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WO2024187960A1 - Method for preparing spherical aluminum oxide by using magnetic rotating arc plasma - Google Patents

Method for preparing spherical aluminum oxide by using magnetic rotating arc plasma Download PDF

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Publication number
WO2024187960A1
WO2024187960A1 PCT/CN2024/073271 CN2024073271W WO2024187960A1 WO 2024187960 A1 WO2024187960 A1 WO 2024187960A1 CN 2024073271 W CN2024073271 W CN 2024073271W WO 2024187960 A1 WO2024187960 A1 WO 2024187960A1
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WIPO (PCT)
Prior art keywords
plasma
aluminum oxide
raw material
alumina
carrier gas
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PCT/CN2024/073271
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French (fr)
Chinese (zh)
Inventor
王佳丽
万玲
张铭
李如龙
杨启炜
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衢州晶洲科技发展有限公司
浙江大学衢州研究院
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Publication of WO2024187960A1 publication Critical patent/WO2024187960A1/en

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/021—After-treatment of oxides or hydroxides
    • C01F7/025—Granulation or agglomeration
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/021—After-treatment of oxides or hydroxides
    • C01F7/027—Treatment involving fusion or vaporisation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres

Definitions

  • the present application relates to the technical field of metal oxides, and in particular to a method for preparing spherical aluminum oxide by using magnetic rotating arc plasma.
  • Alumina is a high-hardness inorganic compound, which is widely used in ceramics, high-hardness materials, coating materials, refractory materials, electronic industry, etc. Among them, spherical alumina has regular morphology, good fluidity, small specific surface area and large bulk density, and is a good thermal interface material.
  • the existing preparation methods of spherical alumina mainly include homogeneous precipitation method, sol-emulsion-gel method, drop ball method, template method, aerosol decomposition method, spray method and flame method, etc.
  • the above preparation methods all have certain problems, such as difficulty in controlling the product particle size, serious product agglomeration phenomenon, high equipment requirements and great technical difficulty, etc.
  • Thermal plasma technology has the advantages of high temperature, high energy, controllable atmosphere, and rapid reaction, and can meet the requirements of spheroidization treatment.
  • Chinese patent CN107176617A discloses a method for preparing submicron spherical alumina powder by thermal plasma, comprising the following steps: (1) uniformly mixing aluminum powder and alumina powder in proportion; (2) using oxygen-containing gas as carrier gas to transport the mixed powder composed of aluminum powder and alumina powder into a thermal plasma reactor; (3) in the plasma reactor, aluminum powder undergoes a gasification-oxidation-deposition process in sequence, and alumina powder undergoes a gasification-deposition process in sequence; (4) the product with aluminum powder as raw material is first deposited to generate nano alumina particles, and the product with aluminum powder as raw material is subsequently deposited on the nano alumina particles; (5) the generated submicron alumina powder enters the plasma product collection system with the air flow to obtain submicron alumina powder.
  • the spheroidization rate of s
  • the purpose of the present application is to provide a method for preparing spherical alumina using magnetic rotating arc plasma.
  • the spherical alumina prepared by the method provided in the present application has a high spheroidization rate.
  • the present application provides a method for preparing spherical aluminum oxide using magnetic rotating arc plasma, comprising the following steps:
  • a plasma generator is used to provide thermal plasma; the operating power of the plasma arc in the plasma generator is 10 to 10000 kW;
  • the aluminum oxide raw material is transported to the region of the thermal plasma by using a carrier gas, and the surface of the aluminum oxide raw material is melted under the action of the thermal plasma to obtain aluminum oxide particles with melted surface;
  • the flow rate of the carrier gas is 1-5000 Nm 3 /h;
  • the aluminum oxide particles with the surface melted are cooled to obtain spherical aluminum oxide.
  • the plasma generating device comprises a magnetic rotating arc plasma torch.
  • the thermal plasma includes at least one of arc plasma, radio frequency plasma and combustion plasma.
  • the atmosphere gas of the thermal plasma is nitrogen.
  • the carrier gas includes one or more of nitrogen, argon and hydrogen.
  • the feed rate of the alumina raw material is 0.5-1500 kg/h.
  • the cooling is quench gas cooling.
  • the cooling rate of the quenching gas cooling is ⁇ 2000K/s.
  • the present application provides a method for preparing spherical alumina using magnetic rotating arc plasma, comprising the following steps: using a plasma generator to provide thermal plasma; the operating power of the plasma arc in the plasma generator is 10 to 10,000 kW; using a carrier gas to transport alumina raw materials to the region of the thermal plasma, the alumina raw materials undergo surface melting under the action of the thermal plasma to obtain surface-molten alumina particles; the flow rate of the carrier gas is 1 to 5,000 Nm 3 /h; the surface-molten alumina particles are cooled to obtain spherical alumina.
  • the present application controls the speed of the alumina raw materials through the high-temperature zone in the plasma region by controlling the flow rate of the carrier gas of the alumina raw materials and the operating power of the plasma arc, so that the alumina raw materials are fully melted and spheroidized, the spheroidization rate of the alumina is improved, and the particle size uniformity is good.
  • the method provided by the present application does not require a subsequent deposition growth step, the spherical alumina does not agglomerate, the particles have high dispersion, the process is simple, the operation is simple, and the production is efficient. The production cost is low, the production efficiency is high, and it is suitable for industrial production.
  • the smaller the feed amount of alumina raw material the smaller the possibility of unspheroidized raw material appearing in the alumina product.
  • too small alumina feed amount will lead to too low production efficiency of spherical alumina.
  • the present application achieves low-cost and high-efficiency preparation of spherical alumina by controlling the feed amount of alumina raw material, which has good economic benefits.
  • FIG1 is a SEM image of spherical alumina at different operating powers of plasma arc, wherein A is Example 1, B is Example 2, C is Example 3, D is Example 4, and E is Comparative Example 1;
  • FIG2 is a SEM image of spherical alumina under different cathode gas and carrier gas flow conditions, wherein A is Example 5, B is Example 6, and C is Example 7.
  • the present application provides a method for preparing spherical aluminum oxide using magnetic rotating arc plasma, comprising the following steps:
  • a plasma generator is used to provide thermal plasma; the operating power of the plasma arc in the plasma generator is 10 to 10000 kW;
  • the aluminum oxide raw material is transported to the region of the thermal plasma by using a carrier gas, and the surface of the aluminum oxide raw material is melted under the action of the thermal plasma; the flow rate of the carrier gas is 1-5000 Nm 3 /h;
  • the present application uses a plasma generator to provide thermal plasma.
  • the operating power of the plasma arc in the plasma generator is 10 to 10000 kW, preferably 25 to 200 kW; under low power conditions, it is difficult for the temperature to fully liquefy the surface of the raw aluminum oxide, resulting in a low spheroidization rate of spherical aluminum oxide; as the power increases, the spheroidization rate of spherical aluminum oxide gradually increases.
  • the plasma generator preferably includes a magnetic rotating arc plasma torch.
  • the thermal plasma preferably includes at least one of arc plasma, radio frequency plasma and combustion plasma, more preferably rotating arc plasma;
  • the atmosphere gas of the thermal plasma is preferably nitrogen;
  • the flow rate of the atmosphere gas is preferably 1 to 600 Nm 3 /h, more preferably 1 to 50 Nm 3 /h, and further preferably 1 to 20 Nm 3 /h.
  • the present application uses a carrier gas to transport the aluminum oxide raw material to the thermal plasma region, where the aluminum oxide raw material undergoes surface melting under the action of the thermal plasma to obtain aluminum oxide particles with melted surfaces; the flow rate of the carrier gas is 1-5000 Nm 3 /h.
  • the feed rate of the alumina raw material is preferably 0.5 to 1500 kg/h, more preferably 0.6 to 200 kg/h, and further preferably 0.7 to 100 kg/h.
  • the carrier gas preferably includes one or more of nitrogen, argon and hydrogen, more preferably includes nitrogen or a nitrogen-hydrogen mixed gas; the flow rate of the carrier gas is 1-5000Nm 3 /h, preferably 2-1000Nm 3 /h, and more preferably 2-30Nm 3 /h.
  • the alumina raw material is preferably a type with a concentrated particle size distribution; in the present application, the operating power of the plasma arc and the gas (cathode gas and carrier gas) flow rate affect the speed at which the alumina raw material enters the high temperature zone of the plasma, thereby affecting the time for the alumina raw material to pass through the high temperature zone of the plasma, thereby affecting the spheroidization effect.
  • the present application cools the surface-molten aluminum oxide particles to obtain spherical aluminum oxide.
  • the cooling method is preferably quenching gas cooling; the cooling rate of the quenching gas cooling is preferably ⁇ 2000K/s, more preferably ⁇ 2500K/s, and further preferably 2500-20000K/s.
  • the present application preferably further comprises collecting the spherical alumina.
  • the collection is preferably to transport the spherical alumina to a product collection device using the carrier gas.
  • the present application has no special limitation on the product collection device, and an alumina collection device well known to those skilled in the art can be used.
  • the present application does not specifically limit the preparation device of the spherical alumina, and the spherical alumina can be prepared using a magnetic rotating arc plasma device well known to those skilled in the art.
  • the alumina raw material (Al 2 O 3 ) used in the following examples was purchased from Shanghai Yide Chemical Co., Ltd.
  • a magnetic rotating arc plasma torch (the operating power of the plasma arc is 13 kW) is used to generate thermal plasma, wherein the thermal plasma is generated by nitrogen gas with a flow rate of 1 Nm 3 /h;
  • Alumina raw materials feeding amount of 0.72 kg/h
  • carrier gas nitrogen flow rate of 2.5 Nm 3 /h
  • the alumina raw materials are melted under the action of the thermal plasma to obtain alumina particles with melted surfaces
  • the surface-molten aluminum oxide particles are cooled and solidified under a condition of 2500 K/s and then collected to obtain spherical aluminum oxide.
  • Spherical alumina was prepared according to the method of Example 1, the only difference from Example 1 being that the operating power of the plasma arc was 16 kW.
  • Spherical alumina was prepared according to the method of Example 1, the only difference from Example 1 being that the operating power of the plasma arc was 19 kW.
  • Spherical alumina was prepared according to the method of Example 1, the only difference from Example 1 being that the operating power of the plasma arc was 22 kW.
  • Spherical alumina was prepared according to the method of Example 1, the only difference from Example 1 being that the operating power of the plasma arc was 26 kW.
  • Figure 1 is a SEM image of spherical alumina (Examples 1 to 5) at different operating powers of plasma arcs, wherein A is Example 1, B is Example 2, C is Example 3, D is Example 4, and E is Example 5.
  • the spheroidization rate also gradually increases, and the spheroidization rate of spherical alumina increases from 65% to 72%, but fine powder (gasification product) attached to the surface of the alumina ball appears.
  • the power reaches 20kW
  • the spheroidization rate is increased to 85%, the sphericity is good, and no obvious agglomeration occurs.
  • Some nano-scale fine powder still adheres to the surface of the alumina ball.
  • the power is further increased, many melt balls will appear in the product.
  • SEM characterization found a large amount of fine powder, as well as some raw materials, and the proportion of spherical particles dropped to less than 40%.
  • Spherical aluminum oxide was prepared according to the method of Example 1, the only difference from Example 1 being that the plasma
  • the operating power of the arc was 20 kW
  • the nitrogen flow rate for generating the thermal plasma was 1.5 Nm 3 /h
  • the carrier gas flow rate was 2 Nm 3 /h.
  • Spherical aluminum oxide was prepared according to the method of Example 1, the only difference from Example 1 being that the operating power of the plasma arc was 20 kW and the carrier gas flow rate was 2 Nm 3 /h.
  • Spherical alumina was prepared according to the method of Example 1, the only difference from Example 1 being that the operating power of the plasma arc was 20 kW.
  • Figure 2 is a SEM image of spherical alumina under different cathode gas and carrier gas flow conditions, where A is Example 5, B is Example 6, and C is Example 7. As shown in Figure 2, the gas volume also has a significant effect on the spheroidization rate. Excessive gas flow causes the raw material to pass through the high temperature area of the plasma arc too fast, affecting the spheroidization effect and reducing the spheroidization rate.
  • a magnetic rotating arc plasma torch (power of 200 kW) was used to generate thermal plasma, wherein the thermal plasma was generated by nitrogen gas with a nitrogen gas flow rate of 20 Nm 3 /h;
  • Alumina raw materials feeding amount of 6 kg/h
  • carrier gas flow rate of 30 Nm 3 /h
  • the alumina raw materials are melted under the action of the thermal plasma to obtain alumina particles with melted surfaces
  • the surface-molten aluminum oxide particles are cooled and solidified at a temperature gradient of 2500 K/s and then collected to obtain spherical aluminum oxide.
  • a magnetic rotating arc plasma torch (power of 7000 kW) was used to generate thermal plasma, wherein the thermal plasma was generated by nitrogen gas with a nitrogen gas flow rate of 600 Nm 3 /h;
  • Alumina raw materials feeding amount of 80 kg/h
  • carrier gas flow rate of 500 Nm 3 /h
  • the alumina raw materials are melted under the action of the thermal plasma to obtain alumina particles with melted surfaces
  • the surface-molten aluminum oxide particles are cooled and solidified at a temperature gradient of 4000 K/s and then collected to obtain spherical aluminum oxide.

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Abstract

The present invention relates to the technical field of metal oxides, and provides a method for preparing spherical aluminum oxide by using magnetic rotating arc plasma. The method for preparing spherical aluminum oxide by using magnetic rotating arc plasma comprises the following steps: providing thermal plasma by using a plasma generating device, conveying an aluminum oxide raw material to a region of the thermal plasma by using a carrier gas, subjecting same to surface melting under the action of the thermal plasma, and then cooling same, so as to obtain spherical aluminum oxide. By controlling the flow of the carrier gas for the aluminum oxide raw material and the operating power of a plasma arc, the speed of the aluminum oxide raw material passing through a plasma high-temperature region is controlled, such that the aluminum oxide raw material is fully molten and spheroidized, the spheroidization rate of the aluminum oxide is improved, and the particle size uniformity is good. Moreover, the method does not require a subsequent deposition growth step, spherical aluminum oxide does not agglomerate, and the dispersity of particles is high.

Description

一种利用磁旋转弧等离子体制备球形氧化铝的方法A method for preparing spherical aluminum oxide using magnetic rotating arc plasma
本申请要求于2023年3月13日提交中国专利局、申请号为CN202310268826.5、发明名称为“一种利用磁旋转弧等离子体制备球形氧化铝的方法”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。This application claims the priority of the Chinese patent application filed with the China Patent Office on March 13, 2023, with application number CN202310268826.5 and invention name “A method for preparing spherical alumina using magnetic rotating arc plasma”, the entire contents of which are incorporated by reference in this application.
技术领域Technical Field
本申请涉及金属氧化物技术领域，具体涉及一种利用磁旋转弧等离子体制备球形氧化铝的方法。The present application relates to the technical field of metal oxides, and in particular to a method for preparing spherical aluminum oxide by using magnetic rotating arc plasma.
背景技术Background Art
氧化铝是一种高硬度无机化合物，在陶瓷、高硬材料、涂层材料、耐火材料、电子行业等领域等均有广泛应用。其中，球形氧化铝具有形貌规则、较好的流动性、较小的比表面积以及较大的堆积密度，是一种良好的热界面材料。Alumina is a high-hardness inorganic compound, which is widely used in ceramics, high-hardness materials, coating materials, refractory materials, electronic industry, etc. Among them, spherical alumina has regular morphology, good fluidity, small specific surface area and large bulk density, and is a good thermal interface material.
现有球形氧化铝的制备方法主要包括均相沉淀法、溶胶-乳液-凝胶法、滴球法、模板法、气溶胶分解法、喷射法和火焰法等。然而，上述制备方法都存在一定的问题，例如难以控制产品粒径、产品团聚现象严重、设备要求高和技术难度大等。The existing preparation methods of spherical alumina mainly include homogeneous precipitation method, sol-emulsion-gel method, drop ball method, template method, aerosol decomposition method, spray method and flame method, etc. However, the above preparation methods all have certain problems, such as difficulty in controlling the product particle size, serious product agglomeration phenomenon, high equipment requirements and great technical difficulty, etc.
热等离子体技术具有高温、高能、气氛可控、反应迅速等优点，能满足球化处理的要求。例如，中国专利CN107176617A公开了一种热等离子体制备亚微米级球形氧化铝粉体的方法，包括以下步骤：(1)将铝粉和氧化铝粉按比例均匀混合；(2)用含氧气体作为载气，将铝粉和氧化铝粉组成的混合粉体输送入热等离子体反应器；(3)在等离子体反应器中，铝粉依次经历气化-氧化-沉积过程，氧化铝粉依次经历气化-沉积过程；(4)以氧化铝粉为原料的产物首先沉积生成纳米氧化铝颗粒，以铝粉为原料的产物后续沉积在纳米氧化铝颗粒上；(5)生成的亚微米级氧化铝粉体随气流进入等离子体产物收集系统，获得亚微米级氧化铝粉体。然而，上述制备方法制备得到的球形氧化铝的球化率较低。Thermal plasma technology has the advantages of high temperature, high energy, controllable atmosphere, and rapid reaction, and can meet the requirements of spheroidization treatment. For example, Chinese patent CN107176617A discloses a method for preparing submicron spherical alumina powder by thermal plasma, comprising the following steps: (1) uniformly mixing aluminum powder and alumina powder in proportion; (2) using oxygen-containing gas as carrier gas to transport the mixed powder composed of aluminum powder and alumina powder into a thermal plasma reactor; (3) in the plasma reactor, aluminum powder undergoes a gasification-oxidation-deposition process in sequence, and alumina powder undergoes a gasification-deposition process in sequence; (4) the product with aluminum powder as raw material is first deposited to generate nano alumina particles, and the product with aluminum powder as raw material is subsequently deposited on the nano alumina particles; (5) the generated submicron alumina powder enters the plasma product collection system with the air flow to obtain submicron alumina powder. However, the spheroidization rate of spherical alumina prepared by the above preparation method is low.
发明内容 Summary of the invention
有鉴于此，本申请的目的在于提供一种利用磁旋转弧等离子体制备球形氧化铝的方法，本申请提供的方法制备得到的球形氧化铝的球化率高。In view of this, the purpose of the present application is to provide a method for preparing spherical alumina using magnetic rotating arc plasma. The spherical alumina prepared by the method provided in the present application has a high spheroidization rate.
为了实现上述发明目的，本申请提供以下技术方案：In order to achieve the above-mentioned invention object, this application provides the following technical solutions:
本申请提供了一种利用磁旋转弧等离子体制备球形氧化铝的方法，包括以下步骤：The present application provides a method for preparing spherical aluminum oxide using magnetic rotating arc plasma, comprising the following steps:
利用等离体发生装置提供热等离子体；所述等离体发生装置中等离子电弧的运行功率为10～10000kW；A plasma generator is used to provide thermal plasma; the operating power of the plasma arc in the plasma generator is 10 to 10000 kW;
利用载气将氧化铝原料输送至所述热等离子体的区域，所述氧化铝原料在热等离子体作用下发生表面熔融，得到表面熔融的氧化铝微粒；所述载气的流量为1～5000Nm3/h；The aluminum oxide raw material is transported to the region of the thermal plasma by using a carrier gas, and the surface of the aluminum oxide raw material is melted under the action of the thermal plasma to obtain aluminum oxide particles with melted surface; the flow rate of the carrier gas is 1-5000 Nm 3 /h;
将所述表面熔融的氧化铝微粒进行冷却，得到球形氧化铝。The aluminum oxide particles with the surface melted are cooled to obtain spherical aluminum oxide.
优选地，所述等离体发生装置包括磁旋转弧等离子体炬。Preferably, the plasma generating device comprises a magnetic rotating arc plasma torch.
优选地，所述热等离子体包括电弧等离子体、射频等离子体和燃烧等离子体中的至少一种。Preferably, the thermal plasma includes at least one of arc plasma, radio frequency plasma and combustion plasma.
优选地，所述热等离子体的氛围气体为氮气。Preferably, the atmosphere gas of the thermal plasma is nitrogen.
优选地，所述载气包括氮气、氩气和氢气中的一种或几种。Preferably, the carrier gas includes one or more of nitrogen, argon and hydrogen.
优选地，所述氧化铝原料的进料量为0.5～1500kg/h。Preferably, the feed rate of the alumina raw material is 0.5-1500 kg/h.
优选地，所述冷却为淬冷气冷却。Preferably, the cooling is quench gas cooling.
优选地，所述淬冷气冷却的冷却速率≥2000K/s。Preferably, the cooling rate of the quenching gas cooling is ≥2000K/s.
本申请提供了一种利用磁旋转弧等离子体制备球形氧化铝的方法，包括以下步骤：利用等离体发生装置提供热等离子体；所述等离体发生装置中等离子电弧的运行功率为10～10000kW；利用载气将氧化铝原料输送至所述热等离子体的区域，所述氧化铝原料在热等离子体作用下发生表面熔融，得到表面熔融的氧化铝微粒；所述载气的流量为1～5000Nm3/h；将所述表面熔融的氧化铝微粒进行冷却，得到球形氧化铝。本申请通过控制氧化铝原料的载气的流量以及等离子电弧的运行功率，实现了对氧化铝原料通过等离子体区域中的高温区速度的控制，使得氧化铝原料充分熔融并发生球化，提高了氧化铝的球化率，粒径均一性好。而且，本申请提供的方法无需后续的沉积生长步骤，球形氧化铝不发生团聚，颗粒分散性高，工艺简单，操作简单，生 产成本低，生产效率高，适宜工业化生产。The present application provides a method for preparing spherical alumina using magnetic rotating arc plasma, comprising the following steps: using a plasma generator to provide thermal plasma; the operating power of the plasma arc in the plasma generator is 10 to 10,000 kW; using a carrier gas to transport alumina raw materials to the region of the thermal plasma, the alumina raw materials undergo surface melting under the action of the thermal plasma to obtain surface-molten alumina particles; the flow rate of the carrier gas is 1 to 5,000 Nm 3 /h; the surface-molten alumina particles are cooled to obtain spherical alumina. The present application controls the speed of the alumina raw materials through the high-temperature zone in the plasma region by controlling the flow rate of the carrier gas of the alumina raw materials and the operating power of the plasma arc, so that the alumina raw materials are fully melted and spheroidized, the spheroidization rate of the alumina is improved, and the particle size uniformity is good. Moreover, the method provided by the present application does not require a subsequent deposition growth step, the spherical alumina does not agglomerate, the particles have high dispersion, the process is simple, the operation is simple, and the production is efficient. The production cost is low, the production efficiency is high, and it is suitable for industrial production.
进一步的，氧化铝原料的进料量越小，氧化铝产品内出现未发生球化原料的可能性越小，然而氧化铝进料量太小会导致球形氧化铝的生产效率太低，本申请通过控制氧化铝原料的进料量实现了球形氧化铝的低成本、高效率的制备，具有很好的经济效益。Furthermore, the smaller the feed amount of alumina raw material, the smaller the possibility of unspheroidized raw material appearing in the alumina product. However, too small alumina feed amount will lead to too low production efficiency of spherical alumina. The present application achieves low-cost and high-efficiency preparation of spherical alumina by controlling the feed amount of alumina raw material, which has good economic benefits.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
图1为不同等离子电弧的运行功率下球形氧化铝的SEM图，其中，A为实施例1，B为实施例2，C为实施例3，D为实施例4，E为对比例1；FIG1 is a SEM image of spherical alumina at different operating powers of plasma arc, wherein A is Example 1, B is Example 2, C is Example 3, D is Example 4, and E is Comparative Example 1;
图2为不同阴极气和载气流量条件下的球形氧化铝的SEM图，其中，A为实施例5，B为实施例6，C为实施例7。FIG2 is a SEM image of spherical alumina under different cathode gas and carrier gas flow conditions, wherein A is Example 5, B is Example 6, and C is Example 7.
具体实施方式DETAILED DESCRIPTION
本申请提供了一种利用磁旋转弧等离子体制备球形氧化铝的方法，包括以下步骤：The present application provides a method for preparing spherical aluminum oxide using magnetic rotating arc plasma, comprising the following steps:
利用等离体发生装置提供热等离子体；所述等离体发生装置中等离子电弧的运行功率为10～10000kW；A plasma generator is used to provide thermal plasma; the operating power of the plasma arc in the plasma generator is 10 to 10000 kW;
利用载气将氧化铝原料输送至所述热等离子体的区域，所述氧化铝原料在热等离子体作用下发生表面熔融；所述载气的流量为1～5000Nm3/h；The aluminum oxide raw material is transported to the region of the thermal plasma by using a carrier gas, and the surface of the aluminum oxide raw material is melted under the action of the thermal plasma; the flow rate of the carrier gas is 1-5000 Nm 3 /h;
将所述表面熔融的氧化铝微粒进行冷却，得到球形氧化铝；Cooling the aluminum oxide particles with the surface melted to obtain spherical aluminum oxide;
在本申请中，若无特殊说明，所有的原料组分均为本领域技术人员熟知的市售商品。In the present application, unless otherwise specified, all raw material components are commercially available products well known to those skilled in the art.
本申请利用等离体发生装置提供热等离子体。在本申请中，所述等离体发生装置中等离子电弧的运行功率为10～10000kW，优选为25～200kW；低功率条件下温度难以使原料氧化铝表面充分液化，导致球形氧化铝的球化率较低；随着功率的提高，球形氧化铝的球化率逐步上升。在本申请中，所述等离体发生装置优选包括磁旋转弧等离子体炬。在本申请中，所述热等离子体优选包括电弧等离子体、射频等离子体和燃烧等离子体中的至少一种，更优选为旋转电弧等离子体；所述热等离子体的氛围气体优选为氮气；所述氛围气体的流量优选为1～600Nm3/h，更优选为1～50Nm3/h，进一步优选为1～20Nm3/h。 The present application uses a plasma generator to provide thermal plasma. In the present application, the operating power of the plasma arc in the plasma generator is 10 to 10000 kW, preferably 25 to 200 kW; under low power conditions, it is difficult for the temperature to fully liquefy the surface of the raw aluminum oxide, resulting in a low spheroidization rate of spherical aluminum oxide; as the power increases, the spheroidization rate of spherical aluminum oxide gradually increases. In the present application, the plasma generator preferably includes a magnetic rotating arc plasma torch. In the present application, the thermal plasma preferably includes at least one of arc plasma, radio frequency plasma and combustion plasma, more preferably rotating arc plasma; the atmosphere gas of the thermal plasma is preferably nitrogen; the flow rate of the atmosphere gas is preferably 1 to 600 Nm 3 /h, more preferably 1 to 50 Nm 3 /h, and further preferably 1 to 20 Nm 3 /h.
得到热等离子体后，本申请利用载气将氧化铝原料输送至所述热等离子体的区域，所述氧化铝原料在热等离子体作用下发生表面熔融，得到表面熔融的氧化铝微粒；所述载气的流量为1～5000Nm3/h。After obtaining the thermal plasma, the present application uses a carrier gas to transport the aluminum oxide raw material to the thermal plasma region, where the aluminum oxide raw material undergoes surface melting under the action of the thermal plasma to obtain aluminum oxide particles with melted surfaces; the flow rate of the carrier gas is 1-5000 Nm 3 /h.
在本申请中，所述氧化铝原料的进料量优选为0.5～1500kg/h，更优选为0.6～200kg/h，进一步优选为0.7～100kg/h。In the present application, the feed rate of the alumina raw material is preferably 0.5 to 1500 kg/h, more preferably 0.6 to 200 kg/h, and further preferably 0.7 to 100 kg/h.
在本申请中，所述载气优选包括氮气、氩气和氢气中的一种或几种，更优选包括氮气或氮气-氢气混合气体；所述载气的流量为1～5000Nm3/h，优选为2～1000Nm3/h，进一步优选为2～30Nm3/h。In the present application, the carrier gas preferably includes one or more of nitrogen, argon and hydrogen, more preferably includes nitrogen or a nitrogen-hydrogen mixed gas; the flow rate of the carrier gas is 1-5000Nm 3 /h, preferably 2-1000Nm 3 /h, and more preferably 2-30Nm 3 /h.
在本申请中，所述氧化铝原料优选为粒径分布集中的种类；在本申请中，所述等离子电弧的运行功率和气体(阴极气和载气)流量对氧化铝原料进入等离子体高温区的速度有影响，进而影响氧化铝原料通过等离子体高温区的时间，从而影响球化效果。In the present application, the alumina raw material is preferably a type with a concentrated particle size distribution; in the present application, the operating power of the plasma arc and the gas (cathode gas and carrier gas) flow rate affect the speed at which the alumina raw material enters the high temperature zone of the plasma, thereby affecting the time for the alumina raw material to pass through the high temperature zone of the plasma, thereby affecting the spheroidization effect.
得到表面熔融的氧化铝微粒后，本申请将所述表面熔融的氧化铝微粒进行冷却，得到球形氧化铝。在本申请中，所述冷却的方式优选为淬冷气冷却；所述淬冷气冷却的冷却速率优选≥2000K/s，更优选为≥2500K/s，进一步优选为2500～20000K/s。After obtaining the surface-molten aluminum oxide particles, the present application cools the surface-molten aluminum oxide particles to obtain spherical aluminum oxide. In the present application, the cooling method is preferably quenching gas cooling; the cooling rate of the quenching gas cooling is preferably ≥2000K/s, more preferably ≥2500K/s, and further preferably 2500-20000K/s.
所述冷却后，本申请优选还包括收集所述球形氧化铝。在本申请中，所述收集优选为利用所述载气将球形氧化铝输送至产物收集装置中，本申请对于所述产物收集装置没有特殊限定，采用本领域技术人员熟知的氧化铝收集装置即可。After the cooling, the present application preferably further comprises collecting the spherical alumina. In the present application, the collection is preferably to transport the spherical alumina to a product collection device using the carrier gas. The present application has no special limitation on the product collection device, and an alumina collection device well known to those skilled in the art can be used.
本申请对于所述球形氧化铝的制备装置没有特殊限定，采用本领域技术人员熟知的磁旋转弧等离子体装置制备即可。The present application does not specifically limit the preparation device of the spherical alumina, and the spherical alumina can be prepared using a magnetic rotating arc plasma device well known to those skilled in the art.
下面将结合本申请中的实施例，对本申请中的技术方案进行清楚、完整地描述。显然，所描述的实施例仅仅是本申请一部分实施例，而不是全部的实施例。基于本申请中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本申请保护的范围。The technical solutions in this application will be described clearly and completely below in conjunction with the embodiments in this application. Obviously, the described embodiments are only part of the embodiments of this application, not all of them. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.
以下实施例中使用的氧化铝原料(Al2O3)购买于上海易德化工有限公司。The alumina raw material (Al 2 O 3 ) used in the following examples was purchased from Shanghai Yide Chemical Co., Ltd.
实施例1 Example 1
利用磁旋转弧等离子体炬(等离子电弧的运行功率为13kW)产生热等离子体，其中，热等离子体由氮气产生，氮气的流量为1Nm3/h；A magnetic rotating arc plasma torch (the operating power of the plasma arc is 13 kW) is used to generate thermal plasma, wherein the thermal plasma is generated by nitrogen gas with a flow rate of 1 Nm 3 /h;
利用载气(氮气流量为2.5Nm3/h)输送氧化铝原料(进料量为0.72kg/h)，氧化铝原料在所述热等离子体作用下进行熔融，得到表面熔融的氧化铝微粒；Alumina raw materials (feeding amount of 0.72 kg/h) are transported by carrier gas (nitrogen flow rate of 2.5 Nm 3 /h), and the alumina raw materials are melted under the action of the thermal plasma to obtain alumina particles with melted surfaces;
所述表面熔融的氧化铝微粒在2500K/s条件冷却固化后收集，得到球形氧化铝。The surface-molten aluminum oxide particles are cooled and solidified under a condition of 2500 K/s and then collected to obtain spherical aluminum oxide.
实施例2Example 2
按照实施例1的方法制备球形氧化铝，与实施例1的区别仅在于等离子电弧的运行功率为16kW。Spherical alumina was prepared according to the method of Example 1, the only difference from Example 1 being that the operating power of the plasma arc was 16 kW.
实施例3Example 3
按照实施例1的方法制备球形氧化铝，与实施例1的区别仅在于等离子电弧的运行功率为19kW。Spherical alumina was prepared according to the method of Example 1, the only difference from Example 1 being that the operating power of the plasma arc was 19 kW.
实施例4Example 4
按照实施例1的方法制备球形氧化铝，与实施例1的区别仅在于等离子电弧的运行功率为22kW。Spherical alumina was prepared according to the method of Example 1, the only difference from Example 1 being that the operating power of the plasma arc was 22 kW.
对比例1Comparative Example 1
按照实施例1的方法制备球形氧化铝，与实施例1的区别仅在于等离子电弧的运行功率为26kW。Spherical alumina was prepared according to the method of Example 1, the only difference from Example 1 being that the operating power of the plasma arc was 26 kW.
图1为不同等离子电弧的运行功率下球形氧化铝(实施例1～5)的SEM图，其中，A为实施例1，B为实施例2，C为实施例3，D为实施例4，E为实施例5。由图1可知，随着功率的增加，球化率也逐渐增大，球形氧化铝的球化率为从65％上升到72％，但均出现附着在氧化铝球表面的细粉(气化产物)。在功率达到20kW时，球化率提升到85％，球形度较好，且未出现明显团聚，仍有部分纳米级细粉附着在氧化铝球表面，当功率进一步增加，产品中会出现很多融球，SEM表征发现大量细粉，也有部分原料，球形颗粒占比降至40％以下。Figure 1 is a SEM image of spherical alumina (Examples 1 to 5) at different operating powers of plasma arcs, wherein A is Example 1, B is Example 2, C is Example 3, D is Example 4, and E is Example 5. As shown in Figure 1, with the increase of power, the spheroidization rate also gradually increases, and the spheroidization rate of spherical alumina increases from 65% to 72%, but fine powder (gasification product) attached to the surface of the alumina ball appears. When the power reaches 20kW, the spheroidization rate is increased to 85%, the sphericity is good, and no obvious agglomeration occurs. Some nano-scale fine powder still adheres to the surface of the alumina ball. When the power is further increased, many melt balls will appear in the product. SEM characterization found a large amount of fine powder, as well as some raw materials, and the proportion of spherical particles dropped to less than 40%.
实施例5Example 5
按照实施例1的方法制备球形氧化铝，与实施例1的区别仅在于等离子 电弧的运行功率为20kW，产生热等离子体的氮气流量为1.5Nm3/h，载气流量为2Nm3/h。Spherical aluminum oxide was prepared according to the method of Example 1, the only difference from Example 1 being that the plasma The operating power of the arc was 20 kW, the nitrogen flow rate for generating the thermal plasma was 1.5 Nm 3 /h, and the carrier gas flow rate was 2 Nm 3 /h.
实施例6Example 6
按照实施例1的方法制备球形氧化铝，与实施例1的区别仅在于等离子电弧的运行功率为20kW，载气流量为2Nm3/h。Spherical aluminum oxide was prepared according to the method of Example 1, the only difference from Example 1 being that the operating power of the plasma arc was 20 kW and the carrier gas flow rate was 2 Nm 3 /h.
实施例7Example 7
按照实施例1的方法制备球形氧化铝，与实施例1的区别仅在于等离子电弧的运行功率为20kW。Spherical alumina was prepared according to the method of Example 1, the only difference from Example 1 being that the operating power of the plasma arc was 20 kW.
图2为不同阴极气和载气流量条件下的球形氧化铝的SEM图，其中，A为实施例5，B为实施例6，C为实施例7。由图2可知，气量对球化率也有明显影响，气体流量过大导致原料通过等离子电弧高温区域的速度过快，影响球化效果，降低球化率。Figure 2 is a SEM image of spherical alumina under different cathode gas and carrier gas flow conditions, where A is Example 5, B is Example 6, and C is Example 7. As shown in Figure 2, the gas volume also has a significant effect on the spheroidization rate. Excessive gas flow causes the raw material to pass through the high temperature area of the plasma arc too fast, affecting the spheroidization effect and reducing the spheroidization rate.
实施例8Example 8
利用磁旋转弧等离子体炬(功率为200kW)产生热等离子体，其中，热等离子体由氮气产生，氮气流量为20Nm3/h；A magnetic rotating arc plasma torch (power of 200 kW) was used to generate thermal plasma, wherein the thermal plasma was generated by nitrogen gas with a nitrogen gas flow rate of 20 Nm 3 /h;
利用载气(流量为30Nm3/h)输送氧化铝原料(进料量为6kg/h)，氧化铝原料在所述热等离子体作用下进行熔融，得到表面熔融的氧化铝微粒；Alumina raw materials (feeding amount of 6 kg/h) are transported by carrier gas (flow rate of 30 Nm 3 /h), and the alumina raw materials are melted under the action of the thermal plasma to obtain alumina particles with melted surfaces;
所述表面熔融的氧化铝微粒在2500K/s温度梯度下冷却固化后收集，得到球形氧化铝。The surface-molten aluminum oxide particles are cooled and solidified at a temperature gradient of 2500 K/s and then collected to obtain spherical aluminum oxide.
实施例9Example 9
利用磁旋转弧等离子体炬(功率为7000kW)产生热等离子体，其中，热等离子体由氮气产生，氮气流量为600Nm3/h；A magnetic rotating arc plasma torch (power of 7000 kW) was used to generate thermal plasma, wherein the thermal plasma was generated by nitrogen gas with a nitrogen gas flow rate of 600 Nm 3 /h;
利用载气(流量为500Nm3/h)输送氧化铝原料(进料量为80kg/h)，氧化铝原料在所述热等离子体作用下进行熔融，得到表面熔融的氧化铝微粒；Alumina raw materials (feeding amount of 80 kg/h) are transported by carrier gas (flow rate of 500 Nm 3 /h), and the alumina raw materials are melted under the action of the thermal plasma to obtain alumina particles with melted surfaces;
所述表面熔融的氧化铝微粒在4000K/s温度梯度下冷却固化后收集，得到球形氧化铝。The surface-molten aluminum oxide particles are cooled and solidified at a temperature gradient of 4000 K/s and then collected to obtain spherical aluminum oxide.
以上所述仅是本申请的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本申请原理的前提下，还可以做出若干改进和润 饰，这些改进和润饰也应视为本申请的保护范围。 The above is only a preferred embodiment of the present application. It should be noted that a person skilled in the art can make several improvements and modifications without departing from the principle of the present application. These improvements and modifications should also be considered as the protection scope of this application.

Claims (14)

  1. 一种利用磁旋转弧等离子体制备球形氧化铝的方法，其特征在于，包括以下步骤：A method for preparing spherical aluminum oxide using magnetic rotating arc plasma, characterized in that it comprises the following steps:
    利用等离体发生装置提供热等离子体；所述等离体发生装置中等离子电弧的运行功率为10～10000kW；A plasma generator is used to provide thermal plasma; the operating power of the plasma arc in the plasma generator is 10 to 10000 kW;
    利用载气将氧化铝原料输送至所述热等离子体的区域，所述氧化铝原料在热等离子体作用下发生表面熔融，得到表面熔融的氧化铝微粒；所述载气的流量为1～5000Nm3/h；The aluminum oxide raw material is transported to the region of the thermal plasma by using a carrier gas, and the surface of the aluminum oxide raw material is melted under the action of the thermal plasma to obtain aluminum oxide particles with melted surface; the flow rate of the carrier gas is 1-5000 Nm 3 /h;
    将所述表面熔融的氧化铝微粒进行冷却，得到球形氧化铝。The aluminum oxide particles with the surface melted are cooled to obtain spherical aluminum oxide.
  2. 根据权利要求1所述的方法，其特征在于，所述等离子电弧的运行功率为25～200kW。The method according to claim 1 is characterized in that the operating power of the plasma arc is 25 to 200 kW.
  3. 根据权利要求1所述的方法，其特征在于，所述等离体发生装置包括磁旋转弧等离子体炬。The method according to claim 1, characterized in that the plasma generating device comprises a magnetic rotating arc plasma torch.
  4. 根据权利要求1所述的方法其特征在于，所述热等离子体包括电弧等离子体、射频等离子体和燃烧等离子体中的至少一种。The method according to claim 1 is characterized in that the thermal plasma includes at least one of arc plasma, radio frequency plasma and combustion plasma.
  5. 根据权利要求1或4所述的方法，其特征在于，所述热等离子体的氛围气体为氮气。The method according to claim 1 or 4 is characterized in that the atmosphere gas of the thermal plasma is nitrogen.
  6. 根据权利要求5所述的方法，其特征在于，所述热等离子体的氛围气体的流量为1～600Nm3/h。The method according to claim 5, characterized in that the flow rate of the atmosphere gas of the thermal plasma is 1-600 Nm 3 /h.
  7. 根据权利要求1所述的方法，其特征在于，所述载气包括氮气、氩气和氢气中的一种或几种。The method according to claim 1 is characterized in that the carrier gas comprises one or more of nitrogen, argon and hydrogen.
  8. 根据权利要求1或7所述的方法，其特征在于，所述载气的流量为为2～1000Nm3/h。The method according to claim 1 or 7, characterized in that the flow rate of the carrier gas is 2-1000 Nm 3 /h.
  9. 根据权利要求1所述的方法，其特征在于，所述氧化铝原料的进料量为0.5～1500kg/h。The method according to claim 1 is characterized in that the feed rate of the alumina raw material is 0.5 to 1500 kg/h.
  10. 根据权利要求1或9所述的方法，其特征在于，所述氧化铝原料的进料量为0.6～200kg/h。The method according to claim 1 or 9 is characterized in that the feed rate of the alumina raw material is 0.6 to 200 kg/h.
  11. 根据权利要求1所述的方法，其特征在于，所述冷却为淬冷气冷却。The method according to claim 1, characterized in that the cooling is quenching gas cooling.
  12. 根据权利要求11所述的方法，其特征在于，所述淬冷气冷却的冷却速率≥2000K/s。 The method according to claim 11, characterized in that the cooling rate of the quenching gas cooling is ≥ 2000K/s.
  13. 根据权利要求11或12所述的方法，其特征在于，所述淬冷气冷却的冷却速率≥2500K/s。The method according to claim 11 or 12, characterized in that the cooling rate of the quenching gas cooling is ≥ 2500K/s.
  14. 根据权利要求11或12所述的方法，其特征在于，所述淬冷气冷却的冷却速率为2500～20000K/s。 The method according to claim 11 or 12 is characterized in that the cooling rate of the quenching gas cooling is 2500-20000K/s.
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