CN202219101U - Sublimation purification system - Google Patents
Sublimation purification system Download PDFInfo
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- CN202219101U CN202219101U CN2011202959965U CN201120295996U CN202219101U CN 202219101 U CN202219101 U CN 202219101U CN 2011202959965 U CN2011202959965 U CN 2011202959965U CN 201120295996 U CN201120295996 U CN 201120295996U CN 202219101 U CN202219101 U CN 202219101U
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- sublimation
- sublimation purification
- space blocking
- blocking unit
- purification system
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The utility model relates to a sublimation purification system which comprises a sublimation heating pipe and is characterized in that one or more space blocking units that are arranged continuously are arranged in a collection area of the sublimation heating pipe; each space blocking unit consists of a hollow cylinder and a plate used for fixing the interior of the hollow cylinder and provided with a through hole; the hollow cylinders are clung to the internal wall of the sublimation heating pipe; and the plane directions of the plates are intersected with the axial directions of the cylinders. The novel sublimation purification system is established by arraying the space blocking units in the traditional sublimation heating pipe. With the adoption of the sublimation purification system, the sublimation product yield is increased by 10%-20%, and the purity is also increased; in addition, the performances of fabricated organic electroluminescence devices are improved, for example, approximately 1V start voltage is reduced, the luminous life is prolonged by 1.5 times, etc.
Description
Technical field
The utility model includes the purifying field of organic compounds, particularly a kind of distillation purification system.
Background technology
During decades in the past; Organic electronic device has been made significant headway; Such as: OLED (organic electroluminescence device), OTFT (OTFT), OPV (organic solar batteries) etc.; OLED material especially wherein, owing to have spontaneous optical activity, high contrast, high reaction rate, wide viewing angle, advantage such as low power consumption, full-colorization, manufacturing process are simple; At home and abroad be confirmed to be and can be applicable to follow-on novel flat-plate display technology, the OLED material had received the extensive concern of research circle and industrial circle in the last few years.
After the initiative work that the Deng Qingyun and the Van Slyke of Kodak are directed against the OLED material began, the application of OLED material and industrialization had obtained very fast progress.For the OLED device, in many factors that influences its device performance, the purity of OLED material principal goods matter is one of most important factor, because it not only directly affects the performance of device, but also influences its reliability.In fact, because the OLED material purity directly affects its internal charge (electronics and hole) transmittability, thereby purity is one of most important factor of investigating its performance in organic electronic device.The OLED material is divided into two big types from technique direction at present: little molecular organic material and macromolecular material.From business-like product at present, most producer all uses micromolecular OLED organic material.The purifying process that obtains highly purified little molecular organic material at present mainly contains following several kinds, such as: subregion fusion method, chromatogram comparison method, original position filtering technique, and thermograde sublimation separation method or the like.In these methods, because there is not liquid phase state in most of organic molecule material under atmospheric pressure or low pressure, so the thermograde sublimating technologe is the most useful and modal a kind of purification process of organic semiconductor small molecule material.The OLED investigation of materials person of lot of domestic and foreign all uses this technology to carry out the production of organic molecule OLED high-purity material with production firm at present.The principle of this method mainly is to set a thermograde, purifies thereby adopt the mode that progressively heats up to come the heating sublimation pipe that principal goods matter is separated with impurity.Its sublimation system that adopts is as shown in Figure 1.Distillation heating tube 7 is the closed at both ends formula, and the one of which end offers vavuum pump interface 8, and the other end can be opened maybe can not drive gas port 9 into; Distillation heating tube 7 is from be divided into the thermal treatment zone 1, acquisition zone 2 and impurity range 3 away from 8 beginnings of vavuum pump interface successively; Sublimate is placed in the thermal treatment zone 1 in advance, in the heating process, under inert gas flow existence or non-existent situation; Principal goods matter can be enriched near the inside pipe wall the acquisition zone 2 (setting the thermal treatment zone of specified temp); And more volatile impurity can be transferred and is deposited on the impurity range 3 farther apart from principal goods matter, and non-volatile impurities is then stayed and held not in the purifying boat, takes out cylinder 10 and can collect sublimate and impurity respectively.This purification system principle is simple; Yet; A common heating sublimation purifying can't satisfy the requirement of purity, need principal goods matter carried out distillation for the second time even distil more frequently reaching enough purity, and therefore whole purge process needs very plenty of time and resource.Hence one can see that, and the improvement of sublimation separation purification technique is for obtaining high-purity material, thereby the low cost of obtaining, high efficiency organic electronic device are very urgent.
Summary of the invention
To the deficiency in above-mentioned field, the utility model provides a kind of sublimation purification system, adopts the inner space to stop the operating path that changes sublimate, thereby principal goods matter and impurity are separated in sublimation process better, and the yield that distils is higher.
A kind of sublimation purification system; Comprise a distillation heating tube; It is characterized in that: the space blocking unit that is provided with one or more continuous arrangements in the acquisition zone of said distillation heating tube; Said space blocking unit is made up of a hollow cylinder and the plate of fixing its inner band through hole, and said hollow cylinder is close to the inwall of the heating tube that distils, and the axial direction of said board plane direction and cylinder intersects.
Be provided with the space blocking unit of one or more continuous arrangements in the said distillation heating tube.
Said plate is a plectane, and said plectane is vertical with the axial direction of cylinder.
Said plectane is positioned at cylinder central authorities.
Said plate is a semi-circular plate, and said space blocking unit is a plurality of, and adjacent semi-circular plate is arranged in opposite directions.
Said through hole is evenly distributed on the plectane.
The utility model will be provided with the space blocking unit at acquisition zone, and the space blocking unit is formed with hollow cylinder and plate, and hollow cylinder is close to inwall; Plate with axially intersect, make from thermal treatment zone sublimate pass through the path full of twists and turns, passed from through hole behind the plate resistance retaining; Thereby make principal goods matter can better separate, improved the purity of acquisition zone principal goods matter, simultaneously because the existence of plate with volatile impurity; The amount that makes vavuum pump take away reduces, and loss is few, and yield improves relatively.In like manner, also the space blocking unit can be set, with the above-mentioned effect of further raising at acquisition zone.
Plate intersects with axle, can be different angles, preferential vertical direction, and then plate becomes plectane.
Plate can also be a semi-circular plate, preferably is provided with two space blocking units, and this semi-circular plate can be designed to arrange in opposite directions, staggered parallel.
Material after the utility model distillation is in the deposition space blocking unit one by one, and sublimation purification finishes, and can take out the space blocking unit, can collect principal goods matter or impurity from the two ends of hollow cylinder very easily.
The length of cylinder, the size of through hole on number and the plectane, number can design according to the separation of principal goods matter easily.
Stop the unit through array manifold in traditional distillation heating tube, set up a kind of new sublimation purification system.After adopting this sublimation purification system, the distillation product yield improves 10-20%, and purity also improves, and has improved the performance of the organic electroluminescence device of preparation simultaneously, has for example reduced the cut-in voltage value of about 1V, is that luminescent lifetime has improved 1.5 times etc.
Description of drawings
Fig. 1 has the sublimation purification system schematic now,
Fig. 2 present embodiment 1 sublimation purification system schematic,
Fig. 3 space blocking unit structural representation,
The A-A of Fig. 4 Fig. 3 is to cutaway view,
Fig. 5 embodiment 2 space blocking unit cross-sectional schematic,
Each label is listed as follows among the figure:
The 1-thermal treatment zone, 2-acquisition zone, 3-impurity range, 4-cylinder, 5-through hole, 6-plectane, the 7-heating tube that distils, 8-vavuum pump interface, 9-air inlet, 10-space blocking unit, 11-semi-circular plate, the 12-former material that distils.
The specific embodiment
Embodiment 1:
A kind of sublimation purification system; Comprise a distillation heating tube 7; It is characterized in that: the space blocking unit 10 that is provided with one or more continuous arrangements in the acquisition zone 2 of said distillation heating tube 7; Said space blocking unit 10 is made up of a hollow cylinder 4 and the plate of fixing its inner band through hole 5, and said hollow cylinder 4 is close to the inwall of the heating tube 7 that distils, and the axial direction of said board plane direction and cylinder 4 intersects.Said plate is a plectane 6, and said plectane 6 is vertical with the axial direction of cylinder 4.Feed inert gas (the time spent can not close) from air inlet 9, the distillation gas of the former material 12 of the thermal treatment zone 1 distillation is full of twists and turns through the path, passes from through hole 5 after being stopped by plectane 6; Thereby make principal goods matter can better separate with volatile impurity; Improved the purity of acquisition zone 2 principal goods matter, simultaneously owing to the existence of plectane 6, the amount that makes vavuum pump interface 8 take away reduces; Loss is few, and yield improves relatively.In like manner, said distillation heating tube 7 interior impurity ranges 3 also can be provided with the space blocking unit 10 of one or more continuous arrangements.
These unit materials can adopt quartz, glass or stainless steel etc. according to the difference of institute's sublimator material.The space blocking unit of this a plurality of arrays uses together and can promote principal goods matter and separate impurities.
Plate in the resistance shelves unit 10, space is a semi-circular plate 11, and on the space blocking unit 10 at least two, and adjacent semi-circular plate 11 is arranged in opposite directions.
Contrast experiment's example:
In order to verify the superiority of new system, the utility model has carried out comparative test with it and traditional structure sublimation system, uses common OLED material NPB to distil, and we adopt 100cm distillation heating tube 7, distillation air inlet 9 about 10cm places, raw material position.Argon flow amount is controlled at 0-10sccm, and vacuum degree control is at 1-9x10
-4Torr.
In the legacy system, the material of purifying is deposited on cylinder 4 inwalls of distillation heating tube, and the deposition region covers whole acquisition zone 2 even meeting and impurity range 3 and produces overlapping.Such as: NPB is in legacy system, and to 30cm, most of impurity deposits extrinsic region but can extend in the Alq acquisition zone range of deposition at 15cm.In new system, the range of deposition of NPB is 5cm-15cm, and range of deposition is narrower than legacy system greatly.Through the detection of material behind the calculating of product yield and the purifying being found new system improves 10-20% than the final purifying productive rate of legacy system, can improve product gas purity behind the identical distillation number of times simultaneously.
The result such as the table one of productive rate
Table 1:10g NPB once distil latter two systems yield relatively
Table 2 be NPB thermal weight loss scanning analysis result (DSC, Seiko Instruments, DSC6200).
Table 2:NPB once distils the back thermogravimetic analysis (TGA) relatively
Liquid chromatogram purity and TGA thermal weight loss result show that new method has improved the purity of NPB.Though the otherness of purity is very little, in the OLED organic material, even if the otherness that very little purity changes performance is clearly.
Principle analysis:
The difference of two kinds of sublimation system is; New system stops unit 10 through placement space in distillation heating tube 7; Make in the thermal treatment zone 1 become gaseous state principal goods matter and impurity, in the process that arrives distillation acquisition zone 2, must transport longer distance, improved distillation productive rate and purity.In traditional mode, distillation back product and impurity only can be deposited on distillation heating tube 7 tube walls, in sublimation process; Some molecule can be discharged from the distillation heating tube with vavuum pump; The waste of material after causing distilling, and because the area of tube wall is limited, a lot of principal goods matter molecules can not effectively be deposited in distillation back acquisition zone 2; But along with molecular motion is deposited in impurity range 3; Even because fed distance is shorter, impurity molecule just is deposited in purifying acquisition zone 2 with principal goods matter molecule still not yet in effect the separation, the back material purity that causes distilling promotes not high.
The advantage that is provided with of new system is that gaseous molecular receives the influence that the space stops the unit, and the time that molecule is carried in the space is longer; Thereby can realize that impurity and the effective of purifying substance separate; Improve separating effect, improved material productive rate behind the purifying, improved the purity of material behind the purifying simultaneously.
Conclusion, novel system can improve productive rate, improves purity.
Claims (6)
1. sublimation purification system; Comprise a distillation heating tube; It is characterized in that: the space blocking unit that is provided with one or more continuous arrangements in the acquisition zone of said distillation heating tube; Said space blocking unit is made up of a hollow cylinder and the plate of fixing its inner band through hole, and said hollow cylinder is close to the inwall of the heating tube that distils, and the axial direction of said board plane direction and cylinder intersects.
2. according to the said sublimation purification of claim 1 system, it is characterized in that: the space blocking unit that is provided with one or more continuous arrangements in the said distillation heating tube impurity range.
3. according to claim 1 or 2 said sublimation purification systems, it is characterized in that: said plate is a plectane, and said plectane is vertical with the axial direction of cylinder.
4. according to the said sublimation purification of claim 3 system, it is characterized in that: said plectane is positioned at cylinder central authorities.
5. according to claim 1 or 2 said sublimation purification systems, it is characterized in that: said plate is a semi-circular plate, and said space blocking unit is a plurality of, and adjacent semi-circular plate is arranged in opposite directions.
6. according to the said sublimation purification of claim 1 system, it is characterized in that: said through hole is evenly distributed on the plectane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202959965U CN202219101U (en) | 2011-08-13 | 2011-08-13 | Sublimation purification system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202959965U CN202219101U (en) | 2011-08-13 | 2011-08-13 | Sublimation purification system |
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| Publication Number | Publication Date |
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| CN202219101U true CN202219101U (en) | 2012-05-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011202959965U Expired - Lifetime CN202219101U (en) | 2011-08-13 | 2011-08-13 | Sublimation purification system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016008313A1 (en) * | 2014-07-15 | 2016-01-21 | 广东阿格蕾雅光电材料有限公司 | Continuous distillation device of organic solid material |
-
2011
- 2011-08-13 CN CN2011202959965U patent/CN202219101U/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016008313A1 (en) * | 2014-07-15 | 2016-01-21 | 广东阿格蕾雅光电材料有限公司 | Continuous distillation device of organic solid material |
| CN105311852A (en) * | 2014-07-15 | 2016-02-10 | 广东阿格蕾雅光电材料有限公司 | Organic solid material continuous distillation device |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20120516 |