JP2011194344A - Method for separating and refining inorganic-type hollow fine-particle powder raw material, high-purity fine particle powder and separation refining apparatus - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a separation and refining method which separates, and refines, an inorganic-type hollow fine-particle powder raw material into a fine particle powder with high contents of hollow fine particles with defects such as small holes and chips, and damaged fine particles, and a fine particle powder with high contents of undamaged and flawless hollow fine particles of a perfect sphere, to provide a method for efficient separation and refining by simple operation, and to provide those separated and refined fine particle powders.SOLUTION: The method includes a process of heating the inorganic-type hollow fine-particle powder raw material 1 at a temperature of 100°C or higher, a process of separating the heated hollow particle powder raw material 1 quenched in the water 107 at or below a room temperature, into a sedimented component 2 in the water 107 and a floating component 3 on the surface of the water 107, a process of recovering the floating component 3 and the sedimented component 2 respectively after separation, and a process of drying the floating component 3 and the sedimented component 2 respectively after recovery.

Description

  The present invention relates to a separation and purification technique for inorganic hollow fine particle powder raw materials, and relates to a high-purity fine particle powder obtained by the same method as the separation and purification method, and a separation and purification apparatus.

  Inorganic hollow microparticles obtained from volcanic ash, which is a volcanic eruption product, and fly ash, which is a burnt generated from an oil power plant, are lightweight and have excellent heat insulation properties. Widely used in applications such as materials and heat insulating paints (see Patent Document 1 and Patent Document 2).

  In addition, shirasu, which is also a deposit of volcanic ejecta, is heat-treated as a raw material, and is finely powdered and used for cosmetic additives (see Patent Document 3).

JP-A-7-32392 JP 2007-146605 A JP 2007-186468 A

  In addition to being obtained as a natural raw material, the hollow fine particles are obtained by heat-foaming a glass material or the like, hollow-molding, classifying, and artificially manufacturing the glass. However, the hollow fine particle powder raw material obtained in this way contains many fine particles having defects such as small holes and chips and fine particles having thin shell thickness and easily broken, and lowers the original performance of the hollow fine particles. A major issue has been how to separate and purify defective microparticles or microparticles that are easily destroyed and hollow microparticles that are difficult to destroy with perfect spheres.

  As a result of intensive studies on the above-mentioned problems of the prior art, the present inventors have roasted the hollow ceramic fine particle powder raw material that has been destroyed or mixed with impurities, and then put it into cold water for rapid cooling to complete the Of the hollow ceramic fine particles, the fine particles that have a thin shell part and are easily broken are broken by rapid contraction due to rapid cooling and settle as sedimentary components, and only complete hollow ceramic fine particles are floating components Found to be separated as. Thus, it has been found that all the above problems can be solved, and the present invention has been completed.

  The present invention has been made in view of the above-mentioned problems.From an inorganic hollow fine particle powder raw material, a fine particle powder containing high-purity fine particles having defects such as small holes and chips and fine particles whose shell thickness is thin and easily broken; It is an object of the present invention to provide a separation and purification method for separating and purifying perfect spherical fine particles free from defects and destruction into fine powder containing high purity. It is another object of the present invention to provide a method and apparatus for efficiently separating and purifying by a simple operation, and to provide a fine particle powder separated and purified with high purity.

In order to solve the above problems, the method for separating and purifying inorganic hollow fine particle powder raw material according to the present invention comprises:
A heating step for heating the inorganic hollow fine particle powder raw material, a settling component that is rapidly cooled by introducing the heated hollow fine particle powder raw material into a liquid, and a levitating component that floats in the liquid The main features include a separation step of separating the buoyant component and a recovery step of collecting the separated levitation component.

  Among inorganic hollow microparticle raw materials, when hollow microparticles with defects such as small pores and chips are immersed in a liquid, even if there are small pores or chips due to the micro interfacial tension at the boundary between the liquid and air, Since the air discharge from the inside of the hollow fine particles and the inflow of the liquid are prevented, the bulk specific gravity of the hollow fine particles still remains small, so these hollow fine particles are also defective such as small holes and chips. It floats on the surface of the liquid in the same manner as the hollow spheres of perfect spheres without any spheres.

  In contrast, according to the separation and purification method according to the present invention, the heated hollow fine particle powder raw material is put into a liquid and rapidly cooled, thereby causing abrupt air shrinkage due to the rapid cooling inside the hollow fine particles, resulting in small pores and chips. In the case of hollow fine particles such as those, since the liquid is sucked into the inside, the bulk specific gravity becomes large and settles in the liquid as a sedimentary component. Moreover, even in the case of a perfect sphere, in the case of hollow fine particles having a thin shell portion (for example, less than 0.1 μm), the portion is destroyed by rapid air contraction due to rapid cooling, and becomes a sedimenting component. Settling in the liquid.

  On the other hand, in the case of hollow fine particles having a relatively thick (0.75 to 10 μm) shell thickness that is a perfect sphere with no small holes or chips and is not destroyed by rapid cooling, Surface. This separates the sedimentary component containing a lot of defective hollow fine particles and broken fine particles into the floating component containing many perfect spherical hollow fine particles without defects. Sedimentable components include broken pieces after being broken.

  The separation and purification method according to the present invention is characterized in that the hollow fine particle powder raw material is a hollow ceramic fine particle raw material or a hollow glass fine particle raw material.

  The separation and purification method according to the present invention has a third feature that the liquid is water.

  The separation and purification method according to the present invention is characterized in that the heating temperature in the heating step is 100 ° C. or higher, and the temperature of the liquid for rapidly cooling the heated hollow fine particle powder raw material is kept at room temperature or lower. .

  The separation and purification method according to the present invention is characterized by having a drying step of drying the recovered floating component.

  The separation and purification method according to the present invention is characterized in that the separated sedimentation component is recovered.

  The separation and purification method according to the present invention has a seventh feature of drying the recovered sedimentary component.

  The separation and purification method according to the present invention is characterized in that the recovered floating component is returned to the heating step again as a hollow fine particle powder raw material. It is possible to further improve the separation accuracy of defect-free hollow fine particles, and obtain a hollow fine particle powder containing defect-free hollow fine particles with higher purity.

  The separation and purification method according to the present invention further includes a preheating step of mixing the hollow fine particle powder raw material with the liquid and preheating the mixture of the hollow fine particle powder raw material and the liquid while stirring, and preheating after the liquid is evaporated The ninth feature is that the hollow fine particle powder raw material in a state is subjected to a heating step. When it is difficult to uniformly and efficiently heat the powder as it is, it is possible to efficiently heat the hollow fine particle powder raw material.

  The fine particle powder according to the present invention heats an inorganic hollow fine particle powder raw material, puts the heated hollow fine particle powder raw material into a liquid, rapidly cools, and floats with a sedimentation component that settles in the liquid. It is characterized by being obtained by separating into components, collecting the separated floating component, and drying the collected floating component.

  The fine particle powder according to the present invention heats an inorganic hollow fine particle powder raw material, puts the heated hollow fine particle powder raw material into a liquid, rapidly cools, and floats with a sedimentation component that settles in the liquid. It is characterized by being obtained by separating into components, recovering the separated sedimentation component, and drying the collected sedimentation component.

  Precipitating components separated and purified by the above method, that is, hollow fine particles having defects such as small holes and chips, high-precipitation precipitating fine particle powders containing many broken particles, and debris are abrasives with excellent polishing power. Used as In addition, the high-purity levitation fine particle powder containing a large amount of flocculating components, that is, perfect spheres and thick (0.75 to 10 μm) hollow fine particles, has a soft polishing power and is excellent as a material for cosmetics, etc. It is used as a heat insulating material, and as a filler for moldings.

  An apparatus for separating and purifying an inorganic hollow fine particle powder raw material according to the present invention comprises a heating means for heating an inorganic hollow fine particle powder raw material, and the heated hollow fine particle powder raw material is put into a liquid and rapidly cooled. And a quenching / separating means for separating the sedimentary component that settles in the liquid and the floatable component that floats in the liquid.

  As described above, according to the present invention, from the inorganic hollow fine particle powder raw material, there is a levitating component that contains highly hollow microparticles that are hard to break, and defects such as small holes and chips from an extremely simple operation. It is possible to separate the hollow fine particles, the broken fine particles, and the sedimentation component containing a large amount of debris, and the excellent effect that each fine particle powder can be obtained efficiently is obtained.

  In addition, the high-purity levitation fine particle powder containing a lot of perfect spherical hollow fine particles obtained by the above-described separation operation has a soft polishing power, so that it is suitable for cosmetics such as nail care products, packs, sunscreens, and other excellent materials. On the other hand, hollow fine particles having defects such as small holes and chips, broken fine particles, and high-purity sedimentary fine particle powders containing a large number of debris are excellent in polishing power and can be provided as abrasives. Has an effect.

  In addition, the separation and purification apparatus according to the present invention has an excellent effect that an apparatus excellent in the separation and purification performance of the inorganic hollow fine particle powder material can be obtained with an extremely simple structure.

Overall configuration diagram of the device of the present invention, Flow diagram showing the separation and purification procedure according to the method of the present invention, The figure which shows a mode that hollow ceramic microparticles | fine-particles are destroyed by the method of this invention, The figure which shows a mode that a hollow ceramic fine particle powder raw material is isolate | separated by this invention method, Scanning electron micrograph of the hollow ceramic fine particle powder raw material before being separated and purified by the method of the present invention, It is a scanning electron micrograph of the high purity hollow ceramic fine particle powder separated as a floating component by the method of the present invention.

  BEST MODE FOR CARRYING OUT THE INVENTION The best mode for carrying out the present invention will be described with reference to the drawings. 1 to 6 show an embodiment of the present invention. In FIG. 1, reference numeral 100 denotes a separation and purification apparatus according to the present invention.

  First, the separation and purification device 100 will be described. The separation and purification device 100 includes a heating device 101, a rapid cooling / separation device 102, a drying device 103, and a recovery means 104 as shown in FIG. Here, the heating device 101 heats the heating pot 105 for heating the inorganic hollow fine particle powder raw material, here the hollow ceramic fine particle powder raw material 1 to a temperature (surface temperature) of 100 ° C. or higher, and the heating pot 105. And a heater 106. The rapid cooling / separation apparatus 102 includes a bottomed cylindrical stirring vessel 108 in which water 107 whose water temperature is kept below room temperature is stored, and the heated hollow ceramic fine particle powder raw material 1 is charged into the stirring vessel 108. Then, it is rapidly cooled and separated into a sedimentary component 2 that settles in the water 107 inside the stirring vessel 108 and a floating component 3 that floats in the water 107.

  The drying apparatus 103 includes a drying pan 109 for drying the sedimentary component 2 and the floating component 3 collected by the collecting unit 104, and a heater 110 for heating the drying pan 109. The drying pan 109 and the heater 110 can also be used as the heating pan 105 and the heater 106 in the heating apparatus 101. Moreover, a handle or the like can be used as the collecting means 104.

  Next, a procedure for separating and purifying the hollow ceramic fine particle powder raw material 1 using the separation and purification apparatus 100 will be described with reference to FIG.

(Heating process)
First, in the heating step S1 shown in FIG. 2, the hollow ceramic fine particle powder raw material 1 is put into the heating pan 105 heated by the heater 106, and the hollow ceramic fine particle powder raw material 1 is stirred in the heating pan 105. Heat so that surface temperature becomes 100 degreeC or more. Here, each hollow ceramic fine particle of the hollow ceramic fine particle powder raw material 1 has an average particle diameter of 20 to 800 μm.

(Rapid cooling / separation process)
Next, in the rapid cooling / separation step S2 shown in FIG. 2, the heated hollow ceramic fine particle powder raw material 1 is put into the stirring vessel 108, rapidly cooled in the water 107 therein, and stirred with a stirring rod. Then, the hollow ceramic fine particle powder raw material 1 in the water 107 is uniformly dispersed and then left to stand. Then, rapid air shrinkage due to rapid cooling occurs inside the hollow ceramic fine particles 4, and in the hollow ceramic fine particles 4A having defects such as small holes and chips, the water 107 is sucked into the inside to increase its bulk specific gravity, It settles in the water 107 as the sedimentation component 2. Further, as shown in FIG. 3, even in a perfect sphere, in the hollow ceramic fine particle 4A ′ having a thin shell portion (less than 0.1 μm), the thin portion is caused by rapid air contraction due to rapid cooling. It is destroyed and settles in the water 107 as the sedimentary component 2.

  On the other hand, in the case of a perfect sphere having no small holes or chips and having a relatively thick (0.75 to 10 μm) hollow ceramic fine particle 4B that was not destroyed by rapid cooling, the floating component 3 As it floats in the liquid. As a result, as shown in FIG. 4, it is separated into a sedimentation component 2 containing a lot of hollow ceramic fine particles 4A having defects and breakage, and a levitation component 3 containing a large amount of hollow ceramic fine particles 4B having no defects. The sedimentation component 2 includes broken pieces.

(Recovery process)
Next, in the recovery step S3 shown in FIG. 2, the floating component 3 and the sedimentary component 2 separated in the vertical direction in the stirring vessel 108 are recovered by the recovery means 104, respectively. The sedimentation component 2 collects the floating component 3 and then tilts the stirring vessel 108 to drain the water 107 and collects the sedimentation component 2 remaining at the bottom.

(Drying process)
Next, in the drying step S4 shown in FIG. 2, the recovered sedimentary component 2 and the levitation component 3 are independently put into the drying pan 109, and the former sedimentary component 2 is dried by As a result, hollow ceramic fine particles having defects such as small holes and chips, broken ceramic fine particles, ceramic fine particle powder containing a large amount of broken pieces, that is, high purity sedimentary ceramic fine particle powder 5 can be obtained. Further, in the latter levitation component 3, a ceramic fine particle powder containing a large number of full sphere-like thick hollow ceramic fine particles, that is, a high purity levitating ceramic fine particle powder 6 is obtained.

  Thus, in the high-purity sedimentary ceramic fine particle powder 5 containing many hollow ceramic fine particles having defects such as small pores and chips, broken ceramic fine particles, and broken pieces by drying, it is used as an abrasive having excellent polishing power. In the high-purity levitating ceramic fine particle powder 6 containing a large number of perfect spherical spherical ceramic fine particles, the polishing power is soft and used as a material for cosmetics.

  The inorganic-based hollow fine particle powder raw material in the present invention is not particularly limited, but preferably the apparent specific gravity is relatively small like the hollow ceramic fine particle raw material or the hollow glass fine particle raw material, and the apparent specific gravity is large due to the shell fracture. Such raw materials are preferred.

  In the present invention, the kind of liquid used as a medium for rapidly cooling the heated hollow fine particle powder raw material and separating and purifying it by the difference in apparent specific gravity is not particularly limited. Organic substances that are simply water or liquid can be used. Further, an aqueous solution in which sugar, polysaccharides or other water-soluble substances are dissolved can be used for adjusting the specific gravity and viscosity.

  Furthermore, the separation and purification method into two components by simple sedimentation and levitation is improved, and more precise separation is performed using the separation principle that separates into multiple components using the balance between the buoyancy of fine particles and the specific gravity of the liquid. For the purpose of realizing purification, a solution having a solute concentration gradient can also be used.

  In the separation and purification method described above, the purification purity of the inorganic fine particle powder is further improved by repeating the step of returning the recovered buoyant component 3 as the hollow fine particle powder raw material once or more in the heating step S1. Is possible.

  Further, before heating the hollow fine particle powder raw material 1, it is put in and suspended in water (liquid) in a preheating container, and the suspension is heated with a heater while stirring to evaporate the water. Even after complete evaporation, the heating is continued and heated to a temperature of 100 ° C. or higher, so that it is possible to efficiently heat the hollow fine particle powder raw material 1 that is difficult to heat uniformly and efficiently with the powder as it is. It becomes like this.

  The method for separating and purifying inorganic hollow fine particle powder according to the present invention and the sedimentable fine particle powder and the floating fine particle powder obtained by the method are configured as described above, but are limited to the above embodiment. Instead, various modifications can be made within the scope of the technical idea of the present invention.

  The inventor put 1 kg of a commercially available hollow ceramic fine particle powder material (trade name: E-SPHERES, average particle size 20 to 800 μm, manufactured by Taiheiyo Cement Co., Ltd.) into a drying / heating pan, and a wooden stirring rod. While stirring the powder raw material as needed, the pan was covered and heated with an electric heater. When the powder raw material is sufficiently dried and the surface temperature reaches 120 to 180 ° C., the powder raw material is poured into water stretched in a metal bucket and rapidly cooled. Was stirred to uniformly disperse the powder raw material in the suspension, and then left to stand until the sedimentation component and the floating component were separated. When both components are separated vertically and accumulated on the bottom and water surface of the bucket, the floating components on the water surface are scooped with a metal handle and transferred to the drying / heating pan described above, and the sedimenting components on the bottom of the bucket. After draining as much as possible by tilting the bucket, it was transferred to another drying and heating pan.

  The pans containing these components were each heated with an electric heater, and the contents were dried with stirring with a stirring bar as needed. As a result, 179 g of high purity sedimentary ceramic fine particle powder and 802 g of high purity levitating ceramic fine particle powder were obtained. FIG. 5 shows a scanning electron micrograph of the hollow ceramic fine particle powder material before separation and purification, and FIG. 6 shows the floating ceramic fine particle powder after separation and purification. According to this example, in the fine particle powder raw material before separation and purification shown in FIG. 5, a large number of fine particles and broken pieces such as chips can be confirmed, whereas in the fine particle powder after separation and purification shown in FIG. Was confirmed to be separated and refined into a fine particle powder containing perfectly spherical hollow fine particles with high purity.

  Separation and purification method according to the present invention comprises inorganic hollow fine particle powder raw material, hollow fine particles having defects such as small pores and chips, fine particle powder containing a lot of broken fine particles, and perfect spherical hollow fine particles without defects. It can be used as a method for separating and refining into a fine particle powder containing a large amount of. In addition, fine particle powder containing a large amount of fine particles having defects and breakage is provided as an abrasive having excellent polishing power, and can be used as a cleanser material or as an industrial abrasive. In addition, fine particle powders containing a large amount of perfect spherical hollow particles have a soft polishing power, and can be used as cosmetics and other materials such as nail care products, packs, sunscreens and the like.

1 Hollow ceramic fine particle powder raw material (Inorganic hollow fine particle powder raw material)
2 Sedimentable component 3 Floating component 4 Hollow ceramic fine particle 4A Hollow ceramic fine particle with defects such as small holes and chips 4A 'Completely spherical but thin hollow ceramic fine particle
4B Thick hollow hollow ceramic fine particles without defects 100 Separation and purification device 101 Heating device 102 Rapid cooling / separation device 103 Drying device 104 Recovery means 105 Heating pan 106, 110 Heater 107 Water 108 Stirring vessel 109 Drying pan

Claims (12)

  A heating step for heating the inorganic hollow fine particle powder raw material, a settling component that is rapidly cooled by introducing the heated hollow fine particle powder raw material into a liquid, and a levitating component that floats in the liquid A method for separating and purifying an inorganic hollow fine particle powder raw material, comprising a separation step for separating the raw material, and a recovery step for collecting the separated floating component.   2. The method for separating and purifying inorganic hollow fine particle powder material according to claim 1, wherein the hollow fine particle powder material is a hollow ceramic fine particle material or a hollow glass fine particle material.   The method for separating and purifying an inorganic hollow fine particle powder raw material according to claim 1 or 2, wherein the liquid is water.   The inorganic hollow fine particles according to any one of claims 1 to 3, wherein the heating temperature in the heating step is 100 ° C or higher, and the temperature of the liquid for rapidly cooling the heated hollow fine particle powder raw material is room temperature or lower. A method for separating and purifying powder raw materials.   The method for separating and purifying an inorganic hollow fine particle powder raw material according to any one of claims 1 to 4, further comprising a drying step of drying the recovered floating component.   The method for separating and purifying an inorganic hollow fine particle powder raw material according to any one of claims 1 to 5, wherein in the collecting step, the separated sedimentary component is collected.   The method for separating and purifying the inorganic hollow fine particle powder raw material according to any one of claims 1 to 6, wherein the recovered sedimentary component is dried in the drying step.   The method for separating and purifying an inorganic hollow fine particle raw material according to any one of claims 1 to 7, wherein the recovered floating component is returned again to the heating step as a hollow fine particle powder raw material.   The method further comprises a preheating step of mixing the hollow fine particle powder raw material with the liquid and preheating the mixture of the hollow fine particle powder raw material and the liquid while stirring, and heating the preheated hollow fine particle powder raw material after the liquid is evaporated The method for separating and purifying the inorganic hollow fine particle powder raw material according to any one of claims 1 to 8, wherein   The inorganic hollow fine particle powder raw material is heated, the heated hollow fine particle powder raw material is put into a liquid and rapidly cooled, and separated into a sedimentary component that settles in the liquid and a floating component that floats. A high-purity inorganic fine particle powder obtained by collecting a floating component and drying the collected floating component.   The inorganic hollow fine particle powder raw material is heated, the heated hollow fine particle powder raw material is put into a liquid and rapidly cooled, and separated into a sedimentary component that settles in the liquid and a floating component that floats. A high-purity inorganic fine particle powder obtained by collecting the settled component and drying the collected settled component.   Heating means for heating inorganic-based hollow fine particle powder raw material, settling component that is rapidly cooled by introducing the heated hollow fine particle powder raw material into liquid, and floating component that floats in the liquid An apparatus for separating and purifying an inorganic hollow fine particle powder material, comprising a rapid cooling / separation means for separating the raw material.

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