JP3375700B2 - Manufacturing method of electrorheological fluid - Google Patents
Manufacturing method of electrorheological fluidInfo
- Publication number
- JP3375700B2 JP3375700B2 JP30831593A JP30831593A JP3375700B2 JP 3375700 B2 JP3375700 B2 JP 3375700B2 JP 30831593 A JP30831593 A JP 30831593A JP 30831593 A JP30831593 A JP 30831593A JP 3375700 B2 JP3375700 B2 JP 3375700B2
- Authority
- JP
- Japan
- Prior art keywords
- dispersion medium
- membrane
- electrorheological fluid
- monomer
- producing
- 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
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- Lubricants (AREA)
- Polymerisation Methods In General (AREA)
Description
【発明の詳細な説明】Detailed Description of the Invention
【０００１】[0001]
【産業上の利用分野】本発明は、新規な電気粘性流体の
作製方法に関するものである。FIELD OF THE INVENTION The present invention relates to a novel method for producing an electrorheological fluid.
【０００２】[0002]
【従来の技術と解決しようとする課題】電気粘性流体
は、親水性の固体粒子からなる分散相で電気絶縁性の分
散媒の中に分散せしめてなる懸濁液で、電場の作用の
下、可逆的にその流体の粘度を変化させることのできる
ものであり、例えば自動車のエンジンマウント、クラッ
チ、ブレーキなどに用いられる。２個の導電性部材の表
面間にこの流体をおき、そこに電圧を印加することによ
りその流体に粘性の可逆的増減をおこさせて導電性部材
が回転体の場合には、両部材表面間にトルクを制御して
伝達させることができる。2. Description of the Related Art An electrorheological fluid is a suspension obtained by dispersing a hydrophilic solid particle in a disperse medium having an electrically insulating property in a dispersed phase. It is capable of reversibly changing the viscosity of the fluid, and is used, for example, in automobile engine mounts, clutches, brakes and the like. If this fluid is placed between the surfaces of two conductive members and a voltage is applied to the fluid to cause the fluid to reversibly increase or decrease its viscosity, and if the conductive member is a rotating body, the space between the surfaces of both members is increased. The torque can be controlled and transmitted to.
【０００３】このような電気粘性流体としては従来各種
分散相からなるものが提案され、例えば多価アルコール
粒子を分散させた流体（特開昭５１−３３７８３号公
報）やアクリレート乃至メタクリレート系ポリマーの固
体粒子を分散させた流体（特公昭６３−２６１５１号公
報）などが知られている。As such an electrorheological fluid, there have conventionally been proposed fluids composed of various dispersed phases. For example, a fluid in which polyhydric alcohol particles are dispersed (JP-A-51-33783) or a solid of an acrylate or methacrylate polymer. A fluid in which particles are dispersed (Japanese Patent Publication No. Sho 63-26151) is known.
【０００４】このように電気粘性流体の製造方法は種々
提案されているが、本発明者らもさきに１ミクロン以下
の微粒子を用いて充分な電気粘性効果による粘度変化を
示す電気粘性流体を開発するべく研究して逆相懸濁重合
法、逆乳化重合法などにより親水性ポリマー粒子を作製
するに当り超音波を用いて分散させてミクロエマルジョ
ンをつくる方法を開発し特許出願した（特願平５−１４
５１８０号）。As described above, various methods for producing an electrorheological fluid have been proposed, but the present inventors have previously developed an electrorheological fluid which exhibits a sufficient viscosity change due to the electrorheological effect by using fine particles of 1 micron or less. In order to make hydrophilic polymer particles by reverse phase suspension polymerization method, inverse emulsion polymerization method, etc., ultrasonic wave was used to disperse them to form a microemulsion. 5-14
5180).
【０００５】この方法によるときは粒子径１ミクロン以
下にして且つシャープな粒度分布に制御されたミクロエ
マルジョンがえられ、これから充分な電気粘性効果を有
する電気粘性流体がえられる。According to this method, a microemulsion having a particle size of 1 micron or less and a controlled sharp particle size distribution is obtained, and from this, an electrorheological fluid having a sufficient electrorheological effect is obtained.
【０００６】本発明者らはかかる逆相懸濁重合法、逆乳
化重合法により電気粘性流体を製造する方法について更
に研究を進めたところ、分散媒中に分散相を分散させて
エマルジョンをつくるに当って膜乳化装置を用いて分散
させることにより、粒度分布の狭い粒子径の制御し易い
粒子からなるミクロエマルジョンを得、これより有効な
電気粘性流体を得ることができることを見い出して本発
明に至ったものである。The present inventors have conducted further research on a method for producing an electrorheological fluid by such a reverse phase suspension polymerization method and a reverse emulsion polymerization method. As a result, a dispersion phase is dispersed in a dispersion medium to form an emulsion. By using a membrane emulsifier to disperse the microemulsion, a microemulsion composed of particles whose particle size distribution is narrow and whose particle size can be easily controlled is obtained. It is a thing.
【０００７】[0007]
【課題を解決するための手段】よって本発明は疎水性、
電気絶縁性液体からなる分散媒に親水性モノマーを分散
させて逆ミセルあるいは油中水滴型ミクロエマルジョン
をつくり、後上記モノマーを重合せしめて電気粘性流体
を製造する方法において、前記分散の手段として膜乳化
装置を用いることを特徴とする電気粘性流体の製法を提
供するものである。Therefore, the present invention is hydrophobic.
In a method for producing an electrorheological fluid by dispersing a hydrophilic monomer in a dispersion medium made of an electrically insulating liquid to form a reverse micelle or a water-in-oil type microemulsion, and then polymerizing the monomer, a membrane is used as the dispersing means. The present invention provides a method for producing an electrorheological fluid characterized by using an emulsifying device.
【０００８】以下、本発明について詳しく説明する。ま
ず、本発明について分散媒として用いられる疎水性電気
絶縁性液体としてシリコンオイル、トルエン、フッ素オ
イル等が用いられ、この中特にシリコンオイルが好んで
用いられる。この分散媒には通常界面活性剤等の分散剤
が加えられる。この分散剤としてはたとえば有機官能基
変性シリコンオイルを用いるのが、好ましい。この変性
シリコンオイルとしてはたとえば日本ユニカーkkからＭ
ＡＣ２１０１の商品名で市販されていたものがある。The present invention will be described in detail below. First, as the hydrophobic electrically insulating liquid used as the dispersion medium in the present invention, silicone oil, toluene, fluorine oil and the like are used, and among them, silicone oil is particularly preferably used. A dispersant such as a surfactant is usually added to this dispersion medium. As the dispersant, for example, organic functional group-modified silicone oil is preferably used. As this modified silicone oil, for example, M from Nippon Unicar kk
There is a product sold under the trade name of AC2101.
【０００９】かくて上記疎水性液体に、たとえば有機官
能基変性シリコンオイルを約１％量溶解させて分散媒と
する。Thus, for example, about 1% of an organic functional group-modified silicone oil is dissolved in the above hydrophobic liquid to form a dispersion medium.
【００１０】次にこの分散媒に分散相として分散される
親水性モノマーとしては特に限定はないがアクリル酸、
メタクリル酸またはこれらの金属塩等の親水性モノマー
が好んで用いられる。通常このモノマーに対して更に架
橋剤、重合開始剤等が用いられる。架橋剤としては例え
ばＮ，Ｎ−メチレンビスアクリルアミドのような２官能
性乃至多官能性の試薬が好んで用いられる。重合開始剤
としてたとえば過硫酸カリウムが用いられる。Next, the hydrophilic monomer dispersed as a dispersed phase in this dispersion medium is not particularly limited, but acrylic acid,
A hydrophilic monomer such as methacrylic acid or a metal salt thereof is preferably used. Usually, a crosslinking agent, a polymerization initiator or the like is further used for this monomer. As the cross-linking agent, a bifunctional or polyfunctional reagent such as N, N-methylenebisacrylamide is preferably used. For example, potassium persulfate is used as the polymerization initiator.
【００１１】このように疎水性電気絶縁性液体からなる
分散媒に親水性モノマーからなる分散相を分散させる手
段として、本発明では膜乳化装置を用いるのである。こ
こに膜乳化装置は微細な孔を有する多孔質膜、好ましく
はシラスよりつくられたシラスポーラスガラス等の多孔
質ガラス膜にモノマーを通して分散媒中に一定粒径の液
滴からなるエマルジョンを得る装置である。上記シラス
ポーラスガラス（ＳＰＧ）を用いる場合、ガラス膜本体
中の細孔径はシラス原料の熱処理温度と処理時間によっ
て調整することができる。通常この細孔径は０．０３〜
１０ミクロンの大きさを有する。ＳＰＧ膜を通して液滴
を形成する場合、膜孔径の約３倍の大きさになる。よっ
て、所定の大きさの液滴を得るには、ＳＰＧ膜の孔径を
制御することで可能である。In the present invention, a membrane emulsifying device is used as a means for dispersing the dispersed phase composed of the hydrophilic monomer in the dispersion medium composed of the hydrophobic electrically insulating liquid. Here, the membrane emulsification device is a device for obtaining an emulsion consisting of droplets of a certain particle size in a dispersion medium by passing a monomer through a porous membrane having fine pores, preferably a porous glass membrane such as shirasu porous glass made of shirasu. Is. When the above-mentioned shirasu porous glass (SPG) is used, the pore size in the glass film body can be adjusted by the heat treatment temperature and the treatment time of the shirasu raw material. Usually this pore size is 0.03 ~
It has a size of 10 microns. When a droplet is formed through the SPG film, the size is about three times the film pore size. Therefore, it is possible to obtain a droplet of a predetermined size by controlling the pore diameter of the SPG film.
【００１２】かかる膜乳化装置の一例の略図を図１に示
す。この図において、容器１、２には夫々モノマー３、
分散媒４が充填されている。５は多孔質ガラス膜モジュ
ールである。A schematic view of an example of such a film emulsifying apparatus is shown in FIG. In this figure, the containers 1 and 2 are respectively provided with a monomer 3,
The dispersion medium 4 is filled. 5 is a porous glass membrane module.
【００１３】乳化の操作は以下の手順で行う。
まず分散媒４をポンプ１３で経路１４に供給し、膜
モジュール５に通す。
分散媒４は膜モジュール５内の膜６の内側７を通
る。
膜モジュール５を出た分散媒４は再び容器２に戻
る。
分散媒４をたえず循環させておく。
モノマー３を加圧ポンプ８で経路９に供給し膜モジ
ュール５に通す。
モノマー３は膜モジュール５内の膜６の外側１５を
通る。このときモノマー３と分散媒４は膜６で分けられ
ている。
圧力計１０をみながら徐々に加圧していくと、ある
圧力で膜６を通ってモノマー３が分散媒４中へ入り、均
一なミクロエマルジョンを形成する。
モノマーがなくなるまで供給する。分散媒は循環さ
せておく。
以上の操作により均一な液滴径のミクロエマルジョ
ンが得られる。
図１において１１，１２は圧力計である。The emulsification operation is performed according to the following procedure. First, the dispersion medium 4 is supplied to the path 14 by the pump 13 and passed through the membrane module 5. The dispersion medium 4 passes through the inside 7 of the membrane 6 in the membrane module 5. The dispersion medium 4 exiting the membrane module 5 returns to the container 2 again. The dispersion medium 4 is constantly circulated. The monomer 3 is supplied to the passage 9 by the pressure pump 8 and passed through the membrane module 5. Monomer 3 passes outside 15 of membrane 6 in membrane module 5. At this time, the monomer 3 and the dispersion medium 4 are separated by the film 6. When the pressure is gradually increased while watching the pressure gauge 10, the monomer 3 enters the dispersion medium 4 through the membrane 6 at a certain pressure to form a uniform microemulsion. Feed until there is no monomer. The dispersion medium is circulated. By the above operation, a microemulsion having a uniform droplet size can be obtained. In FIG. 1, 11 and 12 are pressure gauges.
【００１４】このようにしてえられた分散液を用いて重
合した後調整して作製された電気粘性流体は粒度分布の
狭いかつ粒子径の制御しやすい粒子を分散相とし、充分
な電気粘性効果を有している。The electrorheological fluid prepared by polymerizing the dispersion obtained in this way and then adjusting it has particles having a narrow particle size distribution and easy to control the particle size as the dispersed phase, and has a sufficient electrorheological effect. have.
【００１５】[0015]
【実施例】以下、実施例により本発明を説明するが、本
発明の範囲がこれら実施例のみに限定されるものではな
い。EXAMPLES The present invention will be described below with reference to examples, but the scope of the present invention is not limited to these examples.
【００１６】容量２０００cm3 のビーカーーに信越化学
工業（株）製ＫＦ５６（フェニルシリコンオイル）を１
５００cm3 入れた。次に分散剤の日本ユニカー（株）Ｍ
ＡＣ２１０１ １５．００ｇをシリコンオイルに溶解さ
せた。これを「分散媒」とする。A KF56 (phenyl silicone oil) manufactured by Shin-Etsu Chemical Co., Ltd. was placed in a beaker having a capacity of 2000 cm 3.
I put in 500 cm 3 . Next, the dispersant, Nippon Unicar Co., Ltd. M
15.00 g of AC2101 was dissolved in silicone oil. This is referred to as "dispersion medium".
【００１７】次にアクリル酸（和光純薬工業（株）製）
１８．８ｇに３０．８ｇの水酸化ナトリウム（和光純薬
工業（株）製）２５．４％水溶液で氷冷しつつ中和し、
アクリル酸ナトリウム水溶液に調整した後室温に戻し
た。これを「モノマー」とする。Next, acrylic acid (manufactured by Wako Pure Chemical Industries, Ltd.)
18.8 g was neutralized with 30.8 g of a 25.4% aqueous solution of sodium hydroxide (manufactured by Wako Pure Chemical Industries, Ltd.) while cooling with ice.
After adjusting to an aqueous sodium acrylate solution, the temperature was returned to room temperature. This is referred to as "monomer".
【００１８】添付図１の膜乳化装置の容器１に「分散
媒」を、容器２に「モノマー」をそれぞれ入れる。「分
散媒」を循環させながら「モノマー」を適当な条件で加
圧しつつ多孔質膜モジュール５の細孔径約０．２ミクロ
ンのＳＰＧ膜６を通して液滴を形成させた。形成させた
液滴の粒度分布を図２に示す。これにより粒度分布の狭
い液滴のミクロエマルジョンのえられていることが明ら
かであろう。図２において●は液滴の度数分布を、○は
その積算値分布を示す。The "dispersion medium" is put in the container 1 and the "monomer" is put in the container 2 of the membrane emulsification device of the attached FIG. Droplets were formed through the SPG film 6 of the porous membrane module 5 having a pore size of about 0.2 micron while pressurizing the "monomer" under appropriate conditions while circulating the "dispersion medium". The particle size distribution of the formed droplets is shown in FIG. From this, it is clear that a microemulsion of droplets having a narrow particle size distribution is obtained. In FIG. 2, ● indicates the frequency distribution of the droplets, and ○ indicates the integrated value distribution thereof.
【図１】膜乳化装置略図FIG. 1 Schematic diagram of membrane emulsification device
【図２】膜乳化装置による生成液滴の粒度分布測定結果
を示すグラフFIG. 2 is a graph showing the measurement result of particle size distribution of generated droplets by a film emulsification device.
１，２ 容器 ３ 親水性モノマー ４ 分散媒 ５ 多孔質ガラス膜モジュール ６ 膜（ＳＰＧ膜） ７ 膜内部 ８ 加圧ポンプ ９ モノマー経路 １０，１１，１２ 圧力計 １３ 供給ポンプ １４ 分散媒経路 １５ 膜外部 1, 2 containers 3 Hydrophilic monomer 4 dispersion medium 5 Porous glass membrane module 6 film (SPG film) 7 Inside the membrane 8 pressure pump 9 Monomer pathway 10, 11, 12 pressure gauge 13 Supply pump 14 Dispersion medium path 15 outside the membrane
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ Ｃ１０Ｎ 30:04 Ｃ１０Ｎ 30:04 40:14 40:14 70:00 70:00 (56)参考文献 特開 平７−3282（ＪＰ，Ａ) 特開 平７−3281（ＪＰ，Ａ) 特開 平５−320683（ＪＰ，Ａ) 特開 平６−1854（ＪＰ，Ａ) 特開 平６−49104（ＪＰ，Ａ) 特開 平５−295265（ＪＰ，Ａ) 特開 平３−79605（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C10M 177/00 C10M 155/02 C10M 171/06 C10N 20:06 C10N 30:04 C10N 40:14 C10N 70:00 C08F 2/22 - 2/32 ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 7 Identification code FI C10N 30:04 C10N 30:04 40:14 40:14 70:00 70:00 (56) References Japanese Patent Laid-Open No. 7-3228 ( JP, A) JP 7-3281 (JP, A) JP 5-320683 (JP, A) JP 6-1854 (JP, A) JP 6-49104 (JP, A) JP HEI 5-295265 (JP, A) JP HEI 3-79605 (JP, A) (58) Fields investigated (Int.Cl. 7 , DB name) C10M 177/00 C10M 155/02 C10M 171/06 C10N 20 : 06 C10N 30:04 C10N 40:14 C10N 70:00 C08F 2/22-2/32
Claims (4)
親水性モノマーを分散させて逆ミセルあるいは油中水滴
型ミクロエマルジョンをつくり、後上記モノマーを重合
せしめて電気粘性流体を製造する方法において、前記分
散の手段として膜乳化装置を用いることを特徴とする電
気粘性流体の製法。1. A method of producing an electrorheological fluid by dispersing a hydrophilic monomer in a dispersion medium composed of a hydrophobic and electrically insulating liquid to prepare a reverse micelle or a water-in-oil type microemulsion, and then polymerizing the monomer. 2. A method for producing an electrorheological fluid, characterized in that a film emulsifying device is used as the means for dispersing.
有機官能基変性シリコンオイルを溶解させたものが用い
られる請求項１記載の方法。2. The method according to claim 1, wherein the dispersion medium is a hydrophobic electrically insulating liquid in which organic functional group-modified silicone oil is dissolved.
ラス膜が用いられる請求項１記載の方法。3. The method according to claim 1, wherein a porous glass membrane is used as the membrane in the membrane emulsifying device.
流体。4. An electrorheological fluid produced by the method of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30831593A JP3375700B2 (en) | 1993-12-08 | 1993-12-08 | Manufacturing method of electrorheological fluid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30831593A JP3375700B2 (en) | 1993-12-08 | 1993-12-08 | Manufacturing method of electrorheological fluid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07157788A JPH07157788A (en) | 1995-06-20 |
| JP3375700B2 true JP3375700B2 (en) | 2003-02-10 |
Family
ID=17979577
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30831593A Expired - Fee Related JP3375700B2 (en) | 1993-12-08 | 1993-12-08 | Manufacturing method of electrorheological fluid |
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| Country | Link |
|---|---|
| JP (1) | JP3375700B2 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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1993
- 1993-12-08 JP JP30831593A patent/JP3375700B2/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| JPH07157788A (en) | 1995-06-20 |
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