JP3467220B2 - Droplet generator - Google Patents

Droplet generator

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Publication number
JP3467220B2
JP3467220B2 JP34206899A JP34206899A JP3467220B2 JP 3467220 B2 JP3467220 B2 JP 3467220B2 JP 34206899 A JP34206899 A JP 34206899A JP 34206899 A JP34206899 A JP 34206899A JP 3467220 B2 JP3467220 B2 JP 3467220B2
Authority
JP
Japan
Prior art keywords
liquid
ejection holes
droplet
porous member
droplets
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.)
Expired - Fee Related
Application number
JP34206899A
Other languages
Japanese (ja)
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JP2001151803A (en
Inventor
英明 久保
直樹 片田
純 志田
清二 玉置
宏宣 長崎
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kao Corp
Original Assignee
Kao Corp
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Filing date
Publication date
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Priority to JP34206899A priority Critical patent/JP3467220B2/en
Publication of JP2001151803A publication Critical patent/JP2001151803A/en
Application granted granted Critical
Publication of JP3467220B2 publication Critical patent/JP3467220B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Description

【発明の詳細な説明】 【0001】 【発明の属する技術分野】本発明は、例えば粒径のそろ
ったポリマービーズを得るために利用される液滴生成装
置に関する。 【0002】 【従来の技術】連続相状態の液体を貯留する容器と、こ
の容器の内部に配置される噴出孔を有する多孔部材と、
この多孔部材に液滴化対象液を供給する手段と、その噴
出孔から噴出される液滴化対象液を振動させる手段とを
備え、その噴出される液滴化対象液を振動数に応じて分
散させて液滴とする液滴生成装置が従来より提案されて
いる(特公平1‐28761号公報参照)。 【0003】上記のような液滴生成装置は、例えばモノ
マーの液滴を重合させて粒径の揃ったポリマービーズを
得るのに利用されるが、工業的に利用するためには、多
孔部材に形成する噴出孔の数を多くする必要がある。そ
こで、図5に示すように多数の噴出孔101が均等に配
列された多孔部材102が用いられていた。 【0004】しかし、多数の噴出孔101を均等に配列
すると粒径の揃った液滴を生成することが困難になる。
すなわち、図4に示すように、連続相状態の液体103
を貯留する容器104の内部に多数の噴出孔101が均
等配列された多孔部材102を配置し、その多孔部材1
02に液滴化対象液を供給して噴出孔101から噴出さ
せると共に、その噴出液を振動させて液滴105を生成
した場合、その液滴105は連続相状態の液体103を
同伴して上昇する。そのため、連続相状態の液体103
が図中矢印で示すように液滴105の上昇流の中心に向
かって流れ、液滴105の上昇流に縮流部105′が生
じる。その縮流部105′において液滴105が互いに
衝突して合一あるいは分裂するため、液滴105のサイ
ズが不均一になってしまう。 【0005】このような問題を解決するため、多孔部材
に形成される多数の噴出孔を環状領域に配列することで
液滴の上昇流の縮流を低減して液滴のサイズの均一化を
図ることが提案されている(特開平3‐249931号
公報参照)。 【0006】 【発明が解決しようとする課題】多孔部材に形成する噴
出孔を環状領域に配列することで、液滴の上昇流の中心
部に連続相状態の液体が存在することになり、連続相状
態の液体が上昇流の中心部に向かう流れが弱くなり、あ
る程度の液滴のサイズの均一化を図ることができる。 【0007】しかし、上記従来技術では噴出孔は環状領
域の全域に亘って配列されるものであるため、噴出孔の
配列ピッチを小さくしたような場合、液滴の上昇流の縮
流により周方向に隣接する液滴同士の衝突が生じて液滴
のサイズが不均一になってしまう。 【0008】本発明は上記従来技術の課題を解決するこ
とのできる液滴生成装置を提供することを目的とする。 【0009】 【課題を解決するための手段】本発明の特徴とするとこ
ろは、連続相状態の液体を貯留する容器と、この容器の
内部に配置される多数の噴出孔を有する多孔部材と、こ
の多孔部材に液滴化対象液を供給する手段と、その噴出
孔から噴出される液滴化対象液を振動させる手段とを備
え、その多数の噴出孔が環状領域に配列されている液滴
生成装置であって、前記噴出孔が配列される多孔部材の
環状領域に、周方向に間隔をおいて噴出孔が配列されな
い複数の空域が設けられ、前記空域の周方向幅は前記噴
出孔の配列ピッチよりも大きくされている点にある。 【0010】 【作用】本発明の構成によれば、噴出孔が配列される多
孔部材の環状領域に、周方向に間隔をおいて複数の空域
が設けられるので、液滴の上昇流の中心部と周方向間に
液滴の存在しない領域が生じる。この液滴の存在しない
領域は連続相状態の液体が上昇流の中心に向かう通路に
なるので、液滴の上昇流の縮流を小さくすることができ
る。 【0011】 【発明の実施の形態】以下、図面を参照して本発明の実
施形態を説明する。 【0012】図3に示す液滴生成装置1は、連続相状態
の液体2を貯留する容器3と、この容器3の内部に配置
されるプレート状の多孔部材4を備えている。図1に示
すように、その多孔部材4の環状領域に多数の噴出孔5
が配列されている。また、その噴出孔5が配列される多
孔部材4の環状領域には、周方向に間隔をおいて噴出孔
5が配列されない複数の空域6が設けられている。その
多孔部材4の下方にハウジング7が設けられ、そのハウ
ジング7に、液滴化対象液を貯留するタンク8が配管9
とポンプ10を介し接続されている。これにより、多孔
部材4に供給された液滴化対象液は噴出孔5から連続相
状態の液体2中に噴出される。その噴出液を振動させる
圧電振動子11がハウジング7の内部に設けられてい
る。 【0013】上記噴出孔5から噴出される液滴化対象液
を振動子11の振動数に応じて分散させて均一な液滴群
を生成するには、生成しようとする液滴径、連続相状態
の液体2の物性あるいは液滴化対象液の物性等に応じ、
噴出孔5の径や配列ピッチ、液滴化対象液の噴出速度や
振動数を試行錯誤的に定める必要がある。 【0014】その噴出孔5の径は、連続相状態の液体2
や液滴化対象液の物性、振動の条件を含む種々の因子の
影響を受けるが、主として生成しようとする液滴のサイ
ズにより決定される。一般に生成しようとする液滴のサ
イズは20〜10000μmであり、噴出孔5の径は1
0〜5000μmとされる。 【0015】噴出孔5から噴出される液滴化対象液の流
れは、均一な液滴群を得るためには層流にする必要があ
る。そのため、液滴化対象液の密度をρ、噴出速度を
u、オリフィス孔の径をD、液滴化対象液の粘度をμと
した場合に、Re=D・u・ρ/μで表されるレイノル
ズ数の大きさは、10〜2000好ましくは15〜10
00、特に好ましくは20〜300の範囲とするのが好
ましい。レイノルズ数が10より小さいと流量が小さく
生産効率が低く、2000を超えると乱流領域になるた
め均一な液滴群が生成されないからである。 【0016】噴出孔5から噴出する液滴化対象液を振動
させる手段は、その噴出流を均一な液滴群に分散させる
ことができる振動特性を有するものであればよく、その
振動数は一般に10〜50000Hzが好ましい。具体
的な振動手段としては、機械的振動子、電音響的振動
子、水音響的振動子、電磁的振動子、磁気抵抗的トラン
スジューサー等を用いることができ、これら振動子を多
孔部材に接続して多孔部材を振動させるようにしてもよ
いし、図3に示したように液滴化対象液を振動させるよ
うにしてもよい。 【0017】また、各噴出孔5の配列ピッチPは孔径の
15倍以上が好ましく、空域6の周方向幅sはそのピッ
チPよりも大きくする。空域6の数は2〜30、好まし
くは3〜15がよい。また空域6の周方向幅sの総和
は、環状領域の周長の0.1〜0.8倍、好ましくは
0.2〜0.7倍がよい。また、噴出孔5を配列する環
状領域の中心から外径までの半径をrとした場合、内径
は0.3r以上とするのが良く、好ましくは0.5r以
上とし、より好ましくは0.7r以上とする。また、各
噴出孔5は図1では多角形の各辺上に配列されている
が、円周上に配列するようにしてもよく、環状領域に配
列されれば具体的配置は限定されない。 【0018】上記液滴生成装置1において、容器3に連
続相状態の液体2として1wt%のPVA溶液を貯留
し、液滴化対象液としてモノマー溶液を多孔部材4に供
給して噴出孔5から1孔あたり1.2g/minの流量
で噴出させ、その噴出流に振動子11により1700H
zの正弦波振動を与えた。そのモノマー溶液として、ラ
ウロイルアクリレート/酢酸ビニル/ジビニルベンゼン
/ラウロイルパーオキサイド=80/10/9/1のも
のを用いた。また、噴出孔5の径は80μm、配列ピッ
チPは1.5mmとし、図1に示すように多孔部材4の
環状領域であって平面視正6角形の各項点部分におい
て、噴出孔5が配列されない空域6を設けた。空域6ヶ
所の周方向幅の総和は、環状領域の周長の0.18倍で
あった。また環状領域の外接円の半径は13.5mmで
あった。 【0019】これにより、図2に示すように非常に均一
な単分散液滴12が生成された。すなわち、その液滴1
2の上昇流は周囲のPVA溶液2を伴って上昇するが、
その液滴の上昇流の中心部と周方向間の双方に液滴12
の存在しない領域が生じる。この液滴の存在しない領域
はPVA溶液2が上昇流の中心に向かう通路になるの
で、液滴12の上昇流に生じる縮流が小さくなり、液滴
12相互の衝突が防止される。これにより得られた液滴
を常法により重合させた結果、直径約265μmの均一
な径のポリマービーズが得られた。 【0020】 【発明の効果】本発明による液滴生成装置によれば、多
数の噴出孔が配列される多孔部材の環状領域に、周方向
に間隔をおいて噴出孔が配列されない複数の空域を設け
るという簡単な構成で液滴の均一化を図ることができ
る。
Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a droplet generating apparatus used for obtaining, for example, polymer beads having a uniform particle size. 2. Description of the Related Art A container for storing a liquid in a continuous phase, a porous member having an ejection hole disposed inside the container,
A means for supplying the liquid to be dropletized to the porous member; and a means for vibrating the liquid to be dropletized ejected from the ejection hole, wherein the ejected liquid to be dropletized is changed in accordance with the frequency. 2. Description of the Related Art A droplet generation apparatus that disperses and forms droplets has been conventionally proposed (see Japanese Patent Publication No. 1-28761). [0003] The above-described droplet generating apparatus is used, for example, to polymerize droplets of a monomer to obtain polymer beads having a uniform particle size. It is necessary to increase the number of orifices to be formed. Therefore, as shown in FIG. 5, a porous member 102 in which a large number of ejection holes 101 are uniformly arranged has been used. However, if a large number of ejection holes 101 are evenly arranged, it becomes difficult to generate droplets having a uniform particle diameter.
That is, as shown in FIG.
A porous member 102 in which a large number of ejection holes 101 are evenly arranged is disposed inside a container 104 for storing
When the liquid to be dropletized is supplied to 02 and ejected from the ejection hole 101, and the ejected liquid is vibrated to generate a droplet 105, the droplet 105 rises along with the liquid 103 in a continuous phase state. I do. Therefore, the liquid 103 in the continuous phase state
Flows toward the center of the upward flow of the droplet 105 as shown by the arrow in the figure, and a contraction portion 105 ′ is generated in the upward flow of the droplet 105. The droplets 105 collide with each other at the contraction portion 105 ′ so as to be united or split, so that the size of the droplets 105 becomes uneven. In order to solve such a problem, by arranging a large number of ejection holes formed in a porous member in an annular region, the contraction of the upward flow of the droplet is reduced, and the size of the droplet is made uniform. It has been proposed to achieve this (see Japanese Patent Application Laid-Open No. 3-249931). [0006] By arranging the ejection holes formed in the porous member in an annular region, the liquid in the continuous phase exists at the center of the upward flow of the droplet, and the continuous liquid is present. The flow of the liquid in the phase state toward the center of the upward flow is weakened, and the size of the droplets can be made uniform to some extent. However, in the above-mentioned prior art, the ejection holes are arranged over the entire annular region. Therefore, when the arrangement pitch of the ejection holes is reduced, the circumferential direction is reduced by the contraction of the upward flow of the droplets. The droplets adjacent to each other collide with each other, and the size of the droplets becomes non-uniform. An object of the present invention is to provide a droplet generating apparatus which can solve the above-mentioned problems of the prior art. A feature of the present invention is that a container for storing a liquid in a continuous phase, a porous member having a large number of ejection holes arranged inside the container, Means for supplying the liquid to be dropletized to the porous member, and means for vibrating the liquid to be dropletized ejected from the ejection holes, the droplets having a large number of ejection holes arranged in an annular region In the generator, a plurality of voids in which the orifices are not arranged at intervals in the circumferential direction are provided in the annular region of the porous member in which the orifices are arranged, and the circumferential width of the void is the same as that of the jet.
The point is that it is made larger than the arrangement pitch of the outlet holes . According to the structure of the present invention, a plurality of cavities are provided at intervals in the circumferential direction in the annular region of the porous member in which the ejection holes are arranged, so that the central portion of the upward flow of the droplets is provided. In the circumferential direction, a region where no droplet exists is generated. Since the liquid in the continuous phase forms a passage toward the center of the upward flow in the region where the droplet does not exist, the contraction of the upward flow of the droplet can be reduced. An embodiment of the present invention will be described below with reference to the drawings. A droplet generating apparatus 1 shown in FIG. 3 includes a container 3 for storing a liquid 2 in a continuous phase, and a plate-shaped porous member 4 disposed inside the container 3. As shown in FIG. 1, a large number of ejection holes 5 are provided in the annular region of the porous member 4.
Are arranged. In the annular region of the porous member 4 in which the ejection holes 5 are arranged, a plurality of air spaces 6 in which the ejection holes 5 are not arranged are provided at intervals in the circumferential direction. A housing 7 is provided below the porous member 4, and a tank 8 for storing the liquid to be dropletized is provided in the housing 7 with a pipe 9.
And a pump 10. Thus, the liquid to be dropletized supplied to the porous member 4 is ejected from the ejection holes 5 into the liquid 2 in a continuous phase state. A piezoelectric vibrator 11 for vibrating the ejected liquid is provided inside the housing 7. In order to disperse the liquid to be formed into droplets ejected from the ejection hole 5 in accordance with the frequency of the vibrator 11 to produce a uniform droplet group, the droplet diameter to be produced, the continuous phase According to the physical properties of the liquid 2 in the state or the physical properties of the liquid to be dropletized,
It is necessary to determine the diameter and arrangement pitch of the ejection holes 5 and the ejection speed and frequency of the liquid to be dropletized by trial and error. [0014] The diameter of the ejection hole 5 is determined by the liquid 2 in a continuous phase.
Although it is affected by various factors including physical properties of the liquid to be formed into droplets and conditions of vibration, it is mainly determined by the size of the droplet to be formed. Generally, the size of the droplet to be formed is 20 to 10000 μm, and the diameter of the ejection hole 5 is 1 μm.
It is 0 to 5000 μm. The flow of the liquid to be formed into droplets ejected from the ejection holes 5 needs to be laminar in order to obtain a uniform droplet group. Therefore, when the density of the liquid to be dropletized is ρ, the ejection speed is u, the diameter of the orifice hole is D, and the viscosity of the liquid to be dropletized is μ, Re = D · u · ρ / μ. The Reynolds number is 10 to 2000, preferably 15 to 10
00, particularly preferably 20 to 300. If the Reynolds number is less than 10, the flow rate is small and the production efficiency is low, and if it exceeds 2,000, a turbulent region is formed, so that a uniform droplet group is not generated. The means for vibrating the liquid to be formed into droplets ejected from the ejection holes 5 may be any means having a vibration characteristic capable of dispersing the ejected flow into a uniform group of droplets. 10 to 50,000 Hz is preferred. As a specific vibration means, a mechanical vibrator, an electroacoustic vibrator, a hydroacoustic vibrator, an electromagnetic vibrator, a magnetoresistive transducer, etc. can be used, and these vibrators are connected to a porous member. Then, the porous member may be vibrated, or the liquid to be dropletized may be vibrated as shown in FIG. The arrangement pitch P of the ejection holes 5 is preferably at least 15 times the hole diameter, and the circumferential width s of the air space 6 is set to be larger than the pitch P. The number of the airspaces 6 is preferably 2 to 30, and more preferably 3 to 15. The total of the circumferential width s of the airspace 6 is 0.1 to 0.8 times, preferably 0.2 to 0.7 times, the circumferential length of the annular region. When the radius from the center to the outer diameter of the annular region in which the ejection holes 5 are arranged is r, the inner diameter is preferably 0.3 r or more, preferably 0.5 r or more, and more preferably 0.7 r or more. Above. Further, although the respective ejection holes 5 are arranged on each side of the polygon in FIG. 1, they may be arranged on the circumference, and the specific arrangement is not limited as long as they are arranged in an annular region. In the above-described droplet generating apparatus 1, a 1 wt% PVA solution is stored in the container 3 as the liquid 2 in the continuous phase state, and a monomer solution is supplied to the porous member 4 as a liquid to be dropletized, and is discharged from the ejection hole 5 It is ejected at a flow rate of 1.2 g / min per hole, and the ejected flow is applied to the
A sinusoidal vibration of z was applied. As the monomer solution, a solution of lauroyl acrylate / vinyl acetate / divinylbenzene / lauroyl peroxide = 80/10/9/1 was used. In addition, the diameter of the ejection hole 5 is 80 μm, the arrangement pitch P is 1.5 mm, and as shown in FIG. An airspace 6 not arranged was provided. The sum of the circumferential widths of the six airspaces was 0.18 times the circumferential length of the annular area. The radius of the circumscribed circle of the annular region was 13.5 mm. As a result, a very uniform monodispersed droplet 12 was produced as shown in FIG. That is, the droplet 1
The ascending flow of 2 rises with the surrounding PVA solution 2,
Droplets 12 are located both between the center of the upward flow of the droplet and the circumferential direction.
There is a region where there is no. Since the area where the droplets do not exist becomes a passage for the PVA solution 2 toward the center of the upward flow, the contraction of the upward flow of the droplets 12 is reduced, and the collision of the droplets 12 is prevented. The resulting droplets were polymerized by a conventional method, and as a result, polymer beads having a uniform diameter of about 265 μm were obtained. According to the droplet generating apparatus of the present invention, a plurality of cavities in which the ejection holes are not arranged at intervals in the circumferential direction are formed in the annular region of the porous member in which a large number of ejection holes are arranged. The droplets can be made uniform with a simple configuration of providing the droplets.

【図面の簡単な説明】 【図1】本発明の実施形態に係る液滴生成装置の多孔部
材の平面図 【図2】本発明の実施形態に係る液滴生成装置の作用説
明図 【図3】本発明の実施形態に係る液滴生成装置の構成説
明図 【図4】従来例に係る液滴生成装置の作用説明図 【図5】従来例に係る液滴生成装置の多孔部材の平面図 【符号の説明】 1 液滴生成装置 2 連続相状態の液体 3 容器 4 多孔部材 5 噴出孔 6 空域 10 ポンプ 11 圧電振動子
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a plan view of a porous member of a droplet generation device according to an embodiment of the present invention. FIG. 2 is an operation explanatory diagram of a droplet generation device according to an embodiment of the present invention. FIG. 4 is an explanatory diagram of a configuration of a droplet generating device according to an embodiment of the present invention. FIG. 4 is an explanatory diagram of an operation of a droplet generating device according to a conventional example. FIG. [Description of Signs] 1 Droplet generating device 2 Liquid in continuous phase 3 Container 4 Porous member 5 Spouting hole 6 Airspace 10 Pump 11 Piezoelectric vibrator

───────────────────────────────────────────────────── フロントページの続き (72)発明者 玉置 清二 和歌山県和歌山市湊1334番地花王株式会 社研究所内 (72)発明者 長崎 宏宣 和歌山県和歌山市湊1334番地花王株式会 社研究所内 (56)参考文献 特開 平3−249931(JP,A) 特開 平2−305802(JP,A) (58)調査した分野(Int.Cl.7,DB名) C08F 2/00 - 2/60 B01J 2/06 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Seiji Tamaki 1334 Minato, Wakayama, Wakayama Pref. References JP-A-3-249931 (JP, A) JP-A-2-305802 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) C08F 2/00-2/60 B01J 2 / 06

Claims (1)

(57)【特許請求の範囲】 【請求項1】 連続相状態の液体を貯留する容器と、こ
の容器の内部に配置される多数の噴出孔を有する多孔部
材と、この多孔部材に液滴化対象液を供給する手段と、
その噴出孔から噴出される液滴化対象液を振動させる手
段とを備え、その多数の噴出孔が環状領域に配列されて
いる液滴生成装置であって、前記噴出孔が配列される多
孔部材の環状領域に、周方向に間隔をおいて噴出孔が配
列されない複数の空域が設けられ、前記空域の周方向幅
は前記噴出孔の配列ピッチよりも大きくされていること
を特徴とする液滴生成装置。
(57) [Claim 1] A container for storing a liquid in a continuous phase state, a porous member having a large number of ejection holes disposed inside the container, and droplets formed on the porous member. Means for supplying a target liquid;
Means for vibrating the liquid to be dropletized to be ejected from the ejection holes, wherein the plurality of ejection holes are arranged in an annular region, wherein the porous member in which the ejection holes are arranged In the annular region, a plurality of air spaces in which the ejection holes are not arranged at intervals in the circumferential direction are provided , and a circumferential width of the air space is provided.
The droplet generation device according to claim 1, wherein the arrangement pitch is larger than the arrangement pitch of the ejection holes .
JP34206899A 1999-12-01 1999-12-01 Droplet generator Expired - Fee Related JP3467220B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
JP34206899A JP3467220B2 (en) 1999-12-01 1999-12-01 Droplet generator

Publications (2)

Publication Number Publication Date
JP2001151803A JP2001151803A (en) 2001-06-05
JP3467220B2 true JP3467220B2 (en) 2003-11-17

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Application Number Title Priority Date Filing Date
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Country Link
JP (1) JP3467220B2 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005044035A1 (en) * 2005-09-14 2007-03-15 Basf Ag Method for dripping liquids

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JP2001151803A (en) 2001-06-05

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