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WO2022156224A1 - 一种超微粉粒子聚集冷却罐式结构及超微粉粒子成形方法 - Google Patents

一种超微粉粒子聚集冷却罐式结构及超微粉粒子成形方法 Download PDF

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WO2022156224A1
WO2022156224A1 PCT/CN2021/116493 CN2021116493W WO2022156224A1 WO 2022156224 A1 WO2022156224 A1 WO 2022156224A1 CN 2021116493 W CN2021116493 W CN 2021116493W WO 2022156224 A1 WO2022156224 A1 WO 2022156224A1
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particles
tank
cooling
powder particle
channel
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PCT/CN2021/116493
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English (en)
French (fr)
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钟笔
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钟笔
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Priority claimed from CN202110099342.3A external-priority patent/CN112915919A/zh
Priority claimed from CN202120198835.8U external-priority patent/CN214636172U/zh
Application filed by 钟笔 filed Critical 钟笔
Priority to JP2023507605A priority Critical patent/JP7566376B2/ja
Priority to US18/035,940 priority patent/US20230415115A1/en
Publication of WO2022156224A1 publication Critical patent/WO2022156224A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium

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  • the invention belongs to the technical field of ultrafine powder particle preparation, in particular to an ultrafine powder particle aggregation cooling tank structure and an ultrafine powder particle forming method.
  • the substance to be prepared is first heated and gasified at high temperature, and then solidified and formed from gaseous state to liquid state. Because the ultrafine powder particles to be prepared are microscopic materials, mostly nanoscale, submicron or micron-scale powders, the formed particles are small in size, very fast in forming speed, and very high in temperature. Although the technical principle of forming is simple, the actual It is very difficult to use. It is more difficult to prepare powder particles with uniform particle size, stable morphology and good dispersion that can be used in batches.
  • Common methods include a flared structure, which slows the flow of the vapor to control particle formation, or a blow-to-cool structure, which allows the vapor to cool quickly. These two methods have the defect of uneven temperature of the inner and outer layers of the air flow, or the defect of the uneven internal flow caused by the inner layer of air blowing and air intake, which will lead to the appearance of a large number of ultra-small and ultra-large particles, which will affect the subsequent use of the powder.
  • the purpose of the present invention is to provide a kind of ultrafine powder particle aggregation cooling tank structure and ultrafine powder particle forming method, to solve the problem that a large number of ultra-small and super-large particles in the prior art affect the subsequent use of the powder.
  • An ultra-fine powder particle aggregation cooling tank structure which is arranged in the ultra-fine powder particle preparation system, including an outlet and return structure, a garbage return structure or a garbage collection structure, a particle forming control structure and a tank-type direction-changing material distribution structure connected in sequence;
  • the front end of the air outlet and return structure is connected to the front high temperature evaporator, and the rear end of the tank-type direction-changing material distribution structure is connected to the rear collection structure;
  • the ultrafine powder particle preparation system also includes a heating system arranged in the high temperature evaporator for providing a heat source, a feeding system for providing raw materials to the high temperature evaporator, a circulating cooling system for providing cooling, and a carrier flow and cooling air source or Circulating gas system, a pressure balance system that provides pressure balance control, and a gas-solid separation system or a gas-solid-liquid separation system for the collection part.
  • the front end of the air outlet and return structure is connected to the air outlet of the high-temperature evaporator, and the interior of the air outlet and return structure at least includes a first channel for the entry of high-temperature steam; or heating device.
  • the interior of the garbage return structure or garbage collection structure at least includes a second channel, the front end of the second channel is connected to the first channel, and the rear end is connected to the inner cavity of the particle forming control structure; the second channel
  • the outer side is provided with a heat preservation or heating device.
  • the front end of the inner cavity of the particle forming control structure is connected to the second channel, and the rear end of the inner cavity is connected to the air inlet pipe of the jet cooling structure or the tank-type direction-changing material distribution structure, and an ultrafine powder particle forming area is arranged inside.
  • a heat preservation or heating or cooling structure is arranged inside the particle forming control structure, and the temperature of the ultrafine powder particle forming area is indirectly controlled by heat conduction or heat radiation, and the particle size is controlled by the carrier gas velocity and the cross-sectional size of the ultrafine powder particle forming area. The velocity with which the carrier gas passes through the ultrafine particle forming area.
  • a jet cooling structure for pre-cooling the formed particles is provided between the particle forming control structure and the tank-type direction-changing material distribution structure, and the jet cooling structure at least includes an inner third channel, and the front end of the third channel is provided. It is connected with the ultrafine powder particle forming area, and the rear end is connected with the tank-type direction-changing material distribution structure, and a porous inner layer plate is arranged outside the third channel to uniformly spray cooling gas into the third channel from the periphery.
  • the tank-type direction-changing material distribution structure includes a direction-changing tank-type cavity, and an air inlet pipe and an air outlet pipe are connected to the direction-changing tank type cavity, wherein the air inlet pipe is connected to the third channel or particle.
  • the forming control structure is connected, and the air outlet pipe is connected with the collecting structure;
  • the interior of the air inlet duct and the air outlet duct is provided with an inner-layer thermal insulation structure or a cooling structure;
  • the included angle between the axial centerline of the air intake duct and the axial centerline of the air outlet duct is 30-150°.
  • the relationship between the volume V of the direction-changing tank cavity and the cross-sectional area S1 of the air inlet interface is as follows:
  • one or more cooling fluid inlets are provided on the direction changing tank cavity, the cooling fluid is gas or liquid, and the cooling fluid enters the direction changing tank cavity through the cooling fluid inlet, and the cooling fluid enters the direction changing tank cavity through the cooling fluid inlet.
  • the carrier gas and powder in the tank cavity are mixed and cooled.
  • a method for forming an ultrafine powder particle aggregation cooling tank structure, using the ultrafine powder particle aggregation cooling tank structure of the present disclosure comprises the following steps:
  • the material to be prepared ultrafine powder particles is added into the high temperature evaporator, the material vapor evaporated by heating is mixed with the carrier gas to form a mixture, and then enters the air outlet and reflux structure from the air outlet of the high temperature evaporator, and the air outlet is controlled by heat preservation or heating
  • the internal temperature of the reflow structure is higher than the melting point of the material to be prepared;
  • the mixed gas enters the particle forming control structure after passing through the air outlet and return structure, the garbage return structure or the garbage collection structure.
  • the temperature of each part of the ultrafine powder particle forming area is indirectly controlled by heat conduction or thermal radiation, and the speed of the particles passing through the internal areas with the carrier gas is controlled by the carrier gas velocity and the cross-sectional size of the pipe, which provides stable and controllable conditions for particle forming, allowing the particles to be formed.
  • the substance to be prepared changes from gaseous state to liquid state, liquid state to solid state, gaseous states collide with each other and condense into smaller liquid nuclei, and smaller liquid nuclei collide with each other to form larger droplets or gaseous state collides with smaller liquid nuclei to form larger liquid nuclei.
  • Droplets larger droplets continue to collide with each other to grow or solidify into solid particles, smaller liquid cores and solid particles combine into larger solid particles or become core-shell structures, gaseous and solid particles combine into larger solid particles or become cores Shell structure, solid particles continue to cool, so as to prepare particles with desired particle size and morphology;
  • step S3 The particles with the desired particle size and shape prepared in step S2 are carried by the carrier gas, and directly enter the tank-type direction-changing material distribution structure, and the defective particles in the particles are separated from the good particles, wherein the good particles are in the carrier gas.
  • the air is carried by the air to move to the next process, and the defective particles converge to the garbage return structure or garbage collection structure;
  • the good particles are carried by the carrier gas into the collection structure, and the formed ultrafine powder particles are separated from the carrier gas, wherein the ultrafine powder particles are collected as products, and the carrier gas is discharged or recycled.
  • the particles with the desired particle size and morphology prepared in step S2 are carried by the carrier gas into the inside of the jet cooling structure, and the cooling gas is uniformly sprayed into the inner channel from the periphery through the porous inner layer plate, and the cooling gas is injected into the inner channel. After the high temperature gas and the formed particles are mixed and cooled, they enter the tank-type direction-changing distribution structure.
  • This patent precisely controls each stage of the ultrafine powder particle forming process through a specific structure, including temperature field control, velocity field control, and control of the connection between the structures, using the steam circulating inside it to pass through each controlled part uniformly. , to provide stable and controllable conditions for the formation of ultrafine powder particles, and the formed particles have uniform particle size, stable morphology and good dispersion.
  • FIG. 1 is a schematic structural diagram of the ultrafine powder particle aggregation cooling tank structure of the present invention.
  • Air outlet and return structure 2. Garbage return structure or garbage collection structure, 3. Particle forming control structure, 4. Air jet cooling structure, 41. Air jet at the jet cooling structure, 5. Tank-type direction-changing material distribution structure, 51, Cooling fluid inlet, 6. Inner cavity in high temperature evaporator, 7. Collector.
  • the terms “installed”, “connected” and “connected” should be understood in a broad sense, unless otherwise expressly specified and limited, for example, it may be a fixed connection or a detachable connection Connection, or integral connection; may be mechanical connection or electrical connection; may be direct connection, indirect connection through an intermediate medium, or internal communication between two elements.
  • installed may be a fixed connection or a detachable connection Connection, or integral connection; may be mechanical connection or electrical connection; may be direct connection, indirect connection through an intermediate medium, or internal communication between two elements.
  • This structure is used to prepare ultrafine powder particles, including but not limited to metal ultrafine powder particles.
  • preparation of metal ultrafine powder particles is taken as an example for description, but it is not limited that this structure can only be used for the preparation of metal ultrafine powder particles.
  • the particle aggregation and cooling tube-pot structure is a channel, and each interface is designed in the channel.
  • the connection method is to connect all parts, and to precisely control each stage in the particle forming process through a specific structure, including temperature field control, velocity field control, and control of the connection between structures, so that the steam circulating inside is evenly distributed. After each controlled part, stable and controllable conditions are provided for particle formation, and conditions are created for microscopic particle formation.
  • the substances to be prepared change from gaseous state to liquid state, liquid state to solid state, gaseous states collide with each other and condense into smaller liquid nuclei, and smaller liquid nuclei collide with each other to form larger droplets, or gaseous state collides with smaller liquid nuclei to form smaller liquid nuclei.
  • Large droplets, larger droplets continue to collide with each other to grow or solidify into solid particles, smaller liquid cores and solid particles combine into larger solid particles or a core-shell structure, gaseous and solid particles combine into larger solid particles or become The core-shell structure, the solid particles continue to cool, so as to prepare the particles with the desired particle size and morphology.
  • the formed particles have uniform particle size, stable morphology and good dispersion.
  • the application provides a kind of ultrafine powder particle aggregation cooling tank structure, which is arranged in the ultrafine powder particle preparation system, and in the ultrafine powder particle preparation system in the present application, it also includes a superfine powder particle preparation system arranged in a high temperature evaporator.
  • a superfine powder particle preparation system arranged in a high temperature evaporator.
  • feeding system providing raw material to high temperature evaporator
  • circulating cooling system providing cooling
  • gas source or circulating gas system providing carrier flow and cooling
  • pressure balance system providing pressure balance control
  • collecting part gas-solid separation system or gas-solid-liquid separation system are all in the prior art, and their connection relationship or structure has not been improved in this application. Therefore, they will not be described in detail in this application, but can be obtained from the previous patent documents here.
  • the present application also provides each functional segment inside the cooling tank structure for gathering ultrafine powder particles.
  • the cross-sectional shape and caliber size of each functional segment can be set to be the same, similar, or deformed, variable diameter, etc. as required, as long as each functional segment can be Function segment connections can be designed as required.
  • the length of each functional segment is selected as needed, which does not affect the realization of the technical solution of the present application.
  • Each functional segment can also be a multi-segment splicing or each part of the overall structure, which is specifically adjusted according to actual needs (such as site, production volume, etc.), and is not a limitation or improvement to the technical solution of the present application.
  • the focus of this application is the gathering cooling tube tank structure arranged between the high temperature evaporator and the collecting structure, including the air outlet and return structure 1 connected in sequence, the garbage return structure or garbage collection structure 2, the particle forming control structure 3 and the tank structure Change the distribution structure 5.
  • the front end of the air outlet and return structure 1 is connected to the air outlet of the front high temperature evaporator, and the rear end of the tank-type direction-changing material distribution structure 5 is connected to the rear collection structure.
  • the inside of the air outlet and return structure 1 at least includes a first channel for high temperature steam to enter, and the outer shell of the air outlet and return structure 1 is provided outside the first channel.
  • a heat preservation structure is arranged between the first passage and the outer shell of the air outlet and return structure 1, and a reinforcement structure or a heating device is arranged outside the first passage.
  • the outer shell of the air outlet and return structure 1 is a jacket structure, and a circulating cooling liquid is passed through the jacket structure.
  • the first channel is made of a material that does not physically or/and chemically react with the material to be prepared.
  • the temperature inside the gas outlet and reflux structure 1 is controlled to be higher than the melting point of the ultrafine powder particle material to be prepared by heat preservation or heating.
  • the garbage return structure or garbage collection structure 2 includes at least a second passage in the interior of the garbage return structure or garbage collection structure 2 .
  • the front end of the second channel is connected to the first channel, and the rear end is connected to the inner cavity of the particle forming control structure 3 .
  • the garbage in the upper pipeline or channel is melted into liquid and then returned, or the garbage in the upper pipeline or channel is collected into the garbage storage bucket to prevent the passage of gas in the channel.
  • the outside of the second channel is provided with a heat preservation or heating device, and the heat preservation or heating device is used to control the temperature inside the garbage return structure to be higher than the melting point of the material to be prepared, or the temperature in the ventilation channel of the garbage collection structure to be higher than the desired preparation temperature.
  • the melting point of the material, the temperature in the garbage storage bucket is lower than the melting point of the material to be prepared.
  • the front end of the inner cavity of the particle forming control structure 3 is connected with the second channel, and the rear end of the inner cavity is connected with the air jet cooling structure 4 or the air inlet pipe of the tank-type changing direction material distribution structure 5, and an ultrafine powder particle forming area is arranged inside.
  • the ultrafine powder particle forming area is a channel structure, which is the main place for particle forming control.
  • a heat preservation or heating or cooling structure is arranged inside the particle forming control structure 3, and the temperature of the ultrafine powder particle forming area is indirectly controlled by heat conduction or heat radiation, and the particles are controlled by the carrier gas velocity and the cross-sectional size of the ultrafine powder particle forming area.
  • the speed of the carrier gas passing through the ultrafine powder particle forming area provides stable and controllable conditions for particle forming.
  • the particle forming control structure 3 includes an outer shell structure, an intermediate thermal insulation layer and an inner thermal conduction layer.
  • the outer shell structure is a jacket structure, and the jacket structure is used for circulating coolant.
  • the intermediate thermal insulation layer has a single-layer or multi-layer structure.
  • the inner heat-conducting layer forms a heat-insulated channel, that is, the ultrafine powder particle forming area, and is used to indirectly control the temperature of the material circulating in the channel through heat conduction or heat radiation.
  • the substance to be prepared is changed from gaseous state to liquid state, liquid state to solid state, and the gaseous state collides with each other to condense into smaller liquid nuclei, and the smaller liquid nuclei collide with each other to form larger droplets or gaseous and smaller liquid nuclei.
  • Small liquid nuclei collide to form larger droplets larger droplets continue to collide with each other to grow or solidify into solid particles, smaller liquid nuclei and solid particles combine into larger solid particles or a core-shell structure, and gaseous and solid particles combine In order to form larger solid particles or to form a core-shell structure, the solid particles continue to cool, thereby producing particles of the desired particle size and morphology.
  • the smaller liquid core only refers to a relative concept, not a specific size
  • a larger droplet also refers to a relative concept, not a specific size. Therefore, the above-mentioned larger and smaller does not mean that it is unclear, but only because it involves the internal changes of the molecule, and is used to express in words, and the following larger and smaller should be understood in this way.
  • a jet cooling structure 4 for pre-cooling the formed particles can be installed between the particle forming control structure 3 and the tank-type diversion distribution structure 5 .
  • the jet cooling structure 4 at least includes an internal third channel, the front end of the third channel is connected with the ultrafine powder particle forming area, and the rear end is connected with the tank-type direction-changing material distribution structure 5 .
  • a porous inner layer plate is arranged in the third channel to uniformly spray cooling gas into the third channel from the periphery to prevent soft agglomeration or hard agglomeration when the formed particles are agglomerated due to high temperature.
  • the tank-type direction-changing material distribution structure 5 includes a direction-changing tank-type cavity, and an air inlet pipe and an air outlet pipe are connected to the direction-changing tank type cavity, wherein the air inlet pipe and the third channel or the particle forming control structure are connected. 3 connection, the outlet pipe is connected with the collecting structure.
  • the included angle between the axial centerline of the air intake duct and the axial centerline of the air outlet duct is 30-150°.
  • the present application also provides a method for forming ultrafine powder particles, using the ultrafine powder particle aggregation cooling tube-pot structure of the present disclosure, comprising the following steps:
  • the material to be prepared ultrafine powder particles is added into the high temperature evaporator, the material vapor evaporated by heating is mixed with the carrier gas to form a mixture, and then enters the air outlet and reflux structure from the air outlet of the high temperature evaporator, and the air outlet is controlled by heat preservation or heating
  • the internal temperature of the reflow structure is higher than the melting point of the material required to be prepared.
  • the mixed gas enters the particle forming control structure after passing through the air outlet and return structure, the garbage return structure or the garbage collection structure.
  • the temperature of each part of the ultrafine powder particle forming area is indirectly controlled by heat conduction or thermal radiation, and the speed of the particles passing through the inner area with the carrier gas is controlled by the carrier gas velocity and the pipe cross-sectional size, providing stable and controllable conditions for particle forming.
  • step S3 The particles with the desired particle size and shape prepared in step S2 are carried by the carrier gas, and directly enter the tank-type direction-changing material distribution structure, and the defective particles in the particles are separated from the good particles, wherein the good particles are in the carrier gas. Carrying by the air, it moves to the next process, and the defective particles converge to the garbage return structure or the garbage collection structure.
  • the good particles are carried by the carrier gas into the collection structure, and the formed ultrafine powder particles are separated from the carrier gas, wherein the ultrafine powder particles are collected as products, and the carrier gas is discharged or recycled.
  • the particles with the desired particle size and morphology prepared in step S2 are carried by the carrier gas into the inside of the jet cooling structure, and the cooling gas is uniformly sprayed into the inner channel from the periphery through the porous inner layer plate, and the incoming high temperature After the gas and the formed particles are mixed and cooled, they enter the tank-type diversion distribution structure.
  • One or more cooling fluid inlets are arranged on the direction-changing tank-type cavity of the tank-type direction-changing material distribution structure.
  • the cooling fluid is gas or liquid, and the cooling fluid enters the direction-changing tank-type cavity through the cooling fluid inlet.
  • the carrier gas and powder are mixed and cooled through the reversing tank cavity.
  • the aggregated, cooled and shaped particles are collected into a product, and the carrier gas is discharged or recycled.
  • the high-temperature evaporator in front, the collection and cooling structure in the rear, the heating system that provides the heat source in the high-temperature evaporator, and the feeding system that provides raw materials in front of the high-temperature evaporator provides cooling.
  • the circulating cooling system, the gas source or circulating gas system that provides carrier flow and cooling, the pressure balance system that provides pressure balance control, and the gas-solid separation system or gas-solid-liquid separation system of the collection part cooperate together to complete the continuous particle aggregation, cooling and forming. Circulate the industrial production process to prepare nanoscale, submicron or micron-scale powders with uniform particle size, stable morphology and good dispersion.

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Abstract

一种超微粉粒子聚集冷却罐式结构及超微粉粒子成形方法，罐式结构设置于超微粉粒子制备系统中，包括依次连接的出气与回流结构（1）、粒子成形控制结构（3）及罐式变向分料结构（5）；出气与回流结构（1）的前端与前置的高温蒸发器连接，罐式变向分料结构（5）的后端与后置的收集器（7）及冷却结构连接。

Description

一种超微粉粒子聚集冷却罐式结构及超微粉粒子成形方法 技术领域
本发明属于超微粉粒子制备技术领域，特别是指一种超微粉粒子聚集冷却罐式结构及超微粉粒子成形方法。
背景技术
在使用蒸发冷凝气相法制备超微粉粒子的成形与冷却技术中，先将所需制备的物质先经过高温加热气化，再由气态经液态后固化成形。因为所需制备的超微粉粒子为微观材料，多为纳米级、亚微米级或微米级粉末，成形的粒子尺寸较小，形成速度非常快，温度非常高，成形的技术原理虽然简单，但是实际运用却非常困难。如需制备出可以批量使用的粒径均匀、形貌稳定，分散良好的粉体粒子，难度更大。
常用方法包括扩口结构，让蒸气流动速度放慢然后去控制粒子成形；或是吹气冷却结构，让蒸气快速冷却。这两种方法存在气流内外层温度不均匀的缺陷，或存在吹气进气内层导致内部流态不均匀的缺陷，都会导致大量超小与超大颗粒的出现，影响粉体的后续使用。
发明内容
本发明的目的是提供一种超微粉粒子聚集冷却罐式结构及超微粉粒子成形方法，以解决现有技术中存在的大量超小与超大颗粒影响粉体的后续使用的问题。
本发明是通过以下技术方案实现的：
一种超微粉粒子聚集冷却罐式结构，设置于超微粉粒子制备系统中，包括依次连接的出气与回流结构、垃圾回流结构或垃圾收集结构、粒子成形控制结构及罐式变向分料结构；
所述出气与回流结构的前端与前置的高温蒸发器连接，罐式变向分料结构的后端与后置的收集结构连接；
所述超微粉粒子制备系统还包括设置于高温蒸发器内用于提供热源的加 热系统，向高温蒸发器内提供原料的加料系统，提供冷却的循环冷却系统，提供载流和冷却的气源或循环气系统，提供压力平衡控制的压力平衡系统，以及收集部分的气固分离系统或气固液分离系统。
可选的，所述出气与回流结构的前端与高温蒸发器的出气口连接，所述出气与回流结构的内部至少包括一用于高温蒸气进入的第一通道；第一通道的外侧设置有保温或加温装置。
可选的，所述垃圾回流结构或垃圾收集结构的内部至少包括一第二通道，所述第二通道的前端与第一通道连接，后端与粒子成形控制结构的内腔连接；第二通道的外侧设置有保温或加温装置。
可选的，所述粒子成形控制结构的内腔前端与第二通道连接，内腔后端与喷气冷却结构或罐式变向分料结构的进气管连接，其内部设置有超微粉粒子成形区域，在所述粒子成形控制结构的内部设置有保温或加温或冷却结构，通过热传导或热辐射间接控制超微粉粒子成形区域的温度，通过载流气速度与超微粉粒子成形区域的截面尺寸控制粒子随载流气通过超微粉粒子成形区域的速度。
可选的，粒子成形控制结构与罐式变向分料结构之间设置有用于对已成形的粒子进行预冷却的喷气冷却结构，喷气冷却结构至少包括内部的第三通道，第三通道的前端与超微粉粒子成形区域连通，后端与罐式变向分料结构连接，在所述第三通道外设置有多孔内层板，以由周边向第三通道内均匀喷入冷却气体。
可选的，所述罐式变向分料结构包括变向罐式腔体，在所述变向罐式腔体上连接有进气管道和出气管道，其中进气管道与第三通道或粒子成形控制结构连接，出气管道与收集结构连接；
所述进气管道与出气管道的内部设置有内层保温结构或冷却结构；
所述进气管道的轴向中线与出气管道的轴向中线的夹角为30-150°。
可选的，所述变向罐式腔体的容积V与进气接口内截面积S1的关系如下：
V/S1>100，其中,V的单位为立方厘米，S1的单位为平方厘米。
可选的，在所述变向罐式腔体上设置有一个或一个以上的冷却流体进口，冷却流体为气体或液体，冷却流体通过冷却流体进口进入变向罐式腔体内，对 通过变向罐式腔体的载流气及粉末进行混合与冷却。
一种超微粉粒子聚集冷却罐式结构成形方法，使用本公开的超微粉粒子聚集冷却罐式结构，包括以下步骤：
S1、待制备超微粉粒子的材料加入到高温蒸发器内，经过加热蒸发的材料蒸气与载流气混合成混合气后从高温蒸发器的出气口进入出气与回流结构，通过保温或加温控制出气与回流结构的内部温度高于所需要制备材料的熔点；
S2、所述混合气在通过出气与回流结构、垃圾回流结构或垃圾收集结构后，进入粒子成形控制结构，在粒子成形控制结构内的超微粉粒子成形区域，通过保温结构或加温结构或冷却结构，通过热传导或热辐射间接控制超微粉粒子成形区域各部分的温度，通过载流气速度与管道截面尺寸控制粒子随着载流气通过内部各区域的速度，为粒子成形提供稳定可控条件，让需制备的物质由气态变为液态，液态变为固态，气态相互碰接凝结为较小液核，较小液核相互碰撞接成为较大液滴或气态与较小液核碰撞结为较大液滴，较大液滴继续相互碰撞长大或固化为固态颗粒，较小液核与固态颗粒结合为较大固态颗粒或成为核壳结构，气态与固态颗粒结合为较大固态颗粒或成为核壳结构，固态颗粒继续冷却，从而制备出期望达到的粒径和形貌的粒子；
S3、步骤S2制备的期望达到的粒径和形貌的粒子在载流气的携带下，直接进入罐式变向分料结构，对粒子中的不良品粒子与良品粒子分离，其中良品粒子在载流气的携带下向下一工序移动，不良品粒子向垃圾回流结构或垃圾收集结构汇聚；
S4、良品粒子在载流气的携带下进入收集结构内，成形的超微粉粒子与载流气分离，其中超微粉粒子被收集为产品，载流气被排出或循环使用。
可选的，步骤S2制备的期望达到的粒径和形貌的粒子在载流气的携带下，进入喷气冷却结构内部，通过多孔内层板由周边向内部通道内均匀喷入冷却气体，与进入的高温气体及已经成形的粒子混合和冷却后，进入罐式变向分料结构。
本发明的有益效果是：
本专利通过特定的结构对超微粉粒子成形过程中的各个阶段进行精准控制，包括温度场控制，速度场控制，各结构之间连接的控制，使用其内部流通 的蒸气均匀地经过各受控部位，为超微粉粒子成形提供稳定可控条件，成形的粒子粒径均匀、形貌稳定，分散良好。
附图说明
图1为本发明超微粉粒子聚集冷却罐式结构的结构示意图。
附图标记说明
1、出气与回流结构，2、垃圾回流结构或垃圾收集结构，3、粒子成形控制结构，4、喷气冷却结构，41、喷气冷却结构处喷气，5、罐式变向分料结构，51、冷却流体进口，6、高温蒸发器内的内腔，7、收集器。
具体实施方式
以下通过实施例对本发明的技术方案进行详细的说明，以下的实施例仅是示例性的，仅能用来解释和说明本发明的技术方案，而不能解释为是对本发明技术方案的限制。
在本发明的描述中，需要说明的是，术语“中心”、“上”、“下”、“左”、“右”、“前”、“后”、“竖直”、“水平”、“内”、“外”等指示方位或位置关系为基于附图所示的方位或位置关系，仅是为了便于描述本发明和简化描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为是对本发明的限制，此外，术语“第一”、“第二”、“第三”仅用于描述目的，而不能理解为指示或暗示相对重要性。
在本发明的描述中，需要说明的是，除非另有明确的规定和限定，术语“安装”、“相连”、“连接”应做广义理解，例如，可以是固定连接，也可以是可拆卸连接，或一体地连接；可以是机械连接，也可以是电连接；可以是直接相连，也可以通过中间媒介间接相连，也可以是两个元件内部的连通。对于本领域的普通技术人员而言，可以根据具体情况理解上述术语在本发明中的具体含义。
本结构用于制备超微粉粒，包括但不限于金属超微粉粒。在以下的实施例中，以制备金属超微粉粒为例进行说明，但不是限定本结构仅能用于金属超微粉粒的制备。
在使用蒸发冷凝气相法制备纳米级、亚微米级或微米级微观粒子粉末时， 使用粒子聚集冷却管罐式结构与粒子成形方法，粒子聚集冷却管罐式结构为一通道，通道内设计各接口的连接方式，将各部位连通，通过特定的结构对粒子成形过程中的各个阶段进行精准控制，包括温度场控制，速度场控制，各结构之间连接的控制，使其内部流通的蒸气均匀地经过各受控部位，为粒子成形提供稳定可控的条件，为微观粒子成形营造条件。让需制备的物质由气态变为液态，液态变为固态，气态相互碰接凝结为较小液核，较小液核相互碰接成为较大液滴或气态与较小液核碰撞结为较大液滴，较大液滴继续相互碰撞长大或固化为固态颗粒，较小液核与固态颗粒结合为较大固态颗粒或成为核壳结构，气态与固态颗粒结合为较大固态颗粒或成为核壳结构，固态颗粒继续冷却，从而制备出期望达到的粒径和形貌的粒子。成形的粒子粒径均匀、形貌稳定、分散良好。
如图1所示，本申请提供一种超微粉粒子聚集冷却罐式结构，设置于超微粉粒子制备系统中，在本申请中的超微粉粒子制备系统中，还包括设置于高温蒸发器内用于提供热源的加热系统，向高温蒸发器内提供原料的加料系统，提供冷却的循环冷却系统，提供载流和冷却的气源或循环气系统，提供压力平衡控制的压力平衡系统，以及收集部分的气固分离系统或气固液分离系统。上述这些部分均为现有技术，其连接关系或结构在本申请中没有改进，因此，在本申请中不进行详细的说明，此处通过在先的专利文献均能获得。
本申请还提供一种超微粉粒子聚集冷却罐式结构内部的各功能段，各功能段的截面形状、口径尺寸等可以根据需要设置为相同、相似，或变形、变径等，只要能够实现各个功能段连接均可以根据需要进行设计。同时，各功能段的长度按需选用，并不影响本申请技术方案的实现。各功能段也可以是多段拼接或整体结构中的各个部分，具体根据实际需要(比如场地、生产量等)进行调整，不作为对本申请技术方案的限制或改进。
本申请的重点为设置于高温蒸发器与收集结构之间的聚集冷却管罐式结构，包括依次连接的出气与回流结构1、垃圾回流结构或垃圾收集结构2、粒子成形控制结构3及罐式变向分料结构5。
其中，出气与回流结构1的前端与前置的高温蒸发器的出气口连接，罐式变向分料结构5的后端与后置的收集结构连接。
出气与回流结构1的内部至少包括用于高温蒸气进入的第一通道，在第一通道外侧设置有出气与回流结构1的外壳。在第一通道与出气与回流结构1的外壳之间设置有保温结构，在第一通道外侧设置有加固结构或加热设备。出气与回流结构1的外壳为夹套结构，夹套结构内部通过循环冷却液。第一通道由不与待制备的材料发生物理或/和化学反应的材料制成。通过保温或加温控制出气与回流结构1内部的温度高于所需要制备的超微粉粒子材料的熔点。
垃圾回流结构或垃圾收集结构2，所述垃圾回流结构或垃圾收集结构2的内部至少包括一第二通道。所述第二通道的前端与第一通道连接，后端与粒子成形控制结构3的内腔连接。在保证气体通过的同时，将上方管道或通道内的垃圾融化成液体后回流，或是将上方管道或通道内的垃圾收集进垃圾留置存放桶内，防止阻碍通道内气体的通过。第二通道的外侧设置有保温或加温装置，通过保温或加温装置控制垃圾回流结构内部的温度高于所需制备材料的熔点，或垃圾收集结构的通气通道内的温度高于所需制备材料的熔点，垃圾留置存放桶内的温度低于所需制备材料的熔点。
所述粒子成形控制结构3的内腔前端与第二通道连接，内腔后端与喷气冷却结构4连接或罐式变向分料结构5的进气管连接，其内部设置有超微粉粒子成形区域。超微粉粒子成形区域为一通道结构，是粒子成形控制的主要场所。在所述粒子成形控制结构3的内部设置有保温或加温或冷却结构，通过热传导或热辐射间接控制超微粉粒子成形区域的温度，通过载流气速度与超微粉粒子成形区域的截面尺寸控制粒子随载流气通过超微粉粒子成形区域的速度，为粒子成形提供稳定可控条件。
粒子成形控制结构3包括外层壳体结构、中间保温层及内层热传导层。
所述外层壳体结构为夹套结构，夹套结构内用于流通冷却剂。
所述中间保温层为单层或多层结构。
所述内层热传导层，形成经过保温处理的通道，即超微粉粒子成形区域，用于将通道内流通的物质的温度通过热传导或热辐射方式进行间接控制。
通过粒子成形控制结构3，将需制备的物质由气态变为液态，液态变为固态，气态相互碰接凝结为较小液核，较小液核相互碰接成为较大液滴或气态与较小液核碰撞结为较大液滴，较大液滴继续相互碰撞长大或固化为固态颗粒， 较小液核与固态颗粒结合为较大固态颗粒或成为核壳结构，气态与固态颗粒结合为较大固态颗粒或成为核壳结构，固态颗粒继续冷却，从而制备出期望达到的粒径和形貌的粒子。在本申请中，较小液核仅是指相对概念，并不是指具体的尺寸，同样，较大液滴也是指相对概念，而不是指具体尺寸。因此，上述较大和较小并不是指代不清楚，仅是因为涉及分子的内部变化，用来进行文字表述，后面的较大和较小均应如此的理解。
粒子成形控制结构3与罐式变向分料结构5之间可以加装用于对已成形的粒子进行预冷却的喷气冷却结构4。所述喷气冷却结构4至少包括内部的第三通道，第三通道的前端与超微粉粒子成形区域连通，后端与罐式变向分料结构5连接。在所述第三通道内设置有多孔内层板，以由周边向第三通道内均匀喷入冷却气体，防止成形的粒子因为温度较高而团聚时发生软团聚或硬团聚。
所述罐式变向分料结构5包括变向罐式腔体，在所述变向罐式腔体上连接有进气管道和出气管道，其中进气管道与第三通道或粒子成形控制结构3连接，出气管道与收集结构连接。所述进气管道的轴向中线与出气管道的轴向中线的夹角为30-150°。
本申请还提供一种超微粉粒子成形方法，使用本公开的超微粉粒子聚集冷却管罐式结构，包括以下步骤：
S1、待制备超微粉粒子的材料加入到高温蒸发器内，经过加热蒸发的材料蒸气与载流气混合成混合气后从高温蒸发器的出气口进入出气与回流结构，通过保温或加温控制出气与回流结构的内部温度高于所需要制备材料的熔点。
S2、所述混合气在通过出气与回流结构、垃圾回流结构或垃圾收集结构后，进入粒子成形控制结构，在粒子成形控制结构内的超微粉粒子成形区域，通过保温结构或加温结构或冷却结构，通过热传导或热辐射间接控制超微粉粒子成形区域各部分的温度，通过载流气速度与管道截面尺寸控制粒子随着载流气通过内部各区域的速度，为粒子成形提供稳定可控条件。让需制备的物质由气态变为液态，液态变为固态，气态相互碰接凝结为较小液核，较小液核相互碰撞接成为较大液滴或气态与较小液核碰撞结为较大液滴，较大液滴继续相互碰撞长大或固化为固态颗粒，较小液核与固态颗粒结合为较大固态颗粒或成为核壳结构，气态与固态颗粒结合为较大固态颗粒或成为核壳结构，固态颗粒继续冷 却，从而制备出期望达到的粒径和形貌的粒子。
S3、步骤S2制备的期望达到的粒径和形貌的粒子在载流气的携带下，直接进入罐式变向分料结构，对粒子中的不良品粒子与良品粒子分离，其中良品粒子在载流气的携带下向下一工序移动，不良品粒子向垃圾回流结构或垃圾收集结构汇聚。
S4、良品粒子在载流气的携带下进入收集结构内，成形的超微粉粒子与载流气分离，其中超微粉粒子被收集为产品，载流气被排出或循环使用。
或者，步骤S2制备的期望达到的粒径和形貌的粒子在载流气的携带下，进入喷气冷却结构内部，通过多孔内层板由周边向内部通道内均匀喷入冷却气体，与进入的高温气体及已经成形的粒子混合和冷却后，进入罐式变向分料结构。
所述罐式变向分料结构的变向罐式腔体的容积V与进气接口内截面积S1的关系如下：
V/S1>100；其中，V为容积，单位为立方厘米；S1为内截面积，单位为平方厘米。
所述罐式变向分料结构的变向罐式腔体上设置有一个或一个以上的冷却流体进口，冷却流体为气体或液体，冷却流体通过冷却流体进口进入变向罐式腔体内，对通过变向罐式腔体的载流气及粉末进行混合与冷却。
所聚集冷却成形的粒子被收集成为产品，载流气被排出或循环使用。
通过上所述各结构配合与连接，与前置的高温蒸发器，后置的收集及冷却结构，高温蒸发器内提供热源的加热系统，高温蒸发器前置的提供原料的加料系统，提供冷却的循环冷却系统，提供载流和冷却的气源或循环气系统，提供压力平衡控制的压力平衡系统，以及收集部分的气固分离系统或气固液分离系统共同配合，完成粒子聚集冷却成形连续循环工业化生产过程，制备出粒径均匀，形貌稳定，分散良好的纳米级、亚微米级或微米级的粉末。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变形，本发明的范围由所附权利要求极其等同限定。

Claims (10)

  1. 一种超微粉粒子聚集冷却罐式结构，其特征在于，设置于超微粉粒子制备系统中，包括依次连接的出气与回流结构、垃圾回流结构或垃圾收集结构、粒子成形控制结构及罐式变向分料结构；
    所述出气与回流结构的前端与前置的高温蒸发器连接，罐式变向分料结构的后端与后置的收集结构连接；
    所述超微粉粒子制备系统还包括设置于高温蒸发器内用于提供热源的加热系统，向高温蒸发器内提供原料的加料系统，提供冷却的循环冷却系统，提供载流和冷却的气源或循环气系统，提供压力平衡控制的压力平衡系统，以及收集部分的气固分离系统或气固液分离系统。
  2. 根据权利要求1所述的超微粉粒子聚集冷却罐式结构，其特征在于，所述出气与回流结构的前端与高温蒸发器的出气口连接，所述出气与回流结构的内部至少包括一用于高温蒸气进入的第一通道；第一通道的外侧设置有保温或加温装置。
  3. 根据权利要求1或2所述的超微粉粒子聚集冷却罐式结构，其特征在于，所述垃圾回流结构或垃圾收集结构的内部至少包括一第二通道，所述第二通道的前端与第一通道连接，后端与粒子成形控制结构的内腔连接；第二通道的外侧设置有保温或加温装置。
  4. 根据权利要求1至3中任一项所述的超微粉粒子聚集冷却罐式结构，其特征在于，所述粒子成形控制结构的内腔前端与第二通道连接，内腔后端与喷气冷却结构或罐式变向分料结构的进气管连接，其内部设置有超微粉粒子成形区域，在所述粒子成形控制结构的内部设置有保温或加温或冷却结构，通过热传导或热辐射间接控制超微粉粒子成形区域的温度，通过载流气速度与超微粉粒子成形区域的截面尺寸控制粒子随载流气通过超微粉粒子成形区域的速度。
  5. 根据权利要求1至4中任一项所述的超微粉粒子聚集冷却罐式结构，其特征在于，粒子成形控制结构与罐式变向分料结构之间设置有用于对已成形的粒子进行预冷却的喷气冷却结构，喷气冷却结构至少包括内部的第三通道，第三通道的前端与超微粉粒子成形区域连通，后端与罐式变向分料结构连接， 在所述第三通道外设置有多孔内层板，以由周边向第三通道内均匀喷入冷却气体。
  6. 根据权利要求1至5中任一项所述的超微粉粒子聚集冷却罐式结构，其特征在于，所述罐式变向分料结构包括变向罐式腔体，在所述变向罐式腔体上连接有进气管道和出气管道，其中进气管道与第三通道或粒子成形控制结构连接，出气管道与收集结构连接；
    所述进气管道与出气管道的内部设置有内层保温结构或冷却结构；
    所述进气管道的轴向中线与出气管道的轴向中线的夹角为30-150°。
  7. 根据权利要求1至6中任一项所述的超微粉粒子聚集冷却罐式结构，其特征在于，所述变向罐式腔体的容积V与进气接口内截面积S1的关系如下：
    V/S1>100，其中,V的单位为立方厘米，S1的单位为平方厘米。
  8. 根据权利要求1至7中任一项所述的超微粉粒子聚集冷却罐式结构，其特征在于，在所述变向罐式腔体上设置有一个或一个以上的冷却流体进口，冷却流体为气体或液体，冷却流体通过冷却流体进口进入变向罐式腔体内，对通过变向罐式腔体的载流气及粉末进行混合与冷却。
  9. 一种超微粉粒子聚集冷却罐式结构成形方法，使用上述权利要求1至8中任一项的超微粉粒子聚集冷却罐式结构，其特征在于，包括以下步骤：
    S1、待制备超微粉粒子的材料加入到高温蒸发器内，经过加热蒸发的材料蒸气与载流气混合成混合气后从高温蒸发器的出气口进入出气与回流结构，通过保温或加温控制出气与回流结构的内部温度高于所需要制备材料的熔点；
    S2、所述混合气在通过出气与回流结构、垃圾回流结构或垃圾收集结构后，进入粒子成形控制结构，在粒子成形控制结构内的超微粉粒子成形区域，通过保温结构或加温结构或冷却结构，通过热传导或热辐射间接控制超微粉粒子成形区域各部分的温度，通过载流气速度与管道截面尺寸控制粒子随着载流气通过内部各区域的速度，为粒子成形提供稳定可控条件，让需制备的物质由气态变为液态，液态变为固态，气态相互碰接凝结为较小液核，较小液核相互碰撞接成为较大液滴或气态与较小液核碰撞结为较大液滴，较大液滴继续相互碰撞长大或固化为固态颗粒，较小液核与固态颗粒结合为较大固态颗粒或成为核壳结构，气态与固态颗粒结合为较大固态颗粒或成为核壳结构，固态颗粒继续冷 却，从而制备出期望达到的粒径和形貌的粒子；
    S3、步骤S2制备的期望达到的粒径和形貌的粒子在载流气的携带下，直接进入罐式变向分料结构，对粒子中的不良品粒子与良品粒子分离，其中良品粒子在载流气的携带下向下一工序移动，不良品粒子向垃圾回流结构或垃圾收集结构汇聚；
    S4、良品粒子在载流气的携带下进入收集结构内，成形的超微粉粒子与载流气分离，其中超微粉粒子被收集为产品，载流气被排出或循环使用。
  10. 根据权利要求9所述的超微粉粒子聚集冷却罐式结构成形方法，其特征在于，步骤S2制备的期望达到的粒径和形貌的粒子在载流气的携带下，进入喷气冷却结构内部，通过多孔内层板由周边向内部通道内均匀喷入冷却气体，与进入的高温气体及已经成形的粒子混合和冷却后，进入罐式变向分料结构。
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