WO2020111207A1 - Tige d'agitateur et dispositif d'agitation - Google Patents

Tige d'agitateur et dispositif d'agitation Download PDF

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Publication number
WO2020111207A1
WO2020111207A1 PCT/JP2019/046678 JP2019046678W WO2020111207A1 WO 2020111207 A1 WO2020111207 A1 WO 2020111207A1 JP 2019046678 W JP2019046678 W JP 2019046678W WO 2020111207 A1 WO2020111207 A1 WO 2020111207A1
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WO
WIPO (PCT)
Prior art keywords
stirring rod
stirring
rod according
liquid contact
section
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2019/046678
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English (en)
Japanese (ja)
Inventor
秀和 重吉
邦英 四方
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Kyocera Corp
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Kyocera Corp
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Publication date
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Priority to JP2020557842A priority Critical patent/JP7279077B2/ja
Publication of WO2020111207A1 publication Critical patent/WO2020111207A1/fr
Anticipated expiration legal-status Critical
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/02—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations

Definitions

  • the present disclosure relates to a stirring rod for stirring a liquid, and a stirring device including the stirring rod.
  • an analyzer that analyzes blood, urine, and other biochemical samples, mainly for medical purposes, is equipped with a stirring device that stirs the sample solution.
  • This stirring device is equipped with a stirring rod for stirring the sample solution.
  • the stir bar is required to have chemical resistance to sample solutions, reagents and the like.
  • the stirring rod is made of, for example, a metal material such as stainless steel or a resin material such as polyethylene or polypropylene which is surface-treated using a fluororesin.
  • a stainless steel stirring rod whose surface is coated with a fluororesin such as tetrafluoroethylene, trifluoroethylene, chlorotrifluoroethylene, FEP (copolymer of tetrafluoroethylene and hexafluoropropylene) has durability and cost. It is preferably used from the viewpoint of (for example, Patent Documents 1 and 2).
  • the stirring rod of the present disclosure is an integrally molded ceramic product having a stirring portion having a cross section orthogonal to the axial center and having a constant shape along the axial direction.
  • the angle between the adjacent convex portions is larger than the angle obtained by dividing 360° by the number of the convex portions.
  • the stirring device of the present disclosure includes the stirring rod described above.
  • FIG. 5 is a schematic view showing a manufacturing process of the stirring rod of the present disclosure. It is a schematic diagram for explaining the warp of the stirring rod of the present disclosure. It is a schematic diagram showing a use state of a stirring rod of the present disclosure.
  • (A) And (b) is a front view which shows other embodiments of the stirring rod of this indication, respectively.
  • the stirring rod 1 has a stirring unit 2 and a stirring unit having the same axial center A as the stirring unit 2 on one end face in the axial direction of the stirring unit 2. 2 and a shaft portion 3 formed integrally.
  • the stirring unit 2 has a cross section orthogonal to the axis A having a constant shape over the entire length of the stirring unit 2 along the axial direction. That is, as shown in FIG. 1B, the cross section of the stirring section 2 has a shape in which a plurality of convex sections 4 are arranged in the circumferential direction. Since the stirring rod 1 according to the present embodiment includes the plurality of convex portions 4, it is possible to stir by generating a flow in the axial direction.
  • the stir bar 1 is made of ceramics integrally molded with excellent chemical resistance. That is, the stirring portion 2 having a cross-sectional shape in which the plurality of convex portions 4 are arranged in the circumferential direction over the entire length can be obtained by, for example, extrusion molding.
  • Extrusion is performed according to the following procedure. First, water and binder (binder) are added to and mixed with the raw material (powder) and continuously supplied into the cylinder to be heated and melted. Next, the molten material is rotated by a screw in the cylinder to rotate the cylinder. Extrude through a front die, cool and mold. The extruded molded product 11 shown in FIG. 2 has the cross-sectional shape shown in FIG. 1(b) over the entire length. After firing the molded product 11, one end is ground and polished while the molded product 11 is rotated in the grinding/polishing process to form the shaft portion 3. At this time, the shaft portion 3 and the stirring portion 2 have the common axis A.
  • the cross-sectional shape of the shaft portion 3 is not particularly limited, and examples thereof include a circular shape, a quadrangular shape, and an elliptical shape.
  • the raw material of such ceramics is not particularly limited as long as it has excellent chemical resistance, and examples thereof include high-purity alumina, zirconia, silicon nitride, silicon carbide, and alumina-zirconia composite material.
  • the plurality of convex portions 4 arranged in the circumferential direction of the stirring unit 2 extend radially from the axis A in the radial direction, and the convex portions 4 are arranged at equal intervals. There is.
  • the convex portion 4 has a tapered shape whose width becomes narrower toward the tip. With such a tapered shape, the resistance (stress) received by the tip of the convex portion 4 is reduced, and the durability is improved.
  • the entire convex portion 4 is formed into a curved surface. Therefore, the space between the adjacent convex portions 4 and 4, that is, the valley portion is also curved.
  • the angle between adjacent protrusions 4 is larger than the angle obtained by dividing 360° by the number of protrusions 4. That is, each convex portion 4 is thinner than the root portion at a position distant from the axis A. Therefore, there is an effect that a reagent or the like is less likely to accumulate in the gap between the convex portions 4. Further, there is an effect that it is easy to polish even during manufacturing.
  • the angle ⁇ between the adjacent convex portions 4 and 4 may be larger than the angle ⁇ by 1/4 ⁇ or more when ⁇ is an angle obtained by dividing 360° by the number of the convex portions 4.
  • the angle ⁇ between the adjacent convex portions 4 and 4 may form an obtuse angle of 90° or more.
  • the angle ⁇ may be in the range of 90° ⁇ 180°.
  • the angle ⁇ means the angle formed by the tangents of the portions of the adjacent convex portions 4 and 4 that are closest to the valley portion.
  • the convex portion 4 having a shape as shown in FIG. 1B, it means the angle between the outer tangent line of one convex portion 4 and the inner tangent line of the other convex portion 4.
  • the stirring rod 1 may have a shape in which the axis A is curved in an arc shape.
  • the stirring portion 2 is shown as warped, but the shaft center A of the shaft portion 3 is also warped.
  • x the distance most distant from the vertical line in the stirring section 2 shown in FIG. 3 is preferably 0.2 mm or less.
  • X shown in FIG. 3 can be measured by, for example, a gap gauge or the like.
  • the stirring efficiency is improved by the warp of the stirring unit 2.
  • the temperature and the firing time during firing of the molded product 11 may be controlled.
  • the stirring rod 1 is inserted into the stirring tank 9 of the stirring device with the stirring unit 2 facing downward.
  • the upper portion of the shaft portion 3 projects from the liquid surface of the sample solution 8.
  • a drive unit (not shown) including a motor for rotating the stirring rod 1 is connected to the shaft portion 3 protruding from the liquid surface, and the stirring rod 1 is rotated.
  • the stirring unit 2 of the stirring rod 1 in this embodiment is located at least near the bottom of the stirring tank 9, stirring can be performed efficiently regardless of the viscosity of the sample solution 8. Particularly, when the stirring section 2 is formed to be long in the axial direction, it is suitable for stirring the high-viscosity sample solution 8.
  • the stirring unit 2 may have a half or less of the depth of the sample solution 8 (the height from the bottom surface of the stirring tank 9 to the liquid surface).
  • the stirring rod of the present disclosure is not limited to the embodiment of FIG. 1, and various modifications are possible.
  • the stirring unit 2 may be at the bottom, and as shown in FIG. 5( b ), a plurality of stirring units 2 a, 2 b, 2 c may be provided along the shaft 3. It may be arranged in the same manner.
  • the number of convex portions 4 provided on the shaft portion 3 is not limited to the four shown in the figure, and can be appropriately selected within the range of 2 to 5.
  • the shaft portion 3 is integrally formed with the stirring portion 2 by extrusion molding or the like.
  • the shaft portion 3 is manufactured separately from the stirring portion 2, and the shaft portion 3 is formed in a recess provided on the end surface of the stirring portion 2.
  • the shaft portion 3 may be attached and fixed.
  • the shaft portion 3 may have a circular or elliptical cross section, or may have a quadrangular shape for preventing idling.
  • the ceramic may have closed pores, and the value (A) obtained by subtracting the average value of the circle equivalent diameters of the closed pores from the distance between the centers of gravity of the adjacent closed pores may be 20 ⁇ m to 85 ⁇ m.
  • the value (A) is 20 ⁇ m or more, void portions are dispersed and arranged without being dense, and thus high mechanical properties are obtained.
  • the value (A) is 85 ⁇ m or less, it is good when processing such as polishing from the outer peripheral surface of the stirring section 2 in the axial direction or from the end surface of the stirring section 2 or the end surface of the shaft section 3 to the inside. Good workability can be obtained. Further, since the space between the adjacent closed pores is narrowed, it is possible to suppress the extension of microcracks caused by thermal shock.
  • the distance between the centers of gravity of closed pores can be obtained by the following method.
  • a copper plate is used for polishing from the end face of the stirring unit 2 toward the inside by using diamond abrasive grains having an average particle diameter D 50 of 3 ⁇ m.
  • a polished surface is obtained by polishing with a tin plate using diamond abrasive grains having an average particle diameter D 50 of 0.5 ⁇ m.
  • the arithmetic average roughness Ra of the polished surface can be 0.01 ⁇ m to 0.2 ⁇ m.
  • the arithmetic average roughness Ra of the polished surface can be determined according to JIS B 0601:1994, the radius of the stylus is 5 ⁇ m, the material of the stylus is diamond, the measurement length is 1.25 mm, and the cutoff value is It may be 0.25 mm.
  • the polished surface is observed at a magnification of 200 times, and an average range is selected.
  • a range in which the area is 0.105 mm 2 (horizontal length 374 ⁇ m, vertical length 280 ⁇ m) is CCD
  • the image analysis software “A image-kun (ver2.52)” registered trademark, manufactured by Asahi Kasei Engineering Co., Ltd.
  • the distance between the centers of gravity of the closed pores was measured by a method called the distance between centers of gravity measurement of the degree of dispersion. Find the distance.
  • the image analysis software “A image-kun” it means image analysis software manufactured by Asahi Kasei Engineering Co., Ltd.
  • a threshold value which is an index showing the brightness of an image, is 86, brightness is dark, small figure removal area is 1 ⁇ m 2 , and a noise removal filter is provided.
  • the threshold value may be adjusted according to the brightness of the observed image. The brightness was set to dark, the binarization method was set to manual, the small figure removal area was set to 1 ⁇ m 2 and a noise removal filter was provided. Adjust the value.
  • the silicon concentration on the liquid contact surface is higher than the silicon concentration on an internal virtual surface parallel to the liquid contact surface.
  • a color mapping image of silicon (electron beam microanalyzer (EPMA)) was used for the polished cross section including the liquid contact surface (horizontal length 120 ⁇ m, vertical length: 90 ⁇ m). You can observe.
  • EPMA electron beam microanalyzer
  • the ceramic on the liquid contact surface of the convex portion 4 has a plurality of crystal grains and a grain boundary phase, and the width (w) of the grain boundary phase located between the adjacent crystal grains is 0.7 ⁇ m to
  • the ratio (d/w) of the depth (d) of the grain boundary phase to the width (w) of the grain boundary phase may be 0.06 to 0.18.
  • the width (w) of the grain boundary phase is in the above range and the ratio (d/w) of the depth (d) of the grain boundary phase is 0.18 or less, the binding force between crystal grains due to the grain boundary phase Is maintained sufficiently, the risk of shedding is reduced even when high-pressure washing is performed using a water-soluble detergent.
  • the width (w) and the depth (d) of the grain boundary phase an atomic force microscope (7500AFM/SPM manufactured by Keysight Technology) was used, the measurement mode was ACAFM mode, and the scanning speed of the probe used for measurement was 0.15lines. /Sec, the measurement area is 20 ⁇ m ⁇ 20 ⁇ m, the length of the measurement target is 7 ⁇ m to 20 ⁇ m, and the resolution is 512 pixels ⁇ 512 pixels, the cross-sectional profile of the liquid contact surface is obtained, and the ratio (d/w) is the grain boundary phase. It may be calculated using the respective measured values of the width (w) and the depth (d).
  • the average diameter of the crystal particles of the ceramics on the liquid contact surface of the convex portion 4 may be 2 ⁇ m to 8 ⁇ m.
  • the contact angle with respect to pure water becomes smaller, so that the efficiency of removing stains can be increased when the particles are washed with a water-soluble detergent.
  • the average diameter of crystal particles of ceramics can be obtained as follows.
  • the observation surface is obtained by etching the polished surface at a temperature of, for example, 1480° C. until the crystal particles and the grain boundary layer can be distinguished from each other.
  • a backscattered electron image of the observation surface was magnified 2000 times in a range of 60 ⁇ m ⁇ 44 ⁇ m, and a straight line of the same length, for example, 30 ⁇ m, was drawn radially around an arbitrary point,
  • the average diameter can be obtained by dividing the total length of the straight line by the total number of crystals existing on the straight line.
  • the contact angle of the liquid contact surface of the convex portion 4 with respect to pure water may be 37° or less and the coefficient of variation thereof may be 0.02 or less.
  • At least one of the side surface and the end surface of the convex portion 4 may be covered with a film made of a compound containing fluorinated polysiloxane. After washing with a water-soluble detergent, the Lotus effect that water droplets adhering to the surface covered with the above film adsorb the dirt can be obtained, so that the dirt removal efficiency can be increased.
  • the contact angle of the liquid contact surface of the membrane with pure water may be 104° or more, and the coefficient of variation may be 0.01 or less.
  • the contact angle of the liquid contact surface can be determined according to JIS R 3257:1999. For example, if a contact angle meter (manufactured by Kyowa Interface Science Co., Ltd., model CA-X) is used, it can be measured at 5 or more points Good. Next, the manufacturing method of the stirring rod of the present disclosure will be described when the stirring rod is made of high-purity alumina ceramics.
  • Aluminum oxide powder (purity of 99.9 mass% or more) as the main component, and magnesium hydroxide, silicon oxide, and calcium carbonate powders were mixed with an organic binder, a plasticizer, a lubricant, and ion-exchanged water. After being stirred using a universal stirrer, a rotary mill, a V-type stirrer, or the like, further kneading is performed using a three-roll mill, a kneader, or the like to obtain a plasticized kneaded clay.
  • the content of the magnesium hydroxide powder is 0.43 to 0.53 mass%
  • the content of the silicon oxide powder is 0.02 to 0.04 mass%
  • the content of the calcium carbonate powder is 100% by mass.
  • the content is 0.020 to 0.071% by mass
  • the balance is aluminum oxide powder and unavoidable impurities.
  • the organic binder is a water-soluble binder such as methyl cellulose or hydroxypropyl methyl cellulose.
  • the kneaded material is molded by an extrusion molding machine, the precursor of the stirring portion having a plurality of convex portions, and the precursor of the shaft portion having the same axial center as this precursor on one end face in the axial direction of the precursor A molded body having and is obtained.
  • the stirring bar of the present disclosure can be obtained by firing the molded body at a firing temperature of 1500° C. to 1700° C. and a holding time of 4 hours to 6 hours.
  • At least one of the side face and the end face of the convex portion may be polished, and then heat-treated at a temperature of 1600° C. to 1700° C. for 1 hour to 4 hours. It is possible to obtain a stirring bar in which the contact angle of the liquid contact surface of the part to pure water is 37° or less and the coefficient of variation is 0.02 or less.
  • a surface pressure applied to the side surface or the end surface to be polished is 0.03 MPa to 0.05 MPa, and a lapping machine made of diamond abrasive grains having an average grain size of 1 ⁇ m to 2 ⁇ m and copper may be used.
  • At least one of the side surface and the end surface of the convex portion is at least a target of coating.
  • the surface of the convex portion may be coated by a method such as flow coating, dipping or spraying, and then dried at, for example, 130°C to 150°C.

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  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Accessories For Mixers (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

Cette tige d'agitation 1 comprend un produit formé d'un seul tenant en céramique et comporte une section d'agitation ayant, dans une section transversale de celle-ci perpendiculaire à un axe, une forme constante dans la direction axiale. Dans la section transversale, une pluralité de saillies 4 sont agencées dans une direction circonférentielle, et l'angle θ entre des saillies adjacentes 4 est supérieur à l'angle obtenu en divisant 360° par le nombre des saillies 4. La tige d'agitation 1 est pourvue de la section d'agitation 2 ayant la pluralité de saillies 4, et d'une section d'arbre 3 formée d'un seul tenant sur une surface d'extrémité axiale de la section d'agitation 2 de façon à être coaxiale à la section d'agitation 2.
PCT/JP2019/046678 2018-11-29 2019-11-28 Tige d'agitateur et dispositif d'agitation Ceased WO2020111207A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2020557842A JP7279077B2 (ja) 2018-11-29 2019-11-28 撹拌棒および撹拌装置

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JP2018223755 2018-11-29
JP2018-223755 2018-11-29

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH041448U (fr) * 1990-04-17 1992-01-08
JP3102011U (ja) * 2003-12-01 2004-06-24 照子 村上 電動納豆攪拌機
JP2015221427A (ja) * 2014-05-22 2015-12-10 ポスコ 攪拌装置
WO2016043269A1 (fr) * 2014-09-17 2016-03-24 積水化学工業株式会社 Dispositif d'appport de poudre, dispositif filmogene et procede filmogene

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH041448U (fr) * 1990-04-17 1992-01-08
JP3102011U (ja) * 2003-12-01 2004-06-24 照子 村上 電動納豆攪拌機
JP2015221427A (ja) * 2014-05-22 2015-12-10 ポスコ 攪拌装置
WO2016043269A1 (fr) * 2014-09-17 2016-03-24 積水化学工業株式会社 Dispositif d'appport de poudre, dispositif filmogene et procede filmogene

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JPWO2020111207A1 (ja) 2021-10-07
JP7279077B2 (ja) 2023-05-22

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