A multi-channel vacuum sublimation device and its usage method

Abstract

This application relates to the technical field of solid organic compound purification devices, and specifically relates to a multi-channel vacuum sublimation device and its usage method, which includes at least two deposition chambers, at least two air extraction connection devices, and a multi-port normalization valve. One end of each of the air extraction connection devices is connected to the port of the deposition chamber; the multi-port normalization valve includes at least two pipelines, a switching valve, and a conversion joint. After the at least two pipelines are connected in parallel, they are connected to the conversion joint. The switching valve is arranged between the parallel connection of the at least two pipelines and the conversion joint. One end of the pipeline is connected to the air extraction connection device, and the conversion joint is used to connect to a vacuum system. The multi-channel vacuum sublimation device provided by this application is flexible in assembly, low in price, small in size, easy to operate, and high in efficiency. At the same time, it can purify multiple samples by vacuum sublimation, is easy to control conditions, and is suitable for popularization and use under laboratory conditions such as universities and research institutes.

Description

Technical Field

[0001] This application belongs to the technical field of solid organic compound purification devices, and particularly relates to a multi-channel vacuum sublimation device and a usage method thereof. Background Art

[0002] In the field of organic chemistry, high-purity organic compound samples are of great scientific research significance for the research of molecular structure identification, spectral properties, and biological activities. For organic compounds with poor solubility, especially organic small molecules containing large π-conjugated systems, there are problems that are difficult to separate and purify by conventional methods such as column chromatography, thin-layer chromatography, and recrystallization. Therefore, it is even more difficult to enrich in large quantities and grow crystals by the solution method. In addition, the products separated by the solution method often contain interference from impurities such as organic solvents, water, and silica gel during structure identification, and it is difficult to obtain high-standard structure characterization spectra and results. Sublimation is a commonly used method for purifying solid compounds, but for organic compounds with relatively high melting and boiling points, it is difficult to purify them by atmospheric sublimation. Vacuum sublimation under reduced pressure conditions, by controlling the conditions, realizes the separation and purification of solid organic compounds and crystal growth, which is an effective way to solve the above problems.

[0003] In the field of organic semiconductor materials, a large number of studies have shown that the purity of organic semiconductor materials has a crucial impact on the performance of organic semiconductor devices. Therefore, how to obtain high-purity organic semiconductor materials has become an urgent problem for scientific researchers to solve. After years of development, the vacuum gradient sublimation technology has become one of the most commonly used methods for purifying organic semiconductor materials because of its high sample purification degree. Target crystals can also be obtained through vacuum sublimation, which has extremely important research significance for determining the molecular structure and spatial packing mode of the target substance, and discussing various intermolecular forces.

[0004] However, currently, almost all commercially available vacuum sublimation devices are integrated and fixed, with advantages such as a wide application range, a large amount of purified samples, and high purity. However, they are generally expensive, large in volume, and complex in operation, which limits their promotion and application in laboratory environments such as universities and research institutes. In addition, the deposition cavity of commercially available vacuum sublimation devices is generally not visible during operation, which is not conducive to controlling the conditions for crystal growth, and usually only one sample can be sublimated and purified at a time. Summary of the Invention

[0005] The technical problem solved by this application is that the existing vacuum sublimation device has a complex structure, a large amount of purified samples, can only purify one sample at a time, and has low purification efficiency. This application provides a vacuum sublimation device with a simple structure that can be used to purify at least two samples at a time.

[0006] This application is implemented through the following technical solutions. A multi-channel vacuum sublimation device includes: at least two deposition chambers, at least two air extraction connection devices, and a multi-port normalization valve. One end of each air extraction connection device is connected to the port of the deposition chamber; the multi-port normalization valve includes at least two pipelines, a switching valve, and a conversion joint. After at least two pipelines are connected in parallel, they are connected to the conversion joint. The switching valve is connected in series with the pipeline. One end of the pipeline is connected to the air extraction connection device, and the conversion joint is used to connect to the vacuum system.

[0007] Preferably, a buffer device or a single-channel filtering device is provided between the air extraction connection device and the multi-port normalization valve. The buffer device is used to collect the samples overflowing from the deposition chamber. The single-channel filtering device allows the samples in the deposition chamber to flow out through the single-channel filtering device, and the samples cannot flow into the deposition chamber from one side of the single-channel filtering device.

[0008] Preferably, the buffer device includes a buffer bottle and a matching cold trap. The cold trap is arranged outside the buffer bottle. The buffer bottle consists of two upper and lower parts that can be opened, and the connection part can be fixed with an iron clamp; the matching cold trap is a long cylinder with a sandwich. The sandwich is in a vacuum, and the inside can be cooled with different refrigerants such as liquid nitrogen, dry ice, and ice-water bath according to needs. The cold trap can also be replaced by a low-temperature cold bath tank with alcohol as the medium. The buffer device can effectively prevent the solvents and sample powders wrapped in the samples from contaminating the vacuum system, and is convenient for disassembly and cleaning.

[0009] Preferably, a sample outer tube, at least two deposition rings, a connecting component, and a fixing tube are arranged in the deposition chamber. The outer wall of the deposition ring is parallel to the inner wall of the sample outer tube. At least part of the deposition ring is composed of two detachable semi-circular deposition rings. Adjacent two deposition rings are detachably and fixedly connected through the connecting component. The fixing tube is arranged at least at the opening end of the deposition chamber for fixing at least two deposition rings. The fixing tube is arranged at least at the opening end of the deposition chamber for fixing at least two deposition rings.

[0010] Preferably, the deposition ring is a quartz deposition ring. The deposition ring includes two types, an integral deposition ring and two symmetric semi-circular deposition rings that are closely combined into a ring. It can be a combination of two types of deposition rings. The inner diameter of the deposition ring is slightly larger than the outer diameter of the crucible, and the length is slightly longer than the crucible.

[0011] Preferably, it further includes a three-way valve and a gas storage device. The first channel of the three-way valve is connected to the conversion joint of the multi-port normalization valve. The second channel of the three-way valve is connected to the gas storage device. The third channel of the three-way valve is used to connect to the vacuum system; when the vacuum system is closed, the three-way valve connects the multi-port normalization valve and the gas storage device; when the vacuum system is opened, the three-way valve connects the multi-port normalization valve and the vacuum system.

[0012] Preferably, it further includes a vacuum gauge, which is arranged between the multi-port unifying valve and the three-way valve; the vacuum system includes a two-stage vacuum system composed of two mechanical pumps, and the vacuum degree of one mechanical pump is higher than that of the other mechanical pump.

[0013] Preferably, the air extraction connection device includes a connection body, a screw plug, a first rubber ring, a switch rotation, a second rubber ring and a conversion joint. The first rubber ring and the second rubber ring are respectively arranged at both ends of the connection body. A screw plug is arranged at one end of the connection body, and the screw plug is used to connect with the deposition cavity; a conversion joint is arranged at the other end of the connection body.

[0014] Preferably, the multi-port unifying valve further includes filters. There are several filters, which are respectively arranged on each pipeline; or there is one filter, which is arranged on the conversion joint. The filter is preferably made of metal, polytetrafluoroethylene or ceramic and other materials, and is attached with an activated carbon film, which can adsorb residual trace solid particles or solvents to protect the vacuum system.

[0015] Furthermore, it further includes at least two heating devices, which are used to provide heat sources for the deposition cavity.

[0016] Preferably, the heating device includes a heating cylinder and a temperature control device. The temperature control device is used to accurately control the temperature of the heating cylinder, and has the characteristics of small volume and easy movement. The size specifications are determined according to specific experiments;

[0017] Furthermore, the heating cylinder includes a heating zone and a heat preservation zone. The outside of the heating cylinder is coated with a heat insulation material layer, and multiple heating cylinders can work in parallel to provide heat sources for multiple deposition cavities at the same time.

[0018] The vacuum system is mainly composed of two mechanical pumps with different vacuum degrees, namely a low-vacuum mechanical pump and a high-vacuum mechanical pump, which constitute a two-stage vacuum system. It can not only meet the requirements of vacuum sublimation purification of general solid organic samples, but also effectively reduce accidental material flushing caused by sudden change of vacuum degree; and it is inexpensive, easy to assemble and convenient to maintain.

[0019] The entire sublimation purification process of the multi-channel vacuum sublimation device of the present application is visual. By observing the sublimation situation of the sample in the deposition cavity, it is possible to accurately control the heating part, temperature and duration, and it is easier to obtain the crystals of the sublimated sample. The multi-channel vacuum sublimation device of the present application can be used for vacuum sublimation purification or crystal growth.

[0020] The present application also includes a second solution, the usage method of the above multi-channel vacuum sublimation device, including:

[0021] The sample is added to the bottom of the deposition cavity, the air extraction connection device is closed, so that the deposition cavity and the multi-port unifying valve are in a non-connected state, and the vacuum system is turned on;

[0022] Slowly open the air extraction connection device to connect the deposition chamber with the vacuum system until the vacuum degree of the multi-channel vacuum sublimation device is stable.

[0023] Furthermore, it also includes turning on the heating device to perform sublimation purification of the sample.

[0024] Beneficial effects:

[0025] (1) For the multi-channel vacuum sublimation device of the present application, by setting at least two deposition chambers and a multi-port normalization valve, a set of vacuum system can be used to form a vacuum system for at least two deposition chambers, enabling at least two samples to be purified simultaneously, or one sample to be purified simultaneously in at least two deposition chambers, effectively improving the purification efficiency and saving the experimental equipment and the space occupied by the equipment.

[0026] (2) For the multi-channel vacuum sublimation device of the present application, by setting a buffer device or a single-channel filtration device, the gas overflowing from the deposition chamber can be filtered by the buffer device to avoid the mutual contamination of samples between the deposition chambers; or by setting a single-channel filtration device, the sample can overflow from the deposition chamber but cannot overflow into the deposition chamber, thereby avoiding the contamination of the sample in the deposition chamber.

[0027] (3) For the multi-channel vacuum sublimation device of the present application, at least two deposition rings are arranged in the deposition chamber, enabling the sample to be deposited inside the deposition rings at different temperature gradients. At the same time, at least part of the deposition rings are composed of two semi-rings, making it easy to take out the deposition ring after the sample sublimation is completed, and the two semi-rings make the collection of the sample more convenient.

[0028] (4) For the multi-channel vacuum sublimation device of the present application, with the three-way valve and the gas storage device, when the vacuum system is closed after the sublimation is completed, since the system is still in a high-temperature state, by connecting the gas storage device with the system, the system is filled with the protective gas, which can improve the service life of each component in the multi-channel vacuum sublimation device and protect the sample at the same time.

[0029] (5) For the multi-channel vacuum sublimation device of the present application, the multi-port normalization valve also includes a filter screen, which can avoid the contamination of the vacuum system by impurities.

[0030] (6) The multi-channel vacuum sublimation device of the present application is flexible in assembly, low in price, small in size, easy to operate and high in efficiency. At the same time, it can perform vacuum sublimation purification on multiple samples, is easy to control conditions, and is especially suitable for the sublimation purification of solid organic small molecule samples, and is suitable for use under laboratory conditions such as universities and research institutes. Description of the drawings

[0031] To more clearly illustrate the technical solutions of the embodiments of the present application, the accompanying drawings of the embodiments will be briefly introduced below. Obviously, the accompanying drawings in the following description only relate to some embodiments of the present application and do not limit the present application.

[0032] Figure 1 It is a schematic structural diagram when the deposition cavity of the multi-channel vacuum sublimation device provided by the embodiment of the present application is horizontally placed.

[0033] Figure 2 It is a schematic structural diagram when the deposition cavity of the multi-channel vacuum sublimation device provided by the embodiment of the present application is vertically placed.

[0034] Figure 3 It is a schematic structural diagram of the heating device provided by the embodiment of the present application.

[0035] Figure 4 It is a schematic structural diagram of the deposition cavity provided by the embodiment of the present application.

[0036] Figure 5 It is a three-dimensional structural diagram of the semi-circular deposition ring provided by the embodiment of the present application.

[0037] Figure 6 It is a schematic structural diagram of the air extraction connection device provided by the embodiment of the present application.

[0038] Figure 7 It is a schematic structural diagram of the multi-port normalization valve provided by the embodiment of the present application. Detailed implementation manners

[0039] The following are embodiments of the present application, which are only used for explaining the present application and not for limiting it.

[0040] Embodiment 1

[0041] Please refer to Figure 1 It is a schematic structural diagram when the deposition cavity of the multi-channel vacuum sublimation device provided by the embodiment of the present application is horizontally placed.

[0042] Specifically, the multi-channel vacuum sublimation device of the embodiment of the present application includes two deposition cavities 2, two air extraction connection devices 3 and a multi-port normalization valve 7. One end of each air extraction connection device 3 is connected to the port of the deposition cavity 2; among them, as Figure 7 shown, the multi-port normalization valve 7 includes four pipelines 7-1, four switching valve valves 7-2, a filter screen 7-3 and a conversion joint 7-4. The four pipelines 7-1 are connected in parallel and then connected to the conversion joint 7-4. The four pipelines 7-1 are respectively connected in series with the four switching valve valves 7-2. The four pipelines 7-1 are connected in parallel and then connected in series with the conversion joint 7-4. A filter screen 7-3 is arranged on the conversion joint 7-4. The switching valve 7-2 is used to independently control each pipeline 7-1; continue asFigure 1 As shown, one end of the pipeline 7-1 is connected to the air extraction connection device 3, and the adapter 7-4 is used to connect to the vacuum system 10; the other end of the air extraction connection device 3 is connected to the pipeline 7-1 of the multi-port unifying valve 7, and the filter screen 7-3 is used to protect the vacuum system 10 to prevent the samples in the deposition cavity 2 from flowing into the vacuum system 10.

[0043] It should be noted that there are two deposition cavities 2 in this embodiment. In other embodiments, there may be multiple deposition cavities 2; there are four pipelines of the multi-port unifying valve 7 in this embodiment. In other embodiments, the pipelines of the multi-port unifying valve 7 may be two or three or more than four; the adapter 7-4 of the multi-port unifying valve 7 in this embodiment is provided with a filter screen 7-3. In other embodiments, the filter screen 7-3 may not be provided, or there may be at least two filter screens 7-3, which are respectively arranged on the pipeline 7-1.

[0044] As a preferred solution, in this embodiment, a buffer device 6 is arranged between the air extraction connection device 3 and the multi-port unifying valve 7. The buffer device 6 is used to collect the samples overflowing from the deposition cavity 2 to prevent the samples in one deposition cavity 2 from overflowing and flowing into another deposition cavity 2, thus avoiding sample contamination. In other embodiments, a single-channel filtering device (not shown in the figure) may also be arranged between the air extraction connection device 3 and the multi-port unifying valve 7, which can allow the samples in the deposition cavity 2 to flow out through the single-channel filtering device, and the samples cannot flow into the deposition cavity from one side of the single-channel filtering device, so as to avoid the occurrence of sample contamination between the deposition cavities 2. Of course, in other embodiments, the buffer device 6 may not be arranged between the air extraction connection device 3 and the multi-port unifying valve 7.

[0045] Specifically, the air extraction connection device 3 and the buffer device 6 are connected by a pressure-resistant pipe 5, and a clamp 4 is arranged at the connection to make it detachably and fixedly connected, and the connection has good sealing performance.

[0046] Specifically, in this embodiment, the buffer device 6 is mainly composed of a buffer bottle and a supporting cold trap. The buffer bottle consists of two upper and lower parts and can be separated for easy disassembly and cleaning; the cold trap is a long tube with a vacuum interlayer, and a refrigerant is arranged in the cold trap, and the refrigerant depends on specific experiments.

[0047] In this embodiment, the adapter 7-4 of the multi-port unifying valve 7 is connected to the vacuum system 10, and a vacuum gauge 8 is provided between the adapter 7-4 and the vacuum system 10 to facilitate the detection of the vacuum degree of the device system. As a preferred solution, a three-way valve 9 is provided between the vacuum gauge 8 and the vacuum system 10. The first channel of the three-way valve 9 is connected to the adapter 7-4 of the multi-port unifying valve 7, the vacuum gauge 8 is arranged between the adapter 7-4 and the first channel, the second channel of the three-way valve 9 is connected to the gas storage device 12, and the third channel of the three-way valve 9 is used to connect to the vacuum system 10; when the vacuum system 10 is closed, the three-way valve 9 connects the multi-port unifying valve 7 and the gas storage device 12; when the vacuum system 10 is opened, the three-way valve 9 connects the multi-port unifying valve 7 and the vacuum system 10. By providing the three-way valve 9 and the gas storage device 12 between the adapter 7-4 of the multi-port unifying valve 7 and the vacuum system 10, when the vacuum system 10 is turned on, the connection between the three-way valve 9 and the gas storage device 12 is closed, which does not affect the operation of the multi-channel vacuum sublimation device system; when the sublimation is completed and the vacuum system is closed, the multi-channel vacuum sublimation device system is still in a high-temperature state. By connecting the gas storage device 12 to the multi-channel vacuum sublimation device system, the multi-channel vacuum sublimation device system is filled with a protective gas, which improves the service life of each component in the multi-channel vacuum sublimation device; at the same time, it can be used to protect the sample in the deposition chamber 2.

[0048] Preferably, as Figure 4 and 5 shown, the deposition chamber 2 includes a sample outer tube 2-1, at least two deposition rings 2-3 arranged in the sample outer tube 2-1, a connecting member 2-4, and a fixing tube 2-5. The outer wall of the deposition ring 2-3 is parallel to the inner wall of the sample outer tube 2-1. A part of the deposition rings 2-3 are composed of two detachable semi-circular deposition rings 2-3-1. Adjacent two deposition rings 2-3 are detachably and fixedly connected through the connecting member 2-4. A part of the deposition rings 2-3 are integral deposition rings. The fixing tube 2-5 is arranged at the opening end of the deposition chamber 2 for fixing at least two deposition rings 2-3. In this embodiment, there are five deposition rings 2-3 and connecting members 2-4 respectively. As a variation, the number of deposition rings 2-3 and connecting members 2-4 can also be set as needed, and this embodiment does not make specific limitations. By providing the connecting member 2-4, adjacent two deposition rings 2-3 can be tightly connected, and the two semi-circular deposition rings 2-3-1 will not be misaligned. At least two deposition rings 2-3 are arranged in the deposition chamber 2, so that the sample can be deposited inside the deposition rings 2-3 at different temperature gradients. At the same time, the deposition ring is composed of two semi-circular deposition rings 2-3-1, so that after the sample sublimates, the deposition ring 2-3 is easy to take out, and the two semi-circular deposition rings 2-3-1 make the collection of the sample more convenient.

[0049] Specifically, as Figure 6As shown in the figure, the air extraction connection device 3 includes a connection body 3-6, a screw plug 3-1, a first rubber ring 3-2, a switch rotation 3-3, a second rubber ring 3-5, and an adapter 3-4. The first rubber ring 3-2 and the second rubber ring 3-5 are respectively arranged at both ends of the connection body 3-6. A screw plug 3-1 is arranged at one end of the connection body 3-6, and the screw plug 3-1 is used to connect with the deposition cavity 2; an adapter 3-4 is arranged at the other end of the connection body 3-6.

[0050] Furthermore, in this embodiment, the multi-channel vacuum sublimation device further includes two heating devices 1. The heating device 1 is used to provide a heat source for the deposition cavity 2. In other embodiments, the heating device 1 can also be one or more. The heating devices 1 are arranged in one-to-one correspondence with the deposition cavity 2; or one heating device 1 can correspond to two or more deposition cavities 2. The number of the heating devices 1 is not specifically limited in this embodiment.

[0051] Specifically, as Figure 3 shown, in this embodiment, the heating device 1 includes a temperature control device 1-1 and a heating cylinder. The outside of the heating cylinder is coated with a heat insulation material layer. The heating cylinder includes a heating zone 1-2 and a heat preservation zone 1-3. The heating zone 1-2 is used to heat the deposition cavity 2, and the heat preservation zone 1-3 is used for heat preservation to complete deposition and crystal growth.

[0052] It should be noted that during the process of vacuum sublimation purification using the heating device 1, in order to better control the heating temperature and heating time, an external temperature detector 11 can be closely attached to the sample outer tube 2-1 of the deposition cavity 2 to monitor the temperature change of the sublimation system.

[0053] The vacuum system 10 of the embodiment of the present application is composed of a low-vacuum mechanical pump 10-1 and a high-vacuum mechanical pump 10-2. The two vacuum mechanical pumps form a two-stage vacuum system, which can effectively reduce the occurrence of sample flushing.

[0054] The above is the multi-channel vacuum sublimation device of the embodiment of the present application. In other embodiments, as Figure 2 shown, the deposition cavity 2 can also be placed vertically. The connection method of the vacuum sublimation device is the same as that of this embodiment. Compared with the horizontal placement method, the vertical placement method is less likely to cause flushing and the purification is faster.

[0055] As Figure 1 shown, the embodiment of the present application also includes a second solution. The usage method of the above multi-channel vacuum sublimation device includes:

[0056] 1. Add the sample to the bottom of the deposition cavity 2, close the air extraction connection device 3, so that the deposition cavity 2 and the multi-port normalization valve 7 are in a non-connected state, and turn on the vacuum system 10;

[0057] Second, slowly open the air extraction connection device 3 to connect the deposition chamber 2 with the vacuum system 10, and wait for the vacuum degree of the multi-channel vacuum sublimation device to stabilize.

[0058] Third, turn on the heating device 1 to perform sublimation purification of the sample.

[0059] Specifically, as Figure 1 and Figure 4 shown, first, select and connect the deposition chamber 2 and corresponding components of corresponding specifications according to the mass of the sample to be purified required for the specific experiment. Then evenly spread the sample to be sublimated on the inner wall of the crucible 2-2, place the crucible 2-2 into the integrated deposition ring 2-3, and further fix and place the deposition ring 2-3 assembled by the connection component 2-4 and the semi-circular deposition ring 2-3-1 according to the specific experimental requirements to tightly hoop each deposition ring 2-3. The last section is the integrated deposition ring 2-3; among them, the deposition ring 2-3 assembled by the integrated deposition ring 2-3 and two semi-circular deposition rings 2-3-1 can be used in combination to facilitate scraping and collection of the sublimated sample. After assembly, slowly place the sample outer tube 2-1, and finally place the fixing tube 2-5 to fix, completing the sample loading. Specifically, in this embodiment, the connection component 2-4 is an annular clamp, the inner diameter of the annular clamp is the same as or slightly larger than the outer diameter of the deposition ring 2-3, so that the deposition ring 2-3 can be snapped into the annular clamp. A retaining ring is provided on the inner wall of the annular clamp, and there is a certain distance between the retaining ring and both ends of the annular clamp, which is convenient for the deposition ring 2-3 to be snapped into both sides respectively. The ring radius of the retaining ring is 2 mm - 1 cm. By setting the retaining ring, it is convenient to fix the semi-circular deposition ring 2-3-1 to prevent the semi-circular deposition ring 2-3-1 from being misaligned along the central axis direction. In other embodiments, the connection component 2-4 can also be of other types, as long as it can fix two adjacent deposition rings 2-3, and the present application does not specifically limit the connection component 2-4.

[0060] It should be noted that in other embodiments, when using a multi-channel vacuum sublimation device with the deposition chamber placed vertically as Figure 2 shown, the sample loading sequence is to first place the sample at the bottom of the quartz crucible 2-2, then fix the quartz crucible 2-2, the deposition ring 2-3 and the connection component 2-4 in sequence, slowly place them into the sample outer tube 2-1, then place the fixing tube 2-5, and slowly place the entire assembled deposition chamber 2 vertically to complete the sample loading.

[0061] As Figure 1 and Figure 6As shown in the figure, the deposition chamber 2 filled with samples is slowly connected to the evacuation connection device 3 with the switching rotary valve 3-3 closed. It is tightened with the screw plug 3-1 and the rubber ring 3-2 to ensure sealing. Connect the pressure-resistant pipe 5 through the adapter 3-4, and then connect the buffer device 6, the multi-port unifying valve 7, the vacuum gauge 8, the three-way valve 9 and the vacuum system 10 in sequence. The connection points are tightened with the clamp 4 to ensure sealing. Finally, the deposition chamber 2 is slowly placed into the heating cylinder 1-2 of the heating device 1. Among them, the outer tube 2-1 of the sample is longer than the heating cylinder, so that the sample can complete heating sublimation in the heating area of the heating cylinder, deposition and crystal growth in the heat preservation area, and the outer tube 2-1 of the sample exposed outside the heating cylinder cools down in the air. The assembly of the entire multi-channel vacuum sublimation device is completed, waiting for evacuation and heating sublimation.

[0062] Slowly start the mechanical pump with low vacuum degree in the vacuum system 10 to evacuate, and open the three-way valve 9, the switch valve 7-2 and the switching rotary valve 3-3 on the entire gas path in sequence. After the reading of the vacuum gauge 8 is stable, close the valve of the mechanical pump with low vacuum degree, and start the mechanical pump 10-2 with high vacuum degree to evacuate. After the reading of the vacuum gauge 8 is stable, open the valve of the mechanical pump with low vacuum degree. The mechanical pump 10-2 with high vacuum degree and the mechanical pump 10-1 with low vacuum degree in the vacuum system 10 work together to provide a vacuum environment for the deposition chamber 2. After the reading of the vacuum gauge 8 is stable again, turn on the heating device 1 to start vacuum sublimation purification. The vacuum system 10 in the embodiment of the present application is a two-stage vacuum system, which can effectively reduce the occurrence of sample flushing.

[0063] On the basis of previously measuring the melting point or decomposition temperature of each sample, as shown in 1 and 3, precisely control the temperature through the temperature control device 1-1 of the heating device, slowly heat the outer tube 2-1 of each sample with the heating cylinder, and set the corresponding heating rate gradient and stable heating duration according to the difference in thermal stability of each sample. During the heating and vacuum sublimation process, the heating cylinder 1-2 can be moved to observe the purification situation. When a sample is purified, the independent evacuation connection device 3 and the heating device 1 can be closed. After cooling, remove the deposition chamber 2 to complete vacuum sublimation purification. That is, it improves the purification efficiency and reduces unnecessary energy consumption. The sublimation purification process has strong visibility and high controllability.

[0064] After completing the vacuum sublimation purification, the gas storage device 12 connected to the three-way valve 9 can be opened. The gas storage device 12 stores inert gas, and inert gas is introduced into the deposition chamber 2 to prevent the sample from being affected by water and oxygen in the air, which is convenient for long-term storage of the sublimation purification product.

[0065] Embodiment 2

[0066] This embodiment uses the multi-channel vacuum sublimation device of Embodiment 1 to test the multi-channel vacuum sublimation device based on the sublimation purification effects of bi-thiazole, bi-pyridine, and fluorenone compounds. All the sample compounds involved have poor solubility and good thermal stability. Among them, the samples numbered 1 to 3 in Table 1 are bi-thiazole compounds, the sample numbered 4 is a bi-pyridine compound, and the samples 5 to 6 are fluorenone compounds. The specific experimental results are shown in Table 1 below.

[0067] Since the solubility of each of the above compounds is poor, the crude reactants are directly subjected to vacuum sublimation purification; after the first sublimation purification, no purity detection and yield calculation were carried out, and the second sublimation purification was directly carried out. After detection by nuclear magnetic resonance or elemental analysis, the purity of the products after the second sublimation purification was all >98%; there was still a small amount of cross-products that were not further purified; generally, the more times the sample is sublimated and purified, the higher the relative purity, but the relative loss during the scraping process is greater, especially when the sublimation amount is small, the loss caused by incomplete scraping is significantly increased.

[0068] Table 1: Results of sample sublimation purification

[0069]

[0070] It should be noted that after the thermal decomposition temperature of the crude product of the above samples was tested in advance, generally 2 to 4 samples with similar thermal stabilities were selected. In this embodiment, the samples numbered 1 to 4 in Table 1 above were taken as a group and sublimated and purified using the multi-channel vacuum sublimation device of Embodiment 1. Four deposition cavities 2 corresponding to those in Embodiment 1 were sufficient. The samples numbered 5 and 6 in the above table were taken as a group and sublimated and purified using the multi-channel vacuum sublimation device of Embodiment 1. As can be seen from Table 1 above, the multi-channel vacuum sublimation device involved in the present application has achieved the purification of several organic compounds with good conjugation, and has a good purification effect, and can obtain target products with high purity. By controlling the vacuum sublimation conditions, crystals of multiple target products can be obtained, and the crystal formation rate is relatively high.

[0071] It should be noted that in this embodiment, the multi-channel vacuum sublimation device of Embodiment 1 is used to purify different samples, and it can also perform vacuum sublimation purification on the same sample placed in multiple deposition cavities 2 to achieve the enrichment of the same sample quality.

[0072] Combined with the description and practice of the present application disclosed herein, other embodiments of the present application are readily conceivable and understandable to those skilled in the art. The description and embodiments are only considered to be exemplary, and the true scope and gist of the present application are defined by the claims.

Claims

1. A multi-channel vacuum sublimation device, characterized in that, Comprising: At least two deposition chambers (2); At least two air extraction connection devices (3), one end of each of the air extraction connection devices being connected to the port of the deposition chamber (2); And a multi-port normalization valve (7), including at least two pipelines (7-1), a switching valve (7-2) and an adapter (7-4), the at least two pipelines (7-1) being connected in parallel and then connected to the adapter (7-4), the switching valve (7-2) being connected in series with the pipeline (7-1), one end of the pipeline (7-1) being connected to the air extraction connection device (3), and the adapter (7-4) being used for connection to a vacuum system (10); A buffer device (6) or a single-channel filtering device is provided between the air extraction connection device (3) and the multi-port normalization valve (7), the buffer device (6) being used for collecting the samples overflowing from the deposition chamber (2), and the single-channel filtering device allowing the samples in the deposition chamber to flow out through the single-channel filtering device, and samples not flowing into the deposition chamber from one side of the single-channel filtering device.

2. The multi-channel vacuum sublimation device according to claim 1, wherein The deposition chamber (2) includes a sample outer tube (2-1) and at least two deposition rings (2-3), a connecting member (2-4) and a fixing tube (2-5) provided therein, the outer wall of the deposition ring (2-3) being parallel to the sample outer tube (2-1), at least part of the deposition ring (2-3) being composed of two detachable semi-circular deposition rings (2-3-1), and adjacent two deposition rings (2-3) being detachably and fixedly connected through the connecting member (2-4), and the fixing tube (2-5) being provided at least at the opening end of the deposition chamber (2) for fixing the at least two deposition rings (2-3).

3. The multi-channel vacuum sublimation device according to claim 1, wherein, Also included are a three-way valve (9) and a gas storage device, a first channel of the three-way valve (9) being connected to the adapter (7-4) of the multi-port normalization valve (7), a second channel of the three-way valve (9) being connected to the gas storage device (12), and a third channel of the three-way valve (9) being used for connection to the vacuum system (10).

4. The multi-channel vacuum sublimation device according to claim 3, characterized in that, Also included is a vacuum gauge (8), provided between the multi-port normalization valve (7) and the three-way valve (9); the vacuum system (10) includes a two-stage vacuum system composed of two mechanical pumps, and the vacuum degree of one of the mechanical pumps is higher than that of the other mechanical pump.

5. The multi-channel vacuum sublimation device according to claim 1, wherein The air extraction connection device (3) includes a connection body (3-6), a screw plug (3-1), a first rubber ring (3-2), a switch rotary valve (3-3), a second rubber ring (3-5) and an adapter (3-4), the first rubber ring (3-2) and the second rubber ring (3-5) being respectively provided at both ends of the connection body (3-6), the screw plug (3-1) being provided at one end of the connection body (3-6) for connection to the deposition chamber (2); and the adapter (3-4) being provided at the other end of the connection body (3-6).

6. The multi-channel vacuum sublimation device according to claim 1, characterized in that, The multi-port normalization valve (7) further includes a filter screen (7-3). There are several filter screens (7-3), which are respectively arranged on each pipeline (7-1); or there is one filter screen (7-3), which is arranged on the adapter (7-4).

7. The multi-channel vacuum sublimation device according to claim 1, wherein It further includes at least two heating devices (1), and the heating devices (1) are used to provide heat sources for the deposition chamber (2).

8. The method of using the multi-channel vacuum sublimation device according to any one of claims 1-7, characterized in that, Including: The sample is added to the bottom of the deposition chamber (2), the air extraction connection device (3) is closed, so that the deposition chamber (2) and the multi-port normalization valve (7) are in a non-connected state, and the vacuum system (10) is turned on; The air extraction connection device (3) is slowly opened, so that the deposition chamber (2) is connected to the vacuum system (10), and wait for the vacuum degree of the multi-channel vacuum sublimation device to be stable.

9. The method of using a multi-channel vacuum sublimation device according to claim 8, characterized in that, After the vacuum degree of the multi-channel vacuum sublimation device is stable, it further includes turning on the heating device (1) to perform sublimation purification of the sample.

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