CN211158659U - Multi-channel vacuum sublimation device - Google Patents

Abstract

The application relates to the technical field of solid organic compound purification devices, in particular to a multi-channel vacuum sublimation device which comprises at least two deposition cavities, at least two air extraction connecting devices and a multi-port normalization valve, wherein one end of each air extraction connecting device is connected with a port of each deposition cavity; the multi-port normalization valve comprises at least two pipelines, a switch valve and a first conversion joint, wherein the at least two pipelines are connected in parallel and then are connected with the first conversion joint, the switch valve is arranged between the at least two pipelines which are connected in parallel and the first conversion joint, one end of each pipeline is connected with the air suction connecting device, and the first conversion joint is used for being connected with a vacuum system. The application provides a multichannel vacuum sublimation device equipment is nimble, low price, small in size, easy operation and efficient, can purify a plurality of sample vacuum sublimation simultaneously, and easily control condition is suitable for and uses widely under laboratory conditions such as colleges and universities and scientific research institutions.

Description

Multi-channel vacuum sublimation device

Technical Field

The application belongs to the technical field of solid organic compound purification devices, and particularly relates to a multi-channel vacuum sublimation device.

Background

In the field of organic chemistry, high-purity organic compound samples have very important scientific research significance on molecular structure identification, spectral properties and biological activity research. For organic compounds with poor solubility, especially small organic molecules containing large pi conjugated systems, etc., there is a problem that separation and purification are difficult by conventional methods such as column chromatography, thin layer chromatography, recrystallization, etc., and therefore, it is more difficult to enrich a large amount and grow crystals by a solution method. In addition, the product obtained by the solution method often contains the interference of impurities such as organic solvent, water, silica gel and the like when the structure identification is carried out, and a high-specification structure characterization spectrogram and a high-specification structure characterization result are difficult to obtain. Sublimation is a common method for purifying solid compounds, but it is difficult to purify organic compounds having a relatively high melting point by sublimation at atmospheric pressure. Vacuum sublimation is carried out under the condition of reduced pressure, and separation and purification of solid organic compounds and crystal growth are realized by controlling the conditions, so that the method is an effective way for solving the problems.

For the field of organic semiconductor materials, a great deal of research has shown that the purity of organic semiconductor materials has a crucial influence on the performance of organic semiconductor devices. Therefore, how to obtain high-purity organic semiconductor materials becomes a difficult problem to be solved urgently by researchers. After many years of development, the vacuum gradient sublimation technology has been developed as one of the most commonly used methods for purifying organic semiconductor materials because of its advantage of high sample purification degree. The target crystal can be obtained through vacuum sublimation, and the method has extremely important research significance for determining the molecular structure and the space accumulation mode of the target and discussing various acting forces existing among molecules.

However, most of the commercial vacuum sublimation devices are fixed integrally at present, and have the advantages of wide application range, large amount of purified samples, high purity and the like, but generally have high price, large volume and complex operation, and limit popularization and application in laboratory environments such as universities and scientific research institutions. In addition, the deposition cavity is generally invisible in the operation of the commercial vacuum sublimation device, which is not beneficial to controlling the condition for growing crystals, and only one sample can be purified by sublimation at a time.

Disclosure of Invention

The technical problem that this application was solved lies in, current vacuum sublimation device structure is complicated, and purification sample volume is great, only can purify a sample once, and purification efficiency is low. The application provides a simple structure, once can be used for purifying the vacuum sublimation device of two kinds of at least samples.

This application is realized through following technical scheme, a multichannel vacuum sublimation device, includes: the device comprises at least two deposition cavities, at least two air extraction connecting devices and a multi-port normalization valve, wherein one end of each air extraction connecting device is connected with a port of each deposition cavity; the multi-port normalization valve comprises at least two pipelines, a switch valve and a first conversion joint, wherein the at least two pipelines are connected in parallel and then connected with the first conversion joint, the switch valve is connected with the pipelines in series, one end of each pipeline is connected with the air suction connecting device, and the first conversion joint is used for being connected with the vacuum system.

Preferably, a buffering device or a single-channel filtering device is arranged between the air exhaust connecting device and the multi-port normalizing valve, the buffering device is used for collecting samples overflowing from the deposition cavity, the single-channel filtering device can enable the samples in the deposition cavity 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.

Preferably, the buffer device comprises a buffer bottle and a matched cold trap, the cold trap is arranged outside the buffer bottle, the buffer bottle consists of an upper part and a lower part which can be opened, and the joint can be fixed by an iron clamp; the matched cold trap is a long cylinder with an interlayer, the interlayer is vacuum, the interior of the cold trap can be cooled by different refrigerants such as liquid nitrogen, dry ice, ice water bath and the like according to requirements, and the cold trap can also be replaced by a low-temperature cold bath taking alcohol as a medium. The buffer device can effectively prevent the solvent and sample powder wrapped in the sample from polluting a vacuum system, and is convenient to disassemble and clean.

Preferably, a sample outer tube, at least two deposition rings arranged in the sample outer tube, a connecting part and a fixing tube are arranged in the deposition cavity, the outer wall of each deposition ring is parallel to the inner wall of the sample outer tube, at least part of the deposition rings are formed by two detachable semicircular deposition rings, the adjacent two deposition rings are detachably and fixedly connected through the connecting part, the fixing tube is at least arranged at the opening end of the deposition cavity and used for fixing the at least two deposition rings, and the fixing tube is at least arranged at the opening end of the deposition cavity and used for fixing the at least two deposition rings.

Preferably, the deposition ring is a quartz deposition ring, the deposition ring comprises two types, an integral deposition ring and two symmetrical semicircular deposition rings are tightly combined into a ring, and the two types of deposition rings can be combined, wherein the inner diameter of the deposition ring is slightly larger than the outer diameter of the crucible, and the length of the deposition ring is slightly longer than the crucible.

Preferably, the vacuum pump further comprises a three-way valve and an air storage device, wherein a first channel of the three-way valve is connected with a first switching joint of the multi-port return valve, a second channel of the three-way valve is connected with the air storage device, and a third channel of the three-way valve is used for being connected with a vacuum system; when the vacuum system is closed, the three-way valve is communicated with the multi-port normalization valve and the gas storage device; when the vacuum system is turned on, the three-way valve communicates the multi-port return valve with the vacuum system.

Preferably, the device also comprises a vacuum meter which is arranged between the multi-port normalization valve and the three-way valve; the vacuum system comprises a two-stage vacuum system formed by two mechanical pumps, wherein the vacuum degree of one mechanical pump is higher than that of the other mechanical pump.

Preferably, the air exhaust connecting device comprises a connecting body, a threaded cock, a first rubber ring, a switch rotation, a second rubber ring and a second adapter, the first rubber ring and the second rubber ring are respectively arranged at two ends of the connecting body, the threaded cock is arranged at one end of the connecting body, and the threaded cock is used for being connected with the deposition cavity; the other end of the connecting body is provided with a second adapter.

Preferably, the multi-port normalizing valve further comprises a plurality of filter screens which are respectively arranged on each pipeline; or the filter screen is one and is arranged on the first conversion joint. The filter screen is preferably made of metal, polytetrafluoroethylene or ceramic, and an active carbon film is attached on the filter screen, so that residual micro solid particles or solvent can be adsorbed, and the vacuum system is protected.

Further, the device also comprises at least two heating devices, and the heating devices are used for providing a heat source for the deposition cavity.

Preferably, the heating device comprises a heating cylinder and a temperature control device, the temperature control device is used for accurately controlling the temperature of the heating cylinder, and the heating device has the characteristics of small volume and easy movement, and the size specification is determined by specific experiments;

further, the heating cylinder comprises a heating area and a heat preservation area, the outside of the heating cylinder is coated with a heat insulation material layer, a plurality of heating cylinders can work in parallel, and a heat source is provided for a plurality of deposition cavities.

The vacuum system mainly comprises two mechanical pumps with different vacuum degrees, namely a low-vacuum-degree mechanical pump and a high-vacuum-degree mechanical pump, so that a two-stage vacuum system is formed, the vacuum sublimation purification requirement of a common solid organic sample can be met, and accidental material flushing caused by sudden change of the vacuum degree can be effectively reduced; and the cost is low, the assembly is convenient and fast, and the maintenance is convenient.

The utility model provides a whole purification process of sublimating of multichannel vacuum sublimation device is visual, through observing the sublimation condition of sample in the deposit cavity, can realize accurate control heating position, temperature and time length, obtains the crystal of sublimating the sample more easily. The multichannel vacuum sublimation device of this application can be used to the vacuum sublimation purification, also can be used to crystal growth.

Has the advantages that:

(1) the utility model provides a multichannel vacuum sublimation device through setting up two at least deposit cavitys and multiport normalizing valve for adopt one set of vacuum system both can so that two at least deposit cavitys form the vacuum system, can purify two at least samples simultaneously, or a sample two at least deposit cavitys purify simultaneously, effectively improve purification efficiency, practice thrift the space that experimental facilities and equipment occupy.

(2) According to the multi-channel vacuum sublimation device, the buffer device or the single-channel filtering device is arranged, so that gas overflowing from the deposition cavity can be filtered through the buffer device, and the mutual pollution of samples among the deposition cavities is avoided; or by arranging the single-channel filtering device, the sample can overflow from the deposition cavity but cannot overflow into the deposition cavity, so that the sample in the deposition cavity is prevented from being polluted.

(3) The utility model provides a multichannel vacuum sublimation device sets up two at least deposit rings in the deposit cavity for the sample can deposit in the inside of the deposit ring of different temperature gradient departments, and at least partial deposit ring is constituteed for two semi-rings simultaneously, makes the sample sublimate the back, and the deposit ring easily takes out, and two semi-rings make the collection of sample more convenient.

(4) The utility model provides a multichannel vacuum sublimation device, three-way valve and gas storage device, after the sublimation is accomplished, when closing vacuum system, because the system still is in the high temperature state, through gas storage device and system intercommunication for fill protective gas in the system, can improve the life of each part among the multichannel vacuum sublimation device, protect the sample simultaneously.

(5) The utility model provides a multichannel vacuum sublimation device, multiport return valve still include the filter screen, can avoid impurity contamination vacuum system.

(6) The utility model provides a multichannel vacuum sublimation device, the equipment is nimble, low price, small in size, easy operation and efficient, can purify a plurality of sample vacuum sublimation simultaneously, and easily control the condition is particularly suitable for the sublimation purification of solid organic micromolecule sample, is suitable for using under laboratory conditions such as colleges and universities and scientific research institutions.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings of the embodiments will be briefly introduced below, and it is apparent that the drawings in the following description only relate to some embodiments of the present application and are not limiting on the present application.

Fig. 1 is a schematic structural diagram of a deposition chamber of a multi-channel vacuum sublimation apparatus provided in an embodiment of the present application, which is horizontally disposed.

Fig. 2 is a schematic structural diagram of a deposition chamber of the multi-channel vacuum sublimation device provided by the embodiment of the application when the deposition chamber is vertically arranged.

Fig. 3 is a schematic structural diagram of a heating device provided in an embodiment of the present application.

Fig. 4 is a schematic structural diagram of a deposition chamber provided in an embodiment of the present application.

Fig. 5 is a schematic perspective view of a semicircular deposition ring according to an embodiment of the present disclosure.

Figure 6 is a schematic structural view of a suction connection provided in an embodiment of the present application.

Fig. 7 is a schematic structural diagram of a multi-port normalization valve provided in an embodiment of the present application.

Detailed Description

The following are examples of the present application which are intended to be illustrative only and not limiting.

Example 1

Fig. 1 is a schematic structural diagram of a deposition chamber of a multi-channel vacuum sublimation apparatus according to an embodiment of the present disclosure, which is horizontally disposed.

Specifically, the multi-channel vacuum sublimation device in the embodiment of the application comprises two deposition cavities 2, two air extraction connecting devices 3 and a multi-port normalization valve 7, wherein one end of each air extraction connecting device 3 is connected with a port of each deposition cavity 2; as shown in fig. 7, the multi-port normalization valve 7 includes four pipelines 7-1, four switch valve valves 7-2, a filter screen 7-3, and a first conversion connector 7-4, the four pipelines 7-1 are connected in parallel and then connected to the first conversion connector 7-4, the four pipelines 7-1 are respectively connected in series with the four switch valve valves 7-2, the four pipelines 7-1 are connected in parallel and then connected in series with the first conversion connector 7-4, the filter screen 7-3 is disposed on the first conversion connector 7-4, and the switch valve 7-2 is used for individually controlling each pipeline 7-1; continuing with FIG. 1, one end of the line 7-1 is connected to the suction connection 3, and the first adapter 7-4 is adapted to be connected to the vacuum system 10; the other end of the air suction connecting device 3 is connected with a pipeline 7-1 of a multi-port return valve 7, and a filter screen 7-3 is used for protecting the vacuum system 10 so as to prevent the sample in the deposition cavity 2 from flowing to the vacuum system 10.

It should be noted that there are two deposition chambers 2 in this embodiment, and in other embodiments, there may be a plurality of deposition chambers 2; in the present embodiment, the number of the pipelines of the multi-end return valve 7 is four, and in other embodiments, the number of the pipelines of the multi-end return valve 7 may be two or three or more; in the embodiment, the strainer 7-3 is arranged on the first adapter 7-4 of the multi-port return valve 7, and in other embodiments, the strainer 7-3 is not arranged, or at least two strainers 7-3 are arranged on the pipeline 7-1 respectively.

Preferably, in this embodiment, a buffer device 6 is disposed between the suction connection device 3 and the multi-port normalization valve 7, and the buffer device 6 is used for collecting the samples overflowing from the deposition chambers 2, so as to prevent the samples in one deposition chamber 2 from overflowing and flowing to another deposition chamber 2, and prevent contamination between the samples. In other embodiments, a single-channel filter (not shown) may be disposed between the evacuation connection device 3 and the multi-port normalization valve 7, so that the sample in the deposition chamber 2 flows out through the single-channel filter, and the sample cannot flow into the deposition chamber from one side of the single-channel filter, thereby avoiding sample contamination between the deposition chambers 2. Of course, in other embodiments, the buffer device 6 may not be provided between the suction connection 3 and the multiport return valve 7.

Specifically, the air exhaust connecting device 3 is connected with the buffer device 6 through the pressure-resistant pipe 5, the clamp 4 is arranged at the joint of the air exhaust connecting device and the buffer device so that the air exhaust connecting device can be detachably and fixedly connected, and the sealing performance of the joint is good.

Specifically, in this embodiment, the buffer device 6 mainly comprises a buffer bottle and a matched cold trap, and the buffer bottle is composed of an upper part and a lower part which are separable, so that the buffer bottle is convenient to disassemble and clean; the cold trap is a long cylinder with a vacuum interlayer, and a refrigerant is arranged in the cold trap and is determined by specific experiments.

In this embodiment, the first adapter 7-4 of the multi-port normalization valve 7 is connected to the vacuum system 10, and the vacuum gauge 8 is disposed between the first adapter 7-4 and the vacuum system 10, so as to facilitate detection of the vacuum degree of the device system. As a preferred scheme, a three-way valve 9 is arranged between a vacuum meter 8 and a vacuum system 10, a first channel of the three-way valve 9 is connected with a first conversion joint 7-4 of a multi-port normalization valve 7, the vacuum meter 8 is arranged between the first conversion joint 7-4 and the first channel, a second channel of the three-way valve 9 is connected with a gas storage device 12, and a third channel of the three-way valve 9 is used for being connected with the vacuum system 10; when the vacuum system 10 is closed, the three-way valve 9 is communicated with the multi-port normalization valve 7 and the gas storage device 12; when the vacuum system 10 is turned on, the three-way valve 9 communicates the multi-port return valve 7 and the vacuum system 10. By arranging the three-way valve 9 and the gas storage device 12 between the first conversion joint 7-4 of the multi-port normalization valve 7 and the vacuum system 10, when the vacuum system 10 is opened, the three-way valve 9 and the gas storage device 12 are closed, so that the operation of a multi-channel vacuum sublimation device system is not influenced; after sublimation is finished, when the vacuum system is closed, the multi-channel vacuum sublimation device system is still in a high-temperature state and is communicated with the multi-channel vacuum sublimation device system through the gas storage device 12, so that the multi-channel vacuum sublimation device system is filled with protective gas, and the service life of each component in the multi-channel vacuum sublimation device is prolonged; while also serving to protect the sample within the deposition chamber 2.

Preferably, as shown in fig. 4 and 5, the deposition chamber 2 includes an outer sample tube 2-1, at least two deposition rings 2-3 disposed in the outer sample tube 2-1, a connecting member 2-4, and a fixing tube 2-5, wherein an outer wall of the deposition ring 2-3 is parallel to an inner wall of the outer sample tube 2-1, a portion of the deposition rings 2-3 is formed by two detachable semicircular deposition rings 2-3-1, two adjacent deposition rings 2-3 are detachably and fixedly connected by the connecting member 2-4, a portion of the deposition rings 2-3 is an integral deposition ring, and the fixing tube 2-5 is disposed at an open end of the deposition chamber 2 and is used for fixing at least two deposition rings 2-3. In this embodiment, the deposition rings 2 to 3 and the connecting members 2 to 4 are five, and as a modification, the number of the deposition rings 2 to 3 and the connecting members 2 to 4 may be set as required, and this embodiment is not particularly limited. The connecting parts 2-4 can be arranged to tightly connect two adjacent deposition rings 2-3, and the two semicircular deposition rings 2-3-1 can not be dislocated. At least two deposition rings 2-3 are arranged in the deposition cavity 2, so that a sample can be deposited in the deposition rings 2-3 at different temperature gradients, and meanwhile, the deposition rings are composed of two semicircular deposition rings 2-3-1, so that the deposition rings 2-3 are easy to take out after the sample is sublimated, and the two semicircular deposition rings 2-3-1 make the collection of the sample more convenient.

Specifically, as shown in fig. 6, the air suction connection device 3 comprises a connection body 3-6, a threaded cock 3-1, a first rubber ring 3-2, a switch rotation 3-3, a second rubber ring 3-5 and a second adapter 3-4, wherein the two ends of the connection body 3-6 are respectively provided with the first rubber ring 3-2 and the second rubber ring 3-5, one end of the connection body 3-6 is provided with the threaded cock 3-1, and the threaded cock 3-1 is used for connecting with the deposition chamber 2; the other end of the connecting body 3-6 is provided with a second adapter 3-4.

Further, in this embodiment, the multi-channel vacuum sublimation device further includes two heating devices 1, the heating devices 1 are used for providing heat sources for the deposition cavities 2, in other embodiments, one or more heating devices 1 may be provided, and the heating devices 1 and the deposition cavities 2 are arranged in one-to-one correspondence; or one heating device 1 may correspond to two or more deposition chambers 2, and the number of the heating devices 1 is not particularly limited in this embodiment.

Specifically, as shown in fig. 3, in the present embodiment, the heating device 1 includes a temperature control device 1-1 and a heating cylinder, an insulating material layer is coated outside the heating cylinder, the heating cylinder includes a heating area 1-2 and a holding area 1-3, the heating area 1-2 is used for heating the deposition chamber 2, and the holding area 1-3 is used for holding to complete deposition and crystal growth.

It should be noted that, in the process of performing vacuum sublimation purification by using the heating device 1, in order to better control the heating temperature and the heating time, the external temperature detector 11 may be closely attached to the sample outer tube 2-1 of the deposition chamber 2 to monitor the temperature change of the sublimation system.

The vacuum system 10 of the embodiment of the application consists of a low-vacuum mechanical pump 10-1 and a high-vacuum mechanical pump 10-2, and the two vacuum mechanical pumps form a two-stage vacuum system, so that the sample flushing condition can be effectively reduced.

Above be the multichannel vacuum sublimation device of this application embodiment, in other embodiments, as shown in fig. 2, deposition cavity 2 also can adopt the vertical mode of placing, and the connected mode of its air sublimation device is the same with this embodiment, compares horizontal mode of placing, and the vertical mode of placing is more difficult for towards the material, purification is more swift.

As shown in fig. 1, the method for using the multi-channel vacuum sublimation apparatus includes:

firstly, adding a sample into the bottom end of a deposition cavity 2, closing an air-extracting connecting device 3 to enable the deposition cavity 2 and a multi-port normalization valve 7 to be in a non-communicated state, and opening a vacuum system 10;

and secondly, slowly opening the air exhaust connecting device 3 to ensure that the deposition cavity 2 is communicated with the vacuum system 10 and the vacuum degree of the multi-channel vacuum sublimation device is stable.

And thirdly, starting the heating device 1 to carry out sublimation purification on the sample.

Specifically, as shown in fig. 1 and 4, the deposition chamber 2 and the corresponding components of the respective specifications are first selected and connected according to the quality of the purified sample required for the specific experiment. Then uniformly paving a sample to be sublimated on the inner side wall of the crucible 2-2, putting the crucible 2-2 into the integrated deposition ring 2-3, further fixedly placing a connecting part 2-4 and a deposition ring 2-3 assembled by the semicircular deposition ring 2-3-1 according to specific experimental requirements so as to tightly clamp each deposition ring 2-3, and finally forming the integrated deposition ring 2-3 in the last section; wherein, the deposition ring 2-3 formed by assembling the integral deposition ring 2-3 and the two semicircular deposition rings 2-3-1 can be matched for use, so that the sublimation sample can be scraped and collected conveniently; and slowly placing the sample outer tube 2-1 after the assembly is finished, and finally placing the sample outer tube 2-5 for fixation to finish sample loading. Specifically, in this embodiment, the connecting component 2-4 is an annular clamp, the inner diameter of the annular clamp is the same as the outer diameter of the deposition ring 2-3, or slightly larger than the outer diameter of the deposition ring 2-3, so that the deposition ring 2-3 can be clamped into the annular clamp, a circle of check rings are arranged on the inner wall of the annular clamp, the check rings are spaced from both ends of the annular clamp by a certain distance, so that the deposition ring 2-3 can be clamped into both sides of the annular clamp, the ring radius of the check rings is 2mm-1cm, and the semicircular deposition ring 2-3-1 can be fixed by arranging the check rings, so as to prevent the semicircular deposition ring 2-3-1 from being dislocated along the. In other embodiments, the connecting members 2-4 may be of other types as long as they can fix the two adjacent deposition rings 2-3, and the connecting members 2-4 are not particularly limited in this application.

It should be noted that, in other embodiments, when the multi-channel vacuum sublimation apparatus with the deposition chamber vertically arranged as shown in fig. 2 is adopted, 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 connecting part 2-4 in sequence, slowly place the sample in the sample outer tube 2-1, then place the fixed tube 2-5, and slowly vertically arrange the whole assembled deposition chamber 2, thereby completing the sample loading.

As shown in fig. 1 and fig. 6, the deposition chamber 2 filled with the sample is slowly connected with the suction connecting device 3 closed by the switch rotary valve 3-3, and is tightly clamped by the screw cock 3-1 and the rubber ring 3-2 to ensure sealing; the second adapter 3-4 is connected with a pressure pipe 5, then a buffer device 6, a multi-port integrated valve 7, a pressure gauge 8, a three-way valve 9 and a vacuum system 10 are sequentially connected, and the joint is tightened by a hoop 4 to ensure sealing. Finally, slowly placing the deposition cavity 2 into a heating cylinder 1-2 of the heating device 2; wherein, the sample outer tube 2-1 is longer than the heating cylinder, so that the sample is heated and sublimated in the heating area of the heating cylinder, the deposition and crystal growth are completed in the heat preservation area, and the sample outer tube 2-1 exposed outside the heating cylinder is cooled in the air. And after the whole multi-channel vacuum sublimation device is assembled, vacuumizing, heating and sublimating.

Slowly starting the low-vacuum degree mechanical pump in the vacuum system 10 for vacuum pumping, and sequentially opening a three-way valve 9, a switch valve 7-2 and a switch rotary valve 3-3 on the whole gas path; after the indication number of the vacuum meter 8 is stable, closing the valve of the low-vacuum-degree mechanical pump, and starting the high-vacuum-degree mechanical pump 10-2 for vacuumizing; after the indication number of the vacuum meter 8 is stable, a low-vacuum-degree mechanical pump valve is opened, and a high-vacuum-degree mechanical pump 10-2 and a low-vacuum-degree mechanical pump 10-1 in the vacuum system 10 work together to provide a vacuum environment for the deposition cavity 2; after the number indicated by the vacuum gauge 8 is stabilized again, the heating device 1 is started, and vacuum sublimation purification is started. The vacuum system 10 of the embodiment of the application is a two-stage vacuum system, and the occurrence of the sample material flushing situation can be effectively reduced.

On the basis of measuring the melting point or the decomposition temperature of each sample in advance, as shown in 1 and 3, the temperature is accurately controlled by a temperature control device 1-1 of a heating device, a heating cylinder is used for slowly heating an outer tube 2-1 of each sample, and corresponding temperature rise gradient and stable heating time length are set according to the difference of thermal stability of each sample; in the heating vacuum sublimation process, the movable heating cylinder 1-2 is used for observing the purification condition, and the independent air extraction connecting device 3 and the heating device 1 can be closed after the sample is purified; and cooling, and taking down the deposition cavity 2 to finish vacuum sublimation purification. Not only improves the purification efficiency, but also reduces unnecessary energy consumption, and has strong visibility and high controllability in the sublimation purification process.

After the vacuum sublimation purification is completed, the gas storage device 12 connected with the three-way valve 9 can be opened, inert gas is stored in the gas storage device 12, and the inert gas is introduced into the deposition cavity 2, so that the sample is prevented from being influenced by water and oxygen in the air, and the sublimation purification product can be conveniently stored for a long time.

Example 2

In this embodiment, the multi-channel vacuum sublimation apparatus of embodiment 1 is adopted, and the multi-channel vacuum sublimation apparatus is inspected through the sublimation purification effect based on the bithiazole, the bipyridine and the fluorenone compounds, and the related sample compounds have poor solubility and good thermal stability, wherein the samples of numbers 1 to 3 in table 1 are the bithiazole compounds, the sample of number 4 is the bipyridine compounds, the samples of numbers 5 to 6 are the fluorenone compounds, and the specific experimental results are shown in table 1 below.

Because the solubility of each compound is poor, the crude product of the reactant is directly subjected to vacuum sublimation purification; after the first sublimation purification, purity detection and yield calculation are not carried out, secondary sublimation purification is directly carried out, and the purity of products obtained by secondary sublimation purification is more than 98% through nuclear magnetism or element analysis and detection; a small amount of cross-products are not further purified; generally, the more times of sublimation purification of a sample, the higher the relative purity, but the greater the loss in the scraping process, and particularly when the sublimation amount is small, the loss caused by incomplete scraping is obviously increased.

Table 1: sublimation and purification of sample

After the thermal decomposition temperature of the crude product is tested in advance, 2-4 samples with similar thermal stability are selected, in the embodiment, the serial numbers 1-4 in the table 1 are a group of multi-channel vacuum sublimation devices in the embodiment 1 for sublimation and purification, and four deposition cavities 2 in the embodiment 1 are correspondingly adopted. The samples numbered 5 and 6 in the above table are a set of samples that were purified by sublimation using the multi-channel vacuum sublimation apparatus of example 1. As can be seen from table 1 above, the multi-channel vacuum sublimation device provided by the application realizes purification of several types of organic compounds with good conjugation, has a good purification effect, and can obtain a target product with high purity. By controlling the vacuum sublimation conditions, a plurality of crystals of the target product can be obtained, and the crystal generation rate is high.

It should be noted that, in this embodiment, the multi-channel vacuum sublimation apparatus in embodiment 1 is used to purify different samples, and it is also possible to perform vacuum sublimation purification on the same sample in the multiple deposition chambers 2, so as to realize enrichment of the same sample mass.

Other embodiments of the present application will be apparent to those skilled in the art from consideration of the specification and practice of the present application disclosed herein. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the application being indicated by the following claims.

Claims (8)

1. A multi-channel vacuum sublimation apparatus, comprising:

at least two deposition chambers (2);

at least two air-extracting connecting devices (3), wherein one end of each air-extracting connecting device is connected with a port of the deposition cavity (2);

and the multi-port normalization valve (7) comprises at least two pipelines (7-1), a switch valve (7-2) and a first conversion joint (7-4), the at least two pipelines (7-1) are connected with the first conversion joint (7-4) after being connected in parallel, the switch valve (7-2) is connected with the pipelines (7-1) in series, one end of each pipeline (7-1) is connected with the air suction connecting device (3), and the first conversion joint (7-4) is used for being connected with the vacuum system (10).

2. A multi-channel vacuum sublimation apparatus according to claim 1, wherein a buffer device (6) or a single-channel filter device is arranged between the suction connection device (3) and the multi-port normalization valve (7), the buffer device (6) is used for collecting the sample overflowed from the deposition chamber (2), the single-channel filter device can make the sample in the deposition chamber flow out through the single-channel filter device, and the sample can not flow into the deposition chamber from one side of the single-channel filter device.

3. Multi-channel vacuum sublimation device according to claim 1, wherein the deposition chamber (2) comprises a sample outer tube (2-1) and at least two deposition rings (2-3), connecting members (2-4) and stationary tubes (2-5) arranged therein, the outer wall of the deposition ring (2-3) is parallel to the sample outer tube (2-1), at least part of the deposition ring (2-3) is composed of two detachable semicircular deposition rings (2-3-1), two adjacent deposition rings (2-3) are detachably and fixedly connected through the connecting part (2-4), the fixing pipe (2-5) is at least arranged at the opening end of the deposition cavity (2) and is used for fixing the at least two deposition rings (2-3).

4. The multi-channel vacuum sublimation apparatus according to claim 1, further comprising a three-way valve (9) and a gas storage device, wherein a first channel of the three-way valve (9) is connected with the first adapter (7-4) of the multi-port normalization valve (7), a second channel of the three-way valve (9) is connected with the gas storage device (12), and a third channel of the three-way valve (9) is used for connecting with the vacuum system (10).

5. Multi-channel vacuum sublimation device according to claim 4, further comprising a vacuum gauge (8) arranged between the multiport normalizing valve (7) and the three-way valve (9); the vacuum system (10) comprises a two-stage vacuum system formed by two mechanical pumps, wherein the vacuum degree of one mechanical pump is higher than that of the other mechanical pump.

6. The multi-channel vacuum sublimation device according to claim 1, wherein the suction connection device (3) comprises a connection body (3-6), a threaded cock (3-1), a first rubber ring (3-2), a switch rotary valve (3-3), a second rubber ring (3-5) and a second conversion joint (3-4), the two ends of the connection body (3-6) are respectively provided with the first rubber ring (3-2) and the second rubber ring (3-5), one end of the connection body (3-6) is provided with the threaded cock (3-1), and the threaded cock (3-1) is used for connecting with the deposition chamber (2); the other end of the connecting body (3-6) is provided with the second adapter (3-4).

7. The multi-channel vacuum sublimation device according to claim 1, wherein the multi-port normalization valve (7) further comprises a plurality of sieves (7-3), the plurality of sieves (7-3) being respectively arranged on each pipeline (7-1); or the number of the filter screens (7-3) is one, and the filter screens are arranged on the first conversion joint (7-4).

8. A multi-channel vacuum sublimation device according to claim 1, further comprising at least two heating devices (1), the heating devices (1) being adapted to provide a heat source for the deposition chamber (2).

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