JPH0459255A - Uniform liquid drop-forming method - Google Patents
Uniform liquid drop-forming methodInfo
- Publication number
- JPH0459255A JPH0459255A JP17176390A JP17176390A JPH0459255A JP H0459255 A JPH0459255 A JP H0459255A JP 17176390 A JP17176390 A JP 17176390A JP 17176390 A JP17176390 A JP 17176390A JP H0459255 A JPH0459255 A JP H0459255A
- Authority
- JP
- Japan
- Prior art keywords
- nozzle
- droplets
- electrode
- voltage
- hole
- 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.)
- Granted
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000002612 dispersion medium Substances 0.000 claims abstract description 49
- 230000001360 synchronised effect Effects 0.000 claims abstract description 11
- 230000005684 electric field Effects 0.000 abstract description 20
- 230000000694 effects Effects 0.000 abstract description 11
- 238000005260 corrosion Methods 0.000 abstract description 8
- 230000007797 corrosion Effects 0.000 abstract description 8
- 230000035515 penetration Effects 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 22
- 239000000178 monomer Substances 0.000 description 17
- 239000006185 dispersion Substances 0.000 description 16
- 239000002904 solvent Substances 0.000 description 14
- 239000002245 particle Substances 0.000 description 13
- 239000000243 solution Substances 0.000 description 13
- 229920000642 polymer Polymers 0.000 description 12
- 238000007796 conventional method Methods 0.000 description 9
- 239000003350 kerosene Substances 0.000 description 8
- 230000002209 hydrophobic effect Effects 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 6
- 229920002554 vinyl polymer Polymers 0.000 description 6
- 238000004581 coalescence Methods 0.000 description 5
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- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 4
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- 239000010935 stainless steel Substances 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
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- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
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- 150000001298 alcohols Chemical class 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
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- CMCBDXRRFKYBDG-UHFFFAOYSA-N 1-dodecoxydodecane Chemical compound CCCCCCCCCCCCOCCCCCCCCCCCC CMCBDXRRFKYBDG-UHFFFAOYSA-N 0.000 description 1
- RZRNAYUHWVFMIP-KTKRTIGZSA-N 1-oleoylglycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-KTKRTIGZSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
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- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
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- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- CQRQNIOKOWFIGF-UHFFFAOYSA-N C=CC1=CC=CC=C1C=C.O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 Chemical compound C=CC1=CC=CC=C1C=C.O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 CQRQNIOKOWFIGF-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Particle Formation And Scattering Control In Inkjet Printers (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、均一で微小な径を有する液滴の形成方法に関
す・る。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for forming droplets having a uniform and minute diameter.
［従来の技術］
高分子物質の溶液やビニル重合性上ツマー溶液を均一で
微小な液滴とし、この液滴をゲル化あるいは重合させて
えられる均一で微小な径を有する粒子は、機能性吸着剤
や担体として極めて有用なものである。[Prior art] A solution of a polymeric substance or a vinyl polymerizable supernatant solution is made into uniform and minute droplets, and the particles with a uniform and minute diameter obtained by gelling or polymerizing the droplets have functional properties. It is extremely useful as an adsorbent or carrier.
こうした均一で微小な液滴の形成方法としては、従来よ
り、機械的に一定周期の振動を加える方法（以下、機械
式という）、または交流電圧を印加する方法（以下、電
気式という）が知られている。Conventionally, methods for forming such uniform, minute droplets include a method of applying mechanical vibrations at a constant frequency (hereinafter referred to as the "mechanical method") or a method of applying an alternating current voltage (hereinafter referred to as the "electric method"). It is being
機械式は、気体中あるいは分散媒中にノズルから液体を
液柱として噴出させる際、一定周期の機械的な振動を加
えて、この振動数と同期した均一な液滴を形成するもの
である（特開昭５７−１０２０９５号公報、特開昭８１
−８３２０２号公報）。しかし、この方法においては液
滴を小さくするためには振動数を大きくしなければなら
ないが、この大きな振動数と同期状態をうるためにはノ
ズル径を小さくしかつ噴出速度を大きくしなければなら
ない。ところが、分散媒中に噴出させる方法では噴出速
度を大きくすると分散媒との摩擦で液柱が破壊されてし
まい、一方、気体中に噴出する方法では気体中に長時間
浮遊するため液滴同士が合体してしまうという問題があ
り、前者ではせいぜい５００ａｍ、後者でも２００加ま
での液滴しか形成できない。In the mechanical method, when a liquid is ejected as a liquid column from a nozzle into a gas or a dispersion medium, a constant period of mechanical vibration is applied to form uniform droplets that are synchronized with this vibration frequency ( JP-A-57-102095, JP-A-81
-83202). However, in this method, the frequency must be increased in order to make the droplets smaller, but in order to achieve synchronization with this large frequency, the nozzle diameter must be reduced and the jetting speed must be increased. . However, in the method of jetting into the dispersion medium, if the jetting speed is increased, the liquid column will be destroyed by friction with the dispersion medium, while in the method of jetting into the gas, the droplets will remain suspended in the gas for a long time, causing the droplets to break up with each other. There is a problem of coalescence, and the former can only form droplets with a diameter of at most 500 am, while the latter can only form droplets with a diameter of up to 200 am.
電気式は、分散媒中に設置したノズルと電極の間に一定
周期の高圧交流電圧を印加しながら液体をノズルから噴
出させることにより、交流周期と同期した数の液滴を分
散媒中に形成させる方法であり（特開昭５８−１７５８
６８号公報）、この電気式では、ノズルと電極の間に一
定周期で変化する電場を与え、その電場の変化により、
ノズルから分散媒中に噴出しだ液柱を切断するため、直
接、微小液滴の懸濁液をうろことができるほか、機械的
振動による環境問題もなく、また振動数の安定維持も容
易である。The electric type applies a high-voltage AC voltage with a constant cycle between the nozzle installed in the dispersion medium and the electrode, and jets the liquid from the nozzle, forming a number of droplets in the dispersion medium that are synchronized with the AC cycle. (Japanese Patent Laid-Open No. 58-1758)
In this electric method, an electric field that changes at a constant period is applied between the nozzle and the electrode, and due to the change in the electric field,
Since the liquid column ejected from the nozzle into the dispersion medium is cut, the suspension of minute droplets can be directly suspended, there are no environmental problems caused by mechanical vibration, and it is easy to maintain a stable vibration frequency. be.
［発明が解決しようとする課題］
このように電気式は数々の点で機械式よりも優れた方法
ではあるが、液柱の切断に必要な同期状態をうるために
はノズルの液体噴出孔を除いて電気的に絶縁しておく必
要があると共に高電圧を必要とする。そのためノズルの
絶縁被膜が破れたりノズルや電極に腐食が生じたりし、
均一な液滴を継続的に安定して製造することが困難であ
る。また、電気式においても機械式はどではないが、生
成した微小液滴が液滴生成域に残留しているため、液滴
同士の合体の防止が不充分となっている。さらに、電場
の変化を分散媒に反映させて液滴を生成するため、使用
できる分散媒の電気物性に厳しい制限がある。[Problem to be solved by the invention] As described above, the electric method is superior to the mechanical method in many respects, but in order to obtain the synchronized state necessary for cutting the liquid column, it is necessary to adjust the liquid jet hole of the nozzle. They must be electrically insulated from the outside, and require high voltage. As a result, the insulating coating on the nozzle may be torn or corrosion may occur on the nozzle or electrode.
It is difficult to consistently and stably produce uniform droplets. Further, even in the electric type, although not in the case of the mechanical type, since the generated minute droplets remain in the droplet generation area, it is insufficient to prevent the droplets from coalescing. Furthermore, since droplets are generated by reflecting changes in the electric field on the dispersion medium, there are severe limitations on the electrical properties of the dispersion medium that can be used.
本発明はこうした電気式の均一微小液滴の形成方法の問
題点を解消した方法に関するものであり、低電圧で合体
防止効果に優れ、かつ使用分散媒の制限が緩和された均
一な液滴の形成方法を提供するものである。The present invention relates to a method that solves the problems of the electric method for forming uniform micro droplets, and is a method for forming uniform droplets that uses low voltage, has an excellent coalescence prevention effect, and has relaxed restrictions on the dispersion medium used. A forming method is provided.
［課題を解決するための手段］
本発明の均一な液滴の形成方法は、分散媒中に、液体噴
出ノズルと該液体の通過孔を設けた電気的絶縁板と電極
とをこの順に配置し、ノズルと電極間に一定周期の電圧
を加えながらノズルから液体を噴出させることにより、
該電圧の周期と同期した数の均一な液滴を生成させる方
法である。[Means for Solving the Problems] The method for forming uniform droplets of the present invention includes disposing a liquid jet nozzle, an electrically insulating plate provided with passage holes for the liquid, and an electrode in this order in a dispersion medium. By ejecting liquid from the nozzle while applying a constant voltage between the nozzle and the electrode,
This is a method of generating uniform droplets in a number synchronized with the period of the voltage.
［作用］
本発明の方法を第１〜２図に基づいて説明する。第１図
は本発明の方法を実施するときに採用しうる分散装置の
一実施態様の概略縦断面図であり、第２図は第１図に示
す実施態様において形成される電界を説明するための概
略断面図である。[Operation] The method of the present invention will be explained based on FIGS. 1 and 2. FIG. 1 is a schematic longitudinal sectional view of an embodiment of a dispersion device that can be employed when carrying out the method of the present invention, and FIG. 2 is for explaining the electric field formed in the embodiment shown in FIG. FIG.
第１図に示す液滴形成用分散装置の実施態様のばあい、
外壁部分は電気的な絶縁体、たとえばポリテトラフルオ
ロエチレン、アクリル樹脂などで作製されている。液滴
（１）とする液体は導電性のノズル（２の噴出孔（３）
から分散媒（４）中へ噴出される。ノズル（′２Ｊの前
方には電気的絶縁板（５）がノズルと平行するように配
置されており、該絶縁板（５）の孔（６）はノズルの噴
出孔（３）と同軸する位置に設けられている。さらに絶
縁板（５）の後方には電極０１）が絶縁板（５）と平行
に配置されており、その中央部分に液滴などの通過孔■
が設けられている。そして、ノズル（２）と電極０１）
との間には電源０４１から交流電圧が印加されている。In the case of the embodiment of the dispersion device for forming droplets shown in FIG.
The outer wall portion is made of an electrical insulator such as polytetrafluoroethylene or acrylic resin. The liquid to be made into droplets (1) is passed through a conductive nozzle (spout hole (3) of 2).
is ejected into the dispersion medium (4). An electrically insulating plate (5) is placed in front of the nozzle ('2J) parallel to the nozzle, and the hole (6) of the insulating plate (5) is positioned coaxially with the jet hole (3) of the nozzle. Further, behind the insulating plate (5), an electrode 01) is arranged parallel to the insulating plate (5), and a hole for passing liquid droplets etc. is provided in the center of the electrode 01).
is provided. And nozzle (2) and electrode 01)
An alternating current voltage is applied from a power source 041 between the two.
本発明の方法によれば、均一な微小液滴を低電圧でかつ
液滴の合体を防止しながら形成することができる。According to the method of the present invention, uniform microdroplets can be formed at low voltage while preventing droplets from coalescing.
すなわち、孔（６）を設けた絶縁板（５）を電極口）と
ノズル（２との間に配置することにより、第２図に電気
力線で示すようにノズルと電極の間の電界が絶縁板（５
）の孔（６）で収束し、その部分の電界密度が大幅に高
くなる。その結果、孔（６）の付近ではノズルと電極間
に実際に印加した電圧が増幅された形となり、低電圧で
も従来法で高電圧を加えたときと同じ効果を奏する。こ
のことは、本発明の方法における液滴の生成が孔（６）
付近で生じていることからも明らかである。この電界収
束作用により印加電圧を従来の数百骨の１にまで下げる
ことができ、その結果、ノズルや電極の腐食を抑えるこ
とができる。In other words, by placing an insulating plate (5) with holes (6) between the electrode port) and the nozzle (2), the electric field between the nozzle and the electrode is increased as shown by the lines of electric force in Figure 2. Insulating board (5
) converges at the hole (6), and the electric field density at that part becomes significantly high. As a result, the voltage actually applied between the nozzle and the electrode is amplified in the vicinity of the hole (6), and even at a low voltage, the same effect as when applying a high voltage in the conventional method can be achieved. This means that the generation of droplets in the method of the present invention occurs at the hole (6).
This is clear from the fact that it is occurring nearby. Due to this electric field convergence effect, the applied voltage can be lowered to 1 compared to the conventional voltage of several hundred, and as a result, corrosion of the nozzle and electrode can be suppressed.
また液体および分散媒の通路は絶縁板（５）の孔（６）
のみであり（縮流作用）、孔（６）付近で生成した液滴
（１）はその付近に滞留することなく直ちにその流れに
乗って孔（６）から遠避けられる。したがって、生成し
た液滴同士が衝突して合体する確率は大幅に減る（合体
防止効果）。In addition, the liquid and dispersion medium passages are provided through holes (6) in the insulating plate (5).
(contraction effect), and the droplet (1) generated near the hole (6) does not stay in the vicinity but immediately rides on the flow and is far away from the hole (6). Therefore, the probability that the generated droplets collide with each other and coalesce is significantly reduced (coalescence prevention effect).
さらに、従来法では電気伝導度の大きな分散媒は使用で
きなかったのであるが、絶縁板（５）で分散媒を仕切っ
ているので、絶縁板以降の分散媒、すなわち液滴の生成
に関与しない分散媒については電気的性質による制限は
不要となり、合体防止に有効な分散媒の使用が可能とな
る。Furthermore, in the conventional method, a dispersion medium with high electrical conductivity could not be used, but since the dispersion medium is partitioned by an insulating plate (5), the dispersion medium after the insulating plate does not participate in the formation of droplets. The dispersion medium does not need to be restricted by electrical properties, and it becomes possible to use a dispersion medium that is effective in preventing coalescence.
以上に本発明の方法の基本的な態様および作用効果を述
べたが、その他の態様や作用効果は以下に示す実施例で
明らかにする。The basic aspects and effects of the method of the present invention have been described above, and other aspects and effects will be clarified in the Examples shown below.
［実施例］
本発明に好適に使用される液滴形成用の液体は、高分子
物質の溶液またはビニル重合性モノマーを含む液体であ
る。これらの液体を本発明の方法によって均一な液滴に
分散させたのち、液体が高分子物質の溶液のばあいには
加熱によりこの液滴中の溶剤を揮発させるか、冷却によ
ってゲル化させるか、もしくはこの分散液にゲル化促進
剤を添加することによって液滴を凝固させ、また液体が
ビニル重合性モノマーを含む液体のばあいにはそれを重
合させることによって、これらの液滴から均一な粒子径
をもった粒子かえられる。これらの粒子は優れた機能性
吸着剤や担体として有用である。[Example] The liquid for forming droplets preferably used in the present invention is a solution of a polymeric substance or a liquid containing a vinyl polymerizable monomer. After these liquids are dispersed into uniform droplets by the method of the present invention, if the liquid is a solution of a polymeric substance, the solvent in the droplets is evaporated by heating, or the solvent in the droplets is gelled by cooling. , or by adding a gelling promoter to this dispersion to solidify the droplets, or if the liquid contains a vinyl polymerizable monomer, polymerize it to obtain a homogeneous form from these droplets. Particles with a certain particle size can be changed. These particles are useful as excellent functional adsorbents and carriers.
まず、高分子物質の溶液を使用するばあいについてさら
に詳しく説明する。First, the case where a solution of a polymeric substance is used will be explained in more detail.
この高分子物質には、一般に溶剤に可溶な任意のものが
使用できるので、利用目的に適したものを選べばよい。Generally, any solvent-soluble polymer can be used as this polymeric substance, so it is sufficient to select one suitable for the purpose of use.
該高分子物質は、天然高分子物質であってもよく、合成
高分子物質であってもよい。The polymeric substance may be a natural polymeric substance or a synthetic polymeric substance.
天然高分子物質の例としては、たとえばセルロース、ア
ガロース、カラゲーナン、アルギン酸塩、絹フィブロイ
ン、コラーゲン、キチンなどの天然高分子物質やそれら
の誘導体があげられる。また、合成高分子物質としては
、たとえばポリビニルアルコール、ポリーγ−メチルー
Ｌ−グルタメート、メチルメタクリレート／ヒドロキシ
エチルメタクリレート共重合体などがあげられる。スチ
レン／ブタジェン共重合体、スチレン／クロルメチル化
スチレン共重合体のように架橋とイオン交換基を導入す
ることができるポリマーはイオン交換樹脂の母材として
も有用である。Examples of natural polymeric substances include natural polymeric substances such as cellulose, agarose, carrageenan, alginate, silk fibroin, collagen, and chitin, and derivatives thereof. Further, examples of synthetic polymer substances include polyvinyl alcohol, poly γ-methyl-L-glutamate, methyl methacrylate/hydroxyethyl methacrylate copolymer, and the like. Polymers into which crosslinking and ion exchange groups can be introduced, such as styrene/butadiene copolymers and styrene/chloromethylated styrene copolymers, are also useful as base materials for ion exchange resins.
これらの高分子物質は疎水性または親水性の溶剤に溶解
して本発明に使用される。該溶剤には、後述する分散媒
と非相溶性もしくは貧相溶性の液体が選ばれる。These polymeric substances are used in the present invention after being dissolved in a hydrophobic or hydrophilic solvent. A liquid that is incompatible or poorly compatible with the dispersion medium described below is selected as the solvent.
天然高分子物質およびその誘導体の溶剤は、高分子学会
高分子実験学編集委員会編、「天然高分子Ｊ （１９８
４）共立出版−発行、あるいはＳＡＭＵＥＬ Ｍ、ＨＵ
ＤＳＯＮ ａｎｄ ＪＯＨＮ Ａ、ＣＵＣＵＬＯ５Ｊｏ
ｕｎａｌｏｆ ｍａｃｒｏｓｏｌｅｃｕｌａｒ Ｓｃｉ
ｅｎｃｅ−Ｒｅｖｉｅｗｓ ｉｎＭａｃｒｏ−＋＊ｏｌ
ｅｅｕｌａｒ Ｃｈｅｍｌｓｔｒｙ ａｎｄ Ｐ
ｈｙｓｉｃｓ 。Solvents for natural polymer substances and their derivatives are described in "Natural Polymer J (198
4) Published by Kyoritsu Shuppan or SAMUEL M, HU
DSON and JOHN A, CUCULO5Jo
unalof macrosolecular Sci
ence-Reviews inMacro-+*ol
eeular Chemlstry and P
hysics.
Ｃ１８（１）、１−８２頁、１９８０などを参照して選
ぶことができる。また、合成高分子物質の溶剤は、Ｊ、
Ｂｒａｎｄｒｕｐ、Ｐｏｌｙｍｅｒ Ｈａｎｄｂｏｏ
ｋ、２ｎｄ ｅｄｉｔｉｏｎ 。C18(1), pp. 1-82, 1980, etc., for selection. In addition, the solvent for the synthetic polymer substance is J,
Brandrup, Polymer Handboo
k, 2nd edition.
Ｊｏｈｎ Ｗｉｌｅｙ ａｎｄ ５ｏｎｓ Ｉｎｃ、、
１９７５などを参考にして選ぶことができる。John Wiley and 5ons Inc.
You can choose by referring to 1975, etc.
疎水性の溶剤としては、たとえば塩化メチレン、クロロ
ホルム、ジクロロエタンなどの塩素化炭化水素を単独ま
たは２種以上混合して通常用いられる。これらの溶剤に
凝固促進剤として少量のメタノール、エタノールなどの
低級アルコールを添加することができる。さらに、ポリ
マー粒子を多孔質にするために炭素数が４〜１２の脂肪
族アルコールを加えることもできる。親水性の溶剤とし
ては、たとえば水、アセトン、テトラヒドロフラン、ジ
オキサン、ジメチルホルムアミド、ジメチルアセトアミ
ド、ジメチルスルホキシド、Ｎ−メチル−２−ピロリド
ンなどの水溶性溶剤が通常用いられる。これらに凝固促
進のため、またはポリマー粒子を多孔質にするために水
溶性低級アルコール、水溶性多価アルコール、無機塩類
などを加えることもできる。As the hydrophobic solvent, chlorinated hydrocarbons such as methylene chloride, chloroform, and dichloroethane are commonly used alone or in combination of two or more. A small amount of lower alcohol such as methanol or ethanol can be added to these solvents as a coagulation accelerator. Furthermore, an aliphatic alcohol having 4 to 12 carbon atoms can be added to make the polymer particles porous. As the hydrophilic solvent, water-soluble solvents such as water, acetone, tetrahydrofuran, dioxane, dimethylformamide, dimethylacetamide, dimethyl sulfoxide, and N-methyl-2-pyrrolidone are usually used. Water-soluble lower alcohols, water-soluble polyhydric alcohols, inorganic salts, etc. can also be added to these to promote coagulation or to make the polymer particles porous.
高分子物質の溶液の粘度は、５０ｃｐｓ以下、好ましく
は２０ｃｐｓ以下である。粘度が５０ｃｐｓよりも大き
くなると交流電圧と同期した液滴にはなりにくい。また
、この溶液の電気伝導度にはとくに制限はない。The viscosity of the solution of the polymeric substance is 50 cps or less, preferably 20 cps or less. When the viscosity is greater than 50 cps, it is difficult to form droplets that are synchronized with the AC voltage. Further, there is no particular restriction on the electrical conductivity of this solution.
本発明において、前記の高分子物質の溶液を、ノズルか
ら該溶剤と非相溶性ないし貧相溶性の分散媒中に噴出さ
せることにより、液滴が形成される。In the present invention, droplets are formed by ejecting the solution of the polymeric substance from a nozzle into a dispersion medium that is incompatible or poorly compatible with the solvent.
分散媒としては、高分子物質の溶剤が疎水性のばあいに
は０／Ｗ型の分散液ができるように非イオン性の界面活
性剤、たとえばゼラチン、メチルセルロース、ポリビニ
ルアルコール、ポリオキシエチレンソルビタンモノラウ
リルエーテル、ポリエチレングリコールモノステアレー
トなどを０．２〜５％（重量％、以下同様）添加した水
溶液が通常用いられる。逆に、高分子物質の溶剤が親水
性のばあいには分散媒として疎水性の有機液体が用いら
れる。たとえば、流動パラフィン、リグロイン、テトラ
リンなどの炭化水素系液体、なたね油、綿実油などの植
物油、四塩化炭素、１．１，２．２．−テトラクロロエ
タンなどのハロゲン化炭化水素系溶剤などが用いられる
。これらにはＷ２Ｏ型の分散液ができるようにＨＬ Ｂ
（Ｈｙｄｒｏｐｈｌｌｌｃｍｌｌｐｏｐｈｉｌｉｃ−
Ｂａｌａｎｃｅ ）（堀口 博、“新界面活性剤”、６
３〜７０頁、三共出版−発行、１９８１参照）が３〜７
の界面活性剤、たとえばグリセロールモノステアレート
、グリセロールモノオレエート、ソルビタンモノオレエ
ートなどが０．５〜５％添加される。As a dispersion medium, nonionic surfactants such as gelatin, methyl cellulose, polyvinyl alcohol, polyoxyethylene sorbitan monomer can be used to form a 0/W type dispersion when the solvent for the polymer substance is hydrophobic. An aqueous solution to which lauryl ether, polyethylene glycol monostearate, etc. is added in an amount of 0.2 to 5% (by weight, hereinafter the same) is usually used. Conversely, when the solvent for the polymeric substance is hydrophilic, a hydrophobic organic liquid is used as the dispersion medium. For example, hydrocarbon liquids such as liquid paraffin, ligroin, and tetralin, vegetable oils such as rapeseed oil and cottonseed oil, carbon tetrachloride, 1.1, 2.2. - Halogenated hydrocarbon solvents such as tetrachloroethane are used. These include HL B to form a W2O type dispersion.
(Hydrophlllcmllpophilic-
Balance ) (Hiroshi Horiguchi, “New Surfactant”, 6
Pages 3-70, published by Sankyo Publishing, 1981) are 3-7
A surfactant such as glycerol monostearate, glycerol monooleate, sorbitan monooleate, etc. is added in an amount of 0.5 to 5%.
分散媒の粘度は５０ｃｐＳ以下が好ましく、２０ｃｐｓ
がさらに好ましく 、５ｃｐｓ以下がとくに好ましい。The viscosity of the dispersion medium is preferably 50 cps or less, and 20 cps
is more preferable, and 5 cps or less is particularly preferable.
粘度が大きくなるとノズルから高流速で液体を噴出させ
たとき粘性抵抗によって噴流が破壊され均一な液滴がで
きにくくなる傾向がある。When the viscosity increases, when liquid is ejected from a nozzle at a high flow rate, the jet stream tends to be destroyed by viscous resistance, making it difficult to form uniform droplets.
分散媒の電気伝導度は１０−” 〜１００ ｕｓ／ｃｓ
、さらには１０−７〜ｌＯμｓ／ｃｍであるのが好まし
い。The electrical conductivity of the dispersion medium is 10-” to 100 us/cs
, more preferably 10-7 to 10 μs/cm.
また、液滴形成用液体と分散媒との誘電率の差が大きす
ぎても小さすぎても均一な液滴はできにくくなる傾向が
ある。その理由は充分解明されてはいないが、おそらく
電気伝導度が大きすぎると絶縁板の孔付近の電界の収束
部分における電気的緊張力が生じに（くなるためであろ
うと思われる。また、電気伝導度が小さく、誘電率も小
さいばあいには絶縁板の孔付近への電界の収束度合が小
さくなるためであろうと思われる。Furthermore, if the difference in dielectric constant between the droplet-forming liquid and the dispersion medium is too large or too small, uniform droplets tend to be difficult to form. The reason for this is not fully understood, but it is probably because when the electrical conductivity is too high, electrical tension is generated in the area where the electric field converges near the hole in the insulating plate. This seems to be because when the conductivity is low and the dielectric constant is also low, the degree of convergence of the electric field near the hole in the insulating plate becomes small.
同期状態をうるための電圧は、分散媒の電気伝導度が比
較的大きいばあいは数ボルトから数百ボルトの間である
が、電気伝導度の小さい分散媒のばあい１００ボルト前
後から数千ボルトの間である。なお、従来の電気式によ
れば前者のばあい数百ボルト以上必要であり、後者のば
あいは数千ボルト以上必要としていた。The voltage required to obtain a synchronized state is between several volts and several hundred volts when the dispersion medium has relatively high electrical conductivity, but between around 100 volts and several thousand volts when the dispersion medium has low electrical conductivity. between the bolts. In addition, according to the conventional electric type, the former requires several hundred volts or more, and the latter requires several thousand volts or more.
本発明では、液体の噴出が分散媒中で行なわれるため、
気体中で液滴を形成する方法のようにあとから噴出した
液滴と合体して粒径が大きくなったり、液滴がノズルや
電極に付着することがほとんど生じなくなる。また、液
滴が電圧の周期的変化により形成され、機械的振動によ
らないため、噴出速度をそれほど大きくしなくても粒径
を小′さくすることができ、騒音の問題がなく、しかも
周期が安定しているので液滴の粒径が安定する。In the present invention, since the liquid is ejected in a dispersion medium,
Unlike methods in which droplets are formed in a gas, there is almost no chance that the droplets will coalesce with later ejected droplets to increase the particle size or that the droplets will adhere to the nozzle or electrode. In addition, since the droplets are formed by periodic changes in voltage and are not dependent on mechanical vibrations, the droplet size can be reduced without increasing the jetting speed, and there is no noise problem. is stable, so the droplet size is stable.
つぎに本発明の液滴形成方法を第１〜３図に従って具体
的に説明する。第３図は本発明の方法に使用可能な別の
分散装置の電界の状態を示す概略断面図である。なお第
１〜３図中の四回部分は導電性の材料であることを示し
、ｌｌの部分は絶縁材料であることを示す。第２〜３図
中の曲線は電気力線が絶縁板（５）の孔（６）で収束し
ている状態を示す。Next, the droplet forming method of the present invention will be specifically explained with reference to FIGS. 1 to 3. FIG. 3 is a schematic cross-sectional view showing the electric field conditions of another dispersion device that can be used in the method of the invention. Note that in FIGS. 1 to 3, the 4th part indicates a conductive material, and the 11 part indicates an insulating material. The curves in FIGS. 2 and 3 show the state in which the lines of electric force converge at the holes (6) of the insulating plate (5).
第１図に示すように、液滴形成用分散装置に、高分子物
質の溶液は矢印で示すように一定流量で送り込まれ、ノ
ズル（２１の噴出孔（３）から絶縁板（５）の孔（６）
に向って噴出される。第１図に示す実施態様では、ノズ
ル（′２Ｊは金属などの導電性のものであるが、第３図
に示すようにノズル孔（３）周辺を絶縁性として他の部
分を導電性のものにしてもよい。これらのノズルには従
来の方法のような絶縁被膜は一切施こされていない。図
面に例示する装置では単孔のノズルが使用されているが
、多孔ノズルを使用することももちろん可能である。ノ
ズルの孔（３）の口径は通常２０〜２５０−であるが、
２５０−以下の比較的粒径の小さい液滴を形成するため
には口径を２０ロー以下とするのが好ましく、ノズルの
目詰りを避けるためには３０ＪＪｒＩ以上が好ましい。As shown in Fig. 1, a solution of a polymeric substance is fed into a droplet-forming dispersion device at a constant flow rate as shown by the arrow, and is passed through a nozzle (21) from the ejection hole (3) to a hole in an insulating plate (5). (6)
It is ejected towards. In the embodiment shown in Fig. 1, the nozzle ('2J) is made of conductive material such as metal, but as shown in Fig. 3, the area around the nozzle hole (3) is insulating and the other parts are made of conductive material. These nozzles are not coated with any insulating coating as in conventional methods.Although a single-hole nozzle is used in the device illustrated in the drawing, a multi-hole nozzle may also be used. Of course it is possible.The diameter of the nozzle hole (3) is usually 20-250-
In order to form droplets with a relatively small particle size of 250 mm or less, the diameter is preferably 20 rows or less, and in order to avoid nozzle clogging, 30 JJrI or more is preferred.
絶縁板（５）の孔（６）の径はノズルの口径の２〜１０
０倍が好ましい。絶縁板に孔を設けるのは電界を集中す
るためであり、１００倍を超えるのは好ましくない。し
かしながら、小さすぎると必要以上に高い組み立て精度
が要求されたり、絶縁板に大きな圧力が加わるなどの問
題が生しるため２倍以上が好ましい。The diameter of the hole (6) in the insulating plate (5) is 2 to 10 times the diameter of the nozzle.
0 times is preferable. The purpose of providing holes in the insulating plate is to concentrate the electric field, and it is not preferable for the hole to exceed 100 times. However, if it is too small, problems such as unnecessarily high assembly precision being required and large pressure being applied to the insulating plate arise, so it is preferable that it be twice or more.
また、ノズル（２］と絶縁板（５）の間隔は５０−〜ｌ
Ｏ關が好ましい。この間隔が５０遍未満であると従来の
方法と同じように絶縁板の孔（６）の近傍のノズル部分
に電界が集中して腐食が生じることがある。また、ノズ
ルから噴出する液体を同伴した分散媒の流れが不均一に
なるおそれがある。しかし、この間隔がｌ０ＬＩＩ１１
を超えると液滴か形成される位置で電界が集中されない
ことになり、均一な液滴ができない。Also, the distance between the nozzle (2) and the insulating plate (5) is 50 - ~ l
O-guan is preferred. If this interval is less than 50 degrees, the electric field may concentrate on the nozzle portion near the hole (6) of the insulating plate, causing corrosion, as in the conventional method. Furthermore, there is a risk that the flow of the dispersion medium accompanied by the liquid ejected from the nozzle may become non-uniform. However, this interval is l0LII11
If it exceeds this, the electric field will not be concentrated at the position where the droplet is formed, and uniform droplets will not be formed.
初めの分散媒（４ａ）は矢印で示すように人口（刀から
ノズル（２）と絶縁板の空間（８）に送られる。分散媒
（４ａ）はノズルの孔（３）から出る液体を同伴しなが
ら絶縁板の孔（６）から噴出する。このとき、分散媒の
流量を調節して同伴する液体を縮流させ、同じノズルを
用いて、さらに小さな液滴をつくることも可能である。The initial dispersion medium (4a) is sent from the blade to the nozzle (2) and the space (8) between the insulating plates as shown by the arrow.The dispersion medium (4a) entrains the liquid coming out of the nozzle hole (3). At this time, it is also possible to adjust the flow rate of the dispersion medium to cause the entrained liquid to contract, thereby creating even smaller droplets using the same nozzle.
また本発明では、初めの分散媒（４ａ）とは異なる分散
媒（４ｂ）を入口（９）から分散槽（ト））に供給する
こともてきる。この分散ａｔ （４ｂ）に、たとえば界
面活性剤を添加して液滴の分散を安定に維持し、生成し
た液滴の合体を防止する効果を与えることもてきる。Further, in the present invention, a dispersion medium (4b) different from the initial dispersion medium (4a) can be supplied from the inlet (9) to the dispersion tank (g). For example, a surfactant may be added to this dispersion at (4b) to maintain stable dispersion of the droplets and to provide an effect of preventing coalescence of the generated droplets.
電極旧）は、第１図に示すように、たとえばステンレス
スチールなどの金属製とし、ノズルからｌＯ〜５０龍程
度の距離に設置してもよいし、第２図に示すように分散
装置の絶縁板（５）以降の外壁を導電性材料とし、それ
を電極ａＺとして用いてもよい。第１図の電極旧）には
分散槽ＱＯＩ内で形成された液滴が通過する直径ＩＯ〜
２０ｍ１程度の孔にか開いている。電極０１）は一定の
周期で変化する電圧を与える電源（１４）を介してノズ
ル（２）と接続されている。電極を通過した均一な液滴
の分散液には、通常、前記したような液滴を高分子物質
の粒子に変える処理（図示されていない）がさらに加え
られる。As shown in Figure 1, the electrode may be made of metal such as stainless steel and may be installed at a distance of about 10 to 50 mm from the nozzle, or as shown in Figure 2, the electrode may be made of metal such as stainless steel. The outer wall after the plate (5) may be made of a conductive material and used as the electrode aZ. The electrode (old) in Figure 1 has a diameter of IO~ through which the droplet formed in the dispersion tank QOI passes.
The hole is about 20m1 in size. The electrode 01) is connected to the nozzle (2) via a power source (14) that provides a voltage that changes at regular intervals. The uniform droplet dispersion that has passed through the electrode is typically further subjected to a process (not shown) for converting the droplets into particles of polymeric material as described above.
ノズルからの液滴の吐出量はレイノルズ数に換算したと
き１０〜１０００の範囲であることが好ましく、さらに
好ましくは２０〜５００である。レイノルズ数がＩＯ以
下では液滴の生成量が少なくなり、一方１０００を超え
ると同期状態に達する交流の周期が数１０ＫＨｚを超え
、安定した状態を維持することが難しくなる。The amount of droplets discharged from the nozzle is preferably in the range of 10 to 1000, more preferably 20 to 500, when converted to Reynolds number. If the Reynolds number is less than IO, the amount of droplets generated will be small, while if it exceeds 1000, the cycle of alternating current that reaches a synchronized state will exceed several tens of KHz, making it difficult to maintain a stable state.
本発明が従来の方法に対して著しく優れた点は、とくに
同期状態かえられる最小電圧が従来の方法に比べてはる
かに小さいことである。前記したように従来の方法では
最低でも数百ボルト以上の電圧が必要であり、しかも電
界が絶縁被覆の施されていないノズルの孔部分に集中す
るためにこの部分が腐食されやすかったが、本発明の方
法では数ボルトでよいたけてなく、ノズル、電極ともに
導電性部分の面積にはとくに制限がないので広くするこ
とができ、電界が導電性の部分て集中するためにこの部
分が腐食するということかない。したがって、かりに電
圧を数百ボルト以上加えたばあいでもノズルあるいは電
極の腐食は生じない。A significant advantage of the present invention over conventional methods is, in particular, that the minimum voltage required to change the synchronization state is much smaller than that of conventional methods. As mentioned above, the conventional method requires a voltage of at least several hundred volts, and the electric field concentrates on the nozzle hole, which is not coated with insulation, which is prone to corrosion. In the method of the invention, only a few volts is sufficient, and since there is no particular limit to the area of the conductive part of both the nozzle and the electrode, it can be made wide, and the electric field concentrates on the conductive part, causing corrosion of this part. That's not the case. Therefore, even if a voltage of several hundred volts or more is applied, corrosion of the nozzle or electrode will not occur.
本発明の方法では従来の電気式で必要とされる高電圧で
は均一な液滴が形成されにくくなる。In the method of the present invention, uniform droplets are difficult to form at the high voltages required by conventional electric methods.
その理由は必ずしも明白ではないが、液柱の自励振動と
絶縁板の孔（６）に電界が集中する効果の相乗作用によ
ると考えられる。実際に液滴はこの孔（６）の付近で形
成される。Although the reason for this is not necessarily clear, it is thought to be due to the synergistic effect of the self-excited vibration of the liquid column and the effect of concentration of the electric field in the holes (6) of the insulating plate. Droplets are actually formed near this hole (6).
一定の周期で変化する電圧には、通常の交流電圧を使用
することもできるが、半波整流波形の電圧もしくはパル
ス状の電圧のほうが周波数、電圧ともに同期範囲が広く
、好ましい。適用可能な電圧は液体、分散媒の種類によ
って異なるが通常３〜２０００ボルト、好ましくは５〜
５００ボルト、振動数は通常０．３〜２０ＫＨｚ 、好
ましくは０．５〜１ＯＫＨｚである。Although a normal alternating current voltage can be used as the voltage that changes at a constant cycle, a half-wave rectified waveform voltage or a pulsed voltage is preferable because it has a wider synchronization range for both frequency and voltage. The applicable voltage varies depending on the type of liquid and dispersion medium, but is usually 3 to 2,000 volts, preferably 5 to 2,000 volts.
500 volts, and the frequency is usually 0.3 to 20 KHz, preferably 0.5 to 1 OKHz.
分散媒の流量は分散液中の液滴の濃度が５容量％以下に
なるようにするのが好ましく、さらに好ましくは３容量
％以下である。このような流量で分散媒を流すことによ
り電極のまわりに液滴が滞留して液滴同士の再結合や電
極への付着が生じることがなく、液滴が液滴生成域から
分散媒で流し去られる。The flow rate of the dispersion medium is preferably such that the concentration of droplets in the dispersion liquid is 5% by volume or less, more preferably 3% by volume or less. By flowing the dispersion medium at such a flow rate, the droplets will not accumulate around the electrode and will not recombine with each other or adhere to the electrode, and the dispersion medium will flow the droplets from the droplet generation area. be left.
以上のようにしてえられた均一な液滴は通常前記したよ
うな追加処理が加えられ、完全に凝固した粒子に変えら
れる。The uniform droplets obtained as described above are usually subjected to additional processing as described above to convert them into completely solidified particles.
つぎに、液体として高分子物質の溶液ではなく、ビニル
重合性モノマー液を使用したばあいについて説明する。Next, a case will be described in which a vinyl polymerizable monomer liquid is used as the liquid instead of a solution of a polymeric substance.
このばあいには、前記と同様にして分散媒中に均一な液
滴として分散された重合性モノマーは公知の懸濁重合法
よって重合性させて均一なポリマー粒子とされる。分散
液は０／Ｗ型、Ｗ２Ｏ型いずれでもよいためモノマーは
親水性でも疎水性でもよい。またビニル重合性モノマー
は単独で用いてもよいし２種類以上併用してもよい。こ
のような七ツマ−からなるビニル重合性モノマー液には
、えられるポリマー粒子の構造を調整するために非反応
性の希釈剤を加えてもよい。希釈剤の具体例としては、
たとえばベンゼン、ジエチルベンゼン、キシレン、トル
エンなど、炭素数が５〜１２の脂肪族飽和炭化水素、炭
素数が５〜１２の脂肪族低級アルコールなどがあげられ
る。In this case, the polymerizable monomer dispersed as uniform droplets in the dispersion medium in the same manner as described above is polymerized into uniform polymer particles by a known suspension polymerization method. Since the dispersion liquid may be either O/W type or W2O type, the monomer may be hydrophilic or hydrophobic. Further, the vinyl polymerizable monomers may be used alone or in combination of two or more types. A non-reactive diluent may be added to the vinyl-polymerizable monomer solution consisting of such seven polymers in order to adjust the structure of the obtained polymer particles. Specific examples of diluents include:
Examples include aliphatic saturated hydrocarbons having 5 to 12 carbon atoms, aliphatic lower alcohols having 5 to 12 carbon atoms, such as benzene, diethylbenzene, xylene, and toluene.
前記疎水性モノマーの具体例としては、たとえばスチレ
ン、エチルスチレン、クロルメチル化スチレン、アクリ
ル酸メチル、メタクリル酸メチル、アクリロニトリル、
無水マレイン酸、酢酸ビニルなどのモノビニルモノマー
ジビニルベンゼン、エチレングリコールジメタクリレ
ート、ポリエチレングリコールジメタクリレート、フタ
ル酸ジアリルなどのポリビニルモノマーなどがある。こ
れらのうちで、スチレン−ジビニルベンゼン、クロルメ
チル化スチレン−ジビニルベンゼン、スチレン−無水マ
レイン酸−ジビニルベンゼン、メタクリル酸メチル−ジ
ビニルベンゼン、メタクリル酸メチル−エチレングリコ
ールジメタクレートなどの組み合わせがとくに好ましい
。これらのモノマー液の重合は、紫外線あるいは熱を加
えることによって、あらかじめ少量添加した重合開始剤
、たとえば過酸化ベンゾイル、アゾビスイソブチロニト
リルなどにフリーラジカルを生成させることによって行
なわれる。Specific examples of the hydrophobic monomer include styrene, ethylstyrene, chloromethylated styrene, methyl acrylate, methyl methacrylate, acrylonitrile,
Monovinyl monomers such as maleic anhydride and vinyl acetate; polyvinyl monomers such as divinylbenzene, ethylene glycol dimethacrylate, polyethylene glycol dimethacrylate, and diallyl phthalate. Among these, combinations such as styrene-divinylbenzene, chloromethylated styrene-divinylbenzene, styrene-maleic anhydride-divinylbenzene, methyl methacrylate-divinylbenzene, and methyl methacrylate-ethylene glycol dimethacrylate are particularly preferred. Polymerization of these monomer liquids is carried out by generating free radicals in a polymerization initiator, such as benzoyl peroxide, azobisisobutyronitrile, etc., added in advance in a small amount by applying ultraviolet rays or heat.
親水性モノマーの具体例としては、たとえばアクリルア
ミド、種々のアルキルアクリルアミド、ヒドロキシエチ
ルメタクリレート、アクリル酸、ビニルスルホン酸、Ｎ
−ビニルピロリドンなどがあげられる。これらのポリマ
ーは水溶性であるので通常架橋剤と共重合して不溶化す
る。Specific examples of hydrophilic monomers include acrylamide, various alkyl acrylamides, hydroxyethyl methacrylate, acrylic acid, vinyl sulfonic acid, N
- Examples include vinylpyrrolidone. Since these polymers are water-soluble, they are usually copolymerized with a crosslinking agent to make them insolubilized.
架橋剤には、たとえばメチレンビスアクリルアミド、ポ
リエチレングリコールジメタクリレートなどがある。さ
らに重合開始剤として、たとえば親水性の過硫酸アンモ
ニウムなどが添加される。Examples of crosslinking agents include methylene bisacrylamide and polyethylene glycol dimethacrylate. Further, as a polymerization initiator, for example, hydrophilic ammonium persulfate or the like is added.
前記モノマー液の粘度は、前記の高分子物質の溶液と同
様に５０ｃｐｓ以下、好ましくは２０ｃｐｓ以下である
。また、この液の電気伝導度にはとくに制限はない。The viscosity of the monomer liquid is 50 cps or less, preferably 20 cps or less, similar to the polymer substance solution described above. Further, there is no particular limit to the electrical conductivity of this liquid.
これらのモノマー液の分散媒としては、疎水性上ツマ−
を用いるばあい、前記高分子物質を含む溶液の分散媒と
同じように通常ゼラチン、メチルセルロース、ポリビニ
ルアルコールなどの非イオン性の界面活性剤を０．２〜
５％程度添加した水溶液が用いられる。As a dispersion medium for these monomer liquids, hydrophobic
When using a nonionic surfactant such as gelatin, methyl cellulose, or polyvinyl alcohol, the amount of a nonionic surfactant such as gelatin, methyl cellulose, or polyvinyl alcohol is usually used in the same manner as the dispersion medium of the solution containing the polymeric substance.
An aqueous solution containing about 5% is used.
また、親水性モノマーのばあいには、分散媒としてたと
えばトルエン、キシレン、テトラリン、リグロイン、流
動パラフィンなどの炭化水素系溶剤、四塩化炭素、トリ
クロロエチレン、１．１．２．２．− ）ラクロロエチ
レン、クロルベンゼンなどのハロゲン化物、ひまし油、
綿実油などの植物油、シリコーンオイルなどが用いられ
る。In the case of hydrophilic monomers, the dispersion medium may be hydrocarbon solvents such as toluene, xylene, tetralin, ligroin, liquid paraffin, carbon tetrachloride, trichloroethylene, etc. 1.1.2.2. −) Halides such as lachloroethylene and chlorobenzene, castor oil,
Vegetable oils such as cottonseed oil, silicone oil, etc. are used.
これらにＨＬＢ値が３〜６の界面活性剤、たとえばソル
ビタンモノオレエート、グリセロールモノステアレート
などが０．５〜５％添加される。A surfactant having an HLB value of 3 to 6, such as sorbitan monooleate and glycerol monostearate, is added in an amount of 0.5 to 5%.
この七ツマー液および分散媒を使用し、前記と同様にし
て数〜数千ボルトの一定周期で変化する電圧の周期と同
期して液滴が形成される。Using this 7-mer solution and dispersion medium, droplets are formed in the same manner as described above in synchronization with the period of the voltage that changes at a constant cycle of several to several thousand volts.
このようにして分散媒中に懸濁させた均一なモノマー液
滴は、通常さらに加熱や紫外線照射によって重合させる
ことにより、種々の目的の均一なポリマー粒子とするこ
とができる。使用目的によってはさらに親水性基、イオ
ン交換基、抗体などの生理活性物質などを導入する処理
が加えられる。The uniform monomer droplets thus suspended in the dispersion medium can be made into uniform polymer particles for various purposes, usually by further polymerizing them by heating or UV irradiation. Depending on the purpose of use, further treatments may be added to introduce hydrophilic groups, ion exchange groups, physiologically active substances such as antibodies, etc.
以上に説明したように、本発明の方法によれば、液滴径
が２０〜２５０ Ｊｌの微小な均−滴を従来の方法に比
べてはるかに低い電圧を用いて安定してうろことができ
る。As explained above, according to the method of the present invention, minute uniform droplets with a droplet diameter of 20 to 250 Jl can be stably flowed using a much lower voltage than conventional methods. .
つぎに本発明の方法を実施例によってさらに具体的に説
明する。実施例では液滴とその分散媒の組み合わせとし
て水と灯油を用いているが、もちろん前記した種々の組
み合わせが可能である。Next, the method of the present invention will be explained in more detail with reference to Examples. In the embodiment, water and kerosene are used as a combination of droplets and their dispersion medium, but of course the various combinations described above are possible.
実施例１
液滴用の液体（分散相）として非イオン性界面活性剤を
４％添加した灯油（室温での粘度は１ ｃｐｓ未満、電
気伝導度は２ Ｘ １０−９ ｓ／ｃｍ ）を用い、分
散媒として蒸留水（電気伝導度は４．６×１０’ｓ／ａ
ｍ）を用い、第１図に示す装置により以下の条件で均一
な灯油の液滴の水懸濁液を製造した。Example 1 Kerosene (viscosity at room temperature less than 1 cps, electrical conductivity 2 x 10-9 s/cm) to which 4% nonionic surfactant was added was used as the liquid (dispersed phase) for droplets. , distilled water as a dispersion medium (electrical conductivity is 4.6 x 10's/a
A uniform aqueous suspension of kerosene droplets was produced using the apparatus shown in FIG. 1 under the following conditions.
ノズル（′２Ｊには口径が１００道の孔（３）を有する
ステンレススチール板を使用した。このノズルには、前
記特開昭５８−１７５６６８号公報に記載されているよ
うな絶縁被膜は一切施こさなかった。ステンレススチー
ル製電極０１）には直径１０■ｍの孔Ｑ３）を開けた。A stainless steel plate having a hole (3) with a diameter of 100 was used for the nozzle ('2J).This nozzle was not coated with any insulating coating as described in JP-A-58-175668. A hole Q3) with a diameter of 10 μm was drilled in the stainless steel electrode 01).
ノズルと電極の間に直径４００Ｉの孔（６）の開いた厚
さ２００通のポリテトラフルオロエチレン製の絶縁板（
５）を配設した。ノズル（２］と絶縁板（５）の間隔は
２００虜、ノズル（′２Ｊと電極口）の間隔は１０＋ａ
ｍとした。これらを第１図に示す配置で透明なアクリル
樹脂製の容器に固定した。均一な液滴が生成しているか
どうかは、透明容器の外部からストロボスコープを点滅
させながら観察して確認した。また、実験はすべて室温
で行なった。A 200-thick polytetrafluoroethylene insulating plate with 400 I diameter holes (6) between the nozzle and the electrode (
5) was installed. The distance between the nozzle (2) and the insulating plate (5) is 200mm, and the distance between the nozzle ('2J and the electrode port) is 10+a.
It was set as m. These were fixed in a transparent acrylic resin container in the arrangement shown in FIG. Whether uniform droplets were being generated was confirmed by observing from outside the transparent container with a flashing stroboscope. Furthermore, all experiments were conducted at room temperature.
灯油を１．３ Ｘ １０’ ｍｌ ／ｓｉｎでノズルに
送った。Kerosene was delivered to the nozzle at 1.3 x 10' ml/sin.
また、蒸留水をその入口（力からノズルと絶縁板の間に
４．２ ｍｌ／ｓＩｎで送った。交流電源０４）の交流
周期を７００Ｈｚに設定し、印加電圧を徐々に上げてい
くと、５．２ボルトに達したときに同期状態になり、直
径１８０−の均一な液滴が連続してえられた。このとき
の電流は測定限界の１μＡ以下であった。さらに電圧を
上げていき４００ボルトに達したときに１周期の間に大
小二つの液滴が生成しはじめ、この電圧以上では均一な
液滴の形成は不可能となった。In addition, when the AC cycle of the inlet of distilled water (4.2 ml/sIn was sent between the nozzle and the insulating plate, AC power supply 04) was set to 700 Hz, and the applied voltage was gradually increased, 5. When 2 volts were reached, synchronization was achieved and uniform droplets of 180 mm diameter were obtained in succession. The current at this time was below the measurement limit of 1 μA. When the voltage was further increased and reached 400 volts, two large and small droplets began to be generated during one cycle, and it became impossible to form uniform droplets above this voltage.
実施例２
０径が５０−のノズルに変えたほかは、実施例１と同じ
装置を使用して灯油の液滴を作製した。Example 2 Kerosene droplets were produced using the same apparatus as in Example 1, except that the nozzle had a diameter of 50 mm.
灯油、蒸留水の流量をそれぞれ７ ｘ １０’ ｍｌ
／■１ｎおよび４．２ ｍｌ／ｓｉｎとした。交流周期
を４０００Ｈｚに設定し、印加電圧を徐々に上げた。５
．８ボルトに達すると同期状態になり１周期に１個の均
一な液滴（直径８２ｒ）が連続して形成された。The flow rate of kerosene and distilled water is 7 x 10' ml each.
/■1n and 4.2 ml/sin. The AC cycle was set to 4000 Hz, and the applied voltage was gradually increased. 5
．． When the voltage reached 8 volts, a synchronous state was reached and one uniform droplet (diameter 82r) was continuously formed in one cycle.
さらに電圧を上げると５４０ボルトで大小混ざり合った
液滴が生じ、それ以上の電圧では均一な液滴の形成が不
可能になった。When the voltage was further increased to 540 volts, droplets of mixed sizes were formed, and it became impossible to form uniform droplets at higher voltages.
実施例３
実施例１て用いた装置を用い、灯油を分散媒とし蒸留水
の液滴を生成するべく、以下の条件で行なった。Example 3 Using the apparatus used in Example 1, the following conditions were used to generate droplets of distilled water using kerosene as a dispersion medium.
水、灯油の流量をそれぞれ３．２ ｘ １０’ ｍｌ
／ｗｉｎおよび８．３ ｍｌ／ｓｉｎとした。交流周期
を１１００Ｈｚに設定し、印加電圧を徐々に上げると、
１３０ボルトで同期状態に達し、２０００ボルトで同期
状態が壊れた。生成した均一な液滴の直径は２１０通で
あった。The flow rate of water and kerosene is 3.2 x 10' ml each.
/win and 8.3 ml/sin. When the AC cycle is set to 1100Hz and the applied voltage is gradually increased,
Synchronization was reached at 130 volts, and synchronization was broken at 2000 volts. The diameter of the uniform droplets produced was 210.
［発明の効果］
本発明の方法では従来の方法に比べて極めて低い電圧で
同期状態かえられるので、ノズルの腐食が生じず、また
液滴のノズルや電極への付着がなく、均一で微少な液滴
を長時間安定して製造することができる。[Effects of the Invention] The method of the present invention can change the synchronized state with an extremely low voltage compared to conventional methods, so there is no corrosion of the nozzle, no adhesion of droplets to the nozzle or electrode, and uniform and minute droplets. Droplets can be produced stably for a long time.
第１図は本発明の方法に用いる分散装置の一実施態様の
概略縦断面図、第２図は第１図に示す実施態様の電界の
状態を示す概略断面図、第３図は本発明の方法に用いる
分散装置の別の実施態様における電界の状態を示す概略
断面図である。
（図面の主要符号）
（１）：液滴
（ａ：ノズル
（４）：分散媒
（５）：絶縁板
（６）：絶縁板の孔
旧）、０２）：電極
■：交流電源
第２図FIG. 1 is a schematic vertical cross-sectional view of an embodiment of the dispersion device used in the method of the present invention, FIG. 2 is a schematic cross-sectional view showing the electric field state of the embodiment shown in FIG. 1, and FIG. FIG. 3 is a schematic cross-sectional view showing the state of the electric field in another embodiment of the dispersion device used in the method. (Main symbols in the drawing) (1): Droplet (a: Nozzle (4): Dispersion medium (5): Insulating plate (6): Old hole in insulating plate), 02): Electrode ■: AC power supply Figure 2
Claims (1)
けた電気的絶縁板と電極とをこの順に配置し、ノズルと
電極の間に一定周期の電圧を加えながらノズルから液体
を噴出させることにより、該電圧の周期と同期した数の
均一な液滴を生成させることを特徴とする均一な液滴の
形成方法。1. A liquid ejection nozzle, an electrically insulating plate provided with a passage hole for the liquid, and an electrode are arranged in this order in a dispersion medium, and the liquid is ejected from the nozzle while applying a constant voltage between the nozzle and the electrode. A method for forming uniform droplets, the method comprising: generating uniform droplets in a number synchronized with the period of the voltage.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17176390A JP2854390B2 (en) | 1990-06-28 | 1990-06-28 | Method for forming uniform droplets |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17176390A JP2854390B2 (en) | 1990-06-28 | 1990-06-28 | Method for forming uniform droplets |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0459255A true JPH0459255A (en) | 1992-02-26 |
| JP2854390B2 JP2854390B2 (en) | 1999-02-03 |
Family
ID=15929229
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17176390A Expired - Lifetime JP2854390B2 (en) | 1990-06-28 | 1990-06-28 | Method for forming uniform droplets |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2854390B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004028815A1 (en) * | 2002-09-24 | 2004-04-08 | Konica Minolta Holdings, Inc. | Method for manufacturing electrostatic attraction type liquid discharge head, method for manufacturing nozzle plate, method for driving electrostatic attraction type liquid discharge head, electrostatic attraction type liquid discharging apparatus, and liquid discharging apparatus |
| WO2004028813A1 (en) | 2002-09-24 | 2004-04-08 | Konica Minolta Holdings, Inc. | Liquid jetting device |
| WO2004028814A1 (en) * | 2002-09-24 | 2004-04-08 | Konica Minolta Holdings, Inc. | Liquid jetting device |
| WO2004028812A1 (en) * | 2002-09-24 | 2004-04-08 | Sharp Kabushiki Kaisha | Electrostatic suction type fluid jettint device |
| JP2007331127A (en) * | 2006-06-12 | 2007-12-27 | Ricoh Co Ltd | Liquid droplet delivering apparatus, image forming apparatus, image forming method, and method for manufacturing liquid droplet delivering apparatus |
| CN100398320C (en) * | 2002-09-24 | 2008-07-02 | 夏普株式会社 | Electrostatic attraction fluid jet device |
-
1990
- 1990-06-28 JP JP17176390A patent/JP2854390B2/en not_active Expired - Lifetime
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004028815A1 (en) * | 2002-09-24 | 2004-04-08 | Konica Minolta Holdings, Inc. | Method for manufacturing electrostatic attraction type liquid discharge head, method for manufacturing nozzle plate, method for driving electrostatic attraction type liquid discharge head, electrostatic attraction type liquid discharging apparatus, and liquid discharging apparatus |
| WO2004028813A1 (en) | 2002-09-24 | 2004-04-08 | Konica Minolta Holdings, Inc. | Liquid jetting device |
| WO2004028814A1 (en) * | 2002-09-24 | 2004-04-08 | Konica Minolta Holdings, Inc. | Liquid jetting device |
| WO2004028812A1 (en) * | 2002-09-24 | 2004-04-08 | Sharp Kabushiki Kaisha | Electrostatic suction type fluid jettint device |
| US7314185B2 (en) | 2002-09-24 | 2008-01-01 | Konica Minolta Holdings, Inc. | Liquid jetting device |
| US7337987B2 (en) | 2002-09-24 | 2008-03-04 | Konica Minolta Holdings, Inc. | Liquid jetting device |
| CN100398320C (en) * | 2002-09-24 | 2008-07-02 | 夏普株式会社 | Electrostatic attraction fluid jet device |
| US7449283B2 (en) | 2002-09-24 | 2008-11-11 | Sharp Kabushiki Kaisha | Producing method of electrostatic sucking type liquid jetting head, producing method of nozzle plate, driving method of electrostatic sucking type liquid jetting head, electrostatic sucking type liquid jetting apparatus and liquid jetting apparatus |
| US7520592B2 (en) | 2002-09-24 | 2009-04-21 | Sharp Kabushiki Kaisha | Electrostatic attraction fluid jet device |
| JP2007331127A (en) * | 2006-06-12 | 2007-12-27 | Ricoh Co Ltd | Liquid droplet delivering apparatus, image forming apparatus, image forming method, and method for manufacturing liquid droplet delivering apparatus |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2854390B2 (en) | 1999-02-03 |
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