CN203609915U - Sublimation purification device - Google Patents
Sublimation purification device Download PDFInfo
- Publication number
- CN203609915U CN203609915U CN201320648979.4U CN201320648979U CN203609915U CN 203609915 U CN203609915 U CN 203609915U CN 201320648979 U CN201320648979 U CN 201320648979U CN 203609915 U CN203609915 U CN 203609915U
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- organic compound
- heating furnace
- vacuum
- purifying plant
- plant according
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- 238000000746 purification Methods 0.000 title claims abstract description 19
- 238000000859 sublimation Methods 0.000 title abstract description 8
- 230000008022 sublimation Effects 0.000 title abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 15
- 238000000605 extraction Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 5
- 238000007689 inspection Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000009792 diffusion process Methods 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 230000008878 coupling Effects 0.000 claims description 2
- 238000010168 coupling process Methods 0.000 claims description 2
- 238000005859 coupling reaction Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 238000011031 large-scale manufacturing process Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 239000004065 semiconductor Substances 0.000 description 9
- 238000004821 distillation Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 4
- 238000002061 vacuum sublimation Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 244000144985 peep Species 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The utility model discloses a sublimation purification device for organic compounds. The device comprises a vacuum extraction system, a material vacuum maintaining system, a multi-temperature-zone heating furnace, a micro photographing and observation system as well as a computer control and image display system. The device has the characteristics of precise control, in-situ observation, and rapidness and convenience in operation, the improvement on the purification technology is facilitated, and requirements of mass production are met.
Description
Technical field
The utility model includes organic compounds purification technique field, is specifically related to a kind of for high speed, easy and with low cost heating in vacuum sublimation apparatus.
Background technology
Along with organic semiconductor is in the panchromatic display screen of light emitting diode composition and the application of white-light illuminating, the application of organic semiconductor transistor on logic circuit, and the application of organic semiconductor photovoltaic cell, have recognized that the effect that organic semiconducting materials purification technique is more and more important.High-purity organic semi-conductor uses and often can make the performance of above-mentioned organic semiconductor device and working life bring the raising that exceedes several times.Thereby quick and easy organic semiconductor purification technique tool is of great significance.
Conventionally the method for purification of organic semiconducting materials can be divided into recrystallization or vacuum sublimation method.Vacuum sublimation method refers to after (under reduced pressure) is heated solid under vacuum state and directly becomes gaseous state, then (as quartz glass tube) condenses into solid-state in a thermograde pipe.Because material to be purified and impurity have different sublimation temperatures and condensation temperature, and reach purifying object.In some cases, for the gas flow that makes to distil is effectively along distributing and separate in thermograde pipe, can use carrier gas and the gas that makes to distil from high-temperature stream to low temperature.The factor of controlling distillation purification quality mainly comprises: the temperature of each warm area and thermograde, vacuum and carrier gas flux, and distillation time.The final inspection of refined product depends on the analytical test of final products, but this mode could realize after often requiring distillation purification to finish.In actual production, be vital if detect for improvement and the control of timely technique in purification is carried out.For this reason, patent application CN201010206088.4(Dong Yi, Liu Zhihua, Hou Xiaoyuan) disclose a kind of window structure of rectangle sublimation purification device, be convenient to the observation of full pipeline.This large area watch window has but brought this thermal treatment zone large area heat dissipation problems, thereby and can bring the temperature difference to affect refining effect along pipeline section direction.
As adopt separation neglect window observation panel, the heat that can greatly reduce large area form is stirred consumption and the temperature difference along pipeline section direction.But this often causes and visually observes difficulty again.The utility model has adopted and in small form, has embedded fixing microimaging probe, has solved form and has been difficult to the difficulty of observing, the larger temperature difference problem of having avoided again large form thermal losses and having brought thus simultaneously.
Summary of the invention
The purpose of this utility model is to provide a kind of heating in vacuum sublimation purification device, comprise a vacuum extraction system, a vacuum tube material keeping system, the heating furnace of warm area more than (being formed by 2 ~ 10 temperature thermals treatment zone), one miniature video camera observing system, a computer control and image display system; Described vacuum extraction system is by an oil-sealed rotary pump, or the molecular diffusion pump of mechanical vacuum series connection of pumps composition; Described vacuum extraction system is by vacuum pipe and flange seal, is connected into vacuum material keeping system with one or one group of glass tube; Described many warm areas heating furnace is by resistance wire or electric coupling eddy-current heating silk, ceramic insulation body of heater, heating temperature control device composition; Described many warm areas heating furnace is comprising 2 ~ 7 micropore peepholes, is convenient to embed micropore camera, thereby purifying technique is followed the tracks of and improved to achieve effective control purification quality, is convenient to large-scale production.Wherein many warm areas heating furnace can be Heat Emission Pipe in Cylindrical Furnace, two semicircle open-type heating furnaces.Described many warm areas heating furnace is placed on a liftable trestle table and the heating furnace body that makes to open is realized and moved up and down and reach effective heating or effective cooling object.Described lifting support platform can be realized oscilaltion function by mechanical, hand-driven or by electro-motor.
Described micropore peephole is by quartz glass face, and diameter is the adiabatic tubular sheath composition of 2 ~ 20mm.
Described miniature video camera observing system is embedded in many warm areas heating furnace body micropore peephole, and using diameter is 2 ~ 20mm drum type brake micropore camera, the instant on-site-inspection of convenient enforcement.
Described miniature video camera observing system, is made up of micropore camera, wireless receiver and optional computer.Described minisize pick-up head around subsidiary LED Light-Emitting Diode, as light source, is convenient to clear observation.Described miniature video camera observing system is made up of micropore camera, signal on line and computer recipient processor.
Described miniature video camera observing system, by wired connection or wireless receiving mode, is connected with the computer control system of display screen with one, convenient observation and view data storage.
Described sublimable organic compound purifying plant, can be used for organic semiconductor or its raw material, and the distillation of medicine intermediate and polymer monomer organic compound is purified.Described add alternatively-carrier gas conduit of sublimable organic compound purifying plant is for controlling the speed of organic material distillation, the general many nitrogen of carrier gas, argon gas, helium or wherein 2 ~ 3 kinds of mists.
The utility model beneficial effect is: by adopting technique scheme, the utility model compared with prior art has the following advantages: can overcome the rapid heat dissipation of the rectangular watch window of large area, reduce the shortcoming along the cross-wise direction surrounding temperature difference; The drum type brake watch window that uses diameter little (2 ~ 20mm), is equipped with the pore type camera in microexamination mirror, thereby has overcome in the past by visually observing unclear or being difficult to observe the shortcoming of sublimation chamber intercrystalline size, reaches the object of effective control purifying technique.
Accompanying drawing explanation
Fig. 1 is a kind of sublimation purification device schematic diagram of the utility model.
Fig. 2 is the utility model micropore camera operation principle schematic diagram.
The specific embodiment
By the more specifically explanation of the preferred embodiment of the present utility model shown in accompanying drawing, above-mentioned and other object of the present utility model, Characteristics and advantages will be more clear.In whole accompanying drawings, identical Reference numeral is indicated identical part, does not deliberately draw in proportion accompanying drawing, focuses on illustrating purport of the present utility model.
Below in conjunction with drawings and the specific embodiments, the utility model is described in further detail.
As shown in Figure 1, wherein 100 is an oil-sealed rotary pump to a kind of sublimation purification device of the utility model, and 101 is a part diffusion pump, makes system can reach higher vacuum.103 is that a cold hydrazine pipe makes the liquid nitrogen or the dry ice/acetone solution that add from 105 funnels pass through the possible organic volatile of cold hydrazine inwall condensation, protection service life of vacuum pump, the vacuum of raising vacuum system.104 is a vacuum tube adpting flange 501.Flange 500 and flange 501 make glass outer tube 800 fix and be connected to vacuum system.801 for filling the organic compound glass tube of purification.600 is bracing frame.300 is the bracing frame of adjustment height, supports tubular heater 200.After adjustable supporter can allow the heating furnace of distillation open easily, make whole heating furnace and distillation glass tube produce larger space herein, be conducive to by air or fan air blast makes charge pipe be cooled to quickly the temperature of discharging (to be generally less than 80
oc).Tubular heater 200 is a multiple temperature sections (as four sections) heating furnace.900 is diameter 2 ~ 20mm garden cylinder observation panel.900 for embedding peep hole Zhong garden cylinder pinhole cameras.Pinhole cameras is connected with a display screen, with computer control, records all video recording details of sublimation process, has not only realized on-site-inspection, also with video record whole purification process.920 is an external light source, is conducive to pinhole cameras and observes.
The utility model micropore camera operation principle, as shown in Figure 2, wherein 21 is micropore camera; 22 for embedding 8 minute white LED on camera; 23 is the cylinder that comprises camera and protection, and diameter is 2-20mm; 24 for being connected to computer and display signal line; 25 is optional wireless receiver; 26 is that a computer is for receiving, show and store image pickup signal.26 also join with vacuum, heating furnace alternatively, overall process vacuum, heating and image pickup signal.
Above, be only preferred embodiment of the present utility model, not the utility model done to any pro forma restriction.Any those of ordinary skill in the art, do not departing from technical solutions of the utility model scope situation, all can utilize the technology contents of above-mentioned announcement to make many possible variations or modification to technical solutions of the utility model, or be revised as the equivalent embodiment of equivalent variations.Therefore, every content that does not depart from technical solutions of the utility model, any simple modification, equivalent variations and the modification above embodiment done according to technical spirit of the present utility model, all still belong in the protection domain of technical solutions of the utility model.
Claims (2)
1. a sublimable organic compound purifying plant, is characterized in that: comprise a vacuum extraction system, a vacuum tube material keeping system, the heating furnace of warm area more than, an observing system, a display system;
Described vacuum extraction system is by an oil-sealed rotary pump, or the molecular diffusion pump of mechanical vacuum series connection of pumps composition.
Described vacuum extraction system is by vacuum pipe and flange seal, and vacuum material tube retainer system is connected with one or one group of glass tube;
Described many warm areas heating furnace is by resistance wire or electric coupling eddy-current heating silk, ceramic insulation body of heater, heating temperature control device composition;
Described many warm areas heating furnace is comprising 2 ~ 7 micropore peepholes, is convenient to embed micropore camera, thereby purifying technique is followed the tracks of and improved to achieve effective control purification quality, is convenient to large-scale production.
2. sublimable organic compound purifying plant according to claim 1, is characterized in that heating furnace is made up of 2 ~ 10 heating regions; Heating furnace profile can be Heat Emission Pipe in Cylindrical Furnace or two semicircle open-type heating furnaces.
3. sublimable organic compound purifying plant according to claim 2, is characterized in that: described many warm areas heating furnace is placed on a liftable trestle table and makes the heating furnace physical efficiency of opening move up and down and reach effective heating or effective cooling object.
4. sublimable organic compound purifying plant according to claim 3, is characterized in that: described lifting support platform can be realized oscilaltion function by mechanical, hand-driven or by electro-motor.
5. sublimable organic compound purifying plant according to claim 1, is characterized in that: described micropore peephole is by quartz glass face, and diameter is the adiabatic tubular sheath composition of 2 ~ 20mm.
6. sublimable organic compound purifying plant according to claim 1, is characterized in that: described observing system is embedded in many warm areas heating furnace body micropore peephole, and using diameter is 2 ~ 20mm drum type brake micropore camera, the instant on-site-inspection of convenient enforcement.
7. sublimable organic compound purifying plant according to claim 6, is characterized in that: described observing system is made up of micropore camera, wireless receiver and computer.
8. sublimable organic compound purifying plant according to claim 6, is characterized in that: described micropore camera around subsidiary LED Light-Emitting Diode, as light source, is convenient to clear observation.
9. sublimable organic compound purifying plant according to claim 6, is characterized in that: described observing system is made up of micropore camera, signal on line and computer recipient processor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320648979.4U CN203609915U (en) | 2013-03-06 | 2013-10-21 | Sublimation purification device |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320100943.2 | 2013-03-06 | ||
| CN201320100943 | 2013-03-06 | ||
| CN201320648979.4U CN203609915U (en) | 2013-03-06 | 2013-10-21 | Sublimation purification device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN203609915U true CN203609915U (en) | 2014-05-28 |
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ID=50762598
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201320648979.4U Expired - Lifetime CN203609915U (en) | 2013-03-06 | 2013-10-21 | Sublimation purification device |
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| Country | Link |
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| CN (1) | CN203609915U (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108854136A (en) * | 2018-07-20 | 2018-11-23 | 合肥欧莱迪光电技术有限公司 | A kind of visual small organic molecule of open-type purification high vacuum purifies special equipment |
| CN109030542A (en) * | 2017-06-09 | 2018-12-18 | 武汉尚赛光电科技有限公司 | A kind of organic material heat stability testing equipment |
| CN109646987A (en) * | 2019-01-10 | 2019-04-19 | 合肥欧莱迪光电技术有限公司 | A kind of continuous feeding and discharging high vacuum small organic molecule purification special equipment |
| CN111450566A (en) * | 2019-01-22 | 2020-07-28 | 陕西坤同半导体科技有限公司 | Sublimation furnace and use method thereof |
-
2013
- 2013-10-21 CN CN201320648979.4U patent/CN203609915U/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109030542A (en) * | 2017-06-09 | 2018-12-18 | 武汉尚赛光电科技有限公司 | A kind of organic material heat stability testing equipment |
| CN108854136A (en) * | 2018-07-20 | 2018-11-23 | 合肥欧莱迪光电技术有限公司 | A kind of visual small organic molecule of open-type purification high vacuum purifies special equipment |
| CN109646987A (en) * | 2019-01-10 | 2019-04-19 | 合肥欧莱迪光电技术有限公司 | A kind of continuous feeding and discharging high vacuum small organic molecule purification special equipment |
| CN109646987B (en) * | 2019-01-10 | 2024-03-26 | 合肥百思智能装备有限公司 | Continuous feeding and discharging high-vacuum organic micromolecule purifying special equipment |
| CN111450566A (en) * | 2019-01-22 | 2020-07-28 | 陕西坤同半导体科技有限公司 | Sublimation furnace and use method thereof |
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| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20140528 |