is methanol: trichloromethane: ammonia water 20: 80: 0.2;

anhydrous methanol and concentrated sulfuric acid are sequentially added into the first reaction kettle 1. The discharging pipe 3 of the first reaction kettle 1 is in a closed state, stirring is started, concentrated sulfuric acid is dripped when the temperature of the materials in the first reaction kettle 1 is reduced to 20 ℃, and the temperature in the first reaction kettle 1 is controlled not to exceed 40 ℃ in the whole process. And finishing the dropwise addition of the concentrated sulfuric acid. The first circulating pump 4 is started to start the material to circulate between the first reaction kettle 1 and the second reaction kettle 2. And simultaneously conveying cooling media into the first interlayer 101 and the second interlayer 201 for cooling in the reaction process. The temperature of the material was controlled to be always between 20 ℃ and 25 ℃. After reacting for 8 hours, sampling and carrying out thin-layer detection reaction, and judging whether the material reaction is fully qualified.

The above-mentioned specific embodiments can not be regarded as the restriction to the scope of protection of the utility model, to technical personnel in this technical field, it is right the utility model discloses any replacement improvement or transform that embodiment made all fall within the scope of protection of the utility model.

The parts of the present invention not described in detail are the known techniques of those skilled in the art.

Claims

1. A photoreaction production apparatus, comprising:

2. The production apparatus of claim 1, wherein the light source lamp is provided in a vertically arranged tube structure, the quartz coil is arranged in a spiral structure along an axially outer side of the light source lamp, and the light source lamp is arranged at a central axis of the quartz coil in the spiral structure.

3. A photoreaction production apparatus according to claim 1 or 2, wherein the second reactor contains a filter liquid covering the quartz coil, and the filter liquid is adapted to filter the unwanted wavelength band of light.

4. A photoreaction production apparatus according to claim 1, wherein the cooling apparatus comprises a coolant tank, the coolant tank is connected to the second interlayer through a drain pipe, a second circulation pump is disposed at the drain pipe, a connection pipe is disposed between the second interlayer and the first interlayer, and the second interlayer is connected to the coolant tank through a liquid return pipe.

5. A photoreaction production equipment according to claim 4, wherein the liquid outlet pipe is connected to an upper inlet of the second interlayer, one end of the connecting pipe is connected to a lower outlet of the second interlayer, the other end of the connecting pipe is connected to an upper inlet of the first interlayer, and the liquid return pipe is connected to a lower outlet of the first interlayer.

6. The photoreaction production equipment as claimed in claim 1, wherein the first circulation pump is connected in series with a frequency converter and a relay via wires, and the frequency converter and the relay are connected with the PLC via wires to control the on/off of the first circulation pump and the flow rate of the transported material.

7. A photoreaction production apparatus according to claim 4 or 5, wherein the second circulation pump is connected to a relay via a wire, and the relay is connected to a PLC controller via a wire; a temperature sensor is arranged in the second reaction kettle and is connected with a PLC (programmable logic controller) through a lead; and after the real-time temperature acquired by the temperature sensor exceeds a preset maximum temperature value, the PLC closes the relay to enable the second circulating pump to work, so that the cooling medium circulates along the pipeline.

8. The photoreaction production apparatus according to claim 1, wherein a liquid level meter is disposed in the second reaction vessel, the liquid level meter is connected to a PLC controller via a wire, the PLC controller is connected to an alarm via a wire, and when the height of the filter liquid in the second reaction vessel is lower than the position of the quartz coil, the PLC controller causes the alarm to send an alarm signal.

9. A photoreaction production apparatus according to claim 1, wherein a stirring rod is disposed in the first reactor, the stirring rod is connected to a servo motor, and the servo motor is connected to a PLC controller via a wire to control the rotation speed of the stirring rod, so as to stir the materials in the first reactor.

10. A light reaction production apparatus as claimed in claim 7, wherein a first electromagnetic valve is provided between the first reaction vessel and the first circulating pump, a second electromagnetic valve is provided at a position of the liquid outlet pipe between the second circulating pump and the coolant tank, and the first electromagnetic valve and the second electromagnetic valve are respectively connected with the PLC controller via wires.