Solid sublimation equipment

By combining oscillator and gas pulse device in the sublimation equipment, three-dimensional mixing of solid materials is achieved, the problem of uneven heat is solved, and the sublimation efficiency is improved. It is suitable for the separation and purification of high-purity solid materials on industrial scale.

CN222238857UActive Publication Date: 2024-12-27JIANGSU NATA OPTO ELECTRONIC MATERIAL CO LTD +1
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Patent Information

Application Number
CN202422871910.9
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-11-25
Publication Date
2024-12-27
Estimated Expiration
2034-11-25

AI Technical Summary

Technical Problem

The prior art has uneven heat in the process of sublimation of solid materials, resulting in a low sublimation rate and it is difficult to meet the demand for large-scale industrial production. Especially in large-scale industrial applications, traditional methods such as fluidized beds, vibration beds and rotary beds exist. Problems of space occupation, insufficient stability or complex mechanical structure.

Method used

By introducing an oscillator and gas pulse device into the sublimation device, the oscillator provides transverse vibration to evenly distribute the material, and the gas pulse device generates periodic high-pressure air flow, achieving three-dimensional mixing, breaking the plate junction layer, and promoting uniform heat transfer.

Benefits of technology

It significantly improves the sublimation efficiency, realizes full mixing and dispersion of solid materials, breaks the dependence on equipment space and complex mechanical structures in traditional technology, and is suitable for the separation and purification of high-purity solid materials on industrial scale.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses solid sublimation equipment. The solid sublimation equipment comprises a sublimation kettle, an oscillator and a gas pulse device, the sublimation kettle is provided with a containing cavity for containing solid materials; the oscillator is connected with the sublimation kettle and is used for vibrating the sublimation kettle; the gas pulse device comprises a high-pressure gas pipeline extending into the containing cavity of the sublimation kettle, gas injection holes are formed in the pipe wall of the high-pressure gas pipeline, and solid materials contained in the containing cavity can cover the gas injection holes; and pulse airflow generated by the gas pulse device can be sprayed out from the gas spraying holes, so that gas pulses are formed in the accommodating cavity. According to the solid sublimation equipment provided by the invention, the gas pulse device and the oscillator are matched with each other, so that materials form efficient three-dimensional mixing in the sublimation kettle, solid materials are fully mixed and dispersed in the sublimation process, the hardening phenomenon can be broken, uniform heat transfer is promoted, and the sublimation efficiency is improved.
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Description

Technical Field

[0001] The utility model belongs to the technical field of sublimation devices, and in particular relates to solid sublimation equipment. Background Art

[0002] Sublimation is a process in which a solid substance is directly converted into a gas under heat without going through a liquid state. This physical phenomenon is widely used in the purification and refining of various substances. For example, in the preparation of high-purity chemicals, the production of electronic materials and other industrial applications, the sublimation process is often used as an efficient and important separation method. During the sublimation process of a solid mixture, the heating and gasification efficiency of the solid components directly determines the rate and effect of the entire purification process. However, the existing technology faces many problems when performing sublimation of solid materials.

[0003] When the amount of sublimated solid material is large, uneven heating is common. As heat is transferred from the outer layer of the solid material to the inner layer, the outer layer material begins to vaporize first, while the inner layer material is unable to reach the temperature required for sublimation due to insufficient heat, causing the sublimation process to stagnate in a local area. This uneven heating phenomenon seriously affects the overall sublimation rate, especially in industrial mass production, where the problem of uneven heating makes it difficult to effectively increase the volume of the sublimation process, thereby limiting the efficiency and scale of industrial production.

[0004] Therefore, it is necessary to provide a new solution to the above technical problems. Utility Model Content

[0005] The utility model aims to provide a solid sublimation device, which can achieve full mixing and dispersion of solid materials during the sublimation process.

[0006] To achieve the above purpose, the technical solution provided by the utility model is as follows:

[0007] The utility model provides a solid sublimation device, which comprises: a sublimation kettle, an oscillator and a gas pulse device; the sublimation kettle has a cavity for accommodating solid materials; the oscillator is connected to the sublimation kettle and is used to make the sublimation kettle vibrate; the gas pulse device comprises a high-pressure gas pipeline extending into the cavity of the sublimation kettle, a gas injection hole is arranged on the pipe wall of the high-pressure gas pipeline, and the solid materials accommodated in the cavity can cover the gas injection hole; wherein the pulsed airflow generated by the gas pulse device can be ejected from the gas injection hole to form a gas pulse in the cavity.

[0008] In one or more embodiments, the high-pressure gas pipeline includes at least two gas pipelines that are separately arranged, and the gas pipelines extend vertically into the cavity of the sublimation reactor to the top of the sublimation reactor.

[0009] In one or more embodiments, the distance between the bottom outlet of the gas pipeline and the bottom of the cavity is 1 / 5 to 1 / 4 of the height of the cavity.

[0010] In one or more embodiments, the pipe wall of the gas pipeline is provided with a plurality of gas injection holes facing in different directions, and the aperture of the gas injection holes is 3-6 mm.

[0011] In one or more embodiments, a solenoid valve for opening and closing the gas pipeline is provided on the gas pipeline.

[0012] In one or more embodiments, a sieve plate is disposed in the chamber of the sublimation reactor, and the outer circumferential surface of the sieve plate is engaged with the inner circumferential surface of the chamber.

[0013] In one or more embodiments, the sieve holes on the sieve plate have an aperture of 0.5 to 2 μm, and the distance between the sieve plate and the top of the cavity is 1 / 5 to 1 / 4 of the height of the cavity.

[0014] In one or more embodiments, the solid sublimation equipment further comprises a collecting container, the collecting container and the cavity of the sublimation kettle are connected via an insulation pipeline, the collecting container is connected to a vacuum pump, and a valve is provided on the insulation pipeline.

[0015] In one or more embodiments, the collection container includes a high-temperature collection zone, a medium-temperature collection zone, and a low-temperature collection zone arranged in sequence, and the high-temperature collection zone, the medium-temperature collection zone, and the low-temperature collection zone are staggered to form a winding flow channel in the collection container.

[0016] In one or more embodiments, a high-temperature vertical furnace for heating the sublimation reactor is disposed outside the sublimation reactor.

[0017] Compared with the prior art, the solid sublimation equipment provided by the present invention, through the cooperation of the gas pulse device and the oscillator, enables the material to form an efficient three-dimensional mixture in the sublimation kettle, realizes the full mixing and dispersion of the solid material during the sublimation process, can break the agglomeration phenomenon and promote uniform heat transfer, thereby improving the sublimation efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings required for use in the embodiments or the prior art descriptions are briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the utility model, and for ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0019] Figure 1 It is a structural schematic diagram of a solid sublimation device in one embodiment of the utility model.

[0020] Description of main reference numerals:

[0021] 1-sublimation kettle, 11-chamber, 12-sieve plate, 2-oscillator, 3-gas pulse device, 31-high-pressure gas pipeline, 311-gas injection hole, 312-gas pipeline, 313-solenoid valve, 4-collecting container, 41-high-temperature collection area, 42-medium-temperature collection area, 43-low-temperature collection area, 5-insulation pipeline, 51-valve, 6-vacuum pumping device, 7-high-temperature vertical furnace, 8-solid material. DETAILED DESCRIPTION

[0022] In order to enable those skilled in the art to better understand the technical solutions in the present invention, the following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work should fall within the scope of protection of the present invention.

[0023] Unless explicitly stated otherwise, throughout the specification and claims, the term “comprise” or variations such as “include” or “comprising”, etc., will be understood to include the stated elements or components but not to exclude other elements or components.

[0024] Sublimation technology is a material separation method that directly converts solids into gases and is widely used in the chemical, pharmaceutical and high-purity material preparation. However, in large-scale industrial applications, existing sublimation devices and methods generally have bottlenecks of low efficiency, which affects production capacity and economic benefits.

[0025] The existing technology usually achieves the sublimation process by simply heating solid materials. However, due to the low efficiency of heat conduction inside the solid, it is difficult to ensure the uniformity of heating of the sublimation material, resulting in a decrease in the overall sublimation rate and being unable to meet the needs of industrial mass production. At the same time, during the heating process, the surface of the material often forms a hardened layer due to uneven heating or partial melting, further hindering heat transfer and material volatilization.

[0026] To solve this problem, a variety of material mixing methods such as fluidized bed, vibrating bed, stirred bed and rotating bed have been proposed one after another. However, these methods all have their limitations: the fluidized bed needs to occupy a large amount of space to achieve material fluidization, which affects the stability of the vacuum environment; although the vibrating bed can mix materials during lateral vibration, the heat conduction effect in the vertical direction is still poor; the mechanical structure of the stirred bed is complex, and there is a risk of equipment jamming during operation, and the maintenance cost is high; and the rotating bed has complex moving parts, and it is difficult to ensure the sealing of the connection with the back-end device, and the equipment stability is insufficient. Therefore, in the traditional sublimation method, how to effectively improve the material mixing effect and heat conduction efficiency has always been a technical problem that the industry needs to solve urgently.

[0027] Based on the above problems, the core technology of the utility model is to achieve full mixing and dispersion of solid materials in the sublimation process through the combination of an oscillator and a gas pulse device, thereby significantly improving the sublimation efficiency. Specifically, the oscillator introduced in the equipment acts on the sublimation kettle in a high-frequency vibration manner, so that the material is evenly distributed in the horizontal direction, preventing local overheating and optimizing heat transfer. Compared with the traditional vibrating mixing device, this scheme further introduces a gas pulse device to generate a periodic high-pressure airflow, which acts on the longitudinal direction of the solid material, thereby achieving a more efficient three-dimensional mixing effect. The gas pulse can not only disturb the material vertically, but also destroy the compaction layer formed on the surface of the material, maintain the looseness and good volatility of the material particles, and avoid efficiency loss during the sublimation process.

[0028] The innovative design of this utility model is that it realizes efficient heat transfer and uniform mixing of solid materials in the sublimation kettle through the synergistic effect of the gas pulse device and the oscillator, breaking through the dependence of the traditional technology on equipment space and complex mechanical structure. This optimized design makes the solid sublimation equipment more applicable in industrial applications and can better meet the needs of different fields for separation and purification of high-purity solid materials.

[0029] Please refer to Figure 1 As shown, the solid sublimation equipment in one embodiment of the utility model includes a sublimation reactor 1, an oscillator 2 and a gas pulse device 3.

[0030] The sublimation vessel 1 has a cavity 11 for accommodating solid materials 8. The oscillator 2 is connected to the sublimation vessel 1 and is used to vibrate the sublimation vessel 1. The gas pulse device 3 includes a high-pressure gas pipeline 31 extending into the cavity 11 of the sublimation vessel 1. A gas injection hole 311 is provided on the wall of the high-pressure gas pipeline 31. The solid materials 8 accommodated in the cavity 11 can cover the gas injection hole 311. The pulsed airflow generated by the gas pulse device 3 can be ejected from the gas injection hole 311 to form a gas pulse in the cavity 11.

[0031] As the core component of the equipment, the sublimation reactor 1 plays the main role of containing solid materials 8 and performing sublimation reactions. The shape and material selection of the cavity 11 of the sublimation reactor 1 meet the requirements of temperature uniformity and airtightness during the sublimation process. The material is usually made of high-temperature resistant and corrosion-resistant materials to ensure that no physical deformation or chemical reaction occurs in a high-temperature environment, thereby ensuring the long-term and stable operation of the equipment. Because the sublimation process needs to be carried out in a controlled vacuum environment to reduce the sublimation temperature of the substance and increase the sublimation rate. Therefore, the structural design of the sublimation reactor 1 takes into account factors such as air leakage prevention and sealing to ensure that the entire device maintains good airtightness during operation.

[0032] The function of the oscillator 2 connected to the sublimation kettle 1 is to act on the sublimation kettle 1 through high-frequency vibration, so that the solid material 8 in the cavity 11 can be fully mixed and dispersed laterally. The design of the oscillator 2 is based on the principle of vibration mixing. It breaks the adhesion and compaction between materials by generating periodic or random vibrations, thereby increasing the fluidity and looseness of the materials. The vibration force applied by the oscillator 2 causes the solid particles to constantly collide and move with each other, thereby avoiding local overheating or reduced sublimation efficiency due to uneven heating. This lateral vibration provides a basic guarantee for the uniform heating of the material in the cavity 11, but the action of the oscillator 2 alone is still not enough to completely eliminate all heat conduction problems, especially when the material volume is large or the cavity 11 is deep. Therefore, the equipment further introduces a gas pulse device 3 to form a unique multi-dimensional mixing mechanism.

[0033] The gas pulse device 3 is directly connected to the interior of the cavity 11 of the sublimation reactor 1, and includes one or more high-pressure gas pipelines 31 extending into the cavity 11. A plurality of gas injection holes 311 are provided on the high-pressure gas pipeline 31. The design of these injection holes takes into account the directionality and coverage of the gas flow to ensure that the gas flow can act on the material in the best form. The injection holes are distributed in different directions of the tube wall, so that the high-pressure gas can be evenly distributed in the entire cavity 11, forming a strong airflow disturbance. This pulsed airflow can produce multi-level impacts in the material, further promoting the mixing of solid particles and heat conduction in the vertical direction. Especially for large or high-density materials, the effect of the gas pulse can effectively destroy the compacted layer, break it up, and maintain the overall uniformity and good volatility of the material.

[0034] The vacuum degree will affect the sublimation process of solid materials (it is not necessary to maintain a specific vacuum degree during the sublimation process of solid materials). Materials with different characteristics can obtain better sublimation effects under appropriate vacuum degrees. In order to further improve the sublimation effect, the pulse injection time and frequency of the high-pressure gas can be flexibly adjusted according to the material characteristics and sublimation requirements to minimize the disturbance to the system vacuum degree. In this way, the entire sublimation process can not only maintain a high efficiency, but also minimize energy consumption and equipment loss. In addition, the gas pulse device 3 can select high-pressure nitrogen as the working medium. This gas has stable chemical properties and will not react with the material, ensuring that no impurities are introduced during the sublimation process, thereby improving the purity of the target substance.

[0035] In an exemplary embodiment, the high-pressure gas pipeline 31 includes at least two separate gas pipelines 312, and the gas pipelines 312 extend vertically from the top of the sublimation vessel 1 into the chamber 11 of the sublimation vessel 1. The gas pipelines 312 are provided with pressure gauges (P1, P2).

[0036] The separated gas pipelines 312 are intended to ensure uniformity of gas flow and full coverage of the effect. Each pipeline is evenly distributed along the top of the sublimation reactor 1 and extends vertically into the cavity 11. This arrangement allows high-pressure gas to be transported vertically downward from the top of the cavity 11 to cover the material layer as much as possible. Through such a design, the gas injection holes 311 can be closer to different areas of the solid material 8, avoiding the problem of local airflow concentration that may be caused by a single gas pipeline 312. This multi-path separated structure not only improves the uniformity of gas distribution, but also effectively regulates the direction and intensity of the airflow, ensuring that each material particle can be fully disturbed by the gas pulse.

[0037] Specifically, the distance between the bottom outlet of the gas pipeline 312 and the bottom of the cavity 11 is 1 / 5 to 1 / 4 of the height of the cavity 11. Setting the bottom outlet of the gas pipeline 312 at a height of 1 / 5 to 1 / 4 of the bottom of the cavity 11 can make the airflow ejected by the high-pressure gas form a better impact force and coverage. At this height, the airflow can not only quickly penetrate the lower layer of materials, but also effectively push the middle and upper layers of materials, forming a strong disturbance from bottom to top. The advantage of this design is that the high-pressure gas pulse will not cause excessive agitation of local materials due to too short a distance, nor will it cause the airflow to lose its impact force and have difficulty penetrating the material layer due to too large a distance.

[0038] The oscillator 2 mainly provides lateral vibration to evenly disperse the material on the horizontal plane, while the high-pressure gas pulse provides disturbance force in the vertical direction. These two forces combined together can form a complex and efficient three-dimensional mixing state in the chamber 11. In this way, the material particles can continuously move and turn over during the sublimation process, improving the uniformity of heat transfer and preventing local overheating or insufficient sublimation.

[0039] Furthermore, a plurality of gas injection holes 311 facing in different directions are provided on the wall of the gas pipeline 312 , and the aperture of the gas injection hole 311 is 3-6 mm.

[0040] The arrangement of the gas injection holes 311 in different directions can achieve all-round airflow distribution. These injection holes are opened at different angles on the wall of the gas pipeline 312, so that each time the high-pressure gas pulse is ejected, it is not concentrated in one direction, but evenly diffused in multiple directions ( Figure 1 The black arrows around the gas injection holes 311 indicate the gas injection direction). This multi-angle airflow distribution can effectively break the static accumulation between the material particles and promote the comprehensive mixing and dispersion of the materials. Through such a disturbance design, the material particles will continuously turn over and move in the sublimation reactor 1, avoiding the formation of a hardened layer or an overheated area in a certain part due to long-term heating, thereby achieving more uniform sublimation.

[0041] The aperture of the gas injection hole 311 is preferably designed to be between 3 and 6 mm. If the aperture is too small, the airflow injection speed will be too high, resulting in an overly concentrated impact force, which may cause local scattering or uneven disturbance of the material, affecting the stability of the overall sublimation process. On the contrary, if the aperture is too large, the airflow will diffuse too quickly, lose the due impact force, and it will be difficult to effectively break the adhesion and compaction between the materials.

[0042] The gas pipeline 312 is provided with a solenoid valve 313 for switching the gas pipeline 312, and its main function is to control the inflow and interruption of high-pressure gas. By adjusting the opening and closing time of the solenoid valve 313, dynamic control of the gas pulse frequency and intensity can be achieved. Different material properties and sublimation requirements have different requirements for airflow disturbance, and the existence of the solenoid valve 313 enables this requirement to be flexibly met. For example, for denser solid materials 8, the solenoid valve 313 can be set to open at high frequency for a short time to provide a stronger airflow impact, thereby effectively breaking the adhesion between the materials and enhancing the mixing effect. For looser materials, the pulse frequency or airflow intensity can be reduced to avoid unnecessary material scattering and ensure the stability and efficiency of the sublimation process.

[0043] In an exemplary embodiment, a sieve plate 12 is provided in the chamber 11 of the sublimation reactor 1, and the outer peripheral surface of the sieve plate 12 is engaged with the inner peripheral surface of the chamber 11. The sieve plate 12 separates the solid material 8 in the chamber 11 from the gas outlet area, playing a filtering and supporting role. The sieve plate 12 is provided with a plurality of tiny sieve holes, and the design of these sieve holes allows the gas generated during the sublimation process to pass smoothly, while the solid particles are effectively blocked on the sieve plate 12, thereby preventing the material from being carried out of the sublimation reactor 1 by the airflow.

[0044] The outer circumference of the sieve plate 12 is joined to the inner circumference of the chamber 11, which ensures the stability and sealing of the sieve plate 12. This joining method prevents the material from leaking from the gap between the sieve plate 12 and the wall of the chamber 11, and effectively improves the overall sealing performance of the equipment. Sealing is crucial in the sublimation process, because for some special solid material sublimation equipment, it is usually necessary to maintain a specific vacuum degree and airflow path to ensure the smooth progress of the sublimation process.

[0045] Specifically, the sieve hole diameter on the sieve plate 12 is 0.5~2μm, and the distance between the sieve plate 12 and the top of the cavity 11 is 1 / 5~1 / 4 of the height of the cavity 11. The sieve hole diameter is set to 0.5~2μm in order to achieve the filtration and separation of particulate materials during the sublimation process. This aperture range is sufficient to allow the gas molecules generated during the sublimation process to pass smoothly, while blocking solid particles and preventing them from being carried out of the cavity 11 by the high-pressure airflow. If the aperture is too small, it may hinder the passage of airflow and increase the pressure burden of the system; if the aperture is too large, it cannot effectively prevent the loss of material particles, affecting the purification effect of the sublimated substance.

[0046] The distance between the sieve plate 12 and the top of the cavity 11 is set to 1 / 5 to 1 / 4 of the height of the cavity 11. Such a distance design is intended to provide sufficient accommodation space for the solid material 8, while ensuring that the material can fully contact and be evenly distributed in the sublimation vessel 1. By placing the sieve plate 12 at this height, the material in the sublimation vessel 1 can form an area that is evenly heated, which not only avoids the overheating problem caused by the material directly accumulating at the bottom of the cavity 11, but also provides sufficient action space for the airflow of the gas pulse device 3, making the disturbance effect more significant.

[0047] In an exemplary embodiment, the solid sublimation device further includes a collecting container 4, the collecting container 4 and the chamber 11 of the sublimation kettle 1 are connected through an insulation pipeline 5, the collecting container 4 is connected to a vacuum pump 6, and a valve 51 is provided on the insulation pipeline 5. A pressure gauge (P3) is provided on the insulation pipeline 5.

[0048] During the sublimation process, the solid material 8 is directly converted into gas by heat energy, and the sublimation gas needs to be quickly and stably transferred from the sublimation reactor 1 to the collection container 4 to prevent condensation or gas leakage. To achieve this, the collection container 4 is connected to the volume 11 of the sublimation reactor 1 through the insulation pipeline 5. The insulation pipeline 5 not only provides a stable gas transmission channel, but also prevents the gas from condensing due to a sudden drop in temperature during the transmission process through insulation measures, thereby maintaining the stability of the sublimation product.

[0049] In order to further optimize the sublimation process, the system is equipped with a vacuum device 6, which is directly connected to the collection container 4 to form an adjustable vacuum environment. The vacuum device 6 is used to form a negative pressure in the collection container 4, and this negative pressure state is transmitted to the sublimation reactor 1 through the insulation pipeline 5, so as to adjust the vacuum degree in the sublimation reactor 1. The adjustment of the vacuum degree will affect the sublimation process, because under a lower pressure environment, the sublimation temperature of the material will decrease, thereby accelerating the sublimation rate and reducing energy consumption. Through the precise control of the vacuum device 6, the equipment can adjust the vacuum degree according to the sublimation characteristics of different materials, thereby achieving more flexible and efficient operation and meeting the diverse industrial production needs.

[0050] Specifically, the collection container 4 includes a high-temperature collection area 41, a medium-temperature collection area 42 and a low-temperature collection area 43 which are arranged in sequence. The high-temperature collection area 41, the medium-temperature collection area 42 and the low-temperature collection area 43 are arranged alternately to form a winding flow channel in the collection container 4.

[0051] The multi-level partition design of the collection container 4 is based on the physical characteristics of the condensation behavior of the substance. During the sublimation process, different substances have different condensation points, and the gaseous products will be condensed in sequence and effectively collected in an environment with gradually decreasing temperature. The high-temperature collection area 41 is set in the part close to the insulation pipe to receive and preliminarily condense those products with higher condensation points. These substances can be transformed into solid state and quickly collected in a high-temperature environment.

[0052] The medium temperature collection area 42 is located in the flow channel after the high temperature area. This area is used to condense substances with a low condensation point but higher than the ambient temperature. As the temperature gradually decreases, the gaseous substances continue to condense into solid particles in the medium temperature environment and are collected, further improving the cleanliness and separation effect. The setting of the medium temperature area ensures that the sublimation products will not flow directly to the low temperature area and cause excessive condensation, and also prevents the sublimation products from being lost or incompletely volatilized at too high a temperature.

[0053] The low temperature collection area 43 is located at the end of the flow channel of the collection container 4, and is used to capture and condense the substances with the lowest condensation point. Here, the remaining gaseous products will be fully condensed and finally collected, thereby realizing the separation and recovery of the substances. The existence of the low temperature area can ensure that the gaseous substances in the entire sublimation process will not be incompletely condensed due to insufficient temperature, and then flow out of the system or pollute the surrounding environment.

[0054] The staggered arrangement of the three collection areas forms a meandering flow channel, which extends the path of gas flow and enhances the condensation effect. The formation of the meandering flow channel allows the gaseous substance to fully contact with each temperature zone when flowing through the collection container 4, increasing the condensation time and thus improving the condensation efficiency. In addition, the meandering flow channel structure helps to slow down the air flow speed, so that the gaseous substance has enough time to condense into a solid state in the flow channel, avoiding rapid passage and reducing the condensation effect.

[0055] In an exemplary embodiment, a high-temperature vertical furnace 7 for heating the sublimation kettle 1 is provided outside the sublimation kettle 1. The high-temperature vertical furnace 7 can wrap the outside of the sublimation kettle 1 to form an all-round heating area. The purpose of this design is to provide a uniform heat source to avoid the phenomenon of low material sublimation efficiency or sintering and hardening of materials in certain areas due to local overheating or uneven heating.

[0056] In summary, the solid sublimation equipment provided by the present invention, through the cooperation between the gas pulse device and the oscillator, enables the material to form an efficient three-dimensional mixture in the sublimation kettle, realizes the full mixing and dispersion of the solid material during the sublimation process, can break the agglomeration phenomenon and promote uniform heat transfer, thereby improving the sublimation efficiency.

[0057] It is obvious to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be regarded as exemplary and non-restrictive from any point of view, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention. Any reference numeral in a claim should not be regarded as limiting the claim to which it relates.

[0058] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A solid sublimation device, characterized in that: include: A sublimation reactor having a cavity for containing solid materials; an oscillator, connected to the sublimation kettle, and used to vibrate the sublimation kettle; A gas pulse device, comprising a high-pressure gas pipeline extending into the chamber of the sublimation reactor, wherein a gas injection hole is provided on the pipe wall of the high-pressure gas pipeline, and the solid material contained in the chamber can cover the gas injection hole; Wherein, the pulsed airflow generated by the gas pulse device can be ejected from the gas injection hole to form a gas pulse in the cavity.

2. The solid sublimation equipment according to claim 1, characterized in that: The high-pressure gas pipeline includes at least two gas pipelines that are separated and arranged, and the gas pipelines extend vertically into the cavity of the sublimation kettle to the top of the sublimation kettle.

3. The solid sublimation equipment according to claim 2, characterized in that: The distance between the bottom outlet of the gas pipeline and the bottom of the cavity is 1 / 5 to 1 / 4 of the height of the cavity.

4. The solid sublimation equipment according to claim 2, characterized in that: The pipe wall of the gas pipeline is provided with a plurality of gas injection holes facing in different directions, and the aperture of the gas injection holes is 3-6 mm.

5. The solid sublimation equipment according to claim 2, characterized in that: The gas pipeline is provided with a solenoid valve for opening and closing the gas pipeline.

6. The solid sublimation equipment according to claim 1, characterized in that: A sieve plate is arranged in the cavity of the sublimation kettle, and the outer peripheral surface of the sieve plate is connected with the inner peripheral surface of the cavity.

7. The solid sublimation equipment according to claim 6, characterized in that: The sieve holes on the sieve plate have an aperture of 0.5-2 μm, and the distance between the sieve plate and the top of the cavity is 1 / 5-1 / 4 of the height of the cavity.

8. The solid sublimation equipment according to claim 1, characterized in that: The solid sublimation equipment further comprises a collecting container, the collecting container and the containing cavity of the sublimation kettle are communicated with each other through a heat-insulating pipeline, the collecting container is connected to a vacuum pumping device, and a valve is arranged on the heat-insulating pipeline.

9. The solid sublimation equipment according to claim 8, characterized in that: The collection container includes a high-temperature collection area, a medium-temperature collection area and a low-temperature collection area which are arranged in sequence. The high-temperature collection area, the medium-temperature collection area and the low-temperature collection area are arranged alternately to form a winding flow channel in the collection container.

10. The solid sublimation equipment according to claim 1, characterized in that: A high-temperature vertical furnace for heating the sublimation kettle is arranged outside the sublimation kettle.