An apparatus and method for the sublimation and purification of organic materials

Abstract

This invention provides a sublimation purification apparatus and method for organic materials. The sublimation purification apparatus includes a sublimation tube and at least one collecting tube connected in sequence. A heat-conducting baffle is provided between the sublimation tube and the adjacent collecting tube. A plate grid is provided inside the sublimation tube, and the plate grid includes vertically arranged axial grid plates and radial grid plates to divide the sublimation tube area. By setting a plate grid inside the sublimation tube, this invention can effectively increase the heat-receiving area and improve the heat transfer efficiency, thereby increasing the sublimation rate. At the same time, the plate grid can form a spatial barrier, effectively preventing impurities or low-boiling-point components in the organic material from being directly splashed out, reducing the risk of contamination of the sublimated material, and improving the purity of the sublimated organic material. The plate grid avoids the problem in traditional methods where the material may be directly discharged during the vacuum process and difficult to condense in the collecting tube. The improved structure of the apparatus is simple and convenient, with significant effects and a wide range of applications.

Description

Technical Field

[0001] This invention belongs to the field of material sublimation and purification technology, and relates to an apparatus and method for sublimation and purification of organic materials. Background Technology

[0002] The efficiency of organic light-emitting devices (OLEDs) is closely related to organic light-emitting materials, which determine important indicators such as the color of light emitted by OLEDs. For example, the purity of organic light-emitting materials is key to affecting indicators such as the color of light emitted and the lifetime of light emitted. In order to meet the material requirements of the field of organic optoelectronic devices, it is necessary to manufacture high-quality, high-purity organic light-emitting materials in order to obtain high-performance organic optoelectronic devices. Therefore, it is necessary to improve the purity of organic light-emitting materials as much as possible.

[0003] Since sublimation is a crucial step in improving the purity of organic materials, vacuum sublimation technology is commonly used for its purification. The vacuum purification apparatus utilizes a combination of mechanical and molecular pumps to create a high vacuum atmosphere. Then, a segmented temperature control method is employed to regulate different temperature zones, taking advantage of the varying sublimation temperatures of different materials to separate and purify them into high-purity organic materials. However, current vacuum sublimation processes suffer from slow sublimation rates, and impurities also sublimate along with the sublimated material. Furthermore, the sputtering effect of low-boiling-point materials makes it difficult to separate the product from the impurities. Additionally, the sublimated organic material tends to condense at the baffles, causing blockages and affecting product purity and the continuity of the sublimation process.

[0004] CN204455272U discloses a novel organic material sublimation sample cell. The sample cell includes a tubular sample sublimation tube and at least one tubular condensation collection tube connected in series. A baffle is installed inside the sample sublimation tube near the opening where the sample sublimation tube and the condensation collection tube connect. The baffle is vertically positioned, and an opening is left between the upper edge of the baffle and the upper wall of the sample sublimation tube. A sample placement stage is also provided inside the sample sublimation tube, and the height of the sample placement stage is lower than the height of the baffle. This sample cell only prevents the sample from being directly carried into the collection area by the baffle, but it does not address or propose any improvements to address issues such as easy blockage caused by the condensation of the sublimated gas phase, slow sublimation rate, and difficulty in separating impurities.

[0005] CN101310812A discloses a vacuum sublimation purification method and apparatus for organic materials. The purification process employs a two-step vacuum sublimation process. The first sublimation temperature is controlled at 30–40°C below the sublimation point of the organic material. To further remove impurities, a second low-temperature vacuum sublimation is required; the second sublimation temperature is controlled at 80–100°C below the sublimation point of the organic material. The purification apparatus mainly includes a glass container with a deposition chamber, a heating furnace, a vacuum pumping system, and a temperature control system. This method uses different glass tube regions as centers for two sublimations to improve product purity. However, it does not explicitly address structural improvements to the glass tube regions where the organic material is placed, nor does it provide any structural improvements to the apparatus to increase the sublimation rate or improve product purity.

[0006] In summary, further structural improvements are needed for vacuum sublimation purification equipment and processes for organic materials to increase the sublimation rate and the purity of the purified product, while ensuring the continuous operation of the sublimation purification process. Summary of the Invention

[0007] To address the problems existing in the prior art, the present invention aims to provide a sublimation purification apparatus and method for organic materials. The apparatus, by setting a plate grid inside the sublimation tube, can effectively increase the heated area of ​​the organic material, improve heat transfer efficiency, and thus increase the sublimation rate. At the same time, the plate grid can form a spatial barrier, effectively preventing impurities or low-boiling-point components in the organic material from being directly splashed out. Furthermore, the combination of the heat-conducting baffle and the above two measures reduces the risk of contamination of the sublimated material and improves the purity of the sublimated sample. The latter can also solve the problem of blockage caused by the easy condensation of the gas phase at the baffle.

[0008] To achieve this objective, the present invention adopts the following technical solution:

[0009] On one hand, the present invention provides a sublimation purification device for organic materials, the sublimation purification device comprising a sublimation tube and at least one collecting tube connected in sequence, a heat-conducting baffle is provided between the sublimation tube and the adjacent collecting tube, and a plate grid is provided inside the sublimation tube, the plate grid comprising vertically arranged axial grid plates and radial grid plates, dividing the sublimation tube region.

[0010] In this invention, the main structure of the sublimation purification device includes a heating furnace, a heating furnace tube, and a vacuum structure. The sublimation tube and the collection tube are located inside the heating furnace tube. The improvements to the sublimation purification device mainly start from the components that come into direct contact with organic materials.

[0011] In this invention, the structural features of the sublimation tube, which holds and heats the organic material to be purified, play a crucial role in the sublimation purification effect. By setting a plate grid in the sublimation tube, specifically with an alternating structure of axial and radial grids, the sublimation tube area is divided into multiple small regions, which can effectively increase the contact and heating area of ​​the organic material, thereby improving its heat transfer efficiency and sublimation rate. The plate grid can also form a spatial barrier, requiring the sublimated material to travel a longer distance to reach the collection tube, avoiding the problem in traditional methods where the material may be directly discharged during the vacuum process and difficult to condense in the collection tube. At the same time, the blocking effect of the plate grid can effectively prevent impurities or low-boiling-point components in the organic material from bubbling and splashing during the sublimation process, reducing the risk of contamination of the sublimated material and improving the purity of the sublimated organic material.

[0012] The heat-conducting baffle set between the sublimation tube and the collection tube in this invention has excellent heat transfer performance, which can effectively prevent the sublimation material from condensing on the baffle due to sudden cooling and blocking the channels of the sublimation tube and the collection tube, ensuring the continuous sublimation process and improving the efficiency of material sublimation and purification. The improved structure of the device is simple and convenient, with obvious effects, and is suitable for the purification of various types of materials, with a wide range of applications.

[0013] The following are preferred technical solutions of the present invention, but are not intended to limit the technical solutions provided by the present invention. The technical objectives and beneficial effects of the present invention can be better achieved and realized through the following technical solutions.

[0014] As a preferred embodiment of the present invention, the collection tube comprises two sections, namely a first collection tube and a second collection tube.

[0015] Preferably, the sublimation tube and the collection tube are integrally disposed in the same heating furnace tube.

[0016] In this invention, based on the structure of commonly used sublimation equipment, the heating furnace tube for loading the sublimation tube and the collecting tube can be a quartz tube. This sublimation equipment has a segmented heating function, and different sections of the heating furnace tube can be set with different temperatures to ensure that the sublimation and condensation of organic materials are completed in the same furnace tube.

[0017] As a preferred technical solution of the present invention, the number of axial grid plates in the plate grid is at least one, such as one, two or three, preferably one.

[0018] Preferably, the length of the axial grid is less than or equal to the length of the inner wall of the sublimation tube.

[0019] Preferably, the number of radial gratings in the plate grid is at least one, for example, one, two, three, four, five, six, seven, eight, nine or ten. The specific number is related to the length of the sublimation tube, the spacing of the radial gratings, and the selection of the sublimation material.

[0020] Preferably, the distance between two adjacent radial grids is 1 to 6 cm, such as 1 cm, 2 cm, 3 cm, 4 cm, 5 cm or 6 cm, but is not limited to the listed values. Other unlisted values ​​within this range are also applicable. In order to obtain a higher yield and a shorter sublimation time, it is preferred to be 1 to 3 cm.

[0021] Preferably, the length of the radial grid is less than or equal to the width of the inner wall of the sublimation tube.

[0022] Preferably, the radial grid is perpendicularly divided by the axial grid on an average basis.

[0023] As a preferred embodiment of the present invention, the axial grating and the radial grating are independently flat or corrugated.

[0024] In this invention, based on the positional relationship between the axial and radial grids, the axial grids are usually selected as flat plates, while the radial grids can be selected as flat plates or corrugated plates to ensure that the size of each partition is basically the same and that the organic material is heated uniformly.

[0025] Preferably, the thickness of the axial and radial gratings is independently 1 to 4 mm, for example 1 mm, 1.5 mm, 2 mm, 2.5 mm, 3 mm, 3.5 mm or 4 mm, but is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0026] Preferably, the axial and radial gratings have the same height, which is 1 / 3 to 2 / 3 of the diameter of the sublimation tube, for example, 1 / 3, 2 / 5, 1 / 2, 3 / 5 or 2 / 3, but is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0027] In this invention, the height of the plate grid has a significant impact on the sublimation process of organic materials. If the height of the plate grid is too large, the upper space will be too small, the sublimation path will be longer, and the sublimation rate will be affected. If the height of the plate grid is too small, the material is more likely to enter the collection tube when heated, which is not conducive to the separation of components.

[0028] As a preferred technical solution of the present invention, the plate grid further includes a base plate, the base plate being arc-shaped and matching the shape of the sublimation tube.

[0029] Preferably, the plate grille is assembled from various parts or formed as a single piece.

[0030] Preferably, the material of the plate grid includes any one or a combination of at least two of titanium, zinc, copper or steel. Typical but non-limiting examples of such combinations include: combinations of titanium and zinc, combinations of copper and zinc, combinations of titanium, zinc and steel, and combinations of zinc, copper and steel, with titanium being the preferred material.

[0031] In this invention, the plate grid may include a base plate in addition to axial and radial grid plates. In this case, the organic material is placed on the base plate. Depending on the material of the plate grid, its heat transfer efficiency is higher, and the setting of the base plate is more conducive to the integrated molding of the plate grid.

[0032] As a preferred embodiment of the present invention, the heat-conducting baffle is disposed between the sublimation tube and the first collection tube.

[0033] Preferably, the height of the heat-conducting baffle is 1 / 3 to 2 / 3 of the diameter of the sublimation tube or the first collecting tube, for example, 1 / 3, 2 / 5, 1 / 2, 3 / 5 or 2 / 3, but is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0034] Preferably, the height of the plate-type grille is equal to or less than the height of the heat-conducting baffle.

[0035] In this invention, the selection of the height of the heat-conducting baffle affects the progress of the sublimation process and the purity of the product. If the height of the heat-conducting baffle is too small, the material is easy to enter the collection tube when heated, which is not conducive to the separation of components. If the height of the heat-conducting baffle is too large, it will result in a slow collection rate of sublimation material and is prone to blockage.

[0036] Preferably, the thickness of the heat-conducting baffle is 5 to 10 mm, such as 5 mm, 5.5 mm, 6 mm, 6.5 mm, 7 mm, 7.5 mm, 8 mm, 8.5 mm, 9 mm, 9.5 mm or 10 mm, but is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0037] As a preferred embodiment of the present invention, the heat-conducting baffle includes a heat-conducting metal plate or a glass plate coated with a heat-conducting metal layer.

[0038] Preferably, the thickness of the thermally conductive metal layer in the glass plate coated with the thermally conductive metal layer is 1 to 4 mm, for example, 1 mm, 1.5 mm, 2 mm, 2.5 mm, 3 mm, 3.5 mm or 4 mm, but is not limited to the listed values. Other unlisted values ​​within this range are also applicable, preferably 1 to 2 mm.

[0039] Preferably, the thermally conductive metal comprises any one or a combination of at least two of titanium, zinc, copper, or steel. Typical but non-limiting examples of such combinations include: combinations of titanium and zinc, combinations of copper and zinc, combinations of titanium, zinc, and steel, and combinations of zinc, copper, and steel, with titanium being the most preferred.

[0040] On the other hand, the present invention provides a method for purifying organic materials using the above-mentioned sublimation purification apparatus, the method comprising:

[0041] The organic material to be purified is dispersed in a plate grid in a sublimation tube, and then heated to sublimate after vacuuming. The temperature inside the sublimation tube and the collection tube is controlled. The sublimated organic material is condensed in the collection tube to obtain the purified organic material.

[0042] As a preferred embodiment of the present invention, the organic material includes organic small molecule luminescent materials.

[0043] In this invention, the organic materials are mainly organic light-emitting materials used in the field of organic optoelectronic devices, one type of which is organic small molecule light-emitting materials. These organic small molecule light-emitting materials can be triazoles and their derivatives, pyrazoline derivatives, triphenylamine derivatives, porphyrin compounds, carbazole, pyrazine, or thiazole derivatives. Preferably, the organic small molecule light-emitting materials can be N,N'-diphenyl-N,N'-(1-naphthyl)-1,1'-biphenyl-4,4'-diamine (NPB), 2,9-dimethyl-4,7-biphenyl-1,10-o-diazaphenanthroline (BCP), 2,3,5,6-tetramethylphenyl-1,4-phthalimide (TMPP), or 4,4',4”-tris(N-carbazolyl)triphenylamine (TCTA).

[0044] Preferably, the absolute pressure after vacuuming is below 3.0 Pa, such as 3.0 Pa, 2.5 Pa, 2.0 Pa, 1.5 Pa, 1 Pa, 0.5 Pa, or 0.1 Pa, but is not limited to the listed values; other unlisted values ​​within this range are also applicable.

[0045] Preferably, the temperatures in the sublimation tube, the first collection tube, and the second collection tube are set in a gradient, with different temperature settings for different sublimation materials.

[0046] Preferably, the temperature of the sublimation tube is 240–260°C, for example, 240°C, 245°C, 250°C, 255°C, or 260°C; the temperature of the first collecting tube is 145–165°C, for example, 145°C, 150°C, 155°C, 160°C, or 165°C; and the temperature of the second collecting tube is 95–115°C, for example, 95°C, 100°C, 105°C, 110°C, or 115°C. However, these are not limited to the listed values, and other unlisted values ​​within their respective ranges are also applicable.

[0047] In this invention, a suitable sublimation temperature is selected based on the chosen organic material, and the material is cooled in stages in two-stage collection tubes to achieve condensation of the sublimated material.

[0048] As a preferred technical solution of the present invention, the sublimation time after heating to the sublimation temperature is 10 to 30 hours, for example, 10 hours, 12 hours, 14 hours, 15 hours, 16 hours, 18 hours, 20 hours, 22 hours, 24 hours, 25 hours, 27 hours, 28 hours or 30 hours. The sublimation time is determined according to different sublimation products and the quality of the product to be sublimated, but is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0049] Preferably, the purified organic material is mainly condensed in the first collection tube, while the second collection tube mainly contains light components.

[0050] Compared with the prior art, the present invention has the following beneficial effects:

[0051] (1) The device described in this invention can effectively increase the heat-receiving area of ​​organic materials and improve the heat transfer efficiency by setting a plate grid inside the sublimation tube, thereby increasing the sublimation rate. At the same time, the setting of the plate grid can form a space barrier, effectively preventing impurities or low-boiling-point components in the organic materials from being directly splashed out, reducing the risk of sublimation material being contaminated, and improving the purity of the sublimated organic materials, which can reach more than 99.8%.

[0052] (2) The plate grid of the present invention makes the sublimation material need to travel a longer distance to reach the collection tube, avoiding the problem that it may be directly discharged during the vacuuming process and difficult to condense in the collection tube in the traditional method, thus improving the product yield, which can reach more than 86.0%.

[0053] (3) The heat-conducting baffle described in this invention has excellent heat transfer performance, which can effectively prevent the sublimation material from condensing on the baffle due to sudden cooling, blocking the channels of the sublimation tube and the collection tube, ensuring the continuous sublimation process, and improving the efficiency of material sublimation and purification.

[0054] (4) The device described in this invention has a simple and convenient structure improvement, obvious effect, and is suitable for the purification of various materials, with a wide range of applications. Attached Figure Description

[0055] Figure 1 This is a top view of the sublimation tube provided in Embodiment 1 of the present invention;

[0056] Figure 2 This is a front view of the sublimation tube provided in Embodiment 1 of the present invention;

[0057] Figure 3 This is a top view of the sublimation tube provided in Embodiment 2 of the present invention;

[0058] Among them, 1-sublimation tube, 2-thermal baffle, 3-axial grid, 4-radial grid. Detailed Implementation

[0059] To better illustrate the present invention and facilitate understanding of its technical solutions, the present invention is further described in detail below. However, the following embodiments are merely simplified examples of the present invention and do not represent or limit the scope of protection of the present invention. The scope of protection of the present invention is determined by the claims.

[0060] The present invention provides a sublimation purification apparatus and method for organic materials. The sublimation purification apparatus includes a sublimation tube 1 and at least one collection tube connected in sequence. A heat-conducting baffle 2 is provided between the sublimation tube 1 and the adjacent collection tube. A plate grid is provided inside the sublimation tube 1. The plate grid includes vertically arranged axial grid plates 3 and radial grid plates 4, which divide the sublimation tube 1 into regions.

[0061] The method includes:

[0062] The organic material to be purified is dispersed in the plate grid of sublimation tube 1, and then heated for sublimation after vacuuming. The temperature inside sublimation tube 1 and collection tube is controlled. The sublimated organic material is condensed in the collection tube to obtain the purified organic material.

[0063] The following are typical but non-limiting embodiments of the present invention:

[0064] Example 1:

[0065] This embodiment provides a sublimation purification device for organic materials. The sublimation purification device includes a sublimation tube 1 and two collection tubes connected in sequence. A top view of the sublimation tube 1 is shown below. Figure 1 As shown, its main view is as follows Figure 2 As shown, a heat-conducting baffle 2 is provided between the sublimation tube 1 and the adjacent collection tube. A plate grid is provided inside the sublimation tube 1. The plate grid includes vertically arranged axial grid plates 3 and radial grid plates 4, which divide the area of ​​the sublimation tube 1.

[0066] The collection tube comprises two sections, namely a first collection tube and a second collection tube.

[0067] The sublimation tube 1 and the collection tube are integrally arranged in the same heating furnace tube.

[0068] The plate grid has one axial grid plate 3, and the length of the axial grid plate 3 is equal to the length of the inner wall of the sublimation tube 1.

[0069] The distance between two adjacent radial grid plates 4 is 3cm, and the radial grid plates 4 are evenly and vertically divided by the axial grid plates 3.

[0070] Both the axial grid plate 3 and the radial grid plate 4 are flat and have a thickness of 2 mm.

[0071] The axial grid plate 3 and the radial grid plate 4 have the same height, which is 1 / 3 of the diameter of the sublimation tube 1.

[0072] The plate-type grille is assembled from various parts and is made of titanium.

[0073] The heat-conducting baffle 2 is disposed between the sublimation tube 1 and the first collection tube.

[0074] The height of the heat-conducting baffle 2 is 2 / 5 of the diameter of the sublimation tube 1.

[0075] The heat-conducting baffle 2 is a glass plate coated with a heat-conducting metal layer, with a total thickness of 6mm and a thickness of 2mm for the heat-conducting metal layer; the heat-conducting metal is titanium.

[0076] Example 2:

[0077] This embodiment provides a sublimation purification device for organic materials. The sublimation purification device includes a sublimation tube 1 and two collection tubes connected in sequence. A top view of the sublimation tube 1 is shown below. Figure 3 As shown, a heat-conducting baffle 2 is provided between the sublimation tube 1 and the adjacent collection tube. A plate grid is provided inside the sublimation tube 1. The plate grid includes vertically arranged axial grid plates 3 and radial grid plates 4, which divide the area of ​​the sublimation tube 1.

[0078] The collection tube comprises two sections, namely a first collection tube and a second collection tube.

[0079] The sublimation tube 1 and the collection tube are integrally arranged in the same heating furnace tube.

[0080] The plate grid has one axial grid plate 3, and the length of the axial grid plate 3 is equal to the length of the inner wall of the sublimation tube 1.

[0081] The distance between two adjacent radial grid plates 4 is 5cm, and the radial grid plates 4 are evenly and vertically divided by the axial grid plates 3.

[0082] The axial grid plate 3 is flat, and the radial grid plate 4 is corrugated, with a thickness of 1 mm.

[0083] The axial grid plate 3 and the radial grid plate 4 have the same height, which is 1 / 2 of the diameter of the sublimation tube 1.

[0084] The plate grid also includes a base plate, which is arc-shaped and matches the shape of the sublimation tube 1.

[0085] The plate-type grille is integrally formed from various parts and is made of steel.

[0086] The heat-conducting baffle 2 is disposed between the sublimation tube 1 and the first collection tube.

[0087] The height of the heat-conducting baffle 2 is half the diameter of the sublimation tube 1.

[0088] The heat-conducting baffle 2 is a glass plate coated with a heat-conducting metal layer, with a total thickness of 5mm and a thickness of 1mm for the heat-conducting metal layer; the heat-conducting metal is steel.

[0089] Example 3:

[0090] This embodiment provides a sublimation purification device for organic materials. The sublimation purification device includes a sublimation tube 1 and two collection tubes connected in sequence. A heat-conducting baffle 2 is provided between the sublimation tube 1 and the adjacent collection tube. A plate grid is provided inside the sublimation tube 1. The plate grid includes vertically arranged axial grid plates 3 and radial grid plates 4, which divide the area of ​​the sublimation tube 1.

[0091] The collection tube comprises two sections, namely a first collection tube and a second collection tube.

[0092] The sublimation tube 1 and the collection tube are integrally arranged in the same heating furnace tube.

[0093] The plate grid has one axial grid plate 3, and the length of the axial grid plate 3 is equal to the length of the inner wall of the sublimation tube 1.

[0094] The distance between two adjacent radial grid plates 4 is 2cm, and the radial grid plates 4 are evenly and vertically divided by the axial grid plates 3.

[0095] Both the axial grid plate 3 and the radial grid plate 4 are flat and have a thickness of 4 mm.

[0096] The axial grid plate 3 and the radial grid plate 4 have the same height, which is 3 / 5 of the diameter of the sublimation tube 1.

[0097] The plate grid also includes a base plate, which is arc-shaped and matches the shape of the sublimation tube 1.

[0098] The plate-type grille is integrally formed from various parts and is made of titanium.

[0099] The heat-conducting baffle 2 is disposed between the sublimation tube 1 and the first collection tube.

[0100] The height of the heat-conducting baffle 2 is 2 / 3 of the diameter of the sublimation tube 1.

[0101] The heat-conducting baffle 2 is a heat-conducting metal plate with a thickness of 4mm; the heat-conducting metal is titanium.

[0102] Example 4:

[0103] This embodiment provides a sublimation purification device for organic materials. The sublimation purification device includes a sublimation tube 1 and two collection tubes connected in sequence. A heat-conducting baffle 2 is provided between the sublimation tube 1 and the adjacent collection tube. A plate grid is provided inside the sublimation tube 1. The plate grid includes vertically arranged axial grid plates 3 and radial grid plates 4, which divide the area of ​​the sublimation tube 1.

[0104] The collection tube comprises two sections, namely a first collection tube and a second collection tube.

[0105] The sublimation tube 1 and the collection tube are integrally arranged in the same heating furnace tube.

[0106] The plate grid has one axial grid plate 3, and the length of the axial grid plate 3 is equal to the length of the inner wall of the sublimation tube 1.

[0107] The distance between two adjacent radial grid plates 4 is 1 cm, and the radial grid plates 4 are evenly and vertically divided by the axial grid plates 3.

[0108] Both the axial grid plate 3 and the radial grid plate 4 are flat and have a thickness of 3 mm.

[0109] The axial grid plate 3 and the radial grid plate 4 have the same height, which is 2 / 3 of the diameter of the sublimation tube 1.

[0110] The plate grid also includes a base plate, which is arc-shaped and matches the shape of the sublimation tube 1.

[0111] The plate-type grille is integrally formed from various parts and is made of titanium.

[0112] The heat-conducting baffle 2 is disposed between the sublimation tube 1 and the first collection tube.

[0113] The height of the heat-conducting baffle 2 is 2 / 3 of the diameter of the sublimation tube 1.

[0114] The heat-conducting baffle 2 is a heat-conducting metal plate with a thickness of 4mm; the heat-conducting metal is titanium.

[0115] Example 5:

[0116] This embodiment provides a sublimation purification device for organic materials. The sublimation purification device includes a sublimation tube 1 and two collection tubes connected in sequence. A heat-conducting baffle 2 is provided between the sublimation tube 1 and the adjacent collection tube. A plate grid is provided inside the sublimation tube 1. The plate grid includes vertically arranged axial grid plates 3 and radial grid plates 4, which divide the area of ​​the sublimation tube 1.

[0117] The collection tube comprises two sections, namely a first collection tube and a second collection tube.

[0118] The sublimation tube 1 and the collection tube are integrally arranged in the same heating furnace tube.

[0119] The plate grid has one axial grid plate 3, and the length of the axial grid plate 3 is equal to the length of the inner wall of the sublimation tube 1.

[0120] The distance between two adjacent radial grid plates 4 is 4 cm, and the radial grid plates 4 are evenly and vertically divided by the axial grid plates 3.

[0121] The axial grid plate 3 is flat, and the radial grid plate 4 is corrugated and has a thickness of 4mm.

[0122] The axial grid plate 3 and the radial grid plate 4 have the same height, which is 2 / 5 of the diameter of the sublimation tube 1.

[0123] The plate grid also includes a base plate, which is arc-shaped and matches the shape of the sublimation tube 1.

[0124] The plate-type grille is integrally formed from various parts and is made of zinc.

[0125] The heat-conducting baffle 2 is disposed between the sublimation tube 1 and the first collection tube.

[0126] The height of the heat-conducting baffle 2 is 2 / 5 of the diameter of the sublimation tube 1.

[0127] The heat-conducting baffle 2 is a glass plate coated with a heat-conducting metal layer, with a total thickness of 10mm and a thickness of 4mm for the heat-conducting metal layer; the heat-conducting metal is titanium.

[0128] Example 6:

[0129] This embodiment provides a method for the sublimation purification of organic materials. The method is carried out using the apparatus described in Embodiment 1, and the method includes:

[0130] The organic material to be purified is dispersed in the plate grid of sublimation tube 1. The organic material is NPB, a small organic molecule luminescent material. The vacuum is drawn to an absolute pressure of 1.5 Pa, and then heated for sublimation. The temperature gradient in sublimation tube 1 and the first and second collection tubes is controlled to decrease. The temperature of sublimation tube 1 is 250°C, the temperature of the first collection tube is 155°C, and the temperature of the second collection tube is 105°C. The sublimation time is maintained for 12.4 h. The sublimated organic material is mainly condensed in the first collection tube to obtain the purified organic material.

[0131] In this embodiment, based on the amount of organic material used before sublimation and the weight of the product in the collection tube, the yield of the purified material was calculated to be 88.10%; the purity of the purified organic material was determined to be 99.87% by liquid chromatography.

[0132] Example 7:

[0133] This embodiment provides a method for the sublimation purification of organic materials. The method is carried out using the apparatus described in Embodiment 1, and the method includes:

[0134] The organic material to be purified is dispersed in the plate grid of sublimation tube 1. The organic material is a small organic molecule luminescent material BCP. The vacuum is drawn to an absolute pressure of 3.0 Pa, and then heated for sublimation. The temperature gradient in sublimation tube 1 and the first and second collection tubes is controlled to decrease. The temperature of sublimation tube 1 is 240°C, the temperature of the first collection tube is 145°C, and the temperature of the second collection tube is 95°C. The sublimation time is maintained for 16.2 h. The sublimated organic material is mainly condensed in the first collection tube to obtain the purified organic material.

[0135] In this embodiment, based on the amount of organic material used before sublimation and the weight of the product in the collection tube, the yield of the purified material was calculated to be 86.50%; the purity of the purified organic material was determined to be 99.81% by liquid chromatography.

[0136] Example 8:

[0137] This embodiment provides a method for the sublimation and purification of organic materials. The method is carried out using the apparatus described in Embodiment 2, and includes:

[0138] The organic material to be purified is dispersed in the plate grid of sublimation tube 1. The organic material is NPB, a small organic molecule luminescent material. The vacuum is evacuated to an absolute pressure of 1.5 Pa, and then heated for sublimation. The temperature gradient in sublimation tube 1 and the first and second collection tubes is controlled to decrease. The temperature of sublimation tube 1 is 245°C, the temperature of the first collection tube is 150°C, and the temperature of the second collection tube is 100°C. The sublimation time is maintained for 12.7 h. The sublimated organic material is mainly condensed in the first collection tube to obtain the purified organic material.

[0139] In this embodiment, based on the amount of organic material used before sublimation and the weight of the product in the collection tube, the yield of the purified material was calculated to be 86.40%; the purity of the purified organic material was determined to be 99.85% by liquid chromatography.

[0140] Example 9:

[0141] This embodiment provides a method for the sublimation and purification of organic materials. The method is carried out using the apparatus described in Embodiment 3, and the method includes:

[0142] The organic material to be purified is dispersed in the plate grid of sublimation tube 1. The organic material is TCTA, a small organic molecule luminescent material. The vacuum is drawn to an absolute pressure of 0.5 Pa, and then heated for sublimation. The temperature gradient in sublimation tube 1 and the first and second collection tubes is controlled to decrease. The temperature of sublimation tube 1 is 260°C, the temperature of the first collection tube is 165°C, and the temperature of the second collection tube is 115°C. The sublimation time is maintained for 19.0 h. The sublimated organic material is mainly condensed in the first collection tube to obtain the purified organic material.

[0143] In this embodiment, based on the amount of organic material used before sublimation and the weight of the product in the collection tube, the yield of the purified material was calculated to be 87.50%; the purity of the purified organic material was determined to be 99.91% by liquid chromatography.

[0144] Example 10:

[0145] This embodiment provides a method for the sublimation purification of organic materials. The method is carried out using the apparatus in Embodiment 4, and the method includes:

[0146] The organic material to be purified is dispersed in the plate grid of sublimation tube 1. The organic material is NPB, a small organic molecule luminescent material. The vacuum is drawn to an absolute pressure of 1.5 Pa, and then heated for sublimation. The temperature gradient in sublimation tube 1 and the first and second collection tubes is controlled to decrease. The temperature of sublimation tube 1 is 245°C, the temperature of the first collection tube is 150°C, and the temperature of the second collection tube is 100°C. The sublimation time is maintained for 12.2 h. The sublimated organic material is mainly condensed in the first collection tube to obtain the purified organic material.

[0147] In this embodiment, based on the amount of organic material used before sublimation and the weight of the product in the collection tube, the yield of the purified material was calculated to be 87.90%; the purity of the purified organic material was determined to be 99.87% by liquid chromatography.

[0148] Example 11:

[0149] This embodiment provides a method for the sublimation and purification of organic materials. The method is carried out using the apparatus described in Embodiment 5, and the method includes:

[0150] The organic material to be purified is dispersed in the plate grid of sublimation tube 1. The organic material is NPB, a small organic molecule luminescent material. The vacuum is drawn to an absolute pressure of 1.5 Pa, and then heated for sublimation. The temperature gradient in sublimation tube 1 and the first and second collection tubes is controlled to decrease. The temperature of sublimation tube 1 is 245°C, the temperature of the first collection tube is 150°C, and the temperature of the second collection tube is 100°C. The sublimation time is maintained for 14.4 h. The sublimated organic material is mainly condensed in the first collection tube to obtain the purified organic material.

[0151] In this embodiment, based on the amount of organic material used before sublimation and the weight of the product in the collection tube, the yield of the purified material was calculated to be 86.70%; the purity of the purified organic material was determined to be 99.83% by liquid chromatography.

[0152] Comparative Example 1:

[0153] This comparative example provides an apparatus and method for the sublimation purification of organic materials. The apparatus is the same as that in Example 1, except that: no plate grid is provided in the sublimation tube 1, and the organic material NPB is directly laid at the bottom of the sublimation tube 1.

[0154] The method described herein is the same as that in Example 6.

[0155] In this comparative example, since no plate grid was installed in the sublimation tube, the heat transfer and sublimation rate were slow, and the sublimation time needed to be extended to 17.4 hours. Due to the lack of space obstruction by the plate grid, the product yield was relatively low, only 70.20%, and there was a risk of impurity sputtering causing contamination of the sublimation material. The purity of the purified organic material was 99.61%.

[0156] As can be seen from the above embodiments and comparative examples, the device of the present invention, by setting a plate grid inside the sublimation tube, can effectively increase the heated area of ​​the organic material, improve the heat transfer efficiency, and thus increase the sublimation rate. Simultaneously, the plate grid forms a spatial barrier, effectively preventing impurities or low-boiling-point components in the organic material from being directly splashed out, reducing the risk of contamination of the sublimated material, and increasing the purity of the sublimated organic material to over 99.8%. The plate grid design causes the sublimated material to travel a longer distance to reach the collection tube, avoiding the problem in traditional methods where it might be directly discharged during the vacuum process and difficult to condense in the collection tube, thus improving the product yield to over 86.0%. The heat-conducting baffle has excellent heat transfer performance, effectively preventing the sublimated material from condensing above the baffle due to sudden cooling, thus preventing blockage of the sublimation tube and collection tube channels, ensuring continuous sublimation, improving the efficiency of material sublimation and purification, and shortening the sublimation time. The improved structure of the device is simple and convenient, with significant effects, suitable for the purification of various types of materials, and has a wide range of applications.

[0157] The present invention has been illustrated with the above embodiments to describe the detailed apparatus and method of the present invention. However, the present invention is not limited to the detailed apparatus and method described above, that is, it does not mean that the present invention must rely on the detailed apparatus and method described above to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent substitutions for the apparatus of the present invention, additions of auxiliary devices, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A sublimation purification apparatus for organic materials, characterized in that, The sublimation purification device includes a sublimation tube and at least one collecting tube connected in sequence. A heat-conducting baffle is provided between the sublimation tube and the adjacent collecting tube. A plate grid is provided inside the sublimation tube. The plate grid includes vertically arranged axial grid plates and radial grid plates to divide the sublimation tube area. The plate grid also includes a base plate, which is arc-shaped and matches the shape of the sublimation tube; The plate grid has one axial grid plate and at least one radial grid plate; the distance between two adjacent radial grid plates is 1 to 6 cm; the radial grid plates are evenly and vertically divided by the axial grid plates; the axial grid plates and the radial grid plates have the same height, which is independently 1 / 3 to 2 / 3 of the diameter of the sublimation tube; The height of the heat-conducting baffle is 1 / 3 to 2 / 3 of the diameter of the sublimation tube; the height of the plate grid is equal to or less than the height of the heat-conducting baffle; the heat-conducting baffle includes a heat-conducting metal plate or a glass plate coated with a heat-conducting metal layer.

2. The sublimation purification apparatus according to claim 1, characterized in that, The collection tube comprises two sections, namely a first collection tube and a second collection tube.

3. The sublimation purification apparatus according to claim 1, characterized in that, The sublimation tube and the collection tube are integrally arranged in the same heating furnace tube.

4. The sublimation purification apparatus according to claim 1, characterized in that, The distance between two adjacent radial gratings is 1 to 3 cm.

5. The sublimation purification apparatus according to claim 1, characterized in that, The axial grating and the radial grating are independently flat or corrugated.

6. The sublimation purification apparatus according to claim 1, characterized in that, The thickness of the axial grating and the radial grating are independently 1 to 4 mm.

7. The sublimation purification apparatus according to claim 1, characterized in that, The panel grille is assembled from various parts or formed as a single piece.

8. The sublimation purification apparatus according to claim 1, characterized in that, The material of the plate grille includes any one or a combination of at least two of titanium, zinc, copper or steel.

9. The sublimation purification apparatus according to claim 8, characterized in that, The material of the plate grille is titanium.

10. The sublimation purification apparatus according to claim 2, characterized in that, The heat-conducting baffle is disposed between the sublimation tube and the first collection tube.

11. The sublimation purification apparatus according to claim 2, characterized in that, The height of the heat-conducting baffle is 1 / 3 to 2 / 3 of the diameter of the first collecting pipe.

12. The sublimation purification apparatus according to claim 1, characterized in that, The thickness of the heat-conducting baffle is 5-10 mm.

13. The sublimation purification apparatus according to claim 1, characterized in that, The thickness of the thermally conductive metal layer in the glass plate coated with the thermally conductive metal layer is 1 to 4 mm.

14. The sublimation purification apparatus according to claim 13, characterized in that, The thickness of the thermally conductive metal layer in the glass plate coated with the thermally conductive metal layer is 1 to 2 mm.

15. The sublimation purification apparatus according to claim 1, characterized in that, Thermally conductive metals include any one or a combination of at least two of titanium, zinc, copper, or steel.

16. The sublimation purification apparatus according to claim 15, characterized in that, The thermally conductive metal is titanium.

17. A method for purifying organic materials using the sublimation purification apparatus according to any one of claims 1-16, characterized in that, The method includes: The organic material to be purified is dispersed in the plate grid of the sublimation tube, and then heated to sublimate after vacuuming. The temperature inside the sublimation tube and the collection tube is controlled. The sublimated organic material is condensed in the collection tube to obtain the purified organic material.

18. The method according to claim 17, characterized in that, The organic materials include organic small molecule luminescent materials.

19. The method according to claim 18, characterized in that, The organic small molecule luminescent material includes any one or a combination of at least two of the following: N,N'-diphenyl-N,N'-(1-naphthyl)-1,1'-biphenyl-4,4'-diamine, 2,9-dimethyl-4,7-biphenyl-1,10-o-diazaphenanthroline, 2,3,5,6-tetramethylphenyl-1,4-phthalimide, or 4,4',4”-tris(N-carbazole-yl)triphenylamine.

20. The method according to claim 17, characterized in that, The absolute pressure after vacuuming is below 3.0 Pa.

21. The method according to claim 17, characterized in that, The temperatures in the sublimation tube, the first collection tube, and the second collection tube are set in a gradient.

22. The method according to claim 21, characterized in that, The temperature of the sublimation tube is 240–260°C, the temperature of the first collection tube is 145–165°C, and the temperature of the second collection tube is 95–115°C.

23. The method according to claim 17, characterized in that, The purified organic material is mainly condensed in the first collection tube.

Images