CN216386773U - Multichannel crystallization screening automated control equipment - Google Patents
Multichannel crystallization screening automated control equipment Download PDFInfo
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- CN216386773U CN216386773U CN202120766738.4U CN202120766738U CN216386773U CN 216386773 U CN216386773 U CN 216386773U CN 202120766738 U CN202120766738 U CN 202120766738U CN 216386773 U CN216386773 U CN 216386773U
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Abstract
The utility model discloses an automatic control device for multi-channel crystal screening, which can realize parallel crystal screening of a plurality of channels of crystal units and comprises a temperature measurement control device, a circulating cooler, a magnetic stirrer, a mechanical stirrer, a feeding pump, a turbidity meter, a grain shape and granularity meter, an infrared concentration measuring instrument and a Raman spectrum measuring instrument, wherein the circulating cooler is matched with a temperature measurement control function device to control the temperature of the multi-channel crystal units, and the channels are independently controlled and do not interfere with each other; each channel is provided with a magnetic stirrer and a mechanical stirrer; the feeding pump provides a feeding function for the crystallization screening process of the multi-path crystallization unit; detecting turbidity values in the multi-path crystallization unit by a turbidity meter; a particle shape and particle size meter is used for measuring the shape and size of particles; the infrared concentration measuring instrument is used for analyzing the concentration of the sample; the Raman spectrum measuring instrument is used for observing the polymorphic transformation, the channels are mutually independent, and the upper computer is matched, so that the automatic control of the crystal screening process is realized.
Description
Technical Field
The utility model relates to the technical field of online measurement process control instruments, in particular to an automatic control device for multi-channel crystal screening.
Background
In the fields of medicine, chemical industry, materials and the like, multiple rounds of crystal form screening are generally needed from research and development to application of new chemical entities. Crystal form screening can rapidly determine the crystal form used for subsequent development. The crystal form screening has great significance for subsequent improvement and patent layout of products. The existing high-throughput crystal screening device has simple functions and can only provide some simple measurement (temperature, turbidity and the like) of crystallization parameters such as: CrystalSCAN by Hel and Crystal16 parallel crystallizer developed by Technobis, Inc. The utility model provides an automatic control instrument for multi-channel crystallization screening, which can measure and control a plurality of important parameters of a crystallization process, including crystal form, crystal habit, turbidity, concentration, particle size distribution and the like, in real time on line.
SUMMERY OF THE UTILITY MODEL
In order to make up for the defects, the utility model provides a multichannel automatic control device for crystal screening, which can monitor and control important parameters of a plurality of crystallization processes in real time on line. The circulating cooler is matched with a temperature measurement control function device to control the temperature of the multi-channel crystallization unit, and the temperature control processes among the channels are relatively independent and do not interfere with each other; detecting turbidity values in the multi-path crystallization unit by a turbidity meter; each channel is provided with a magnetic stirrer and a mechanical stirrer; the feeding pump provides a feeding function for the crystallization screening process of the multi-path crystallization unit; a particle shape and particle size meter is used for measuring the shape and size of particles; the infrared concentration measuring instrument is used for analyzing the concentration of the sample; the polymorphic transformation was observed by raman spectroscopy.
The utility model is realized by the following steps:
an automatic control device for multi-channel crystal screening can realize parallel crystal screening of a plurality of channel crystal units, wherein each channel crystal unit comprises a temperature measurement control device, a circulating cooler, a turbidity instrument, a magnetic stirrer, a mechanical stirrer, a feeding pump, a grain shape and granularity instrument, an infrared concentration measuring instrument, a Raman spectrum measuring instrument and the like,
the temperature measurement control device comprises a crystallization unit, an electric heating unit and a PID controller, wherein the crystallization unit comprises a crystallizer, a metal heat transfer body, a cooling liquid jacket and a temperature measurement unit, a water inlet and a water outlet are respectively arranged on two sides of the cooling liquid jacket, the water outlet is connected with a one-way valve, the water inlet is connected with an electric regulating valve, the circulating cooler is communicated with the cooling liquid jacket and used for supplying and conveying cooling liquid, the PID controller changes the flow of the cooling liquid entering the cooling liquid jacket by controlling the opening degree of the valve, and the metal heat transfer body is used for transferring the temperature of the crystallizer and controlling the temperature reduction process of a sample in the crystallizer;
the electric heating unit is positioned at the bottom of the crystallization unit, the PID controller is used for controlling and heating the sample in the crystallizer, and the PID controller is used for adjusting the output of the electric heating unit and the flow of the cooling liquid through 0-4mA control signals to realize the accurate temperature control of the crystallization unit;
the temperature measuring unit comprises a temperature measuring instrument arranged in the crystallizer and the electric heating unit temperature measuring instrument, and a sample temperature measuring probe in the crystallizer is directly immersed in the crystallizer to measure the temperature of a sample and transmits a temperature signal to the PID controller;
the turbidity measuring instrument, the grain shape particle size analyzer, the infrared concentration measurement and the Raman probe are all led out from the inside of the main case and are fixed at the top of the sealing cover of the crystallizer, and each probe is immersed in a sample or carries out non-contact measurement through a window;
the magnetic stirrer is positioned at the bottom of the crystallization unit, and a stirring switch and the rotating speed of the magnetic stirrer are controlled by upper computer software;
the mechanical stirrer comprises a stirring paddle, the stirring paddle penetrates through the top of the sealing cover of the crystallizer and is positioned in the crystallizer, and clamping platforms are arranged beside the channels and used for fixing a motor of the mechanical stirrer;
the outside of mainframe box is provided with the charge pump, the charge pump is provided with feeding pipeline and a plurality of discharging pipeline all the way, feeding pipeline connects and waits to add the sample cell, and is a plurality of discharging pipeline corresponds respectively and connects a plurality of passageways the crystallizer to pass inside the sealed lid top of crystallizer gets into the crystallizer.
In an embodiment of the utility model, the crystallizer sealing cover is made of polytetrafluoroethylene, and the top of the crystallizer sealing cover is provided with a plurality of hole grooves, the hole grooves are in threaded connection with the probe, and the probe is positioned at the top of the crystallizer sealing cover.
In one embodiment of the utility model, the magnetic stirrer is used for stirring the single or multiple crystallizers in the crystallization unit simultaneously.
In an embodiment of the utility model, the diameter of the turbidity measuring probe is 4mm, and a data transmission module is arranged in the main case and used for transmitting turbidity data to the upper computer software for display.
In one embodiment of the present invention, the number of the crystallization units of the plurality of channels is six, and the channels of each group are independent.
In an embodiment of the present invention, the switches and the communication interfaces of the turbidity measuring apparatus, the magnetic stirrer, the mechanical stirrer, the feeding pump, the grain size analyzer, the infrared concentration measuring apparatus and the raman spectroscopy measuring apparatus are respectively disposed on the back of the main cabinet.
In one embodiment of the present invention, the metal heat transfer body comprises a single-hole metal heat transfer body and a double-hole metal heat transfer body, the single-hole metal heat transfer body is used for realizing crystallization of a single crystallizer, and the double-hole metal heat transfer body is used for realizing simultaneous crystallization of two crystallizers.
In one embodiment of the utility model, the metal heat transfer body is provided with a metal expansion ring in close contact with the metal heat transfer body for expanding the diameter of the crystallizer.
In an embodiment of the present invention, the turbidity measuring apparatus, the particle size analyzer, the infrared concentration measuring apparatus, the raman spectrum measuring apparatus, and the mechanical stirrer are electrically connected to the main cabinet by plugging.
In one embodiment of the utility model, the stirring switches and the rotating speeds of the magnetic stirrer and the mechanical stirrer are controlled by upper computer software.
The utility model has the beneficial effects that:
compared with the prior art, the utility model realizes the multichannel crystal screening automatic control equipment and the multichannel crystal screening automatic control method, the multichannel crystal screening automatic control equipment is provided with a plurality of channels, each channel expands the particle shape and size measurement, the infrared concentration measurement and the Raman spectrum measurement on the basis of realizing the basic functions of temperature control, turbidity measurement, stirring and feeding, the particle shape and size measurement can realize the real-time accurate measurement of the particle shape and size in the crystal screening process, the infrared concentration measurement can utilize infrared spectrum to analyze the concentration of a crystal sample through Fourier transform combined with chemometrics modeling, the in-situ on-line measurement of the concentration and the supersaturation is realized, and the expansion of the Raman spectrum measurement can help to realize the identification of polycrystalline types in the crystal screening process, and the conversion among the polycrystalline types and the conversion from amorphous to crystalline types are observed in real time. This design simple structure provides abundant measurement function for the process of crystallization screening for the screening process is accurate high-efficient fast more.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a schematic perspective view of the present invention.
FIG. 2 is a schematic side-view and rear-view perspective view of the present invention.
FIG. 3 is a schematic view of the structure of the opening of the cover of the crystallizer.
Fig. 4 is a schematic perspective view of a metal heat transfer body.
Fig. 5 is a schematic perspective view of a metal heat transfer body.
In the figure: 1. a crystallization unit; 2. a coolant jacket; 3. electrically plugging the element; 4. an electrical plug-in; 5. a first electrical plug hole; 6. a second electrical plug hole; 7. a third electrical plug hole; 8. a crystallizer sealing cover; 9. A hole groove; 10. a circular hole; 11. a single-hole metal heat transfer body; 12. a double-hole metal heat transfer body.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the utility model, as claimed, but is merely representative of selected embodiments of the utility model. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the equipment or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention.
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 invention, "a plurality" means two or more unless specifically defined otherwise.
Examples
Referring to fig. 1-5, the utility model relates to an automatic control device and method for multi-channel crystal screening, which comprises a temperature measurement control device, a circulation cooler, a turbidity meter, a magnetic stirrer, a mechanical stirrer, a feed pump, a particle size analyzer, an infrared concentration measuring instrument and a raman spectrum measuring instrument.
Referring to fig. 1-2, the present invention includes a plurality of channel crystallization units 1, each channel having a turbidity measuring apparatus, a mechanical stirrer, a magnetic stirrer, a feeding pipeline, a particle size analyzer probe, an infrared concentration measuring apparatus, and a raman spectroscopy measuring apparatus.
As shown in fig. 4-5, the metal heat transfer body has two types, a single-hole metal heat transfer body 11 and a double-hole metal heat transfer body 12, the metal heat transfer body is provided with a round hole 10 for placing a crystallizer, the single-hole heat transfer body 11 realizes the crystallization process of a single crystallizer, the double-hole heat transfer body 12 realizes the simultaneous crystallization process of two crystallizers, and a metal diameter expanding ring is arranged according to the size of the crystallizer and used for expanding the diameter of the small-diameter crystallizer to be in close contact with the metal heat transfer body;
the turbidity meter is used for carrying out turbidity measurement, and is led out from the electric plug-in 4 on the back of the main case and in threaded connection with a hole groove 9 formed in the top of the sealing cover 8 of the crystallizer;
the mechanical stirrer is connected with the mainframe box through an electric plug-pull piece 3 and used in a large-capacity crystallizer, a stirring paddle enters a sample through a hole groove 9 formed in the top of a crystallizer sealing cover 8 to be stirred, the start and stop of stirring and the rotating speed are controlled through upper computer software, a clamping table is arranged beside each channel, and a motor of the mechanical stirrer is fixed;
the feeding pump is arranged outside the mainframe box and is provided with a feeding pipeline and a plurality of discharging pipelines, the feeding pipeline is connected with a sample pool to be added, the discharging pipelines are connected with crystallizers of all channels, and the feeding pipeline enters the crystallizers through a hole groove 9 formed in the top of a sealing cover 8 of the crystallizers;
the grain-shaped granularity measuring probe is connected with the mainframe box through a first electric plugging hole 5 and is fixed inside a hole groove 9 at the top of a crystallizer sealing cover 8;
the infrared concentration measuring probe is connected with the mainframe box through a second electric plug hole 6 and is fixed inside a hole groove 9 at the top of a crystallizer sealing cover 8;
the Raman spectrum measuring probe is connected with the mainframe box through a third electric plug hole 7 and is fixed inside a hole groove 9 at the top of a crystallizer sealing cover 8;
compared with the prior art, the utility model realizes the multi-channel crystal screening automatic control equipment and the method, the six-channel crystal unit 1 is arranged, the particle shape granularity measurement, the infrared concentration measurement and the Raman spectrum measurement are expanded on the basis of realizing the basic functions of temperature control, turbidity measurement, stirring and feeding, the particle shape granularity measurement can realize the real-time accurate measurement of the particle shape and the size in the crystal screening process, the infrared concentration measurement can utilize the infrared spectrum to analyze the concentration of a crystal sample through Fourier transform combined with chemometrics modeling, the in-situ on-line measurement of the concentration and the supersaturation degree is realized, the expansion of the Raman spectrum measurement can help to realize the identification of polymorphic crystals in the crystal screening process, and the conversion among the polymorphic crystals and the conversion from amorphous crystals to crystalline forms are observed in real time. This design simple structure provides abundant measurement function for the process of crystallization screening for the screening process is accurate high-efficient fast more.
It should be noted that the specific model specifications of the cooling cycle, the turbidity meter, the magnetic stirrer, the mechanical stirrer, the feed pump, the particle size analyzer, the infrared concentration measuring instrument and the raman spectroscopy measuring instrument need to be determined by type selection according to the actual specification of the device, and the specific type selection calculation method adopts the prior art in the field, so detailed description is omitted.
It should be noted that the power supply and the principle of the circulation cooler, the turbidimeter, the magnetic stirrer, the mechanical stirrer, the feed pump, the particle size analyzer, the infrared concentration meter and the raman spectrometer are clear to those skilled in the art and will not be described in detail herein.
It should be noted that the control program and the specific operation flow of the upper software are prior art and will be clear to those skilled in the art, and detailed description is not given here.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. An automatic control device for multi-channel crystal screening can realize parallel crystal screening of a plurality of channel crystal units, wherein each channel crystal unit comprises a temperature measurement control device, a circulating cooler, a magnetic stirrer, a mechanical stirrer, a feeding pump, a turbidity meter, a grain shape and granularity meter, an infrared concentration meter and a Raman spectrum meter,
the temperature measurement control device comprises a crystallization unit (1), an electric heating unit and a PID controller, wherein the crystallization unit (1) comprises a crystallizer, a metal heat transfer body, a cooling liquid jacket (2) and a temperature measurement unit, a water inlet and a water outlet are respectively arranged on two sides of the cooling liquid jacket (2), the water outlet is connected with a one-way valve, the water inlet is connected with an electric regulating valve, the circulating cooler is communicated with the cooling liquid jacket (2) and used for supplying and conveying cooling liquid, the PID controller changes the flow of the cooling liquid entering the cooling liquid jacket (2) by controlling the opening degree of the valve, and the metal heat transfer body transfers the temperature of the crystallizer and is used for controlling the temperature reduction process of a sample in the crystallizer;
the electric heating unit is positioned at the bottom of the crystallization unit (1), and the PID controller is used for controlling the heating of the sample in the crystallizer;
the temperature measuring unit comprises a temperature measuring probe arranged in the crystallizer and a temperature measuring probe of the electric heating unit, the temperature measuring probe of the sample in the crystallizer is directly immersed in the crystallizer to measure the temperature of the sample, and the temperature signal is transmitted into the PID controller;
the magnetic stirrer is positioned at the bottom of the crystallization unit (1), and a stirring switch and the rotating speed of the magnetic stirrer are controlled by an upper computer;
the mechanical stirrer comprises a stirring paddle and a motor, the stirring paddle penetrates through a crystallizer sealing cover (8) to enter the interior of the crystallizer, and clamping platforms are arranged beside the channels and used for fixing the motor of the mechanical stirrer;
the feeding pump is arranged outside the mainframe box and is provided with a feeding pipeline and a plurality of discharging pipelines, the feeding pipeline is connected with a sample pool to be added, and the discharging pipelines are respectively correspondingly connected with the crystallizers with a plurality of channels and penetrate through the crystallizer sealing covers (8) to enter the crystallizers;
probes of the turbidity measuring instrument, the grain shape particle size analyzer, the infrared concentration measuring instrument and the Raman spectrum measuring instrument are all led out from the inside of the main case and are fixed in a hole groove of a sealing cover (8) of the crystallizer, and all the probes are immersed in a sample;
the probe size homoenergetic of on-line process monitoring equipment gets into crystallization unit (1), be provided with data transmission module in the mainframe box for with data transmission to show in the host computer.
2. The automatic control equipment for multi-channel crystal screening as claimed in claim 1, wherein the crystallizer sealing cover (8) is made of polytetrafluoroethylene and is provided with a plurality of hole grooves (9), the hole grooves (9) are connected with probes through threaded connectors, and the probes penetrate through the crystallizer sealing cover (8).
3. The automated control equipment for multichannel crystal screening according to claim 1, characterized in that said magnetic stirrer is used to stir single or multiple said crystallizers in the crystallization unit (1) simultaneously.
4. The automated control equipment for multichannel crystal screening as claimed in claim 1, wherein the number of the crystallization units (1) of several channels is six, and the channels of each group are independent.
5. The automated control equipment for multichannel crystal screening as claimed in claim 1, wherein the switches and communication interfaces of the magnetic stirrer, the mechanical stirrer, the feeding pump, the turbidity meter, the grain size analyzer, the infrared concentration meter and the raman spectrometer are respectively disposed on the back of the main cabinet.
6. The automated control equipment for multichannel crystal screening as claimed in claim 1, wherein said metal heat-transfer body comprises a single-hole metal heat-transfer body (11) and a multi-hole metal heat-transfer body (12), said single-hole metal heat-transfer body (11) is used for realizing crystallization of a single said crystallizer, and said multi-hole metal heat-transfer body (12) is used for realizing simultaneous crystallization of a plurality of said crystallizers.
7. The automated control equipment for multi-channel crystal screening as claimed in claim 1, wherein said metal heat-transfer body is provided with a metal diameter-enlarging ring, said metal diameter-enlarging ring is in close contact with said metal heat-transfer body for enlarging the diameter of said crystallizer.
8. The automated control equipment for multichannel crystal screening as claimed in claim 1, wherein said turbidity meter, said particle size analyzer, said infrared concentration meter, said raman spectrometer and said mechanical stirrer are electrically connected to said main cabinet by plugging.
9. The automated control equipment for multichannel crystal screening as claimed in claim 1, wherein the stirring switches and rotation speeds of the magnetic stirrer and the mechanical stirrer are controlled by a host computer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120766738.4U CN216386773U (en) | 2021-04-15 | 2021-04-15 | Multichannel crystallization screening automated control equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120766738.4U CN216386773U (en) | 2021-04-15 | 2021-04-15 | Multichannel crystallization screening automated control equipment |
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| Publication Number | Publication Date |
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| CN216386773U true CN216386773U (en) | 2022-04-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202120766738.4U Active CN216386773U (en) | 2021-04-15 | 2021-04-15 | Multichannel crystallization screening automated control equipment |
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| CN (1) | CN216386773U (en) |
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- 2021-04-15 CN CN202120766738.4U patent/CN216386773U/en active Active
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