CN104649234A - Preparation method of oxide hollow microspheres - Google Patents
Preparation method of oxide hollow microspheres Download PDFInfo
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- CN104649234A CN104649234A CN201310613226.4A CN201310613226A CN104649234A CN 104649234 A CN104649234 A CN 104649234A CN 201310613226 A CN201310613226 A CN 201310613226A CN 104649234 A CN104649234 A CN 104649234A
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- 239000004005 microsphere Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims description 10
- 239000000843 powder Substances 0.000 claims abstract description 67
- 239000002245 particle Substances 0.000 claims abstract description 43
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 19
- 239000001301 oxygen Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- QFXZANXYUCUTQH-UHFFFAOYSA-N ethynol Chemical group OC#C QFXZANXYUCUTQH-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000004088 foaming agent Substances 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 229910052755 nonmetal Inorganic materials 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000000853 adhesive Substances 0.000 claims abstract description 5
- 230000001070 adhesive effect Effects 0.000 claims abstract description 5
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 5
- 239000007921 spray Substances 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 9
- 239000004604 Blowing Agent Substances 0.000 claims description 7
- LNSPFAOULBTYBI-UHFFFAOYSA-N [O].C#C Chemical group [O].C#C LNSPFAOULBTYBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000003822 epoxy resin Substances 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 229920000647 polyepoxide Polymers 0.000 claims description 5
- 210000003934 vacuole Anatomy 0.000 claims description 4
- 239000000839 emulsion Substances 0.000 claims description 2
- 239000006260 foam Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 9
- 150000004706 metal oxides Chemical class 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 230000000717 retained effect Effects 0.000 abstract 1
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000053 physical method Methods 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/32—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process
- C01B13/322—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process of elements or compounds in the solid state
- C01B13/324—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process of elements or compounds in the solid state by solid combustion synthesis
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
- C01G9/03—Processes of production using dry methods, e.g. vapour phase processes
-
- 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
- C01P2004/34—Spheres hollow
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
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Abstract
本发明涉及一种氧化物空心微球的制备方法，本方法是：以球磨细化后的金属粉(或非金属)与发泡剂混合，加入胶粘剂干燥固化后，破碎为细小的团聚颗粒，将团聚颗粒喷射入强氧化性的氧乙炔火焰中，在火焰高温作用下，颗粒中的物质和氧发生强烈的氧化反应生成氧化物熔滴，同时发泡剂分解放出气体，部分气体无法溢出保留在熔滴内部形成空心液泡，经快速冷却固化形成氧化物空心微球。使用本发明方法得到的氧化物空心微球，其工艺具有可控性，并且可以生成各种规格的金属和非金属氧化物成分和空心结构的微球，应用广泛。The invention relates to a method for preparing hollow oxide microspheres. The method is as follows: mixing metal powder (or non-metal) refined by ball milling with a foaming agent, adding an adhesive to dry and solidify, and breaking into fine agglomerated particles. The agglomerated particles are sprayed into a strong oxidizing oxyacetylene flame. Under the high temperature of the flame, the substances in the particles and oxygen undergo a strong oxidation reaction to form oxide droplets. At the same time, the foaming agent decomposes to release gas, and some gas cannot overflow and be retained. Hollow liquid bubbles are formed inside the droplet, and oxide hollow microspheres are formed after rapid cooling and solidification. The process of the oxide hollow microspheres obtained by the method of the invention is controllable, and the microspheres with various specifications of metal and non-metal oxide components and hollow structures can be produced, and are widely used.
Description
技术领域technical field
本发明涉及一种氧化物空心微球的制备方法。The invention relates to a preparation method of oxide hollow microspheres.
背景技术Background technique
空心微球是七十年代发展起来的一种新型材多功能粉体料，具有质轻、流动性好、化学性能稳定、成本低等特点，被誉为空间时代材料。氧化铁空心微粒具有特殊的物理化学性质，已经广泛应用在磁性液体、催化、滤光、磁性吸波材料、磁记录材料、涂料、功能陶瓷等领域。Hollow microspheres are a new type of multifunctional powder material developed in the 1970s. They have the characteristics of light weight, good fluidity, stable chemical properties, and low cost. They are known as space age materials. Iron oxide hollow particles have special physical and chemical properties, and have been widely used in magnetic liquids, catalysis, optical filtering, magnetic absorbing materials, magnetic recording materials, coatings, functional ceramics and other fields.
氧化物微球的制备方法主要有物理方法和化学方法。物理方法制备微球可以采用真空冷凝法、物理粉碎法、机械球磨法等。但是用物理方法制备的样品一般产品纯度低、颗粒分布不均匀，所以在工业生产和试验中很少被采纳。化学方法主要有共沉淀法、溶胶-凝胶法、微乳液法、水解法、水热法等。采用化学方法获得的微粒的粒子一般质量较好，颗粒度较小，但化学方法都存在一定的不足，如产率低、成本高、设备复杂、粉末收集困难等。将氧化物制备成空心微珠还需要昂贵的生产设备，其工艺复杂，成本较高，不宜推广。本发明所涉及的一种铁氧化物空心微球的制备方法，其生产设备简单，成本低，成球率高，有很大的应用和推广前景。The preparation methods of oxide microspheres mainly include physical methods and chemical methods. The microspheres can be prepared by physical methods such as vacuum condensation method, physical pulverization method, mechanical ball milling method, etc. However, samples prepared by physical methods generally have low product purity and uneven particle distribution, so they are rarely adopted in industrial production and testing. Chemical methods mainly include co-precipitation method, sol-gel method, microemulsion method, hydrolysis method, hydrothermal method and so on. The particles obtained by chemical methods generally have better quality and smaller particle size, but chemical methods have certain shortcomings, such as low yield, high cost, complicated equipment, and difficulty in powder collection. The preparation of oxides into hollow microspheres also requires expensive production equipment, the process is complicated, and the cost is high, so it is not suitable for popularization. The preparation method of the iron oxide hollow microspheres involved in the present invention has simple production equipment, low cost and high ball forming rate, and has great application and popularization prospects.
发明内容Contents of the invention
本发明的目的是提供一种氧化物空心微球的制备方法。The purpose of the present invention is to provide a preparation method of oxide hollow microspheres.
其主要内容为以金属(或非金属)粉与发泡剂混合后，加入胶粘剂固化，干燥后破碎为团聚粉体颗粒，然后采用氧-乙炔火焰喷枪，采用纯氧气为送粉气体将团聚粉体颗粒分散喷射入点燃后的氧乙炔火焰中，粉体中的物质在氧乙炔火焰高温的作用下和纯氧发生剧烈氧化反应，放出大量的热形成液态氧化物熔滴，同时发泡剂受热产生的气体将熔滴发泡形成空心球体，之后空心液滴落入去离子水中快速冷却，得到氧化物空心微球。Its main content is to mix metal (or non-metal) powder with foaming agent, add adhesive to solidify, and break into agglomerated powder particles after drying. The bulk particles are dispersed and sprayed into the ignited oxyacetylene flame, and the substance in the powder undergoes a violent oxidation reaction with pure oxygen under the action of the high temperature of the oxyacetylene flame, releasing a large amount of heat to form liquid oxide droplets, while the blowing agent is heated The generated gas foams the droplet to form a hollow sphere, and then the hollow droplet falls into deionized water for rapid cooling to obtain hollow oxide microspheres.
本发明的主要特点Main features of the present invention
1、本发明可用于氧化物空心微球制备。1. The present invention can be used in the preparation of oxide hollow microspheres.
2、本发明设备简单，轻巧，操作方便，应用广泛，成本低。2. The device of the present invention is simple, lightweight, easy to operate, widely used and low in cost.
3、本发明的得到的空心微球成球率高，可达95％以上。3. The obtained hollow microspheres of the present invention have a high ball forming rate, which can reach more than 95%.
4、本发明生成周期短，2-3天就可得到一批成品。4. The production cycle of the present invention is short, and a batch of finished products can be obtained within 2-3 days.
具体实施方式Detailed ways
本发明涉及一种氧化物空心微球的制备方法，具体实施步骤为：The present invention relates to a kind of preparation method of oxide hollow microspheres, and the specific implementation steps are:
(1)制备团聚颗粒粉体：将金属粉(或非金属)与定量发泡剂原料放入球磨机中，球磨12小时以上，使物料颗粒小于10微米；球磨完成后，再将含有胶粘剂(如环氧树脂)的溶液与球磨后的粉料搅拌成乳液状，混合均匀，放入烘箱烘干，温度保持在100-150℃；烘干完成后，将成块的物料取出，粉碎机中粉碎，过325目筛，得到粒径小于45微米的团聚粉颗粒待用。(1) Preparation of agglomerated particle powder: put metal powder (or non-metal) and quantitative foaming agent raw materials into a ball mill, and ball mill for more than 12 hours to make the material particles less than 10 microns; Epoxy resin) solution and ball-milled powder are stirred into an emulsion, mixed evenly, put into an oven for drying, and the temperature is kept at 100-150°C; Pass through a 325 mesh sieve to obtain agglomerated powder particles with a particle size less than 45 microns for use.
(2)将上述步骤制备的团聚粉体颗粒，装入氧-乙炔火焰喷枪的料筒中，采用纯氧气为送粉气体。点燃氧乙炔火焰，调节火焰为中性焰，打开送粉氧气，送粉氧气压力保持在0.6MPa，打开下料桶控制阀，送粉氧气将团聚粉体颗粒射吸入喷枪管路，并分散喷射入点燃后的氧乙炔火焰；粉体中的物质在氧乙炔火焰高温的作用下和纯氧发生剧烈氧化反应，放出大量的热形成液态氧化物熔滴，同时发泡剂受热产生的气体将熔滴发泡形成空心液泡，之后熔融空心液泡落入去离子水中快速冷却，经高速离心机分离后，脱水干燥，获得氧化物空心微球。(2) Put the agglomerated powder particles prepared in the above steps into the barrel of the oxygen-acetylene flame spray gun, and use pure oxygen as the powder feeding gas. Ignite the oxyacetylene flame, adjust the flame to a neutral flame, turn on the powder feeding oxygen, keep the pressure of the powder feeding oxygen at 0.6MPa, open the control valve of the feeding barrel, feed the powder oxygen to inject the agglomerated powder particles into the spray gun pipeline, and disperse the spray into the ignited oxyacetylene flame; the substance in the powder undergoes a violent oxidation reaction with pure oxygen under the high temperature of the oxyacetylene flame, releasing a large amount of heat to form liquid oxide droplets, and at the same time, the gas generated by the blowing agent will melt Droplet foaming forms hollow vacuoles, and then the molten hollow vacuoles are dropped into deionized water for rapid cooling, separated by a high-speed centrifuge, dehydrated and dried to obtain oxide hollow microspheres.
具体实施实例Specific implementation examples
实施例1Example 1
(1)称取200克平均粒径为5微米的Fe粉，聚乙二醇发泡剂20克，混合后放入高能球磨机中，球磨16小时；(1) Take by weighing 200 grams of Fe powder with an average particle diameter of 5 microns, 20 grams of polyethylene glycol blowing agent, put into high-energy ball mill after mixing, and ball mill for 16 hours;
(2)球磨完成后，加入环氧树脂20克和一定量的酒精，充分搅拌均匀；(2) After the ball milling is completed, add 20 grams of epoxy resin and a certain amount of alcohol, and stir well;
(3)将均匀的乳液状混合物倒入干燥皿内，放入鼓风干燥箱内烘干，温度保持在120℃左右；(3) Pour the uniform emulsion-like mixture into a drying dish, put it into a blast drying oven to dry, and keep the temperature at about 120°C;
(4)烘干完成后，将成块的物料取出，在搅拌式粉碎机中粉碎，过350目筛，得到团聚粉颗粒待用；(4) After the drying is completed, the agglomerated material is taken out, pulverized in a stirring pulverizer, and passed through a 350-mesh sieve to obtain agglomerated powder particles for use;
(5)将上述步骤制备的团聚粉体颗粒，装入氧-乙炔火焰喷枪的料筒中，采用纯氧气为送粉气体，送粉氧气压力保持在0.6MPa；(5) The agglomerated powder particles prepared by the above steps are packed into the barrel of the oxygen-acetylene flame spray gun, and pure oxygen is adopted as the powder feeding gas, and the powder feeding oxygen pressure remains at 0.6MPa;
(6)点燃氧乙炔火焰，调节火焰为中性焰，打开送粉氧气，打开下料桶控制阀，送粉氧气将团聚粉体颗粒射吸入喷枪管路，并分散喷射入点燃后的氧乙炔火焰；在火焰下方放置去离子水，反应后的熔融空心液泡落入去离子水中快速冷却，接收反应后的粉粒。(6) Ignite the oxyacetylene flame, adjust the flame to a neutral flame, turn on the powder feeding oxygen, open the control valve of the lower material barrel, feed the powder oxygen to inject the agglomerated powder particles into the spray gun pipeline, and disperse and spray them into the ignited oxyacetylene Flame: Deionized water is placed under the flame, and the molten hollow bubbles after the reaction fall into the deionized water for rapid cooling, and the reacted powder particles are received.
(7)将去离子水中收集的颗粒，经高速离心机分离后，脱水干燥，获得氧化铁空心微球。(7) After the particles collected in deionized water are separated by a high-speed centrifuge, they are dehydrated and dried to obtain iron oxide hollow microspheres.
实施例2Example 2
(1)称取200克平均粒径为5微米的Zn粉，聚乙二醇发泡剂20克，混合后放入高能球磨机中，球磨16小时；(1) Take by weighing 200 grams of Zn powder with an average particle diameter of 5 microns, 20 grams of polyethylene glycol blowing agent, put into a high-energy ball mill after mixing, and ball mill for 16 hours;
(2)球磨完成后，加入环氧树脂20克和一定量的酒精，充分搅拌均匀；(2) After the ball milling is completed, add 20 grams of epoxy resin and a certain amount of alcohol, and stir well;
(3)将均匀的乳液状混合物倒入干燥皿内，放入鼓风干燥箱内烘干，温度保持在120℃左右；(3) Pour the uniform emulsion-like mixture into a drying dish, put it into a blast drying oven to dry, and keep the temperature at about 120°C;
(4)烘干完成后，将成块的物料取出，在搅拌式粉碎机中粉碎，过350目筛，得到团聚粉颗粒待用；(4) After the drying is completed, the agglomerated material is taken out, pulverized in a stirring pulverizer, and passed through a 350-mesh sieve to obtain agglomerated powder particles for use;
(5)将上述步骤制备的团聚粉体颗粒，装入氧-乙炔火焰喷枪的料筒中，采用纯氧气为送粉气体，送粉氧气压力保持在0.6MPa；(5) The agglomerated powder particles prepared by the above steps are packed into the barrel of the oxygen-acetylene flame spray gun, and pure oxygen is adopted as the powder feeding gas, and the powder feeding oxygen pressure remains at 0.6MPa;
(6)点燃氧乙炔火焰，调节火焰为中性焰，打开送粉氧气，打开下料桶控制阀，送粉氧气将团聚粉体颗粒射吸入喷枪管路，并分散喷射入点燃后的氧乙炔火焰；在火焰下方放置去离子水，反应后的熔融空心液泡落入去离子水中快速冷却，接收反应后的粉粒。(6) Ignite the oxyacetylene flame, adjust the flame to a neutral flame, turn on the powder feeding oxygen, open the control valve of the lower material barrel, feed the powder oxygen to inject the agglomerated powder particles into the spray gun pipeline, and disperse and spray them into the ignited oxyacetylene Flame: Deionized water is placed under the flame, and the molten hollow bubbles after the reaction fall into the deionized water for rapid cooling, and the reacted powder particles are received.
(7)将去离子水中收集的颗粒，经高速离心机分离后，脱水干燥，获得氧化锌空心微球。(7) After the particles collected in deionized water are separated by a high-speed centrifuge, they are dehydrated and dried to obtain zinc oxide hollow microspheres.
实施例3Example 3
(1)称取200克平均粒径为5微米的Si粉，聚乙二醇发泡剂20克，混合后放入高能球磨机中，球磨16小时；(1) Take by weighing 200 grams of Si powder with an average particle diameter of 5 microns, 20 grams of polyethylene glycol foaming agent, put into high-energy ball mill after mixing, and ball mill for 16 hours;
(2)球磨完成后，加入环氧树脂20克和一定量的酒精，充分搅拌均匀；(2) After the ball milling is completed, add 20 grams of epoxy resin and a certain amount of alcohol, and stir well;
(3)将均匀的乳液状混合物倒入干燥皿内，放入鼓风干燥箱内烘干，温度保持在120℃左右；(3) Pour the uniform emulsion-like mixture into a drying dish, put it into a blast drying oven to dry, and keep the temperature at about 120°C;
(4)烘干完成后，将成块的物料取出，在搅拌式粉碎机中粉碎，过350目筛，得到团聚粉颗粒待用；(4) After the drying is completed, the agglomerated material is taken out, pulverized in a stirring pulverizer, and passed through a 350-mesh sieve to obtain agglomerated powder particles for use;
(5)将上述步骤制备的团聚粉体颗粒，装入氧-乙炔火焰喷枪的料筒中，采用纯氧气为送粉气体，送粉氧气压力保持在0.6MPa；(5) The agglomerated powder particles prepared by the above steps are packed into the barrel of the oxygen-acetylene flame spray gun, and pure oxygen is adopted as the powder feeding gas, and the powder feeding oxygen pressure remains at 0.6MPa;
(6)点燃氧乙炔火焰，调节火焰为中性焰，打开送粉氧气，打开下料桶控制阀，送粉氧气将团聚粉体颗粒射吸入喷枪管路，并分散喷射入点燃后的氧乙炔火焰；在火焰下方放置去离子水，反应后的熔融空心液泡落入去离子水中快速冷却，接收反应后的粉粒。(6) Ignite the oxyacetylene flame, adjust the flame to a neutral flame, turn on the powder feeding oxygen, open the control valve of the lower material barrel, feed the powder oxygen to inject the agglomerated powder particles into the spray gun pipeline, and disperse and spray them into the ignited oxyacetylene Flame: Deionized water is placed under the flame, and the molten hollow bubbles after the reaction fall into the deionized water for rapid cooling, and the reacted powder particles are received.
(7)将去离子水中收集的颗粒，经高速离心机分离后，脱水干燥，获得氧化硅空心微球。(7) The particles collected in deionized water are separated by a high-speed centrifuge, and dehydrated to obtain hollow silicon oxide microspheres.
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