CN108854136B - Special equipment for purifying visible organic small molecules in high vacuum in open mode - Google Patents
Special equipment for purifying visible organic small molecules in high vacuum in open mode Download PDFInfo
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- CN108854136B CN108854136B CN201810805406.5A CN201810805406A CN108854136B CN 108854136 B CN108854136 B CN 108854136B CN 201810805406 A CN201810805406 A CN 201810805406A CN 108854136 B CN108854136 B CN 108854136B
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- protective sleeve
- movable probe
- test tube
- hearth
- vacuum
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- 150000003384 small molecules Chemical class 0.000 title claims abstract description 8
- 230000001681 protective effect Effects 0.000 claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 238000000746 purification Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000012360 testing method Methods 0.000 claims abstract description 17
- 238000004140 cleaning Methods 0.000 claims abstract description 16
- 230000000007 visual effect Effects 0.000 claims abstract description 3
- 239000000523 sample Substances 0.000 claims description 37
- 238000005092 sublimation method Methods 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 abstract description 6
- 239000000428 dust Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 3
- 238000013021 overheating Methods 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract description 3
- 239000012264 purified product Substances 0.000 abstract description 3
- 238000002061 vacuum sublimation Methods 0.000 description 7
- 238000009792 diffusion process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D7/00—Sublimation
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses open-type purification high-vacuum visual organic small molecule purification special equipment which comprises a furnace frame, a flange plate, a hot gas outlet, an armored thermocouple, a cold gas inlet, a protective sleeve, a sleeve cleaning device, a test tube and a display, wherein the furnace frame is provided with a furnace inlet and a furnace outlet; the furnace frame is provided with an open type hearth heating combination device, the open type hearth heating combination device comprises an upper hearth combination heating plate and a lower hearth combination heating plate, and a test tube is arranged between the upper hearth combination heating plate and the lower hearth combination heating plate; the invention can easily realize convenient observation of purified products in the vacuum tube in a high-temperature environment, the added armored thermocouple effectively protects the products from being damaged due to overheating, the dust filter trap and the cooling filter trap, and under the condition of not influencing vacuum, the problem that the traditional vacuum system pumps material powder and hot gas into a molecular pump to influence the service life of equipment is solved, and the double effects of filtering and cooling are effectively realized.
Description
Technical Field
The invention belongs to the field of organic photoelectric material manufacturing, relates to an open type purification high vacuum visible technology, and particularly relates to open type purification high vacuum visible organic micromolecule purification special equipment.
Background
In order to meet the requirements of the organic photoelectric device field on materials, the organic photoelectric material industry in China needs to manufacture high-quality and high-purity organic photoelectric materials so as to obtain high-performance organic photoelectric devices. In the prior art, the vacuum sublimation technology is often adopted to purify the organic small molecular material. The currently used vacuum sublimation purification equipment adopts a design scheme of three-section temperature control or five-section temperature control, obtains a high vacuum atmosphere by combining a mechanical pump and a molecular pump, then respectively regulates and controls different temperature zones, and separates and purifies by using different sublimation temperatures of different component materials to obtain high-quality and high-purity organic micromolecule materials. The existing vacuum sublimation purification equipment controls the diffusion rate of the organic micromolecule material after sublimation by adjusting the heating temperature of a heating device.
However, the heating device is often adjusted depending on the experience and the feeling of technicians in the specific operation, the purification process is not effectively monitored, the vacuum sublimation purification process of the organic micromolecule material cannot be effectively controlled, and the diffusion rate of the organic micromolecules is not convenient to control; so that the purification speed is influenced when the diffusion rate is low, and further the production efficiency is influenced; when the diffusion rate is high, the organic small molecules can diffuse into the vacuum pump again, which causes serious pollution to the vacuum pump and material waste.
Meanwhile, the purity and quality of the material are poor due to the fact that effective control over the vacuum sublimation purification process of the organic small molecular material cannot be achieved. In summary, a technical problem to be solved by those skilled in the art is how to provide an apparatus for vacuum sublimation and purification of small organic molecule materials to effectively control a vacuum sublimation and purification process of small organic molecule materials, so as to improve the purification speed and purity and quality of the materials and reduce pollution and waste. To solve the above-mentioned drawbacks, a solution is now provided.
Disclosure of Invention
The invention aims to provide special open-type purification equipment for high-vacuum visible organic small molecules.
The purpose of the invention can be realized by the following technical scheme:
an open type high-vacuum visible organic small molecule purification special device comprises a furnace frame, a flange plate, a hot gas outlet, an armored thermocouple, a cold gas inlet, a protective sleeve, a sleeve cleaning device, a test tube and a display;
the furnace frame is provided with an open type hearth heating combination device, the open type hearth heating combination device comprises an upper hearth combination heating plate and a lower hearth combination heating plate, and a test tube is arranged between the upper hearth combination heating plate and the lower hearth combination heating plate;
the test tube is internally provided with a protective sleeve, the protective sleeve is fixedly arranged in the test tube through a flange, and the test tube is in a sealed state;
the flange plate is fixedly connected with the movable probe, the movable probe is positioned at the open type hearth heating combination device, and the movable probe is arranged in the protective sleeve; one side of the protective sleeve is also connected with a cold gas inlet through a guide pipe, the cold gas inlet is connected with a cold gas outlet through a guide pipe, the cold gas outlet is arranged in the protective sleeve, the cold gas outlet is arranged at the position of the movable probe, and a hot gas outlet is also formed in the protective sleeve;
an armored thermocouple is further arranged in the protective sleeve, and a sleeve junction cleaning device is further arranged at the upper end of the protective sleeve.
Furthermore, the movable probe is used for observing the form of the material in the sublimation process in real time, so that the acquisition of experimental data and the observation of the purification process are facilitated.
Furthermore, the movable probe is electrically connected with the display through a wire, and the movable probe is used for transmitting the measured data and the image to the display.
Further, cold air sprayed out of the cold air outlet is used for taking away heat around the movable probe;
the cold air sprayed out of the cold air outlet is heated by the movable probe and then is led out through the hot air outlet, so that the movable probe is protected.
Further, the armored thermocouple is used for monitoring the temperature change at the movable probe in real time;
the sleeve cleaning device removes the agglutinated material on the protective sleeve through axial linear mechanical movement.
The invention has the beneficial effects that: the invention can easily realize convenient observation of purified products in the vacuum tube in a high-temperature environment, the added armored thermocouple effectively protects the products from being damaged due to overheating, the dust filter trap and the cooling filter trap, and under the condition of not influencing vacuum, the problem that the traditional vacuum system pumps material powder and hot gas into a molecular pump to influence the service life of equipment is solved, and the double effects of filtering and cooling are effectively realized;
meanwhile, the movable probe on the flange plate can effectively solve the problem that the probe is invisible in the sublimation process in a vacuum high-temperature environment, and data acquisition and observation of the purification process in an experiment are facilitated.
Drawings
In order to facilitate understanding for those skilled in the art, the present invention will be further described with reference to the accompanying drawings.
FIG. 1 is a front view of the apparatus of the present invention;
FIG. 2 is a side view of the apparatus of the present invention;
fig. 3 is a schematic structural diagram of the casing cleaning device of the present invention.
Detailed Description
As shown in fig. 1-3, an open type purification high vacuum visual organic small molecule purification special device comprises a furnace frame 12, a flange plate 1, a hot gas outlet 2, an armored thermocouple 3, a cold gas inlet 4, a protective sleeve 6, a sleeve cleaning device 5, a test tube 10 and a display 11;
an open-type hearth heating combination device 8 is arranged on the furnace frame 12, the open-type hearth heating combination device 8 comprises upper and lower hearth combination heating plates, and a test tube 10 is arranged between the upper and lower hearth combination heating plates;
the flange plate 1 is fixedly connected with a movable probe 7, and the movable probe 7 is used for observing the form of the material in the sublimation process in real time, so that experimental data can be conveniently acquired and the purification process can be conveniently observed;
a protective sleeve 6 is arranged in the test tube 10, the protective sleeve 6 is fixedly arranged in the test tube 10 through a flange plate 1, and the test tube 10 is in a sealed state; the movable probe 7 is electrically connected with the display 11 through a lead, and the movable probe 7 is used for transmitting measured data and images to the display 11;
the position of the movable probe 7 is positioned at the position of the open hearth heating combination device 8, and the movable probe 7 is arranged inside the protective sleeve 6; a cold gas inlet 4 is connected to one side of the protective sleeve 6 through a guide pipe, the cold gas inlet 4 is connected with a cold gas outlet 9 through a guide pipe, the cold gas outlet 9 is arranged in the protective sleeve 6, the cold gas outlet 9 is arranged at the position of the movable probe 7 and used for taking away heat around the movable probe 7, a hot gas outlet 2 is further formed in the protective sleeve 6, and cold gas sprayed out of the cold gas outlet 9 is heated by the movable probe 7 and then is led out through the hot gas outlet 2, so that the movable probe 7 is protected;
an armored thermocouple 3 is further arranged in the protective sleeve 6, and the armored thermocouple 3 is used for monitoring the temperature change of the movable probe 7 in real time;
the protective sleeve 6 is also provided with a sleeve clearing device 5, and the sleeve cleaning device 5 removes the agglutinated materials on the protective sleeve 6 through axial linear mechanical motion.
The sleeve cleaning device 5 comprises an air cylinder 501, a piston rod 502 is arranged at the front end of the air cylinder 501, a connecting block 503 is fixedly connected to the front end of the piston rod 502, an annular lantern ring 504 is fixed on one side of the connecting block 503, a cleaning block 505 is further fixedly connected to the inner ring of the lantern ring 504, and the cleaning block 505 can be sponge; the cleaning block 505 is a ring-shaped block, the inner diameter of the cleaning block 505 is consistent with that of the protective sleeve 6, and the cleaning block 505 is matched with the protective sleeve 6; the cylinder 501 is fixedly connected to the flange plate 1.
The invention can easily realize convenient observation of purified products in the vacuum tube in a high-temperature environment, the added armored thermocouple effectively protects the products from being damaged due to overheating, the dust filter trap and the cooling filter trap, and under the condition of not influencing vacuum, the problem that the traditional vacuum system pumps material powder and hot gas into a molecular pump to influence the service life of equipment is solved, and the double effects of filtering and cooling are effectively realized;
meanwhile, the movable probe on the flange plate can effectively solve the problem that the probe is invisible in the sublimation process in a vacuum high-temperature environment, and data acquisition and observation of the purification process in an experiment are facilitated.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the invention as defined in the following claims.
Claims (1)
1. An open type purification high-vacuum visual organic small molecule purification special device is characterized by comprising a furnace frame (12), a flange plate (1), a hot gas outlet (2), an armored thermocouple (3), a cold gas inlet (4), a protective sleeve (6), a sleeve cleaning device (5), a test tube (10) and a display (11);
an open-type hearth heating combination device (8) is arranged on the furnace frame (12), the open-type hearth heating combination device (8) comprises upper and lower hearth combination heating plates, and a test tube (10) is arranged between the upper and lower hearth combination heating plates;
wherein a protective sleeve (6) is arranged in the test tube (10), the protective sleeve (6) is fixedly arranged in the test tube (10) through a flange plate (1), and the test tube (10) is in a sealed state;
the flange plate (1) is fixedly connected with a movable probe (7), the movable probe (7) is positioned at the open type hearth heating combination device (8), and the movable probe (7) is arranged inside the protective sleeve (6); one side of the protective sleeve (6) is further connected with a cold gas inlet (4) through a guide pipe, the cold gas inlet (4) is connected with a cold gas outlet (9) through a guide pipe, the cold gas outlet (9) is arranged in the protective sleeve (6), the cold gas outlet (9) is arranged at the position of the movable probe (7), and a hot gas outlet (2) is further formed in the protective sleeve (6);
an armored thermocouple (3) is also arranged in the protective sleeve (6), and a sleeve cleaning device (5) is also arranged at the upper end of the protective sleeve (6);
the movable probe (7) is used for observing the form of the material in the sublimation process in real time, so that the acquisition of experimental data and the observation of the purification process are facilitated;
the device is characterized in that the movable probe (7) is electrically connected with the display (11) through a lead, and the movable probe (7) is used for transmitting measured data and images to the display (11);
the cold air sprayed out of the cold air outlet (9) is used for taking away heat around the movable probe (7);
the cold air sprayed out of the cold air outlet (9) is heated by the movable probe (7) and then is guided out through the hot air guide outlet (2), so that the movable probe (7) is protected;
the armored thermocouple (3) is used for monitoring the temperature change at the position of the movable probe (7) in real time;
the sleeve cleaning device (5) removes the agglutinated material on the protective sleeve (6) through axial linear mechanical movement.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810805406.5A CN108854136B (en) | 2018-07-20 | 2018-07-20 | Special equipment for purifying visible organic small molecules in high vacuum in open mode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810805406.5A CN108854136B (en) | 2018-07-20 | 2018-07-20 | Special equipment for purifying visible organic small molecules in high vacuum in open mode |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108854136A CN108854136A (en) | 2018-11-23 |
| CN108854136B true CN108854136B (en) | 2021-02-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810805406.5A Active CN108854136B (en) | 2018-07-20 | 2018-07-20 | Special equipment for purifying visible organic small molecules in high vacuum in open mode |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2159658C1 (en) * | 1999-07-01 | 2000-11-27 | Сибирский химический комбинат | Desublimation plant |
| CN101403039B (en) * | 2008-11-26 | 2010-09-01 | 株洲冶炼集团股份有限公司 | Sublimation apparatus for metal purification |
| CN201664523U (en) * | 2010-03-26 | 2010-12-08 | 陕西科技大学 | Sublimation purification device of organic materials |
| CN102924207B (en) * | 2011-08-13 | 2015-05-27 | 广东阿格蕾雅光电材料有限公司 | Organic micromolecule sublimation purifying method |
| JP6006516B2 (en) * | 2012-03-30 | 2016-10-12 | 出光興産株式会社 | Organic material purification equipment |
| CN202956215U (en) * | 2012-12-10 | 2013-05-29 | 重庆洋泰科技发展有限公司 | Constant-pressure air blowing thermocouple |
| CN102961890B (en) * | 2012-12-12 | 2014-09-17 | 中国科学院长春应用化学研究所 | Equipment and process for vacuum sublimation purification of small organic molecule material |
| CN203154863U (en) * | 2013-02-09 | 2013-08-28 | 浙江桐庐百草园中药材开发有限公司 | Borneol cinnamomum camphora extraction and purification device |
| CN203609915U (en) * | 2013-03-06 | 2014-05-28 | 江西冠能光电材料有限公司 | Sublimation purification device |
| CN104667563B (en) * | 2015-02-13 | 2017-03-22 | 安徽贝意克设备技术有限公司 | Multi-combined high-vacuum purifying system |
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Effective date of registration: 20220422 Address after: 230000 9th floor, building A12, phase II, gongtou Liheng Plaza, intersection of Chuangxin Avenue and Fanhua Avenue, Taohua Industrial Park Development Zone, Feixi County, Hefei City, Anhui Province Patentee after: Anhui beiyike Intelligent Technology Co.,Ltd. Address before: Room 402, 4th floor, north, management committee, Chaohu Economic Development Zone, Hefei City, Anhui Province Patentee before: HEFEI OULAIDI PHOTOELECTRIC TECHNOLOGY CO.,LTD. |