CN111228846B - Sustainable production of straight barrel purification device and method - Google Patents
Sustainable production of straight barrel purification device and method Download PDFInfo
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- CN111228846B CN111228846B CN202010252403.0A CN202010252403A CN111228846B CN 111228846 B CN111228846 B CN 111228846B CN 202010252403 A CN202010252403 A CN 202010252403A CN 111228846 B CN111228846 B CN 111228846B
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- 238000000746 purification Methods 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000001704 evaporation Methods 0.000 claims abstract description 97
- 230000008020 evaporation Effects 0.000 claims abstract description 76
- 238000003860 storage Methods 0.000 claims abstract description 52
- 238000010438 heat treatment Methods 0.000 claims abstract description 36
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 239000013014 purified material Substances 0.000 claims abstract description 19
- 230000000630 rising effect Effects 0.000 claims abstract description 7
- 238000007790 scraping Methods 0.000 claims description 41
- 239000000463 material Substances 0.000 claims description 30
- 238000007670 refining Methods 0.000 claims description 23
- 239000002699 waste material Substances 0.000 claims description 19
- 239000012159 carrier gas Substances 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 9
- 238000010924 continuous production Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 3
- 238000002485 combustion reaction Methods 0.000 claims 1
- 238000005520 cutting process Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 15
- 238000011068 loading method Methods 0.000 abstract description 2
- 238000009413 insulation Methods 0.000 abstract 1
- 238000007599 discharging Methods 0.000 description 4
- 239000011368 organic material Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000007600 charging Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 229910010272 inorganic material Inorganic materials 0.000 description 3
- 239000011147 inorganic material Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011900 installation process Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- -1 and the like Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
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- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011982 device technology Methods 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D7/00—Sublimation
- B01D7/02—Crystallisation directly from the vapour phase
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Abstract
本发明提供可持续生产的直桶式提纯装置及方法，包括直桶式提纯炉、蒸发炉、导流桶、刮板、加热温控系统和外桶；在底层的蒸发炉中把原材料蒸发成蒸汽流，蒸汽流向上经过多段式不同温区的炉体，在蒸汽流上升过程中只能在导流桶与炉体之间一个狭窄的空间中通过，迫使蒸汽流的温度与炉体的温度更加接近并沉积，通过刮板将提纯料刮到存料槽，再经出料口存入存料器。所述的炉体全部密封在一个外桶内进行保温。整个装料和取料过程在不破坏真空的情况下进行，从而可持续不断的进行此提纯过程，提高了生产效率；由于整个生产过程不破坏真空环境，减少人为参与，以及采用直桶式的炉体结构能够提升炉温的均匀度，从而提高提纯材料的纯度。
The present invention provides a sustainable production straight barrel purification device and method, including a straight barrel purification furnace, an evaporation furnace, a guide barrel, a scraper, a heating temperature control system and an outer barrel; the raw materials are evaporated into a steam flow in the evaporation furnace at the bottom layer, and the steam flow passes through a multi-stage furnace body with different temperature zones upward. During the rising process of the steam flow, it can only pass through a narrow space between the guide barrel and the furnace body, forcing the temperature of the steam flow to be closer to the temperature of the furnace body and deposited, and the purified material is scraped to the storage tank by the scraper, and then stored in the storage device through the discharge port. The furnace body is completely sealed in an outer barrel for insulation. The entire loading and unloading process is carried out without destroying the vacuum, so that the purification process can be carried out continuously, thereby improving production efficiency; because the entire production process does not destroy the vacuum environment, human participation is reduced, and the straight barrel furnace body structure can improve the uniformity of the furnace temperature, thereby improving the purity of the purified material.
Description
Technical Field
The invention belongs to the technical field of physical vapor deposition, relates to a purification device, and particularly relates to a sustainable production straight barrel type purification device and method.
Background
The purification of materials by utilizing different evaporation temperatures of various materials is a very effective method, and particularly, the law that the evaporation temperature changes with the change of parameters such as different chemical compositions, structures, molecular weights and the like in organic materials can be realized by evaporating at different temperatures, so that the method has become a very effective method for solid materials such as organic electroluminescence (OLED), organic solar cells (OPV), organic Thin Film Transistors (OTFT) and the like. The method commonly used at present is to use a tube type purifying device, which is to put an impure organic raw material in a quartz tube with multiple temperature areas under the condition of vacuum or low vacuum airflow to evaporate the impure organic raw material in the high temperature areas and then deposit the organic raw material in different temperature areas, and take the material in each temperature area after the organic raw material is cooled to obtain the high-purity material. The prior art material purification apparatus still has the following problems for vacuum purification of various vaporizable organic materials or inorganic materials with a lower vaporization temperature: (1) After each time of charging and purification, the materials of each component can be taken out and reloaded only by cooling and opening, so that the production efficiency is seriously affected, continuous production is difficult, and industrialization is difficult to realize; (2) The temperature of the horizontal furnace tube is high and low, which affects the purification accuracy. Due to the problems, the price of the high-purity material is high, and the development of the OLED industry is influenced.
Disclosure of Invention
In order to solve the problems of low purification efficiency and low precision of various organic materials or inorganic materials with lower evaporation temperature in the prior art, the invention provides a continuous production straight barrel type purification device and method, raw materials are evaporated into steam flow in an evaporation furnace at the bottom layer, the steam flow upwards passes through a furnace body with different temperature areas in multiple sections, the steam flow only can pass through a narrow space between a guide barrel and the furnace body in the rising process of the steam flow, the temperature of the steam flow is forced to be closer to the temperature of the furnace body and is deposited, and purified materials deposited in each temperature area are scraped to a corresponding storage groove through a scraper plate on the guide barrel and enter a corresponding storage through a discharge port. The furnace body is totally sealed in an outer barrel for heat preservation. The whole charging and taking process is carried out under the condition of not damaging vacuum, so that the purification process can be continuously carried out, and the production efficiency can be greatly improved; and the whole production process does not damage the vacuum environment, so that the artificial participation is reduced, and the uniformity of the furnace temperature can be improved by adopting a straight barrel type furnace body structure. Thereby improving the purity of the purified material.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a sustainable production straight barrel type purification device comprises a straight barrel type purification furnace, an evaporation furnace, a flow guiding barrel, a scraping plate, a heating temperature control system and an outer barrel;
the evaporation furnace is communicated with the bottom of the straight barrel type purification furnace, and the outer barrel is hermetically sleeved at the peripheries of the straight barrel type purification furnace and the evaporation furnace; the guide barrel is sleeved in the straight barrel type purifying furnace, and a channel for steam flow to circulate is formed between the outer wall of the guide barrel and the inner wall of the straight barrel type purifying furnace; the scraping plate is arranged on the outer wall of the guide flow barrel, a notch for installing an annular storage groove is arranged on the scraping plate, and the annular storage groove is fixed on the inner wall of the straight barrel type purifying furnace; the temperature of the outer walls of the evaporation furnace and the straight barrel type purification furnace is controlled by the heating temperature control system.
Preferably, the straight barrel type purifying furnace is formed by connecting a top cover, a plurality of cylinder furnace body sections with the same diameter and a bottommost inverted cone cylinder, wherein a first extraction opening is formed in the top cover, annular storage tanks are arranged at the connecting positions between two adjacent cylinder furnace body sections and between the last cylinder furnace body section and the bottommost inverted cone cylinder, and the bottoms of the storage tanks are connected with discharge pipes.
Preferably, the annular storage groove is provided with a positioning hole, and the positioning hole is matched with a fixed convex point on the inner wall of the straight barrel type purifying furnace, so that the annular storage groove is detachably connected with the inner wall of the straight barrel type purifying furnace.
Preferably, the guide barrel is sleeved in the straight barrel type purifying furnace and comprises a guide barrel body, a rotating shaft and a refining plate arranged at the lower end of the rotating shaft; the rotary shaft and the flow guiding barrel body are coaxially arranged and fixedly connected into a whole, the rotary shaft penetrates through the straight barrel type purifying furnace and is fixed and sealed at the top cover of the straight barrel type purifying furnace through a bearing, the refining plate is positioned in the evaporating furnace, and the refining plate can rotate and lift along with the rotary shaft.
Preferably, the guide barrel body is formed by integrally forming a top plate, an inner cylinder and a bottommost inverted cone-shaped cylinder, a space is reserved between the top plate and a top cover of the straight barrel type purifying furnace body, and a sliding rail for installing a scraping plate is arranged on the outer wall of the inner cylinder.
Preferably, the top plate is provided with a top plate through hole for communicating the inside and the outside of the guide barrel.
Preferably, the scraping plate is arranged on a sliding rail on the outer wall of the inner cylinder, the scraping plate is arranged at the outer edge of the scraping plate and used for scraping the purified material deposited on the inner wall of the straight barrel type purifying furnace into the annular storage tank, and then the scraping plate inserted into the annular storage tank pushes the purified material in the storage tank to the discharge port.
Preferably, the evaporation furnace is of a hollow cavity structure with an evaporation chamber, the top of the evaporation furnace is in sealing connection with the bottom of the straight barrel type purification furnace, the upper end of the side wall of the evaporation furnace is provided with an air inlet pipe for introducing high-purity carrier gas and a feed pipe for feeding raw materials, and the bottom of the evaporation furnace is provided with a waste outlet pipe.
Preferably, the heating temperature control system comprises an evaporation furnace heating temperature control system and a straight barrel type purification furnace heating temperature control system, wherein the evaporation furnace heating temperature control system is used for supplying heat to an evaporation chamber in the evaporation furnace, and the straight barrel type purification furnace heating temperature control system is used for independently controlling the temperature of different temperature areas of the straight barrel type purification furnace, so that the temperature of the different temperature areas of the straight barrel type purification furnace is gradually reduced from bottom to top.
Preferably, the outer barrel comprises a base barrel, an outer barrel body and a connecting cover, wherein the bottom open end of the outer barrel body is detachably and hermetically connected with the base barrel, and the top open end of the outer barrel body is hermetically connected with the outer wall of the straight barrel type purifying furnace through the connecting cover; the connecting cover is provided with a second extraction opening, and the base barrel is provided with a vacuum sealing interface for connecting the pipeline and the electrical connection line to the outside of the outer barrel.
The invention also discloses a method for purifying the vaporizable material by using the continuously-produced straight barrel type purifying device, which comprises the following steps:
1) The starting device is used for vacuumizing the inside and the outside of the straight barrel type purifying furnace respectively, and then setting the temperature of an evaporating chamber in the evaporating furnace and the temperatures of different temperature areas of the straight barrel type purifying furnace formed by a plurality of barrel furnace body sections respectively, wherein the temperature of the straight barrel type purifying furnace gradually decreases from bottom to top; when the evaporation chamber and all the temperature areas reach the preset temperature, the rotary shaft drives the guide flow barrel and the scraping plate to rotate;
2) Before feeding, a rotating shaft is arranged in a lifting state, and at the moment, a space is reserved between the bottom of a refining plate arranged at the lower end of the rotating shaft and the bottom of an evaporation chamber in an evaporation furnace;
3) During feeding, raw materials are conveyed into an evaporation chamber of an evaporation furnace through a spiral feeding device, are uniformly spread into a raw material layer through a material homogenizing plate, and are heated and evaporated in the evaporation chamber; introducing carrier gas from an air inlet pipe of the evaporation furnace, driving steam to rise in a channel between the guide flow barrel and the straight barrel type purifying furnace by the carrier gas to form steam flow, depositing steam components on the inner wall of the straight barrel type purifying furnace in different temperature areas along with the rising of the steam flow to form purified materials, scraping off the purified materials by scrapers arranged on the outer wall of the guide flow barrel, falling into an annular storage groove fixed on the inner wall of the straight barrel type purifying furnace, pushing the purified materials to a discharge hole by the scrapers inserted into the storage groove, and discharging the purified materials through the discharge pipe; the non-condensable components are discharged out of the straight barrel type purifying furnace;
4) The waste which cannot be evaporated in the evaporating chamber is discharged from the waste outlet pipe at the bottom of the refining plate when the rotating shaft is in a falling state.
Repeating steps 2) to 4) of the method can realize continuous production.
Compared with the existing tubular purification device technology, the invention has the following obvious prominent substantive characteristics and remarkable advantages:
1) The invention provides a continuous production straight barrel type purifying device which can carry out charging, discharging and evaporation purification under the conditions of no damage to vacuum, heating and temperature control of the purifying device and can continuously purify raw materials. Compared with the existing tubular purification device, the device saves time and energy for manually taking and loading materials by cooling and breaking vacuum.
2) In the use process, the continuous production straight barrel type purifying device can be used for manually feeding, discharging and purifying, can be fully automated, and is suitable for industrialization.
3) The whole material taking process is completely carried out under the vacuum condition, the scraping plate scrapes the materials deposited in each temperature zone to the corresponding material storage tank, and the materials enter the corresponding material storage device through the material outlet, so that no artificial participation exists, the obtained concentrate is more stable, and the purity is higher; simultaneously, make the detachable installation of storage tank in the oven, also convenient clearance simultaneously is convenient in the maintenance.
4) According to the invention, the evaporation material is heated into steam flow through the bottom-layer evaporation furnace, the steam flow vertically rises to pass through the inner walls of the furnace bodies in different temperature areas, and the steam flow can only pass through a narrow space between the guide flow barrel and the furnace bodies in the rising process of the steam flow, so that the temperature of the steam flow is forced to be more approximate to the temperature of the inner walls of the furnace bodies; the whole furnace body is sealed in the outer barrel, so that the heat preservation effect can be realized, and the uniformity of the furnace temperature is improved.
5) According to the invention, the straight barrel type furnace body is adopted, different temperature areas can be independently arranged on the furnace bodies with different heights, steam flows are parallel to the straight barrel type furnace body in the vertical rising process, the temperature uniformity is easier to control, and the problem of low purification precision caused by the phenomenon that the temperature of the inner wall of a common horizontal furnace tube is higher and lower is solved.
6) The invention can evaporate various organic materials, such as organic electroluminescent materials, organic thin film solar cell materials, organic thin film transistor materials, and the like, and inorganic materials with lower evaporation temperature.
Drawings
FIG. 1 is a partial cut perspective view of a straight barrel type purification apparatus of the present invention;
FIG. 2 is a front cross-sectional view of a straight barrel purification apparatus of the present invention;
FIG. 3 is a side cross-sectional view of a straight barrel purification apparatus of the present invention;
FIG. 4 is a front view of the pod of the present invention;
FIG. 5 is a top view of the pod of the present invention;
FIG. 6 is a schematic view of a screed according to the present invention;
FIG. 7 is an enlarged partial view of a top view of the screed structure of the present invention;
FIG. 8 is a schematic diagram of a storage tank structure according to the present invention;
FIG. 9 is a schematic diagram of a combination of a flow guiding barrel, a material storage tank and a scraping plate;
In the figure: the purifying furnace 1 comprises a straight barrel type purifying furnace 1, barrel furnace body sections 1-1, 1-2, 1-3 and 1-4, annular storage tanks 1-5, 1-6, 1-7 and 1-8, discharge ports 1-9, 1-10, 1-11 and 1-12, discharge pipes 1-13, 1-14, 1-15 and 1-16, an inverted cone barrel 1-17, a top cover 1-18, a first extraction port 1-19 and a bearing 1-20; 2, a vaporization furnace, a feed pipe 2-1, a waste outlet pipe 2-2 and an air inlet pipe 2-3; the device comprises a guide barrel 3, an inner cylinder 3-1, a top plate 3-2, a top plate through hole 3-3, a sliding rail 3-4, an inverted cone cylinder 3-5, a rotating shaft 3-6 and a refining plate 3-7; the scraper 4 comprises the outer edges 4-1, 4-2, 4-3, 4-4, a bent edge 4-5, and scrapers 4-6,4-7, 4-8 and 4-9; the heating temperature control system 5, the evaporating furnace heating temperature control system 5-1, the heating temperature control systems 5-2, 5-3, 5-4 and 5-5 of the straight barrel type purifying furnace; the outer barrel 6, the base barrel 6-1, the outer barrel body 6-2, the connecting cover 6-3 and the second extraction opening 6-4.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The technical features of the embodiments of the invention can be combined correspondingly on the premise of no mutual conflict.
As shown in figures 1-3, the continuous production straight barrel type purifying device comprises a straight barrel type purifying furnace 1, an evaporating furnace 2, a guide barrel 3, a scraping plate 4, a heating temperature control system 5 and an outer barrel 6.
The evaporation furnace 2 is communicated with the bottom of the straight barrel type purification furnace body 1, and the outer barrel 6 is sleeved on the peripheries of the straight barrel type purification furnace 1 and the evaporation furnace 2 to form a sealed space, so that the heat preservation effect is achieved; the guide barrel 3 is sleeved in the straight barrel type purification furnace body 1, a channel for the flow of steam generated by the evaporation furnace to circulate is formed between the outer wall of the guide barrel 3 and the inner wall of the straight barrel type purification furnace 1, when the steam encounters the purification furnace wall of each section with lower temperature, the steam is deposited on the purification furnace wall of each section to become a purification material, and then scraped by the scraping plate 4 to fall into a material storage tank fixed on the inner wall of the straight barrel type purification furnace 1, and the purification material is sent out through a material discharge pipe; the scraping plate 4 is provided with a notch for installing a storage groove, and the outer walls of the evaporation furnace 2 and the straight barrel type purification furnace 1 are provided with a heating temperature control system 5.
In one embodiment of the invention, the straight barrel type purifying furnace 1 is divided into a plurality of cylindrical furnace body sections 1-1, 1-2, 1-3 and 1-4 with the same diameter by 1 straight barrel type cylindrical purifying furnace body, the number is preferably 4, the temperature of each cylindrical furnace body section is gradually reduced from bottom to top so as to deposit purifying materials with different temperatures, and the last cylindrical furnace body section is connected with the bottommost inverted cone cylinder; annular storage tanks 1-5, 1-6, 1-7 and 1-8 with conical surfaces are arranged at the joints between two adjacent cylinder furnace body sections and between the last cylinder furnace body section and the bottommost inverted cone cylinder, discharge ports 1-9, 1-10, 1-11 and 1-12 are arranged at the bottoms of the storage tanks, and the discharge ports 1-9, 1-10, 1-11 and 1-12 are connected with discharge pipes 1-13, 1-14, 1-15 and 1-16.
In one embodiment of the invention, the evaporation furnace 2 is a cup-shaped hollow cavity structure with an evaporation chamber, the top of the evaporation furnace 2 is connected with the bottom of the straight barrel type purification furnace 1 in a sealing way, the upper end of the side wall of the evaporation furnace 2 is provided with an air inlet pipe 2-3 for introducing high-purity carrier gas and a feed pipe 2-1 for allowing raw materials to enter, and the bottom of the evaporation furnace 2 is provided with a waste outlet pipe 2-2. The feeding pipe 2-1 is connected with a feeding mechanism and is used for conveying raw materials from a stock bin to a feeding hole on the evaporation furnace 2, then scraping the raw materials piled near the feeding hole into an evaporation chamber of the evaporation furnace by the refining plate 3-7, the waste outlet pipe is used for discharging waste which cannot be evaporated out of the evaporation furnace, and the air inlet pipe is used for introducing high-purity inert gas when carrying out carrier gas flow purification. The feeding mechanism adopts a spiral feeding device.
The heating temperature control system 5 consists of an evaporation furnace heating temperature control system 5-1 and heating temperature control systems 5-2, 5-3, 5-4 and 5-5 of a straight barrel type purifying furnace, wherein each heating temperature control system is mutually independent and comprises a heating device, a temperature sensor and a temperature controller; the evaporation furnace heating temperature control system 5-1 is used for supplying heat to the evaporation furnace 2, and the heating temperature control systems 5-2, 5-3, 5-4 and 5-5 of the straight barrel type purification furnace are used for controlling the temperatures of different temperature areas of the straight barrel type purification furnace 1 to gradually decrease from bottom to top. The heating device can be a plurality of groups of heating wires wound on the outer walls of the evaporation furnace 2 and the straight barrel type purification furnace 1, the start and stop of each group of heating wires are mutually independent, a temperature sensor is arranged on each cylinder furnace body section of the straight barrel type purification furnace 1, and the temperatures of the four cylinder furnace body sections 1-1, 1-2, 1-3 and 1-4 are controlled to gradually decrease from bottom to top through the temperature controller.
The outer barrel 6 comprises a base barrel 6-1, an outer barrel body 6-2 and a connecting cover 6-3, which are all connected in vacuum to form a low vacuum cavity. The bottom open end of the outer barrel body 6-2 is detachably and hermetically connected with the base barrel 6-1, and the top open end of the outer barrel body 6-2 is hermetically connected with the outer wall of the straight barrel type purifying furnace 1 through a connecting cover 6-3; the connecting cover 6-3 is provided with a second air extraction opening 6-4, the base barrel 6-1 is provided with a connecting hole for connecting a pipeline and an electrical connection line to the outside of the outer barrel 6, and a sealing element is arranged at the connecting hole.
In one embodiment of the present invention, as shown in fig. 4, the guide barrel 3 is composed of a guide barrel body with a diameter smaller than the inner diameter of the straight barrel type purification furnace 1, a rotating shaft 3-6, and a refining plate 3-7 mounted at the lower end of the rotating shaft 3-6. A small space is arranged between the outer wall of the guide barrel 3 and the inner wall of the straight barrel type purifying furnace 1, so that the steam flow of the evaporating material can be forced to be closer to the temperature of the temperature zone in which the steam flow is positioned in the rising process. The rotary shaft 3-6 and the guide barrel body are coaxially arranged and fixedly connected into a whole, the rotary shaft 3-6 penetrates through the straight barrel type purification furnace 1, is fixed and sealed at a top cover 1-18 of the straight barrel type purification furnace 1 through a bearing 1-20, and drives the guide barrel 3 to rotate by external power to play roles in guiding and scraping powder; the refining plate 3-7 extends into the evaporation furnace 2, the refining plate 3-7 can rotate and lift along with the rotating shaft 3-6, the rotation of the rotating shaft 3-6 can be realized through an external stirring motor, and the lifting of the rotating shaft 3-6 can be realized through the driving of the rotating shaft and the stirring motor to integrally move along the axial direction by an external lifting motor; when in a lifting state, the bottom of the refining plate 3-7 is kept at a distance from the bottom of the evaporation chamber, and the refining function is realized in the rotating process, namely raw materials entering from the feed inlet of the evaporation furnace 2 are spread into a thin layer, heated uniformly and easily evaporated; when in a falling state, the bottom of the refining plate 3-7 is in contact with the bottom of the evaporation chamber, and the scraping function is performed in the rotation process, namely, the waste in the evaporation chamber is scraped to a waste outlet and is sent to a waste container through a valve.
The guide barrel body is formed by integrally forming a top plate 3-2, an inner cylinder 3-1 and a bottommost inverted cone cylinder 3-5, a space is reserved between the top plate 3-2 and a top cover of the straight barrel type purification furnace body 1, more than one sliding rail 3-4 for installing scraping plates 4 is arranged on the outer wall of the inner cylinder 3-1, the number of the sliding rails is the same as that of the scraping plates, and the number of the sliding rails is preferably 2 or 3. As shown in FIG. 5, the top plate 3-2 is provided with four top plate through holes 3-3 for communicating the inside and the outside of the guide barrel, and the four top plate through holes are uniformly distributed by taking the rotating shaft 3-6 as the center, so that no pressure difference exists between the inside and the outside of the guide barrel.
In one embodiment of the present invention, as shown in fig. 6, the scraper 4 is mounted on the sliding rail 3-4 of the outer wall of the inner cylinder 3-1 shown in fig. 4, the scraper 4 has a multi-stage structure, and the outer edges 4-1, 4-2, 4-3, 4-4 are optionally mounted with high temperature resistant scrapers 4-6 shown in fig. 7, which face the direction of rotation of the guide cylinder, so that the resistance of the scrapers can be reduced, and the scrapers have a certain elasticity so that the scrapers can be tightly attached to the inner wall of the straight barrel type purification furnace 1 for scraping the purification materials deposited on the inner wall of the straight barrel type purification furnace 1. Gaps for installing annular storage tanks 1-5, 1-6, 1-7 and 1-8 are arranged between each section of scraping plates, so that the shape and the size of the scraping plates 4 are matched with those of the storage tanks. In the specific implementation process, the annular storage groove can be directly and fixedly connected with the inner wall of the straight barrel type purification furnace 1, in the installation process, the scraping plate notch shown in fig. 6 is aligned with the annular storage grooves 1-5, 1-6, 1-7 and 1-8, so that the scraping plate 4 is inserted into the storage groove, then the guide barrel 3 shown in fig. 4 is placed into the straight barrel type purification furnace 1 from top to bottom, in the placement process, the sliding rail shown in fig. 4 and 5 is aligned with the bent edge 4-5 on the inner edge of the quasi-scraping plate 4 shown in fig. 7, so that the guide barrel descends along the sliding rail, and after the guide barrel reaches a certain position, the top cover 1-18 of the straight barrel type purification furnace 1 is installed and sealed. The rotary shaft is driven by external power to rotate, the scraping plate 4 can rotate along with the guide barrel 3, the annular storage tanks 1-5, 1-6, 1-7 and 1-8 are fixed, the purified materials which fall into the annular storage tanks 1-5, 1-6, 1-7 and 1-8 after being scraped down along with the rotation of the scraping plate 4 are scraped to the discharge ports 1-9, 1-10, 1-11 and 1-12, and the purified materials are discharged into the storage tanks through the discharge pipes 1-13, 1-14, 1-15 and 1-16.
In one embodiment of the present invention, as shown in fig. 9, the annular storage tanks 1-5, 1-6, 1-7, 1-8 are not directly and fixedly connected with the inner wall of the straight barrel type purification furnace 1 before being installed, but positioning holes are formed in the annular storage tanks 1-5, 1-6, 1-7, 1-8, and the positioning holes are matched with fixing protruding points on the inner wall of the straight barrel type purification furnace 1, so that the annular storage tanks are detachably installed on the inner wall of the straight barrel type purification furnace 1. Specifically, 4 storage tanks 1-5, 1-6, 1-7 and 1-8 shown in fig. 8 are firstly inserted into 4 notches on 3 scraping plates 4 shown in fig. 6, then the scraping plates are installed on the outer wall of a guide barrel 3 uniformly provided with 3 sliding rails, in the installation process, 3 sliding rails are aligned with the bent edges 4-5 of 3 scraping plates 4 to be inserted into a component A shown in fig. 9, then the whole component A is inserted into a straight barrel type purification furnace 1, and when the annular storage tanks 1-5, 1-6, 1-7 and 1-8 on the component A are inserted into the straight barrel type purification furnace 1, the annular storage tanks are matched with fixed protruding points on the inner wall of the straight barrel type purification furnace 1 by virtue of positioning holes on the annular storage tanks, so that the annular storage tanks can be positioned on the inner wall of the straight barrel type purification furnace 1, and the annular storage tanks cannot rotate along with rotation of the scraping plates.
In one embodiment of the invention, the purification process using a straight barrel purification apparatus is optionally performed under high vacuum or under a low pressure carrier gas stream. The carrier gas is high-purity inert gas, such as high-purity argon, which enters the evaporation furnace through the gas inlet pipe 2-3 under the control of the gas flowmeter, and the high-purity inert gas carrying raw material steam rises to the straight barrel type purification furnace for purification, and the residual gas is discharged from the first extraction opening 1-19.
One specific working procedure of the invention is as follows:
1) Before feeding, the device is started, and the inside and the outside of the straight barrel type purification furnace 1 are respectively pumped into a high vacuum environment and a low vacuum environment through a first pumping hole 1-19 on a top cover 1-18 of the straight barrel type purification furnace 1 and a second pumping hole 6-4 on a cover 6-3 connected with an outer barrel 6; according to the evaporating temperatures of different components in the solid raw materials and the condensing temperatures of different components of steam, the evaporating furnace heating temperature control system 5-1 and the heating temperature control systems 5-2, 5-3, 5-4 and 5-5 of the straight barrel type purifying furnace are independently arranged, namely the heating power of the heating device, and according to each temperature sensor and each temperature controller, different temperature areas of the inner wall of the straight barrel type purifying furnace 1 are set, and the temperature is gradually reduced from bottom to top. The rotating shaft 3-6 in the guide barrel 3 is driven at the top by a motor to drive the guide barrel body in the guide barrel 3, the refining plate 3-7 arranged at the lower end of the rotating shaft and the scraping plate 4 arranged on the outer wall of the guide barrel 3 to rotate. The rotating shaft 3-6 is arranged in a lifting state, and at the moment, a space is reserved between the bottom of the refining plate 3-7 arranged at the lower end of the rotating shaft 3-6 and the bottom of the evaporating chamber in the evaporating furnace 2.
2) During feeding, the vaporizable solid raw material is conveyed to a feed inlet of a feed pipe 2-1 on the side wall of an evaporation furnace 2 by adopting a spiral feeding device, the solid raw material is uniformly spread into a thin raw material layer in an evaporation chamber by a rotary refining plate 3-7 in a lifting state, and different components in the raw material are converted into steam in the evaporation chamber; carrier gas is introduced from an air inlet pipe 2-3 on the side wall of the evaporation furnace 2, and steam is driven by the carrier gas to enter a narrow channel between the guide flow barrel 3 and the straight barrel type purification furnace 1, and rises to form steam flow, and the steam flow can heat the guide flow barrel 3 so that the steam cannot be condensed on the guide flow barrel 3; when the steam flow passes through the inner walls of the cylinder furnace sections 1-1, 1-2, 1-3 and 1-4 in different temperature areas, the temperature of the steam flow is reduced to be close to the temperature of the inner wall of the cylinder furnace section, and deposition is carried out when the steam flow passes through the inner wall of the cylinder furnace section in corresponding temperature, so as to form a solid film or crystal grain; the scraper 4 arranged on the outer wall of the guide barrel 3 scrapes down the deposited purified material along with the rotation of the guide barrel 3, the scraped purified material directly falls into the annular storage tanks 1-5, 1-6, 1-7 and 1-8 fixed on the inner wall of the straight barrel type purifying furnace 1, the purified material in the annular storage tanks is scraped to the discharge ports 1-9, 1-10, 1-11 and 1-12 by the scraper 4 along with the rotation of the guide barrel 3, and is discharged into the corresponding storage tanks through the discharge pipes 1-13, 1-14, 1-15 and 1-16, and the non-condensable components are discharged out of the straight barrel type purifying furnace 1 through the first extraction ports 1-19.
3) After the evaporation is completed, the evaporation chamber is provided with residual waste which cannot be evaporated, the rotating shaft 3-6 is arranged in a falling state, the bottom of the refining plate 3-7 is in contact with the bottom of the evaporation chamber, the rotating refining plate 3-7 scrapes the waste in the evaporation chamber to the waste outlet at the bottom, and the waste is sent into the waste container through the waste outlet pipe 2-2.
In the working process of the device, the spiral feeding device can continuously feed materials into the evaporation furnace 2, purified concentrate automatically falls into a corresponding stock bin, and the whole process can continuously produce without damaging the vacuum, heating and temperature control conditions of the purification device.
The foregoing list is only illustrative of specific embodiments of the invention. Obviously, the invention is not limited to the above embodiments, but many variations are possible. All modifications directly derived or suggested to one skilled in the art from the present disclosure should be considered as being within the scope of the present invention.
Claims (9)
1. The continuous production straight barrel type purification device is characterized by comprising a straight barrel type purification furnace (1), an evaporation furnace (2), a guide barrel (3), a scraping plate (4), a heating temperature control system (5) and an outer barrel (6);
The evaporation furnace (2) is communicated with the bottom of the straight barrel type purification furnace (1), and the outer barrel (6) is hermetically sleeved on the peripheries of the straight barrel type purification furnace (1) and the evaporation furnace (2); the guide barrel (3) is sleeved in the straight barrel type purifying furnace (1), and a channel for steam flow to circulate is formed between the outer wall of the guide barrel (3) and the inner wall of the straight barrel type purifying furnace (1); the scraper (4) is arranged on the outer wall of the guide barrel (3), a notch for installing an annular storage groove is formed in the scraper (4), and the annular storage groove is fixed on the inner wall of the straight barrel type purifying furnace (1); the temperature of the evaporation furnace (2) and the outer wall of the straight barrel type purification furnace (1) is controlled by the heating temperature control system (5);
the straight barrel type purifying furnace (1) is formed by connecting a top cover (1-18), a plurality of cylinder furnace body sections with the same diameter and a bottommost inverted cone cylinder, wherein the top cover (1-18) is provided with a first extraction opening (1-19), annular storage tanks are respectively arranged at the connecting positions between two adjacent cylinder furnace body sections and between the last cylinder furnace body section and the bottommost inverted cone cylinder, and the bottom of each annular storage tank is connected with a discharge pipe;
The guide barrel (3) is sleeved in the straight barrel type purifying furnace (1) and comprises a guide barrel body, a rotating shaft (3-6) and a refining plate (3-7) arranged at the lower end of the rotating shaft; the rotary shaft (3-6) and the diversion barrel body are coaxially arranged and fixedly connected into a whole, the rotary shaft (3-6) penetrates through the straight barrel type purification furnace (1) and is fixed and sealed at the top cover (1-18) of the straight barrel type purification furnace (1) through a bearing (1-20).
2. The sustainable production straight barrel type purification device according to claim 1, wherein the annular storage groove is provided with a positioning hole, the positioning hole is matched with a fixed salient point on the inner wall of the straight barrel type purification furnace (1), and the annular storage groove is detachably connected with the inner wall of the straight barrel type purification furnace (1).
3. The sustainable production straight barrel type purifying device according to claim 1, wherein the outer barrel (6) comprises a base barrel (6-1), an outer barrel body (6-2) and a connecting cover (6-3), the bottom open end of the outer barrel body (6-2) is detachably connected with the base barrel (6-1), and the top open end of the outer barrel body (6-2) is in sealing connection with the outer wall of the straight barrel type purifying furnace (1) through the connecting cover (6-3); the connecting cover (6-3) is provided with a second air extraction opening (6-4), and the base barrel (6-1) is provided with a vacuum sealing interface for connecting a pipeline and an electrical connection line to the outside of the outer barrel (6).
4. The continuous production straight barrel type purifying device according to claim 1, wherein the refining plate (3-7) is positioned in the evaporating furnace (2), and the refining plate (3-7) can rotate and lift along with the rotating shaft (3-6).
5. The sustainable production straight barrel type purifying device according to claim 1, wherein the diversion barrel body is integrally formed by a top plate (3-2), an inner cylinder (3-1) and a bottommost inverted cone cylinder (3-5), a space is reserved between the top plate (3-2) and a top cover of the straight barrel type purifying furnace (1), and a sliding rail (3-4) for installing a scraping plate (4) is arranged on the outer wall of the inner cylinder (3-1).
6. The sustainable-production straight barrel type purifying device according to claim 1, wherein the scraping plate (4) is arranged on a sliding rail (3-4) on the outer wall of the inner barrel (3-1), and a cutting edge (4-6) is arranged on the outer edge of the scraping plate (4) and is used for scraping off purified materials deposited on the inner wall of the straight barrel type purifying furnace (1).
7. The sustainable production straight barrel type purifying device according to claim 1, wherein the evaporating furnace (2) is of a hollow cavity structure with an evaporating chamber, the top of the evaporating furnace (2) is connected with the bottom of the straight barrel type purifying furnace (1) in a sealing mode, an air inlet pipe (2-3) for introducing carrier gas and a feed pipe (2-1) for feeding raw materials are arranged at the upper end of the side wall of the evaporating furnace (2), and a waste outlet pipe (2-2) is arranged at the bottom of the evaporating furnace (2).
8. The sustainable production straight barrel type purification device according to claim 1, wherein the heating temperature control system (5) comprises an evaporation furnace heating temperature control system (5-1) and a straight barrel type purification furnace heating temperature control system, the evaporation furnace heating temperature control system (5-1) is used for supplying heat to a combustion chamber in the evaporation furnace (2), and the straight barrel type purification furnace heating temperature control system is used for independently controlling the temperature of different temperature areas of the straight barrel type purification furnace (1).
9. A method of purifying vaporizable material using the sustainable drum purifying apparatus of claim 1 comprising the steps of:
1) The device comprises a starting device, wherein the inside and the outside of the straight barrel type purifying furnace (1) are vacuumized respectively, and then the temperature of an evaporating chamber in the evaporating furnace (2) and the temperatures of different temperature areas of the straight barrel type purifying furnace (1) formed by a plurality of cylindrical furnace body sections are set respectively, and the temperature of the straight barrel type purifying furnace (1) is gradually reduced from bottom to top; when the evaporation chamber and all the temperature areas reach the preset temperature, the rotating shaft (3-6) drives the guide barrel (3) and the scraping plate (4) to rotate;
2) Before feeding, a rotating shaft (3-6) is arranged in a lifting state, and at the moment, a space is reserved between the bottom of a refining plate (3-7) arranged at the lower end of the rotating shaft (3-6) and the bottom of an evaporation chamber in an evaporation furnace (2);
3) During feeding, raw materials are conveyed into an evaporation chamber of an evaporation furnace (2) through a spiral feeding device, are uniformly spread into a raw material layer through a material-homogenizing plate (3-7), and are heated and evaporated in the evaporation chamber; introducing carrier gas from an air inlet pipe of the evaporation furnace (2), driving steam to rise in a channel between the guide barrel (3) and the straight barrel type purifying furnace (1) by the carrier gas to form steam flow, depositing steam components on the inner walls of the straight barrel type purifying furnace (1) in different temperature areas along with the rising of the steam flow to form purified materials, scraping the purified materials by a scraper (4) arranged on the outer walls of the guide barrel (3), falling into an annular storage groove fixed on the inner walls of the straight barrel type purifying furnace (1), and sending the purified materials out through a discharge pipe; the non-condensable components are discharged out of the straight barrel type purifying furnace (1);
4) The waste material which cannot be evaporated in the evaporating chamber is discharged from the waste material outlet pipe (2-2) scraped to the bottom by the refining plate (3-7) when the rotating shaft (3-6) is in a falling state.
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