Method for collecting solid-state purified matter on two lateral sides of horizontal electric heating equipment

文档序号:1611553 发布日期:2020-01-10 浏览:37次 中文

阅读说明:本技术 固态纯净物卧式电加热设备双侧侧面收集方法 (Method for collecting solid-state purified matter on two lateral sides of horizontal electric heating equipment ) 是由 黄超斌 成友为 于 2018-12-12 设计创作,主要内容包括:固态纯净物卧式电加热设备双侧侧面收集方法,采用卧式电加热设备,先通过卧式电加热设备对固态纯净物进行加热,使得固态纯净物在卧式电加热设备内加热蒸发升华,再通过热扩散方式使得升华的固态纯净物从卧式电加热设备的双侧侧面运动到收集系统装置内,并在收集系统装置内通过冷凝方式还原成固体固态纯净物,达到从侧面收集升华的固态纯净物的目的。本发明采取卧式电加热设备从侧面收集固态纯净物,有利于电加热设备内的坩埚进出,方便操作,还可以方便实现固态纯净物升华的侧向扩散移动的升华与冷凝收集的分区处理,利用升华后的再次冷凝可以大幅提升固态纯净物的纯度,细化固态纯净物,实现高纯度、高效、细化的固态纯净物收集处理。(A method for collecting solid-state purified objects on the two side surfaces of horizontal electric heating equipment adopts the horizontal electric heating equipment, firstly heats the solid-state purified objects through the horizontal electric heating equipment, so that the solid-state purified objects are heated, evaporated and sublimated in the horizontal electric heating equipment, then the sublimated solid-state purified objects move into a collection system device from the two side surfaces of the horizontal electric heating equipment in a thermal diffusion mode, and are reduced into solid-state purified objects in the collection system device in a condensation mode, and the purpose of collecting the sublimated solid-state purified objects from the side surfaces is achieved. The horizontal electric heating equipment is adopted to collect the solid purified substances from the side surface, so that the crucible in the electric heating equipment can be conveniently fed in and out, the operation is convenient, the sublimation and condensation collection partition treatment of lateral diffusion movement of the solid purified substances can be conveniently realized, the purity of the solid purified substances can be greatly improved by utilizing the secondary condensation after sublimation, the solid purified substances are refined, and the high-purity, high-efficiency and refined solid purified substance collection treatment is realized.)

1. A method for collecting solid-state purified substances from the lateral surfaces of two sides of horizontal electric heating equipment is characterized in that: adopt horizontal electrical heating equipment, heat solid-state purities through horizontal electrical heating equipment earlier for solid-state purities heat evaporation sublimation in horizontal electrical heating equipment, rethread thermal diffusion mode makes sublimed solid-state purities move in collecting system device from horizontal electrical heating equipment's two side sides, and reduces into solid-state purities through the condensation mode in collecting system device, reaches the purpose of collecting sublimed solid-state purities from the side.

2. The method for collecting the solid-state purified substance from the lateral surfaces of the two sides of the horizontal electric heating device according to claim 1, wherein the method comprises the following steps: the horizontal electric heating equipment is used for heating the solid purified object, a graphite crucible is arranged on the horizontal electric heating equipment, the raw material of the solid purified object is placed into the graphite crucible, and the solid purified object placed into the graphite crucible is heated to the determined sublimation temperature of the solid purified object through electric heating, so that the solid purified object is sublimated in the graphite crucible in a gasification mode.

3. The method for collecting the solid-state purified substance from the lateral surfaces of the two sides of the horizontal electric heating device according to claim 2, wherein: the gasification and sublimation of the solid purified material in the graphite crucible are carried out in a vacuum environment, and the solid purified material in the graphite crucible is in a vacuum state in the horizontal electric heating equipment through a vacuum system, so that the gasification and sublimation of the solid purified material are facilitated when the horizontal electric heating equipment is used for heating.

4. The method for collecting the solid-state purified substance from the lateral surfaces of the two sides of the horizontal electric heating device according to claim 3, wherein: the vacuum state is that the horizontal electric heating equipment and the collecting system device are sealed, so that inner cavities of the horizontal electric heating equipment and the collecting system device are in a sealed state, a vacuumizing system is connected to a shell of the horizontal electric heating equipment or the collecting system device, and the inner cavities of the horizontal electric heating equipment and the collecting system device are maintained in a vacuum state through the vacuumizing system.

5. The method for collecting the solid-state purified substance from the lateral surfaces of the two sides of the horizontal electric heating device according to claim 1, wherein the method comprises the following steps: the horizontal electric heating equipment and the collecting system device are arranged into two areas with different temperatures, wherein the temperature in the collecting system device is lower than that in the horizontal electric heating equipment; after the solid-state purified substance is gasified and sublimated in the graphite crucible, the gas solid-state purified substance flows and diffuses into the collecting device with low temperature from the side surfaces of the two sides of the horizontal electric heating equipment by utilizing the temperature difference between the horizontal electric heating equipment and the collecting device, and is condensed and reduced into solid powder particles in the collecting device at the same speed.

6. The method for collecting the solid-state purified substance from the lateral surfaces of the two sides of the horizontal electric heating device according to claim 3, wherein: the solid-state purified material sublimated from the crucible of the horizontal electric heating equipment escapes from the crucible in a gaseous state after being sublimated, flows laterally to the two sides of the horizontal electric heating equipment through the upper space of the crucible, and enters the collecting device arranged on the side face of the horizontal electric heating equipment.

7. The method for collecting the solid-state purified substance from the lateral surfaces of the two sides of the horizontal electric heating device according to claim 1, wherein the method comprises the following steps: the solid-state purified object which is collected and sublimated from the side surface is connected with the collecting device at the two side surfaces of the horizontal electric heating equipment, and after the gasified and sublimated solid-state purified object flows into the collecting system device, the solid-state purified object of the gas is rapidly changed into the solid again in a condensing mode, so that the purpose of collecting the sublimated solid-state purified object from the side surface is achieved.

8. The method for collecting the solid-state purified substance from the lateral surfaces of the two sides of the horizontal electric heating device according to claim 1, wherein the method comprises the following steps: the solid purified matter is reduced into solid purified matter in the collecting system device in a condensing mode, namely the collecting system device matched with the section shape of the electric heating cavity is arranged at the side inlet of the end part of the electric heating cavity of the horizontal electric heating equipment, the inner cavity of the collecting system device is communicated with the electric heating cavity of the horizontal electric heating equipment, and the temperature in the collecting system device is maintained below the sublimation temperature of the solid purified matter, so that the temperature of the inner cavity of the collecting system device and the temperature of the electric heating cavity of the horizontal electric heating equipment form a temperature difference; after the solid-state purified substance is heated and sublimated in the crucible by electricity, the solid-state purified substance is diffused from high temperature to low temperature according to the diffusion principle, flows into the inner cavity of the collecting system device from the upper space of the electric heating cavity of the horizontal electric heating equipment, and is reduced into a solid substance when the sublimated gasified solid-state purified substance flows into the inner cavity of the collecting system device due to the fact that the temperature of the inner cavity of the collecting system device is controlled to be lower than the sublimation temperature of the solid-state purified substance, and the solid substance falls into the inner cavity of the collecting system device, so that the purpose of side face collection is achieved.

9. The method for collecting the solid-state purified substance from the lateral surfaces of the two sides of the horizontal electric heating device according to claim 8, wherein: the collecting system device is in a cup shape matched with the cross section of the electric heating cavity and is larger than the size of an electric heating cavity port of the horizontal electric heating equipment, the electric heating cavity of the horizontal electric heating equipment is covered in the port of the collecting system device, so that a gap is formed between the electric heating cavity port of the horizontal electric heating equipment and the port of the collecting system device, the temperature of the inner cavity of the collecting system device is adjusted and controlled by adjusting the size of the gap between the electric heating cavity port of the horizontal electric heating equipment and the collecting system device and the distance between the ports, and the temperature of the inner cavity of the collecting system device is ensured to be lower than the sublimation temperature of the solid pure substances.

10. The method for collecting the solid-state purified substance from the lateral surfaces of the two sides of the horizontal electric heating device according to claim 9, wherein: the collecting system device is matched with a port of an electric heating cavity of the horizontal electric heating equipment in a movable structure, a collecting cover in the collecting system device is matched with the port of the electric heating cavity of the horizontal electric heating equipment in the collecting process, a condensation transition area is formed by adjusting the distance between the two ports, and sublimed solid purified substances are cooled to form solid powder when passing through the condensation transition area; after the collection is finished, the collection system device is moved to open the port of the electric heating cavity of the horizontal electric heating equipment, so that an operator can take out or put in the crucible of the horizontal electric heating equipment conveniently.

Technical Field

The invention relates to a substance smelting and collecting method, in particular to a collecting method for purifying or refining various solid purified substances (such as silicon, magnesium, vanadium and the like), which can effectively improve the collecting efficiency and degree of the solid purified substances; belongs to the technical field of collection of solid pure smelting.

Background art:

the production of simple substance silicon in China has been well established, with the tightening of national energy policy and the development of energy conservation and emission reduction and the advocation of new energy, the smelting of simple substance silicon has become a primary product and process, a series of circulating industrial chains of simple substance silicon, polycrystalline silicon, monocrystalline silicon, solar cells and the like are built in a plurality of domestic emerging energy enterprises, and the development of the whole energy field in China and the application of new energy are influenced in the coming years.

The existing elemental silicon smelting process and flow are processed by a vertical elemental silicon smelting furnace, namely an elemental silicon intermediate frequency smelting furnace, a high-purity graphite crucible is vertically placed into the elemental silicon intermediate frequency smelting furnace, the high-purity graphite crucible is inductively heated to 1650-1750 ℃ by using a magnetic field, and the high-purity graphite crucible is used as a heating body to heat and melt the elemental silicon to smelt the elemental silicon. However, the existing elemental silicon smelting furnace is generally vertical, and the vertical elemental silicon smelting furnace is adopted to collect elemental silicon and needs to be put in and taken out from the top of the furnace, so that the defects of low efficiency, complex operation and the like exist, and the research on the defects is very necessary.

Patent documents in which the same technology as that of the present invention is not found through patent search are reported, and the following patents which have a certain relationship with the present invention are mainly included:

1. the patent number is CN201810323986.4, named as 'a method for producing nanometer submicron spherical silicon powder', and the applicant is: the invention discloses a production method of nanometer submicron silicon powder, which is an invention patent of Tianshuiji chemical industry limited company. The nano spherical silicon is largely used for the silicon-carbon cathode material of the high-energy density lithium ion battery, the energy ratio of the lithium ion battery is improved, and a novel high-temperature gasification physical production method is provided for solving the problems of low unit production efficiency, high cost and low quality of the existing nano silicon powder production method, in particular to the problem of nano-crystallization of the silicon material in the silicon-carbon cathode material of the high-energy density lithium ion battery. The method selects polysilicon, monocrystalline silicon or metal silicon powder as raw materials, and obtains nano-scale or submicron-scale spherical silicon powder through electric heating-laser composite heating, high-temperature gasification, high-temperature growth of silicon vapor, cooling and collection. The process can produce high-purity and high-quality nano silicon powder with the particle size of nano grade (5 nm-100 nm) and submicron grade (0.1 μm-1.0 μm), and the particle size can be accurately controlled.

2. Patent No. CN200710196562 entitled "vacuum purification furnace and purification method especially for silicon metal/silicon dioxide", applicant: the invention patent of the crystal Zhan (Nanchang) science and technology Co., Ltd discloses a vacuum purification furnace for metallic silicon/silica, comprising a crucible for containing the metallic silicon/silica and having an outer wall, and a heating system for heating the crucible and comprising at least a temperature control system for controlling the temperature of the crucible, the vacuum purification furnace being capable of being evacuated and filled with an inert gas or oxygen, characterized in that the temperature control system comprises a plurality of heating elements arranged on at least a part of the outer wall and a computer system connected to the plurality of heating elements, the plurality of heating elements being divided into a plurality of groups in one direction of the crucible, the computer system controlling each group of heating elements in the following manner, for the first group of heating members located foremost in the direction and the first region of the melt in the crucible corresponding to the first group of heating members, the first group of heating members continue to heat the peripheral portion of the first region during the cooling solidification of the first region. This patent also relates to a method for purifying silicon metal/silica using the vacuum purification furnace described above.

3. The patent number is CN201621413960.1, entitled "improved intermediate frequency induction heating equipment", and the applicant is: the patent discloses an improved medium-frequency induction heating device, which is characterized in that the included angle between the central axis of a vacuum furnace shell and the installation ground of the vacuum furnace shell is 1-10 degrees; at least the opening end side of the graphite crucible positioned at the lower part of the central axis of the graphite crucible is provided with a graphite baffle; the end face of the opening end of the graphite crucible is covered with a collector, the collector is in a circular truncated cone shape, and the diameter of the opening end of the collector at the joint of the collector and the graphite crucible is larger than that of the tail end of the collector.

4. The patent number is CN201620391918.8, and the name is 'a device for preparing high-purity nano molybdenum trioxide', the applicant is: the utility model discloses a Australia nanometer material technology limited company's utility model patent in Hubei, this patent discloses a device of preparation high-purity nanometer molybdenum trioxide, including the feed inlet, the bottom and the pay-off auger of feed inlet are linked together, inside the export of pay-off auger stretched into sublimation stove, the bottom of sublimation stove was provided with the bin outlet, the upside and the molybdenum trioxide steam passageway of sublimation stove are linked together, are provided with the dispersant nozzle on the molybdenum trioxide steam passageway, the export and the recoverer of molybdenum trioxide steam passageway are linked together, the bottom of recoverer is provided with the finished product collecting vessel, its characterized in that: the furnace wall of the sublimation furnace is sequentially provided with a silicon nitride liner layer, a graphite cushion layer and a high-temperature heat preservation layer, and the outer wall of the high-temperature heat preservation layer is provided with a medium-frequency induction heating copper pipe.

Although the above patents have been carefully analyzed and referred to the collection and processing method or apparatus of silicon or other pure substances, some improved technical solutions have been proposed, through careful analysis, the proposed patents still adopt a vertical method to work, even though the patent No. CN201621413960.1, entitled "an improved medium frequency induction heating device" proposes a side-lying type silica collection apparatus, but also an upward inclined fixed system apparatus, so that further research on how to simplify the purification and collection method of solid pure substances is needed.

Disclosure of Invention

The invention aims to provide a method for collecting solid-state purified substances, which is simpler and more convenient and has higher operation efficiency, aiming at the defects that various solid-state purified substances or other solid-state substances are collected by a vertical electric heating furnace, so that the operation is inconvenient and the operation efficiency is low.

In order to achieve the purpose, the invention provides a method for collecting the solid-state purified object from the two side surfaces of horizontal electric heating equipment, the horizontal electric heating equipment is adopted, the solid-state purified object is heated by the horizontal electric heating equipment firstly, so that the solid-state purified object is heated, evaporated and sublimated in the horizontal electric heating equipment, the sublimated solid-state purified object moves into a collecting system device from the two side surfaces of the horizontal electric heating equipment in a thermal diffusion mode, and is reduced into the solid-state purified object in the collecting system device in a condensation mode, and the purpose of collecting the sublimated solid-state purified object from the side surfaces is achieved.

Further, the step of heating the solid purified object through the horizontal electric heating device is to arrange a graphite crucible on the horizontal electric heating device, put the raw material of the solid purified object into the graphite crucible, and heat the solid purified object put into the graphite crucible to the determined sublimation temperature of the solid purified object through electric heating, so that the solid purified object is sublimated in the graphite crucible.

Further, the gasification and sublimation of the solid purified material in the graphite crucible are carried out in a vacuum environment, and the solid purified material in the graphite crucible is in a vacuum state in the horizontal electric heating equipment through a vacuum system, so that the gasification and sublimation of the solid purified material are facilitated when the horizontal electric heating equipment is heated.

Furthermore, the vacuum state is to seal the horizontal electric heating device and the collecting system device, so that the inner cavities of the horizontal electric heating device and the collecting system device are in a sealed state, and a vacuumizing system is connected to the shell of the horizontal electric heating device or the collecting system device, so that the inner cavities of the horizontal electric heating device and the collecting system device are maintained in a vacuum state through the vacuumizing system.

Further, the step of enabling the sublimated solid purified substances to move from the two sides of the horizontal electric heating equipment to the collecting system device in a thermal diffusion mode is to arrange the horizontal electric heating equipment and the collecting system device into two areas with different temperatures, wherein the temperature in the arrangement of the collecting system device is lower than that in the horizontal electric heating equipment; after the solid-state purified substance is gasified and sublimated in the graphite crucible, the gas solid-state purified substance flows and diffuses into the collecting device with low temperature from the side surfaces of the two sides of the horizontal electric heating equipment by utilizing the temperature difference between the horizontal electric heating equipment and the collecting device, and is condensed and reduced into solid powder particles in the collecting device at the same speed.

Furthermore, the solid purified material sublimated from the crucible of the horizontal electric heating device moves into the collecting system device from the lateral sides of the horizontal electric heating device in a thermal diffusion mode, and the solid purified material sublimated from the crucible of the horizontal electric heating device escapes from the crucible in a gaseous state after sublimation, flows to the lateral sides of the horizontal electric heating device through the upper space of the crucible, and enters the collecting device arranged on the lateral side of the horizontal electric heating device.

Furthermore, the solid-state purified matter collected and sublimated from the side surface is connected with the collecting device at the side surfaces of the two sides of the horizontal electric heating equipment, and after the gasified and sublimated solid-state purified matter flows into the collecting system device, the solid-state purified matter of the gas is rapidly changed into the solid again in a condensing mode, so that the purpose of collecting the sublimated solid-state purified matter from the side surface is achieved.

Furthermore, the solid purified matter is reduced into solid purified matter in a condensing mode in the collecting system device, namely the collecting system device matched with the section shape of the electric heating cavity is arranged at the side inlet of the end part of the electric heating cavity of the horizontal electric heating equipment, the inner cavity of the collecting system device is communicated with the electric heating cavity of the horizontal electric heating equipment, and the temperature in the collecting system device is maintained below the sublimation temperature of the solid purified matter, so that the temperature of the inner cavity of the collecting system device and the temperature of the electric heating cavity of the horizontal electric heating equipment form a temperature difference; after the solid-state purified substance is heated and sublimated in the crucible by electricity, the solid-state purified substance is diffused from high temperature to low temperature according to the diffusion principle, flows into the inner cavity of the collecting system device from the upper space of the electric heating cavity of the horizontal electric heating equipment, and is reduced into a solid substance when the sublimated gasified solid-state purified substance flows into the inner cavity of the collecting system device due to the fact that the temperature of the inner cavity of the collecting system device is controlled to be lower than the sublimation temperature of the solid-state purified substance, and the solid substance falls into the inner cavity of the collecting system device, so that the purpose of side face collection is achieved.

Furthermore, the collecting system device is in a cup shape matched with the cross section of the electric heating cavity and is larger than the size of the port of the electric heating cavity of the horizontal electric heating equipment, the electric heating cavity of the horizontal electric heating equipment is covered in the port of the collecting system device, so that a gap is formed between the port of the electric heating cavity of the horizontal electric heating equipment and the port of the collecting system device, the temperature of the cavity in the collecting system device is adjusted and controlled by adjusting the size of the gap between the port of the electric heating cavity of the horizontal electric heating equipment and the collecting system device and the distance between the ports, and the temperature of the cavity in the collecting system device is ensured to be lower than the sublimation temperature of the solid purified substances.

Furthermore, the collecting system device is matched with a port of an electric heating cavity of the horizontal electric heating equipment in a movable structure, a collecting cover in the collecting system device is matched with the port of the electric heating cavity of the horizontal electric heating equipment in the collecting process, a condensation transition area is formed by adjusting the distance between the two ports, and the sublimed solid purified substance is cooled to form solid powder when passing through the condensation transition area; after the collection is finished, the collection system device is moved to open the port of the electric heating cavity of the horizontal electric heating equipment, so that an operator can take out or put in the crucible of the horizontal electric heating equipment conveniently.

The invention has the advantages that:

the horizontal electric heating equipment is adopted to collect the solid purified substances from the side surface, so that the crucible in the electric heating equipment can be conveniently fed in and out, the operation is convenient, the sublimation and condensation collection partition treatment of lateral diffusion movement of the solid purified substances can be conveniently realized, the purity of the solid purified substances can be greatly improved by utilizing the secondary condensation after sublimation, the solid purified substances are refined, and the high-purity, high-efficiency and refined solid purified substance collection treatment is realized. Has the following advantages:

1. the horizontal side collection is adopted, so that the crucible in the electric heating equipment can be conveniently fed and discharged, and the operation is convenient;

2. the solid purified materials are collected from the side surface, and the sectional treatment of sublimation and condensation collection can be realized by effectively utilizing the lateral movement of the sublimated solid purified materials; achieve the purpose of high-efficiency collection

3. The solid-state purified object is collected through the side direction, the purity of the solid-state purified object can be greatly improved by utilizing condensation after sublimation, and the recovery of the high-purity solid-state purified object is realized.

Drawings

FIG. 1 is a schematic diagram of the general structure of one embodiment of the present invention;

fig. 2 is a schematic top view of the structure of fig. 1.

Detailed Description

The invention is further illustrated with reference to the following figures and specific examples.

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