JP6423988B2 - Stirring mill and dispersion method of particles in slurry - Google Patents
Stirring mill and dispersion method of particles in slurry Download PDFInfo
- Publication number
- JP6423988B2 JP6423988B2 JP2017009971A JP2017009971A JP6423988B2 JP 6423988 B2 JP6423988 B2 JP 6423988B2 JP 2017009971 A JP2017009971 A JP 2017009971A JP 2017009971 A JP2017009971 A JP 2017009971A JP 6423988 B2 JP6423988 B2 JP 6423988B2
- Authority
- JP
- Japan
- Prior art keywords
- slurry
- partition plate
- cylindrical container
- stirring mill
- rotor
- 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.)
- Active
Links
- 239000002002 slurry Substances 0.000 title claims description 121
- 238000003756 stirring Methods 0.000 title claims description 38
- 238000000034 method Methods 0.000 title claims description 10
- 239000002245 particle Substances 0.000 title description 49
- 239000006185 dispersion Substances 0.000 title description 30
- 238000005192 partition Methods 0.000 claims description 75
- 230000002093 peripheral effect Effects 0.000 claims description 62
- 239000011324 bead Substances 0.000 claims description 54
- 239000010419 fine particle Substances 0.000 claims description 11
- 230000004323 axial length Effects 0.000 claims description 6
- 238000012545 processing Methods 0.000 description 16
- 239000011164 primary particle Substances 0.000 description 13
- 238000000926 separation method Methods 0.000 description 13
- 238000010298 pulverizing process Methods 0.000 description 11
- 239000011163 secondary particle Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 230000006378 damage Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000000498 cooling water Substances 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Description
本発明は、液体中に固体又は液体の粒子が分散している懸濁液（以下、スラリーという）中の凝集している粒子を粉砕するとともに分散させる撹拌ミルと、該撹拌ミルによるスラリー中粒子の分散方法に関する。
本発明でいう分散とは、単一の結晶粒子や非晶質粒子が凝集して形成されている二次粒子を溶液中にばらして、分離することを言い、また本発明でいう粉砕とは、単一粒子を複数の粒子に分解することを言う。
The present invention relates to a stirring mill that pulverizes and disperses agglomerated particles in a suspension in which solid or liquid particles are dispersed in a liquid (hereinafter referred to as slurry), and particles in the slurry by the stirring mill. It is related with the dispersion method.
Dispersion as used in the present invention refers to separating and separating secondary particles formed by aggregation of single crystal particles or amorphous particles into a solution, and pulverization as used in the present invention. , Refers to breaking a single particle into multiple particles.
従来の撹拌ミルは、分散・粉砕を担当する攪拌を行う部分と、分散・粉砕用のビーズを分離するセパレータ部分とに分かれたものと、セパレータ構造において、分散・粉砕とビーズ分離を同時に行うものがあった。前者の装置区分の撹拌ミルとして、例えば下記特許文献１に示す湿式のボールミルが開示されている。この装置では、ビーズが充填される円筒形容器と、該容器内に容器と同軸をなして配置され、モーターを駆動源として回転駆動されるシャフトに固定された攪拌羽とセパレータよりなり、撹拌翼は、分散・粉砕機能を有し、またセパレータはシャフトの上下に固定される円板状のディスクと、上下のディスク間を周方向に一定間隔で連結するブレードよりなってインペラの形態をなしている。粉砕及び分散のためのビーズが充填される当該容器内にスラリーを導入して、攪拌羽とセパレータを回転駆動することにより、スラリー中の粒子を分散・粉砕して、粒子を微細化する。この際に、遠心力の作用によってビーズを分離したスラリーをセパレータの外周端より内周端に移動させ、シャフトの中空な軸心を通して排出させることで、分散・粉砕処理を経た、ビーズ混入の少ないスラリーを製造する。 Conventional agitation mills are divided into a part that performs stirring for dispersion and pulverization and a separator part that separates beads for dispersion and pulverization, and a separator structure that simultaneously performs dispersion and pulverization and bead separation. was there. For example, a wet ball mill shown in Patent Document 1 below is disclosed as the former agitation mill of the apparatus section. This apparatus comprises a cylindrical container filled with beads, a stirring blade fixed to a shaft that is coaxially arranged with the container in the container, and is driven to rotate by using a motor as a driving source, and a separator. Has a function of dispersing and crushing, and the separator is in the form of an impeller comprising a disk-like disk fixed at the top and bottom of the shaft and a blade that connects the upper and lower disks at regular intervals in the circumferential direction. Yes. The slurry is introduced into the container filled with beads for pulverization and dispersion, and the stirring blade and the separator are driven to rotate, whereby the particles in the slurry are dispersed and pulverized to refine the particles. At this time, the slurry in which the beads are separated by the action of centrifugal force is moved from the outer peripheral end of the separator to the inner peripheral end, and discharged through the hollow shaft center of the shaft. A slurry is produced.
また特許文献２には、後者の装置区分の撹拌ミルにあたる従来技術での分散・粉砕に適した粉砕機である。この装置では、円筒形容器及びセパレータが共に大径で、直径Ｄに比べ、軸方向長さＬが小さく、その比率（L／D）が小さい粉砕機が開示されている。また、特許文献３は、前者の装置区分の撹拌ミルであるが、構造的には、後者の装置区分の撹拌ミルに近いものである。上下のディスクの間に仕切板のディスクを入れる発明であり、下方の室において、攪拌による分散・粉砕がなされ、最上段の室でビーズ分離と分散・粉砕を行う装置である。 Patent Document 2 discloses a pulverizer suitable for dispersion and pulverization according to the prior art corresponding to the stirring mill of the latter apparatus section. In this apparatus, a pulverizer is disclosed in which both the cylindrical container and the separator have a large diameter, the axial length L is smaller than the diameter D, and the ratio (L / D) is small. Moreover, although patent document 3 is the stirring mill of the former apparatus division, it is structurally close to the stirring mill of the latter apparatus division. It is an invention in which a partition plate disk is inserted between upper and lower disks, and is a device in which dispersion and pulverization are performed by stirring in the lower chamber, and beads are separated and dispersed and pulverized in the uppermost chamber.
従来技術では、後者の装置区分の攪拌ミルにおいて、特許文献１の例に見られるように、攪拌羽とセパレータの両方を有することから、装置が複雑で製造原価が高であった。更に構造上セパレータブレードの位置が回転軸に近く、かつ短いため、分離性能が悪化する問題があった。これに対応するため、セパレータブレードの設置密度を上げているが、その結果、スラリー通過断面積が小さくなり、スラリー処理量が低下するとともにスラリー送液動力が増加する問題があった。 In the prior art, as shown in the example of Patent Document 1, the stirring mill of the latter apparatus section has both the stirring blades and the separator, so that the apparatus is complicated and the manufacturing cost is high. Furthermore, because of the structure, the position of the separator blade is close to the rotation axis and short, so there is a problem that the separation performance deteriorates. In order to cope with this, the installation density of the separator blades is increased. As a result, there is a problem that the cross-sectional area through which the slurry passes is reduced, the slurry throughput is reduced, and the slurry feeding power is increased.
また、セパレータ位置で、分散・粉砕とビーズ分離の両方の処理をする型式の後者の装置区分においては、特許文献３の例に見られるように、セパレータの直径Ｄと軸方向長さＬの比、Ｌ／Ｄが大きなものでは、容器のスラリー中のビーズ濃度のばらつきが回転軸の方向において大きくなる。この結果、分散不足の粒子と、粒子が過剰に破壊された粒子が混在した状態となって、粒子径が揃い、かつ均一に分散したスラリーが得られなくなる問題があった。特に、高粘性のスラリーにおいては、この現象が顕著であった。
このようなスラリーから得た粒子を使った最終製品では、以下のような問題があった。例えば、酸化物の焼結によって製造される誘電体では、焼結体中の結晶粒子径のばらつきが大きくなり、巨大化した粒子起因の局部的な誘電率異常低下の問題があった。また、インク等の色材においては、色の均一性が確保できない問題があった。
Further, in the latter apparatus type of the type that performs both dispersion / grinding and bead separation at the separator position, as seen in the example of Patent Document 3, the ratio of the separator diameter D to the axial length L When L / D is large, the variation in the bead concentration in the slurry of the container increases in the direction of the rotation axis. As a result, there is a problem in that a particle having a uniform particle size and a uniformly dispersed slurry cannot be obtained because particles having insufficient dispersion and particles in which particles are excessively broken are mixed. In particular, this phenomenon was remarkable in a highly viscous slurry.
The final product using particles obtained from such a slurry has the following problems. For example, a dielectric produced by sintering an oxide has a large variation in crystal particle diameter in the sintered body, and has a problem of local decrease in dielectric constant due to enlarged particles. In addition, color materials such as ink have a problem that color uniformity cannot be ensured.
従って、特許文献２に記載されるように、前述のＬ／Ｄを小さくして、セパレータ全域にわたり均一な処理をすることは有効である。しかし、この装置においても処理上の問題があった。処理量を増加させようとして、セパレータ径を大きくすると、セパレータ外周に近い部分での遠心力と中心に近い部分の遠心力の差が大きくなりすぎて、ビーズが外周部分のみに存在する結果、セパレータ外周部において、仕切板がビーズを巻き込んで、ビーズ混入率が悪化する問題があった。 Therefore, as described in Patent Document 2, it is effective to reduce the above-mentioned L / D and perform uniform processing over the entire separator. However, this apparatus also has a processing problem. If the separator diameter is increased in order to increase the throughput, the difference between the centrifugal force near the separator periphery and the centrifugal force near the center becomes too large. As a result, the beads exist only in the outer periphery. In the outer periphery, the partition plate entrains beads, and there is a problem that the bead mixing rate deteriorates.
このため、特許文献２の装置のように、セパレータ外周部を攪拌することに主眼を置き、ブレードのセパレータ直径方向の長さが短い装置を発明している。しかし、この結果、分散効果が小さくなり、かつビーズ分離が不十分である問題があった。また、従って、分散が不十分で、しかもビーズによる製品の汚染が多いものであった。また、セパレータのブレード長さが短すぎて、ビーズ分離効率が悪く、製品スラリーに不純物が混入する問題があった。 For this reason, as in the apparatus of Patent Document 2, the apparatus focuses on stirring the outer peripheral portion of the separator and invents an apparatus in which the blade is short in the diameter direction of the separator. However, as a result, there are problems that the dispersion effect is reduced and the bead separation is insufficient. Therefore, the dispersion was insufficient and the product was frequently contaminated with beads. Further, the blade length of the separator is too short, the bead separation efficiency is poor, and there is a problem that impurities are mixed into the product slurry.
この問題に対応するため、容器及びセパレータを縦長する場合は、特許文献３に記載されているように、上下のディスクの間に仕切板のディスクを入れる発明がなされている。しかし、この装置においては、スラリーが仕切板で区分された室を順次通過して処理しており、滞留時間が長くなる利点はあるが、装置が大型化する問題と過剰粉砕が起きる問題があった。特に、高粘性のスラリーにおいては、スラリーの流れが複雑で、十分な処理ができなかった。 In order to cope with this problem, when the container and the separator are vertically long, as described in Patent Document 3, an invention has been made in which a disk of a partition plate is inserted between upper and lower disks. However, this apparatus has the advantage that the slurry passes through the chambers divided by the partition plate in order and has the advantage that the residence time becomes long, but there are problems that the apparatus becomes large and excessive crushing occurs. It was. In particular, in the case of a highly viscous slurry, the flow of the slurry is complicated and sufficient treatment cannot be performed.
本発明は、Ｌ／Ｄの最適化を図るとともに、セパレータブレードの設置条件を適正化することにより生産性を低下させることなく、スラリー中の粒子の均一な分散を可能にし、製品特性を向上させることができる撹拌ミルと、該撹拌ミルによるスラリー中微粒子の処理方法を提供することを目的とする。 The present invention optimizes the L / D and optimizes the installation conditions of the separator blade to enable uniform dispersion of particles in the slurry and improve product characteristics without reducing productivity. It is an object of the present invention to provide a stirring mill that can be used and a method for treating fine particles in a slurry using the stirring mill.
請求項１に係る発明の攪拌ミルは、ビーズが充填される円筒容器中に、当該円筒容器と同軸心上に配置されて回転するスラリー排出用中空部を備えた中空シャフト７が配置され、中空シャフト７に接続されるシャフト６、上部円板１０、下部円板１１及び両円板を連結する仕切板９から構成される回転子８が当該円筒容器内にて回転するとともに、当該円筒容器の下蓋４に設けられるスラリー供給口１３から供給されたスラリーが仕切板９間を経由して、中空シャフト７の中空部から装置外に排出されるスラリー経路を形成している攪拌ミルであって、仕切板９の外周端が接する円の直径Ｄと、回転子８の軸方向長さである、前記上部円板１０の上面と下部円板１１の下面間の距離Ｌの比であるＬ／Ｄが０．３〜１．６であることを特徴とする。
In the stirring mill according to the first aspect of the present invention, a hollow shaft 7 having a hollow portion for discharging slurry that is disposed coaxially with the cylindrical container and rotates is disposed in a cylindrical container filled with beads, and is hollow. A rotor 8 composed of a shaft 6 connected to the shaft 7, an upper disk 10, a lower disk 11, and a partition plate 9 connecting both disks rotates in the cylindrical container, and the cylindrical container A stirring mill that forms a slurry path in which the slurry supplied from the slurry supply port 13 provided in the lower lid 4 is discharged from the hollow portion of the hollow shaft 7 to the outside of the apparatus via the partition plate 9. L / is the ratio of the distance L between the upper surface of the upper disk 10 and the lower surface of the lower disk 11, which is the diameter D of the circle that the outer peripheral edge of the partition plate 9 contacts and the axial length of the rotor 8. D is 0.3 to 1.6 .
請求項２に係る発明の攪拌ミルは、ビーズが充填される円筒容器中に、当該円筒容器と同軸心上に配置されて回転するスラリー排出用中空部を備えた中空シャフト７が配置され、中空シャフト７に接続されるシャフト６、上部円板１０、下部円板１１及び両円板１０、１１を連結する仕切板９から構成される回転子８が当該円筒容器内にて回転するとともに、当該円筒容器の上蓋３に設けられるスラリー供給口１４及び下蓋４に設けられるスラリー供給口１３から供給されたスラリーが仕切板９間を経由して、中空シャフト７の中空部から装置外に排出されるスラリー経路を形成している攪拌ミルであって、仕切板９の外周端が接する円の直径Ｄと、回転子８の軸方向長さである、前記上部円板１０の上面と下部円板１１の下面間の距離Ｌの比であるＬ／Ｄが０．３〜３．２であることを特徴とする。
In the stirring mill according to the second aspect of the present invention, a hollow shaft 7 having a hollow portion for discharging slurry rotating coaxially with the cylindrical container is disposed in a cylindrical container filled with beads. A rotor 8 composed of a shaft 6 connected to the shaft 7, an upper disk 10, a lower disk 11, and a partition plate 9 connecting the both disks 10, 11 rotates in the cylindrical container, and The slurry supplied from the slurry supply port 14 provided in the upper lid 3 of the cylindrical container and the slurry supply port 13 provided in the lower lid 4 is discharged from the hollow portion of the hollow shaft 7 to the outside of the device via the partition plate 9. The upper surface of the upper disk 10 and the lower disk, which have a diameter D of a circle with which the outer peripheral edge of the partition plate 9 contacts and the axial length of the rotor 8. 11 of the distance L between the lower surfaces of L / D is equal to or is from 0.3 to 3.2 is.
請求項３に係る発明は、請求項１又は２に係る発明において、仕切板９の内周端が位置する円周の径が、仕切板９の外周端が位置する円周の径の５０〜８５％であることを特徴とする。 The invention according to claim 3 is the invention according to claim 1 or 2, wherein the diameter of the circumference where the inner peripheral end of the partition plate 9 is located is 50 to 50% of the diameter of the circumference where the outer peripheral end of the partition plate 9 is located. It is characterized by 85%.
請求項４に係る発明は、請求項１又は３いずれかに係る発明において、内周端と外周端３の仕切板９のギャップ間隔の比率（Ｇ２／Ｇ１）が１．２≦Ｇ２／Ｇ１≦３であることを特徴とする。 The invention according to claim 4 is the invention according to claim 1 or 3, wherein the ratio (G 2 / G 1 ) of the gap distance between the inner peripheral end and the outer peripheral end 3 of the partition plate 9 is 1.2 ≦ G 2. / G 1 ≦ 3.
請求項５に係る発明は、請求項１から４いずれかに係る発明において、仕切板９が円筒容器の中心から当該円筒容器の側面に向けた直径方向の線に対する角度が回転方向に向いて５〜３０度であることを特徴とする。 The invention according to claim 5 is the invention according to any one of claims 1 to 4, wherein the angle of the partition plate 9 with respect to the diametrical line from the center of the cylindrical container toward the side surface of the cylindrical container is 5 in the rotational direction. It is ˜30 degrees.
請求項６に係る発明は、微細な粒子を含むスラリーを請求項１から３のいずれかに記載の攪拌ミルにて、回転子８を構成する仕切板９の外周端での遠心力が8,000 m/s2以下で処理することを特徴とするスラリー中微粒子の処理方法である。 The invention according to claim 6 is the stirring mill according to any one of claims 1 to 3, wherein the centrifugal force at the outer peripheral end of the partition plate 9 constituting the rotor 8 is 8,000 m. A method for treating fine particles in a slurry, wherein the treatment is performed at / s 2 or less.
請求項７に係る発明は、微細な粒子を含むスラリーを請求項１から３いずれかに記載の攪拌ミルにて、回転子８を構成する仕切板９の外周端と円筒体２の間隔において、仕切板９の外周端での周速と当該間隔により計算されるシェア率が1000〜8000 1/sで処理することを特徴とするスラリー中微粒子の処理方法である。 In the invention according to claim 7, in the gap between the outer peripheral end of the partition plate 9 constituting the rotor 8 and the cylindrical body 2 in the stirring mill according to any one of claims 1 to 3, the slurry containing fine particles, A method for treating fine particles in a slurry, wherein a shear rate calculated based on a peripheral speed at the outer peripheral end of the partition plate 9 and the interval is 1000 to 8000 1 / s.
本発明において、攪拌装置の装置構成を適正にするとともにより、スラリー中の一次粒子破壊が少ない状態で、二次粒子が分解されて一次粒子が均一に分散した製品スラリーが得られるとともに、粉砕用のビーズが処理後のスラリーに混入する比率を低減できる。また、従来の攪拌装置では処理できなかった高粘性スラリー中の微細粒子の分散も可能となる。特に０．５マイクロメートル以下の粒子を含む５００mPa・s以上の高粘度スラリーにおいて、本発明の装置は有効である。更に本発明において、請求項１から５の構成の装置を用いることにより、分散率が高く、かつ一次粒子破壊の少ない処理を安定して実現できる。 In the present invention, the device configuration of the stirring device is made appropriate, and in addition, a product slurry in which the secondary particles are decomposed and the primary particles are uniformly dispersed can be obtained with less primary particle breakage in the slurry. The ratio of the beads mixed into the slurry after processing can be reduced. Further, it becomes possible to disperse the fine particles in the high-viscosity slurry that could not be processed by the conventional stirring device. The apparatus of the present invention is effective particularly in a high-viscosity slurry of 500 mPa · s or more containing particles of 0.5 μm or less. Furthermore, in the present invention, by using the apparatus having the structure of claims 1 to 5, it is possible to stably realize a treatment with a high dispersion rate and a small primary particle destruction.
以下、本発明の実施形態に係る撹拌ミルについて図面により説明する。本図では、装置の回転軸を垂直方向に記載しているが、水平などの他の方向に設置しても良い。
図１は全体を符号１で示す撹拌ミルの断面、図２は図１のＡ−Ａ線断面を示すもので、撹拌ミル１は円筒体２の上下を上蓋３と、下蓋４で固定した密閉形状の円筒容器と、当該円筒容器内に当該円筒容器と同軸をなして配置され、図示してないが、モーターを駆動源として回転駆動されるシャフト６に固定された回転子８よりなり、シャフト６は上側部が横断面円形、下側部が横断面略正方形で、回転子８がシャフト６下側部に回転不可に嵌合している。なお、当該円筒容器は必ずしも、円筒体２、上蓋３，及び下蓋４に分割して構成される必要はなく、例えば、円筒体２と下蓋４が一体化しても良い。
Hereinafter, a stirring mill according to an embodiment of the present invention will be described with reference to the drawings. In this figure, the rotation axis of the apparatus is shown in the vertical direction, but it may be installed in other directions such as horizontal.
FIG. 1 is a cross-sectional view of the agitation mill generally indicated by reference numeral 1, and FIG. 2 is a cross-sectional view taken along line AA of FIG. 1. A cylindrical container having a sealed shape and a rotor 8 fixed to a shaft 6 which is arranged in the cylindrical container and coaxially with the cylindrical container and is not illustrated, but is driven to rotate using a motor as a drive source, The shaft 6 has a circular cross section on the upper side and a substantially square cross section on the lower side, and the rotor 8 is non-rotatably fitted to the lower side of the shaft 6. Note that the cylindrical container does not necessarily need to be divided into the cylindrical body 2, the upper lid 3, and the lower lid 4. For example, the cylindrical body 2 and the lower lid 4 may be integrated.
回転子８は、シャフト６に固着の上部円板１０と、上部円板１０と一定の間隔を存してシャフト６に固着される下部円板１１よりなる一対の円板、及び周方向に等間隔に配置されて、上部円板１０と下部円板１１のそれぞれを連結する軸方向の仕切板９とから構成され、仕切板９の外周端において、周速３〜３０ｍ／秒程度で回転する。 The rotor 8 includes a pair of disks composed of an upper disk 10 fixed to the shaft 6, a lower disk 11 fixed to the shaft 6 with a certain distance from the upper disk 10, and the like in the circumferential direction. It is composed of an axial partition plate 9 arranged at intervals and connecting each of the upper disc 10 and the lower disc 11, and rotates at a peripheral speed of about 3 to 30 m / sec at the outer peripheral end of the partition plate 9. .
中空シャフト７は回転子８の上部円板１０より上方の軸心部を中空にして、中空部を有する中空シャフト７として形成され、中空シャフト７の下端が直径方向の貫通孔１２により仕切板内の回転子８内部に開口している。スラリーの供給口は、円筒容器一側の下蓋４に設置されている第１のスラリー供給口である下部スラリー供給口１３と、円筒容器他側の上蓋３に設置されている第２のスラリー供給口である上部スラリー供給口（図示しない）とからなっているが、いずれか一方が設置されている場合もある。処理中、スラリーは下部供給口１３又は上部スラリー供給口のいずれか、又は両方から供給され、円筒体２の曲面近くを経由して、回転子８の中心方向に流れ、更に中空シャフト７の中空部を通じて装置外に排出される。
The hollow shaft 7 is formed as a hollow shaft 7 having a hollow portion with the axial center portion above the upper disk 10 of the rotor 8 being hollow, and the lower end of the hollow shaft 7 is formed in the partition plate by a diametrical through hole 12. Is opened inside the rotor 8. The slurry supply port includes a lower slurry supply port 13 which is a first slurry supply port installed in the lower lid 4 on one side of the cylindrical container, and a second slurry installed in the upper lid 3 on the other side of the cylindrical container. Although it consists of the upper slurry supply port (not shown) which is a supply port, either one may be installed. During the process, the slurry is supplied from either the lower supply port 13 or the upper slurry supply port or both, flows near the curved surface of the cylindrical body 2, flows toward the center of the rotor 8, and is further hollow in the hollow shaft 7. It will be discharged out of the device through
円筒容器には、図１の矢印で示すように冷媒である冷却水が出入し、冷却水路５を周側面から冷却するようにしているが、上蓋３及び下蓋４にも冷却水を供給し、円筒体２を周側面からだけでなく上下から冷却するようにしてもよい。 As shown by the arrows in FIG. 1, cooling water as a refrigerant enters and exits the cylindrical container and cools the cooling water passage 5 from the peripheral side surface. However, the cooling water is also supplied to the upper lid 3 and the lower lid 4. The cylindrical body 2 may be cooled not only from the peripheral side but also from the top and bottom.
ここで、本発明において、スラリー供給が１方向からのみの場合は、回転子８の仕切板９の外周端の直径（Ｄ）と回転軸方向の長さ（Ｌ）の関係を０．３≦Ｌ／Ｄ≦１．６とする。この条件では、スラリー中粒子の適正な分散と粉砕が行われ、かつ処理後のスラリー中のビーズ汚染が少ない。特に、高粘性スラリーにおいては、本発明の設計要件を備えた装置で処理することの効果が大きい。 Here, in the present invention, when the slurry is supplied from only one direction, the relationship between the diameter (D) of the outer peripheral end of the partition plate 9 of the rotor 8 and the length (L) in the rotation axis direction is 0.3 ≦. L / D ≦ 1.6. Under these conditions, proper dispersion and pulverization of particles in the slurry is performed, and bead contamination in the slurry after treatment is small. Particularly in the case of a highly viscous slurry, the effect of processing with an apparatus having the design requirements of the present invention is significant.
Ｌ／Ｄが０．３以下の場合、ビーズ混入率が増加して、スラリーを製品原料にする際に問題となるレベルとなる。これは、回転子が扁平すぎて、遠心力により円筒体２の周辺に積層しているビーズが撹乱されて、ビーズがスラリーとともに、回転子８内部に流れ込んでしまうためである。 When L / D is 0.3 or less, the bead mixing rate increases, and becomes a problem level when slurry is used as a product raw material. This is because the rotor is too flat, the beads stacked around the cylindrical body 2 are disturbed by centrifugal force, and the beads flow into the rotor 8 together with the slurry.
一方、Ｌ／Ｄ≧１．６の場合、当該円筒容器、回転子８ともに縦長であるため、当該円形容器中のスラリー中ビーズ濃度のばらつきがあり、特に回転軸方向（図中の縦方向）において大きくなる。この結果、ビーズが密な部分では、局所的なせん断力上昇を生じ、ビーズのずり応力が大きくなり、また、ビーズが疎な部分では、せん断力が不足する。更に、スラリーの滞留時間のばらつきも大きくなり、滞留時間の短い粒子は分散不足となる一方、滞留時間の長い粒子では、いわゆる一次粒子破壊が増加する。この結果、分散不足の粒子と、粒子が過剰に破壊された粒子が混在した状態となって、粒子径がそろっており、かつ均一に分散した粒子のスラリーが得られなくなる問題があった。 On the other hand, when L / D ≧ 1.6, since both the cylindrical container and the rotor 8 are vertically long, there is a variation in the bead concentration in the slurry in the circular container, particularly in the direction of the rotation axis (the vertical direction in the figure). At As a result, when the beads are dense, local shear force increases, and the shear stress of the beads increases, and when the beads are sparse, the shear force is insufficient. Further, the dispersion of the residence time of the slurry is increased, and particles having a short residence time are insufficiently dispersed, while particles having a long residence time increase so-called primary particle breakage. As a result, there is a problem in that particles that are insufficiently dispersed and particles in which the particles are excessively broken are mixed, making it impossible to obtain a slurry of uniformly dispersed particles.
一方、スラリーを上下のスラリー供給口であり、第１及び第２のスラリー供給口に相当する下部スラリー供給口１３及び上部スラリー供給口１４から供給する装置構成も本発明を効果的に実施するための装置である。スラリーを上下から供給することで、装置の高さを大きくすることで、大型の装置を製造できる利点がある。スラリー供給口が上下双方に存在する場合は、スラリーの上下方向に流れの中立点が円筒容器中央になるため、一方向からのスラリー供給に対して、約２倍の高さにできる利点がある。なお、スラリー流れを整えるためや製作を容易にするために、上部円板１０と下部円板１１の間に、中間円板を設置することもある。また、当該中間円板が開口部を有する場合もある。 On the other hand, an apparatus configuration that supplies the slurry from the upper and lower slurry supply ports from the lower slurry supply port 13 and the upper slurry supply port 14 corresponding to the first and second slurry supply ports also effectively implements the present invention. It is a device. By supplying the slurry from above and below, there is an advantage that a large apparatus can be manufactured by increasing the height of the apparatus. When the slurry supply ports exist on both the upper and lower sides, since the neutral point of the flow in the vertical direction of the slurry is in the center of the cylindrical container, there is an advantage that it can be about twice as high as the slurry supply from one direction. . An intermediate disk may be installed between the upper disk 10 and the lower disk 11 in order to adjust the slurry flow and facilitate the production. The intermediate disk may have an opening.
上下双方からスラリーを供給する装置においては、L／Dを請求項１の２倍である最大３．２にすることが可能である。スラリー流れが上下対称であり、ビーズ分離はスラリー供給口が１つの場合と同じか良好になるため、同じL／Dの最小値でよい。従って、L／Dの最小値は０．３にすることが可能である。 In the apparatus for supplying the slurry from both the upper and lower sides, the L / D can be set to 3.2 at maximum, which is twice that of the first aspect. Since the slurry flow is vertically symmetric and the bead separation is the same or better as in the case of one slurry supply port, the same minimum L / D value is sufficient. Therefore, the minimum value of L / D can be set to 0.3.
仕切板９が直径方向に短すぎると、ビーズ分離性能が悪化する。これは、仕切り板９によって、円筒容器の内側に、ビーズを送る機能が低下するからである。また仕切り板９が長すぎると、中空シャフト７での流れが屈曲してしまい、流量を増加させようとすると、圧力が過大となる問題がある。したがって、仕切板９の内周端が位置する円周の径が、仕切板９の外周端が位置する円周の径の５０〜８５％であると良く、更に望ましくは、５０〜７０％が良い。 If the partition plate 9 is too short in the diameter direction, the bead separation performance is deteriorated. This is because the function of sending beads to the inside of the cylindrical container is lowered by the partition plate 9. On the other hand, if the partition plate 9 is too long, the flow in the hollow shaft 7 is bent, and there is a problem that the pressure becomes excessive when the flow rate is increased. Therefore, the diameter of the circumference where the inner peripheral end of the partition plate 9 is located is preferably 50 to 85% of the diameter of the circumference where the outer peripheral end of the partition plate 9 is located, and more preferably 50 to 70%. good.
回転子８を構成する仕切板９は図３に示すように、軸心を通る半径となす角αが５〜３０度であることがよい。これは、角αを適正にすることで、回転によるスラリーの回転子８の内側への流れを適正にするためであり、適正な角度であれば、スラリーの回転子８の内部への流れが回転子８の高さ方向で均一化される。この結果、下部での回転子８内部へのスラリー流れが多すぎることによる円筒体２上方でのスラリー流れの減少の防止や、その逆の現象を防止できる。 As shown in FIG. 3, the partition plate 9 constituting the rotor 8 may have an angle α of 5 to 30 degrees with a radius passing through the axis. This is to make the flow of slurry into the rotor 8 by rotation appropriate by making the angle α appropriate, and if the angle is appropriate, the flow of slurry into the rotor 8 is made. It is made uniform in the height direction of the rotor 8. As a result, it is possible to prevent a decrease in the slurry flow above the cylindrical body 2 due to an excessive amount of the slurry flow into the rotor 8 at the lower portion and vice versa.
仕切板９の間隔は本発明で重要な要件である。仕切板の内周端での仕切板間隔ギャップをＧ１とし、外周端での仕切り板間隔ギャップをＧ２とすれば、Ｇ１は１〜７ｍｍ、Ｇ２は１．５〜１０ｍｍが良い。また、Ｇ２はビーズ径の２０倍から１００倍の範囲であると更に良い。また仕切板外周端と容器内周面との間隔ｔは３〜３０ｍｍが良い。前述する仕切板９の総数ｎは多いほどビーズの分離性能が向上し、５００mPa・s以上の高粘度対応が可能となっており、この場合、Ｇ１は１〜５ｍｍ、Ｇ２は１．５〜７ｍｍが良い。 The interval between the partition plates 9 is an important requirement in the present invention. The partition plate spacing gap at the inner peripheral end of the partition plate and G 1, when the partition plate spacing gap at the outer peripheral edge and G 2, G 1 is 1 to 7 mm, G 2 is better 1.5 to 10 mm. Also, G 2 is even better if in the range of 100 times 20 times the bead diameter. The interval t between the outer peripheral edge of the partition plate and the inner peripheral surface of the container is preferably 3 to 30 mm. As the total number n of the partition plates 9 described above increases, the separation performance of the beads improves, and it is possible to cope with a high viscosity of 500 mPa · s or more. In this case, G 1 is 1 to 5 mm, and G 2 is 1.5. ~ 7mm is good.
仕切板９の間の間隔ギャップ比率もビーズ漏れに重要な設計要件である。間隔ギャップ比率をあらわす指標として、次の値を使い説明する。内周端が位置する円周上の径をＤ１、外周端が位置する円周上の径をＤ２、径がＤ１をなす内周上での仕切板内周端のギャップをＧ１、径がＤ２をなす円周上での仕切板外周端のギャップをＧ２とし、また仕切板９の総数をｎとすると、内周端の仕切板間隔ギャップの総和と内周端の円周長との比率は、ｎＧ１／πＤ１となり、仕切板外周端での比率は、ｎＧ２／πＤ２となる。 The gap gap ratio between the partition plates 9 is also an important design requirement for bead leakage. The following values will be used as an index for expressing the gap gap ratio. The diameter on the circumference where the inner peripheral end is located is D 1 , the diameter on the circumference where the outer peripheral end is located is D 2 , and the gap between the inner peripheral ends of the partition plate on the inner circumference where the diameter is D 1 is G 1. , Where G 2 is the gap at the outer periphery of the partition plate on the circumference having a diameter D 2 , and n is the total number of partition plates 9 and n is the circle at the inner periphery, where n is the total number of partition plates 9. The ratio with the circumference is nG 1 / πD 1 , and the ratio at the outer peripheral edge of the partition plate is nG 2 / πD 2 .
本発明を効率的に実施するためには、前出の内周端と外周端での仕切板間隔ギャップの円周長に対する比率が適正である条件の場合、仕切板ギャップ間隔のテーパー率も重要であることから、外周端と内周端の仕切板ギャップ間隔の比率も適正な範囲、１．２≦Ｇ２／Ｇ１≦３とすると更に良い。仕切板９の間隔ギャップが内周側に過剰に狭くなっている場合、円筒体２と仕切板９の間にのみビーズが存在し、破砕の度合いが大きくなりすぎ、またの比率が過剰に小さいと、間隔ギャップ内のスラリー流速が一定となり、より内部までビーズが入り込む結果、ビーズ分離率が低下する。０．１５≦ｎＧ１／πＤ１≦０．６とし、かつ０．２≦ｎＧ２／πＤ２≦０．８とする。つまり、内周端での仕切板間隔ギャップの比率を１５〜６０％、かつ外周端での仕切板間隔ギャップの比率を２０〜８０％とすることで、円筒体２と回転子８の仕切板９との間でのビーズによる粒子の分散・粉砕と回転子８内部へのスラリーの流入量の両者を適正なバランスとすることができる。この結果、ビーズ漏れがなく、適正な分散・粉砕処理ができる。 In order to efficiently carry out the present invention, the taper ratio of the partition plate gap interval is also important when the ratio of the partition plate gap gap to the circumferential length at the inner peripheral end and the outer peripheral end is appropriate. Therefore, it is more preferable that the ratio of the gap between the outer peripheral end and the inner peripheral end of the partition plate gap is in an appropriate range, 1.2 ≦ G 2 / G 1 ≦ 3. When the gap of the partition plate 9 is excessively narrow on the inner peripheral side, beads are present only between the cylindrical body 2 and the partition plate 9, the degree of crushing becomes too large, and the ratio is too small. As a result, the slurry flow rate in the gap is constant, and as a result of the beads getting into the interior, the bead separation rate decreases. 0.15 ≦ nG 1 / πD 1 ≦ 0.6 and 0.2 ≦ nG 2 / πD 2 ≦ 0.8. That is, the ratio of the partition plate gap gap at the inner peripheral end is 15 to 60%, and the ratio of the partition plate gap gap at the outer peripheral end is 20 to 80%. Thus, both the dispersion and pulverization of the particles by the bead 9 and the amount of the slurry flowing into the rotor 8 can be properly balanced. As a result, there is no bead leakage and proper dispersion and pulverization can be performed.
当該円筒容器の下蓋４中央には、下部スラリー供給口１３又は上部スラリー供給口１４が設けられ、溶媒中に粒子を混入した原料スラリーはポンプ圧により下部スラリー供給口１３又は上部スラリー供給口１４より当該円筒容器内に供給されるが、当該円筒容器に供給するのに先立って例えば撹拌機、ホモジナイザー等を用いてスラリーを予備混合しておくのが望ましい。また、下部スラリー供給口１３又は上部スラリー供給口１４の両方から、原料スラリーを供給する場合もある。 A lower slurry supply port 13 or an upper slurry supply port 14 is provided at the center of the lower lid 4 of the cylindrical container, and the raw slurry in which particles are mixed in the solvent is supplied to the lower slurry supply port 13 or the upper slurry supply port 14 by a pump pressure. More preferably, the slurry is preliminarily mixed using, for example, a stirrer, a homogenizer, or the like before being supplied to the cylindrical container. Further, the raw material slurry may be supplied from both the lower slurry supply port 13 or the upper slurry supply port 14.
下部スラリー供給口１３又は上部スラリー供給口１４より当該円筒容器内に供給された原料スラリーは、当該円筒容器内に充填のビーズと回転子８の回転により撹拌混合され、凝集した粒子がほぐされて分散し、遠心力の作用により分離部としての仕切板９外周端より粒子を分離したスラリーが仕切板９間のスラリー経路を経て内周側に移動し、中空シャフト７に形成の開口より中空シャフト７の中空部を通り上方に抜けて排出され、製品スラリーとして回収されるか、或いは再度、供給口１３に送られ、当該円筒容器内のビーズと撹拌混合される。 The raw material slurry supplied into the cylindrical container from the lower slurry supply port 13 or the upper slurry supply port 14 is agitated and mixed in the cylindrical container by the rotation of the filled beads and the rotor 8, and the aggregated particles are loosened. The slurry that has been dispersed and separated from the outer peripheral end of the partition plate 9 as a separation portion by the action of centrifugal force moves to the inner peripheral side through the slurry path between the partition plates 9, and the hollow shaft 7 has an opening formed in the hollow shaft 7. 7 passes through the hollow part 7 and is discharged and collected as product slurry, or sent to the supply port 13 again and stirred and mixed with the beads in the cylindrical container.
なお、当該円筒容器内へのビーズの供給は、上蓋３を取り外した状態の当該円筒容器に上方より供給するか、或いは図示していないが、上蓋３にビーズ供給口を設け、当該供給口を通して行うこともできる。 The beads are supplied into the cylindrical container from above with the cylindrical container with the upper lid 3 removed, or although not shown, the upper lid 3 is provided with a bead supply port, It can also be done.
本装置の運転は以下のような条件で行うのが望ましい。仕切板９外周端の周速も重要な処理条件である。適正な運転条件は、仕切板９の外周端の周速が3〜30ｍ／秒であり、遠心力が8,000m/s2以下である。遠心力は小さいと、ビーズ分離性能が低下するが、1次粒子へのダメージが小さくなる。逆に遠心力が大きいと、ビーズ分離性能は向上するが、1次粒子へのダメージが大きくなる。特に500mPa・s以上の高粘性スラリーの場合は、仕切板９外周端の周速は５〜２５ｍ／秒が良く、遠心力は8,000m/s2以下が良い。遠心力が弱すぎると、ビーズもれがおきるため、望ましくは、800〜8,000 m/s2が良い。なお、ここで遠心力は仕切板９の外周端周速ｖ、仕切板９の外周端の直径Ｄから、G＝2v2/D（m/s2）で計算される値である。 It is desirable to operate this device under the following conditions. The peripheral speed of the outer peripheral edge of the partition plate 9 is also an important processing condition. Appropriate operating conditions are that the peripheral speed of the outer peripheral edge of the partition plate 9 is 3 to 30 m / sec, and the centrifugal force is 8,000 m / s 2 or less. If the centrifugal force is small, the bead separation performance is reduced, but damage to the primary particles is reduced. Conversely, when the centrifugal force is large, the bead separation performance is improved, but the damage to the primary particles is increased. In particular, in the case of a highly viscous slurry of 500 mPa · s or more, the peripheral speed of the outer peripheral end of the partition plate 9 is preferably 5 to 25 m / second , and the centrifugal force is preferably 8,000 m / s 2 or less. If the centrifugal force is too weak, bead leakage occurs, so 800 to 8,000 m / s 2 is desirable. Here, the centrifugal force is a value calculated by G = 2v 2 / D (m / s 2 ) from the outer peripheral end peripheral speed v of the partition plate 9 and the diameter D of the outer peripheral end of the partition plate 9.
仕切板９外周と円筒体２が形成する空間でのスラリーに作用するシェア（せん断力）も重要な処理条件である。本発明では円筒体２と仕切板９外周端が形成する空隙中のシェア率（ｓ）を、仕切板９外周端の周速ｖ（ｍ／秒）、仕切板９外周端と円筒体２との間隔ｔ（ｍ）から計算し、これを用いてS＝ｖ／ｔと計算した場合、Sが1000〜8000（1/s）の条件で運転する。シェア率Sが低いと分散が低下する問題があり、高いと一次粒子へのダメージが大きくなる。 The shear (shearing force) acting on the slurry in the space formed by the outer periphery of the partition plate 9 and the cylindrical body 2 is also an important processing condition. In the present invention, the shear rate (s) in the gap formed by the cylindrical body 2 and the outer peripheral edge of the partition plate 9 is expressed by the peripheral speed v (m / second) of the outer peripheral edge of the partition plate 9, the outer peripheral edge of the partition plate 9 and the cylindrical body 2. When the calculation is made from the interval t (m) and S = v / t is calculated using this, the operation is performed under the condition that S is 1000 to 8000 (1 / s). If the share rate S is low, there is a problem that the dispersion decreases, and if it is high, damage to the primary particles increases.
本装置で使用されるビーズは、一般的には、酸化物粒子、金属粒子などであり、具体的には、ジルコニア、チタニア、ガラス、アルミナ、ジルコン、ステンレススチールなどが用いられ、その比重は原料スラリーより大であれば良く、スラリー比重の２倍以上のものであると更に良い。こうしたビーズは、０．０１〜１ｍｍφ程度の粒子径のものが用いられ、その形状は球状のものが望ましい。スラリー溶媒としては、水、アルコール系有機物、トルエン、アセトン、グリコール類、高粘性のペーストなどが用いられ、処理効率を上げるために分散剤を用いることがある。スラリー粘度は最大3,000mPa・sまで対応できる。本実施形態で対象となるスラリーの粒子は、酸化チタン粉やチタン酸バリウムなどの酸化物、銀やニッケルなどの金属微粒子、微細炭素繊維等である。 The beads used in this apparatus are generally oxide particles, metal particles, etc., and specifically, zirconia, titania, glass, alumina, zircon, stainless steel, etc. are used, and the specific gravity is the raw material. It is sufficient if it is larger than the slurry, and it is even better if it is twice or more the slurry specific gravity. Such beads have a particle diameter of about 0.01 to 1 mmφ, and are preferably spherical. As the slurry solvent, water, alcohol-based organic substances, toluene, acetone, glycols, high-viscosity paste, or the like is used, and a dispersant may be used to increase the processing efficiency. The slurry viscosity can be up to 3,000 mPa · s. The target particles of the slurry in the present embodiment are oxides such as titanium oxide powder and barium titanate, metal fine particles such as silver and nickel, and fine carbon fibers.
図１に記載されるミルを用いた。本装置の主なディメンジョンは、スラリー供給口が１である装置においては、Dが100mm、Lが15mmから226mm、Ｌ／Ｄは0.15〜2.26であった。２つのスラリー供給口ある装置では、Dが100mm、Lが35mmから320mmであった。仕切板９の構成は、間隔については、G１で2〜4mm、G２で3〜6mmであり、外周径D2はDと同じで、D1はD2に対して表１に記載されている比率のものであり、また角度αは５から３０度であった。また、スラリー供給口が２である装置では、Dが100mm、Lが30mmから280mmであり、他の寸法等は、前記の装置と同等であった。比較例として、遠心式ビーズ分離装置と８本の攪拌ピンを持つLが100mmであり、Dが40mmである従来型のビーズミルでの実験結果を示す。原料スラリーは、チタン酸バリウムであり、一次粒子300nm、二次粒子径100μｍのもので、スラリー濃度１０％として処理を行った。スラリー粘度は30mPa・sであった。粉砕・分散用のビーズは、50μmのジルコニアであった。 The mill described in FIG. 1 was used. As for the main dimensions of this apparatus, in an apparatus having a slurry supply port of 1, D was 100 mm, L was 15 mm to 226 mm, and L / D was 0.15 to 2.26. In an apparatus having two slurry supply ports, D was 100 mm and L was 35 mm to 320 mm. The configuration of the partition plate 9 is 2 to 4 mm for G 1 and 3 to 6 mm for G 2 , the outer diameter D2 is the same as D, and D1 is a ratio described in Table 1 with respect to D2. The angle α was 5 to 30 degrees. In the apparatus having the slurry supply port of 2, D is 100 mm, L is 30 mm to 280 mm, and other dimensions are the same as those of the apparatus. As a comparative example, an experimental result in a conventional bead mill in which L having a centrifugal bead separation device and 8 stirring pins is 100 mm and D is 40 mm is shown. The raw material slurry was barium titanate, which had a primary particle size of 300 nm and a secondary particle size of 100 μm, and was processed at a slurry concentration of 10%. The slurry viscosity was 30 mPa · s. The beads for pulverization / dispersion were 50 μm zirconia.
本装置を起動した後、所定の処理時間ごとにミルの排出口からサンプルを採取した。粒子径測定には、株式会社堀場製作所製のレーザー回折・散乱式粒度測定器LA-950を使用した。又１次粒子破壊判定を行うための比表面積測定をmicrometrics社製のFlowSorbII2300を用いてBET一点法にて計測した。 After starting this device, samples were taken from the outlet of the mill every predetermined processing time. For the particle size measurement, a laser diffraction / scattering particle size measuring instrument LA-950 manufactured by HORIBA, Ltd. was used. Moreover, the specific surface area measurement for performing the primary particle fracture determination was measured by the BET single point method using FlowSorbII2300 manufactured by micrometrics.
処理結果を評価するために採用した値は、比較例と実施例１から４及び６から１０では滞留時間が１分４０秒、また実施例５では3分での処理後の処理成績である。評価指標は、二次粒子の平均粒子径（D50：５０％の二次粒子がこのサイズ以下である粒子径）と二次粒子を平均０．３μmまで分散させた際の比表面積を用いた。前者の値では、分散性能を評価する。この値は小さいほど分散性能は良い。後者の値では、一次粒子の破壊度合いを評価する。粒子破壊が起きると、同じ平均二次粒子径であっても、比表面積が大きくなり、一次粒子を破壊したくない場合は、この値が小さいほど良い。 The values adopted for evaluating the treatment results are the treatment results after treatment in the comparative example and Examples 1 to 4 and 6 to 10 after a residence time of 1 minute and 40 seconds, and in Example 5 after 3 minutes. The evaluation index used was the average particle size of secondary particles (D50: particle size in which 50% of secondary particles are less than this size) and the specific surface area when secondary particles were dispersed to an average of 0.3 μm. The former value evaluates the dispersion performance. The smaller this value, the better the dispersion performance. With the latter value, the degree of destruction of primary particles is evaluated. When particle breakage occurs, even if the average secondary particle diameter is the same, the specific surface area becomes large, and if it is not desired to break the primary particles, a smaller value is better.
実施例と比較例を以下の表１に示す。まず、比較例１は従来型の攪拌ローターとビーズセパレーターから構成されるビーズミルのテスト機で処理した例である。この装置の円筒容器は本装置と同一なものを使用したが、回転体は下部に攪拌ロッドがあり、上部にセパレータがあるものを用いた。この結果で、分散性能は良好であるものの、一次粒子破壊が進んでおり、粒子破壊を低減したい処理には不適切であった。 Examples and comparative examples are shown in Table 1 below. First, Comparative Example 1 is an example in which processing was performed with a bead mill tester composed of a conventional stirring rotor and a bead separator. The cylindrical container of this device was the same as that of this device, but the rotating body used was a stirring rod at the bottom and a separator at the top. As a result, although the dispersion performance was good, the primary particle breakage progressed, and it was unsuitable for the treatment for reducing the particle breakage.
表１の実施例は、いずれも本発明の装置用件を満たしたものであり、Ｌ／Ｄは請求項１に係る発明の範囲内で、Ｄ1／Ｄ２、Ｇ ２ ／Ｇ 1 も請求項２及び３に係る発明の範囲である。実施例１から７は、スラリー供給口が１つである装置での例であり、実施例９から１１はスラリー供給口が２つである装置の例である。実施例を解析すると、分散性能については、二次粒子径（D50）が０．４マイクロメートル以下と、良好な分散能力が得られた。一方、比較例２では、Ｌ／Ｄが０．１５と小さいため、０．４６マイクロメートルと分散性能が悪かった。回転子の仕切板外周の周速１２m/sのものの処理結果をＬ／Ｄで整理して、図４にプロットした。このグラフで分るように、Ｌ／Ｄが０．３以下では、急速に分散性能が悪化していた。
All of the examples in Table 1 satisfy the requirements for the apparatus of the present invention, L / D is within the scope of the invention according to claim 1, and D 1 / D 2 and G 2 / G 1 are also claimed. This is the scope of the invention according to Items 2 and 3. Examples 1 to 7 are examples of an apparatus having one slurry supply port, and Examples 9 to 11 are examples of an apparatus having two slurry supply ports. When the examples were analyzed, as for the dispersion performance, the secondary particle diameter (D50) was 0.4 micrometers or less, and a good dispersion ability was obtained. On the other hand, in Comparative Example 2, since the L / D was as small as 0.15, the dispersion performance was 0.46 micrometers, which was poor. The results of processing of the rotor outer peripheral plate with a peripheral speed of 12 m / s were arranged in L / D and plotted in FIG. As can be seen from this graph, when L / D was 0.3 or less, the dispersion performance deteriorated rapidly.
粒子破壊低減の評価結果については、実施例１〜５及び７では、比表面積が７m2/g以下であり、粒子破壊は少ない結果となった。比較例３では、Ｌ／Ｄが２．２６と大きいため、比表面積が８．８m2/gとなり、粒子破壊が進んでいることが判明した。なお、比較例２では所定時間内に平均二次粒子径が３マイクロメートル以下にならなかったので、比表面積の評価はできなかった。L/Dが2.26である比較例３においては、比表面積が回転子の仕切板外周の周速１２m/sのものの処理結果をＬ／Ｄに整理して、図５にプロットした。Ｌ／Ｄは１．６を超えると粒子の比表面積が急に増加しており、粒子破壊が進みやすいことが判明した。したがって、分散性能と一次粒子破壊低減の両方が良好な条件は、Ｌ／Ｄが０．３〜１．６の範囲であった。また、Ｄ1／Ｄ２、Ｇ ２ ／Ｇ 1 も適正な範囲であると更に処理成績がよかった。
As for the evaluation results of particle breakage reduction, in Examples 1 to 5 and 7, the specific surface area was 7 m 2 / g or less, and the particle breakage was small. In Comparative Example 3, since L / D was as large as 2.26, the specific surface area was 8.8 m 2 / g, and it was found that particle destruction was progressing. In Comparative Example 2, since the average secondary particle diameter did not become 3 micrometers or less within a predetermined time, the specific surface area could not be evaluated. In Comparative Example 3 where L / D is 2.26, the treatment results for the specific surface area with a peripheral speed of 12 m / s on the outer periphery of the rotor partition plate are arranged in L / D and plotted in FIG. When L / D exceeded 1.6, the specific surface area of the particles increased rapidly, and it was found that the particle breakage easily progressed. Therefore, L / D was in the range of 0.3 to 1.6 under conditions that both the dispersion performance and the primary particle breakage reduction were good. Further, the processing results were better when D 1 / D 2 and G 2 / G 1 were also in the proper ranges.
同じ実施例の中でも、処理条件の影響もあることが判明した。表１に記載のように、遠心力が所定の範囲であるものと、シェア率が所定の範囲であるものでは、特に処理成績が良かった。一方、遠心力が強すぎる実施例である実施例６では比表面積が若干大きく、粒子破壊がやや進んでいた。遠心力の弱い実施例５では、ビーズ漏れが微少であるが、発生しており、また実施例７では、仕切り板９が短く、D1/D2が0.85でるため、微少なビーズ漏れが発生していたが、いずれも処理上の問題はなかった。 Even in the same example, it has been found that there is an influence of processing conditions. As shown in Table 1, the processing results were particularly good when the centrifugal force was within a predetermined range and when the shear rate was within the predetermined range. On the other hand, in Example 6, which is an example in which the centrifugal force is too strong, the specific surface area is slightly large, and the particle breakage is slightly advanced. In Example 5 where the centrifugal force is weak, the bead leakage is small but has occurred, and in Example 7, the partition plate 9 is short and D1 / D2 is 0.85, so a slight bead leakage occurs. However, there were no processing problems.
実施例８から１０は、スラリーを上下二方向から供給した装置の実施例であり、L／Dが０．３５、１．６、及び３．２で効果的な処理ができていた。 Examples 8 to 10 are examples of the apparatus in which the slurry was supplied from two directions, and the L / D was 0.35, 1.6, and 3.2, and an effective treatment was achieved.
本発明の撹拌ミルおよびスラリー中粒子の分散方法は、微細な粒子を含むスラリーに適用される。スラリーは、炭素粉、セラミック粉、有機物粉などであり、例えばセラミック顔料、インキ、塗料、誘電体原料、磁性体原料、医薬品向け材料、食品向け材料、微細金属粉原料の粒子の分散と粉砕に適している。 The stirring mill and the method for dispersing particles in the slurry of the present invention are applied to a slurry containing fine particles. The slurry is carbon powder, ceramic powder, organic powder, etc., for example, for dispersing and crushing particles of ceramic pigment, ink, paint, dielectric material, magnetic material, pharmaceutical material, food material, fine metal powder material Is suitable.
１‥‥撹拌ミル
２‥‥円筒体
３‥‥上蓋
４‥‥下蓋
５‥‥冷却水路
６‥‥シャフト
７‥‥中空シャフト
８‥‥回転子
９‥‥仕切板
１０‥上部円板
１１‥下部円板
１２‥貫通孔
１３‥下部スラリー供給口
１４‥上部スラリー供給口
DESCRIPTION OF SYMBOLS 1 ... Stirring mill 2 ... Cylindrical body 3 ... Upper lid 4 ... Lower lid 5 ... Cooling water channel 6 ... Shaft 7 ... Hollow shaft 8 ... Rotor 9 ... Partition plate 10 ... Upper disc 11 ... Lower disk 12 ... Through hole 13 ... Lower slurry supply port 14 ... Upper slurry supply port
Claims (7)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2016014168 | 2016-01-28 | ||
| JP2016014168 | 2016-01-28 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2017136586A JP2017136586A (en) | 2017-08-10 |
| JP6423988B2 true JP6423988B2 (en) | 2018-11-14 |
Family
ID=59564499
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2017009971A Active JP6423988B2 (en) | 2016-01-28 | 2017-01-24 | Stirring mill and dispersion method of particles in slurry |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP6423988B2 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109600995A (en) * | 2017-08-02 | 2019-04-09 | 广岛金属与机械株式会社 | The dispersing method and emulsion making process of particle in dispersion machine and slurry |
| IT201800009329A1 (en) | 2018-10-10 | 2020-04-10 | Three Es Srl | Cavitation reactor |
| JP7429039B2 (en) | 2019-04-26 | 2024-02-07 | 株式会社広島メタル＆マシナリー | wet bead mill |
| CN113967981A (en) * | 2021-09-26 | 2022-01-25 | 瞿凯 | Rubber mixing roll |
| JP7408049B1 (en) | 2022-11-11 | 2024-01-05 | 昇 望月 | Stirring blade, stirring method, stirring blade assembly method |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3938171C1 (en) * | 1988-12-30 | 1991-01-03 | Erich Netzsch Gmbh & Co Holding Kg, 8672 Selb, De | |
| JP2003144950A (en) * | 2001-11-09 | 2003-05-20 | Mitsui Mining Co Ltd | Pulverizer |
| JP4741931B2 (en) * | 2005-05-17 | 2011-08-10 | アシザワ・ファインテック株式会社 | Circulation type media stirring mill |
| EP1971439A2 (en) * | 2005-06-08 | 2008-09-24 | Cheshire Dispersion Company Limited | Milling apparatus |
| JP2007229686A (en) * | 2006-03-03 | 2007-09-13 | Mitsui Mining Co Ltd | Media agitation type wet disperser and fine particle dispersion method |
| JP4918272B2 (en) * | 2006-04-11 | 2012-04-18 | アシザワ・ファインテック株式会社 | Circulation type media stirring mill |
| JP5658439B2 (en) * | 2009-05-19 | 2015-01-28 | 花王株式会社 | How to start the beads mill |
| EP2737955B1 (en) * | 2011-07-28 | 2016-07-20 | Ashizawa Finetech Ltd | Medium-stirring pulverizer |
| JP3203625U (en) * | 2016-01-28 | 2016-04-07 | 寿工業株式会社 | Stirring mill |
-
2017
- 2017-01-24 JP JP2017009971A patent/JP6423988B2/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| JP2017136586A (en) | 2017-08-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6423988B2 (en) | Stirring mill and dispersion method of particles in slurry | |
| KR102501892B1 (en) | Agitator ball mill | |
| JP4918226B2 (en) | Media agitation type wet crusher | |
| JP3222139U (en) | Beads mill | |
| KR101310130B1 (en) | Grinding and dispersing apparatus for processing of minute particle of materials | |
| WO2013015237A1 (en) | Medium-stirring pulverizer | |
| JP2006212489A (en) | Grinding method using medium stirring type grinder | |
| JP4886993B2 (en) | Media stirring type wet disperser | |
| JP2017131807A (en) | Disperser, dispersion treatment method, and emulsion manufacturing method | |
| KR20150122228A (en) | Medium stirring type pulverizer | |
| JP5046557B2 (en) | Media stirring type wet disperser and fine particle dispersion method | |
| WO2019026208A1 (en) | Dispersing machine, method for dispersing particles in slurry and emulsion production method | |
| JP2013039508A (en) | Medium stirring type crusher | |
| JP3203625U (en) | Stirring mill | |
| KR101245869B1 (en) | Media-Agitating Wet Pulverizer | |
| JP3209743U (en) | Stirring mill | |
| JP3217671U (en) | Bead mill | |
| JP2008055288A (en) | Media agitation type wet dispersion machine and dispersion process of fine particle | |
| JP7429039B2 (en) | wet bead mill | |
| CN107735182B (en) | Medium circulation type pulverizer | |
| JP2005169340A (en) | Horizontal wet type medium agitating dispersion grinder | |
| TWI755413B (en) | Dispersing machine and method for dispersing particles in slurry and method for producing emulsification | |
| KR101691151B1 (en) | Wet type grinding and dispersing apparatus having preventer of beads flowing | |
| JP2005125192A (en) | Separator and crusher | |
| JP2001190974A (en) | Cracking filter device for powder dispersing machine |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20170713 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20180305 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20180320 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20180501 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20180807 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20180830 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20181016 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20181020 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 6423988 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |