JP2001181309A - Method for manufacturing fine mono disperse solid particle - Google Patents
Method for manufacturing fine mono disperse solid particleInfo
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- JP2001181309A JP2001181309A JP36925699A JP36925699A JP2001181309A JP 2001181309 A JP2001181309 A JP 2001181309A JP 36925699 A JP36925699 A JP 36925699A JP 36925699 A JP36925699 A JP 36925699A JP 2001181309 A JP2001181309 A JP 2001181309A
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- emulsion
- fine particles
- solid fine
- continuous phase
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、医薬、化粧品、液
晶表示装置用スペーサ、標準粒子、分析用充填材、診断
薬の担体、各種標識材等に用いられる単分散固体微粒子
の製造方法に関する。The present invention relates to a method for producing monodispersed solid fine particles used for medicines, cosmetics, spacers for liquid crystal display devices, standard particles, analytical fillers, carriers for diagnostic agents, various labeling materials and the like.
【０００２】[0002]
【従来の技術】固体微粒子の製造方法としては従来から
懸濁重合法や乳化重合法が知られている。懸濁重合法
は、エマルションの分散相を重合させて固体微粒子を合
成する方法であり、乳化重合法は、界面活性剤ミセル中
で重合反応を行うことにより固体微粒子を合成する方法
である。2. Description of the Related Art Suspension polymerization and emulsion polymerization have been known as methods for producing solid fine particles. The suspension polymerization method is a method of synthesizing solid fine particles by polymerizing a dispersion phase of an emulsion, and the emulsion polymerization method is a method of synthesizing solid fine particles by performing a polymerization reaction in a surfactant micelle.
【０００３】このような懸濁重合法では、作製される固
体微粒子の粒径分布は重合前のエマルションの粒径分布
に依存するため、単分散固体微粒子を作製することが困
難である。また、乳化重合法で通常合成できる固体微粒
子の粒径は０．１μｍ程度であり、数μｍ以上の固体微
粒子の合成は困難である。In such a suspension polymerization method, it is difficult to produce monodispersed solid fine particles because the particle size distribution of the solid fine particles produced depends on the particle size distribution of the emulsion before polymerization. The particle size of solid fine particles that can be usually synthesized by an emulsion polymerization method is about 0.1 μm, and it is difficult to synthesize solid fine particles of several μm or more.
【０００４】[0004]
【発明が解決しようとする課題】本発明は、上記現状に
鑑み、粒径が数μｍ以上の単分散固体微粒子の製造方法
を提供することを目的とする。SUMMARY OF THE INVENTION In view of the above situation, an object of the present invention is to provide a method for producing monodispersed solid fine particles having a particle size of several μm or more.
【０００５】[0005]
【課題を解決するための手段】本発明は、反応性モノマ
ーを重合させてなる単分散固体微粒子を製造する方法で
あって、（１）反応性モノマーを含む分散相用組成物を
加圧し、上記分散相用組成物をマイクロチャネルを介し
て連続相中に分散せしめてエマルションを生成する工
程、（２）上記エマルションを重合させることにより固
体微粒子のサスペンジョンを作製する工程、及び、
（３）上記サスペンジョンから連続相を除去することに
より固体微粒子を回収する工程からなる単分散固体微粒
子の製造方法である。以下に本発明を詳述する。SUMMARY OF THE INVENTION The present invention provides a method for producing monodisperse solid fine particles obtained by polymerizing a reactive monomer, wherein (1) a composition for a dispersed phase containing a reactive monomer is pressurized, A step of dispersing the composition for a dispersed phase in a continuous phase through a microchannel to form an emulsion, (2) a step of producing a suspension of solid fine particles by polymerizing the emulsion, and
(3) A method for producing monodisperse solid fine particles, comprising a step of collecting solid fine particles by removing a continuous phase from the suspension. Hereinafter, the present invention will be described in detail.
【０００６】本発明の単分散固体微粒子の製造方法は、
反応性モノマーを重合させてなる。上記反応性モノマー
としては、エマルションを生成して重合によって固体微
粒子を作製することができるものであれば特に限定され
ず、例えば、炭素−炭素二重結合を有する重合性モノマ
ー等が挙げられ、固体微粒子の用途に応じて適宜選定す
ればよい。The method for producing monodisperse solid fine particles of the present invention comprises:
It is obtained by polymerizing a reactive monomer. The reactive monomer is not particularly limited as long as it can produce an emulsion to produce solid fine particles by polymerization, and examples thereof include a polymerizable monomer having a carbon-carbon double bond and the like. What is necessary is just to select suitably according to the use of a microparticle.
【０００７】本発明の単分散固体微粒子の製造方法は、
（１）、（２）及び（３）の工程からなる。上記（１）
の工程は、反応性モノマーを含む分散相用組成物を加圧
し、上記分散相用組成物をマイクロチャネルを介して連
続相中に分散せしめてエマルションを生成する工程であ
る。上記反応性モノマーを含む分散相用組成物は、反応
性モノマー以外の成分を含んでいてもよい。The method for producing monodisperse solid fine particles of the present invention comprises:
It comprises the steps (1), (2) and (3). The above (1)
Is a step of pressurizing the composition for a dispersed phase containing a reactive monomer and dispersing the composition for a dispersed phase in a continuous phase through a microchannel to form an emulsion. The composition for a dispersed phase containing the reactive monomer may contain a component other than the reactive monomer.
【０００８】上記（１）の工程において、固体微粒子の
単分散性を良好とするため、界面活性剤を連続相若しく
は分散相用組成物のいずれか又は両方に添加することが
好ましい。上記界面活性剤としては特に限定されず、例
えば、反応性モノマーの種類、連続相の種類、固体微粒
子の用途等に応じて適宜選定すればよい。上記反応性モ
ノマーを含む分散相用組成物を加圧する圧力としては特
に限定されず、例えば、分散相に要求される大きさ；製
造効率等に応じて適宜設定すればよい。In step (1), a surfactant is preferably added to either or both of the composition for the continuous phase and the dispersed phase in order to improve the monodispersibility of the solid fine particles. The surfactant is not particularly limited, and may be appropriately selected depending on, for example, the type of the reactive monomer, the type of the continuous phase, the use of the solid fine particles, and the like. The pressure at which the composition for a dispersed phase containing the reactive monomer is pressed is not particularly limited, and may be appropriately set according to, for example, the size required for the dispersed phase; production efficiency and the like.
【０００９】上記マイクロチャネルとは、分散相用組成
物を連続相中に分散せしめて分散相を形成させることが
できる一定の形状からなる間隙を意味する。上記マイク
ロチャネルは、製造効率が向上することから、多数の一
定の形状からなる間隙により形成されていることが好ま
しい。上記分散相用組成物をマイクロチャネルを介して
連続相中に分散せしめることにより、分散相用組成物を
連続相中で均一な大きさの微粒子（マイクロスフィア）
からなる分散相とすることができる。上記（１）の工程
において、エマルションを生成する装置としては特に限
定されず、例えば、本出願人が特願平１１−７８８６２
号で提案した装置等を使用することができる。[0009] The above-mentioned microchannel means a gap having a certain shape that can form a dispersed phase by dispersing a composition for a dispersed phase in a continuous phase. It is preferable that the microchannel is formed by a large number of gaps having a constant shape, since manufacturing efficiency is improved. By dispersing the composition for a dispersed phase in a continuous phase through a microchannel, the composition for a dispersed phase can be made into fine particles (microspheres) having a uniform size in the continuous phase.
Can be obtained. In the step (1), an apparatus for producing an emulsion is not particularly limited. For example, the present applicant has filed a Japanese Patent Application No. 11-78862.
And the like.
【００１０】上記（２）の工程は、上記エマルションを
重合させることにより固体微粒子のサスペンジョンを作
製する工程である。上記（２）の工程において、エマル
ションを重合させることにより分散相を形成する微粒子
を固化して固体微粒子のサスペンジョンを作製すること
ができる。上記エマルションの重合方法としては特に限
定されず、例えば、エマルションに重合開始剤を添加し
てから温度を上昇させる方法；あらかじめ重合開始剤を
分散相用組成物に溶解させておいて（１）の工程でエマ
ルションを作製した後、温度を上昇させる方法；光重合
開始剤を用いて特定波長の光を照射する方法等が挙げら
れ、反応性モノマーの種類、反応性、用途等により適宜
選定すればよい。The step (2) is a step of producing a suspension of solid fine particles by polymerizing the emulsion. In the step (2), fine particles forming a dispersed phase are solidified by polymerizing the emulsion, whereby a suspension of solid fine particles can be produced. The method of polymerizing the emulsion is not particularly limited. For example, a method in which a polymerization initiator is added to the emulsion and the temperature is then increased; After the emulsion is prepared in the process, a method of raising the temperature; a method of irradiating light of a specific wavelength using a photopolymerization initiator, and the like. Good.
【００１１】上記重合においては、重合時に粒子同士の
合着を防止するため、エマルションに分散剤を添加して
から重合することが好ましい。また、（１）の工程にお
けるエマルション生成時に、分散相用組成物若しくは連
続相のいずれか又は両方に分散剤を添加することもでき
る。In the above polymerization, in order to prevent coalescence of particles during polymerization, it is preferable to perform polymerization after adding a dispersant to the emulsion. Further, a dispersant may be added to either or both of the composition for the dispersed phase and the continuous phase during the formation of the emulsion in the step (1).
【００１２】上記（３）の工程は、上記サスペンジョン
から連続相を除去することにより固体微粒子を回収する
工程である。上記（３）の工程において、サスペンジョ
ンから連続相を除去し、固体微粒子を回収する方法とし
ては特に限定されず、例えば、真空乾燥法、噴霧乾燥法
等の乾燥方法を用いることができる。また、固体微粒子
の用途によって、未反応モノマー、界面活性剤、分散剤
等が残存すると問題がある場合は、連続相を除去する前
に、抽出操作等により固体微粒子を洗浄することが好ま
しい。The step (3) is a step of recovering solid fine particles by removing a continuous phase from the suspension. In the step (3), the method of removing the continuous phase from the suspension and collecting the solid fine particles is not particularly limited, and for example, a drying method such as a vacuum drying method and a spray drying method can be used. If there is a problem that unreacted monomers, surfactants, dispersants and the like remain depending on the use of the solid fine particles, it is preferable to wash the solid fine particles by an extraction operation or the like before removing the continuous phase.
【００１３】本発明の単分散固体微粒子の製造方法は、
数μｍ以上の単分散固体微粒子を製造することができ
る。上記単分散固体微粒子は、医薬、化粧品、液晶表示
装置用スペーサ、標準粒子、分析用充填剤、診断薬の担
体、各種標識材等に用いることができるものである。The method for producing monodispersed solid fine particles of the present invention comprises:
Monodispersed solid fine particles of several μm or more can be produced. The monodisperse solid fine particles can be used for medicines, cosmetics, spacers for liquid crystal display devices, standard particles, fillers for analysis, carriers for diagnostic agents, various labeling materials, and the like.
【００１４】本発明２は、反応性モノマーを重合させて
なる液晶表示装置用スペーサを製造する方法であって、
（１）反応性モノマーを含む分散相用組成物を加圧し、
上記分散相用組成物をマイクロチャネルを介して連続相
中に分散せしめてエマルションを生成する工程、（２）
上記エマルションを重合させることにより固体微粒子の
サスペンジョンを作製する工程、及び、（３）上記サス
ペンジョンから連続相を除去することにより液晶表示装
置用スペーサを固体微粒子として回収する工程からなる
液晶表示装置用スペーサの製造方法である。[0014] The present invention 2 is a method for producing a spacer for a liquid crystal display device obtained by polymerizing a reactive monomer,
(1) Pressurizing the composition for a dispersed phase containing a reactive monomer,
Dispersing the composition for a dispersed phase in a continuous phase through a microchannel to form an emulsion, (2)
A step of producing a suspension of solid fine particles by polymerizing the emulsion; and (3) a step of collecting a spacer for liquid crystal display devices as solid fine particles by removing a continuous phase from the suspension. It is a manufacturing method of.
【００１５】本発明２の液晶表示装置用スペーサの製造
方法は、本発明１の単分散固体微粒子の製造方法と同様
にして行うことができる。本発明２の液晶表示装置用ス
ペーサの製造方法により得られた液晶表示装置用スペー
サは、粒径が数μｍ以上で単分散性にも優れるものであ
る。上記液晶表示装置用スペーサにより、液晶層の厚み
（セルギャップ）が均一で表示ムラ等の欠陥の少ない液
晶表示装置を得ることができる。The method for manufacturing the spacer for a liquid crystal display device according to the second aspect of the present invention can be performed in the same manner as the method for manufacturing the monodispersed solid fine particles according to the first aspect of the present invention. The spacer for a liquid crystal display device obtained by the method for producing a spacer for a liquid crystal display device according to the second aspect of the present invention has a particle diameter of several μm or more and is excellent in monodispersity. With the spacer for a liquid crystal display device, a liquid crystal display device having a uniform liquid crystal layer thickness (cell gap) and having few defects such as display unevenness can be obtained.
【００１６】[0016]
【発明の実施の形態】以下に本発明の一実施形態を図１
〜５に基づいて説明する。図１は本発明の単分散固体微
粒子の製造方法の概略を工程順に示したブロック図であ
る。上記ブロック図によれば、先ず、反応性モノマーを
含む分散相用組成物を用意する。次いで、（１）工程と
して、この分散相用組成物を加圧し、上記分散相用組成
物をマイクロチャネルを介して水等の連続相中に分散せ
しめてマイクロチャネル乳化を行って、単分散エマルシ
ョンを生成する。次いで、（２）工程として、単分散エ
マルションを加熱等により重合させて単分散サスペンジ
ョンとする。この後、（３）工程として、単分散サスペ
ンジョンから連続相を乾燥除去して単分散固体微粒子を
回収する。DESCRIPTION OF THE PREFERRED EMBODIMENTS One embodiment of the present invention will be described below with reference to FIG.
The description will be made based on .about.5. FIG. 1 is a block diagram showing the outline of the method for producing monodispersed solid fine particles of the present invention in the order of steps. According to the above block diagram, first, a composition for a dispersed phase containing a reactive monomer is prepared. Next, as a step (1), the composition for a dispersed phase is pressurized, and the composition for a dispersed phase is dispersed in a continuous phase such as water through a microchannel to perform microchannel emulsification, thereby obtaining a monodisperse emulsion. Generate Next, as a step (2), the monodispersed emulsion is polymerized by heating or the like to obtain a monodispersed suspension. Thereafter, as a step (3), the continuous phase is dried and removed from the monodispersed suspension to collect monodispersed solid fine particles.
【００１７】以下に単分散エマルションを生成する装置
の一例を図２〜５に基づいて説明する。ここで、図２
は、エマルション生成装置の全体断面図、図３は、同じ
エマルション生成装置の要部の拡大模式図であり、図４
（ａ）は、エマルション生成装置における基板の平面
図、（ｂ）は、エマルション生成装置における基板の裏
面図であり、図５は、マイクロチャネルの部分の拡大斜
視図である。Hereinafter, an example of an apparatus for producing a monodisperse emulsion will be described with reference to FIGS. Here, FIG.
Is an overall cross-sectional view of the emulsion generating apparatus, and FIG. 3 is an enlarged schematic view of a main part of the same emulsion generating apparatus.
(A) is a plan view of a substrate in the emulsion generation device, (b) is a back view of the substrate in the emulsion generation device, and FIG. 5 is an enlarged perspective view of a microchannel portion.
【００１８】図２〜５において、エマルション生成装置
は本体１を恒温槽２につなげて本体１の温度を所定の温
度に制御可能としている。そして、本体１の一方の開口
にガラス板等から構成されるプレート３を嵌め込み、他
方の開口に蓋体４を嵌め込み、蓋体４の中央に分散相用
組成物（Ｏ）の供給口５を形成し、蓋体４の中央から外
れた箇所（図では上方）に連続相（Ｗ）の供給口６を形
成し、更に蓋体４の中央から外れた箇所（図では下方）
にエマルション（Ｅ）の取出口７を形成している。2 to 5, in the emulsion producing apparatus, the main body 1 is connected to a thermostat 2 so that the temperature of the main body 1 can be controlled to a predetermined temperature. Then, a plate 3 made of a glass plate or the like is fitted into one opening of the main body 1, a lid 4 is fitted into the other opening, and a supply port 5 for the dispersed phase composition (O) is placed in the center of the lid 4. A continuous phase (W) supply port 6 is formed at a location (upper in the figure) off the center of the lid 4, and a location (lower in the figure) further off the center of the lid 4.
And an outlet 7 for the emulsion (E).
【００１９】そして、分散相用組成物（Ｏ）の供給口５
には配管を介して分散相用組成物リザーバ８を接続し、
配管の周囲にはヒータ９を設け、また、連続相（Ｗ）の
供給口６には配管を介して連続相リザーバ１０を接続
し、更にエマルション（Ｅ）の取出口７には回収用配管
１１を接続している。ここで、分散相用組成物リザーバ
８及び連続相リザーバ１０は上下位置の調整が可能であ
り、水位差による加圧が行えるよう分散相用組成物
（Ｏ）に作用する圧力及び連続相（Ｗ）に作用する圧力
がそれぞれ調整できる構成になっている。The supply port 5 for the composition for dispersed phase (O)
Is connected to the dispersed phase composition reservoir 8 via a pipe,
A heater 9 is provided around the pipe, a continuous phase reservoir 10 is connected to the continuous phase (W) supply port 6 through the pipe, and a recovery pipe 11 is connected to the emulsion (E) outlet 7. Are connected. Here, the dispersion phase composition reservoir 8 and the continuous phase reservoir 10 can be adjusted up and down, and the pressure acting on the dispersion phase composition (O) and the continuous phase (W ) Can be adjusted respectively.
【００２０】また、プレート３と蓋体４との間の空間に
は基板１２が配置されている。基板１２の中央には開口
１３が形成され、基板１２のプレート３に対向する正面
側には開口１３を矩形状に囲むように突条１４が形成さ
れ、この突条１４の上面を平坦なテラス１５にし、この
テラス１５上に突部１６を一定間隔で多数形成し、これ
ら突部１６、１６間をマイクロチャネル１７としてい
る。マイクロチャネル１７の寸法としては、例えば幅１
６μｍ、高さ２μｍ、テラス長さ３０μｍとする。ま
た、マイクロチャネル１７を含む突条１４の形成方法と
しては、ウェットエッチング又はドライエッチングが適
当である。A substrate 12 is arranged in a space between the plate 3 and the lid 4. An opening 13 is formed at the center of the substrate 12, and a ridge 14 is formed on the front side of the substrate 12 facing the plate 3 so as to surround the opening 13 in a rectangular shape. A large number of protrusions 16 are formed on the terrace 15 at regular intervals, and a microchannel 17 is formed between the protrusions 16. The dimensions of the microchannel 17 are, for example, width 1
6 μm, height 2 μm, terrace length 30 μm. As a method for forming the protrusions 14 including the microchannels 17, wet etching or dry etching is appropriate.
【００２１】更に、基板１２と蓋体４の間にはＯリング
等の隔壁部材１８を介在させ、この隔壁部材１８の弾発
力（弾性力）で上記突部１６をプレート３内側に当接し
ている。そして、隔壁部材１８にて囲まれる内側領域に
は上記分散相用組成物（Ｏ）の供給口５が開口し、外側
領域には連続相（Ｗ）の供給口６及びエマルション
（Ｅ）の取出口７が開口している。尚、プレート３の外
側には、ビデオシステムに繋がるカメラ１９が配置され
ている。Further, a partition member 18 such as an O-ring is interposed between the substrate 12 and the lid 4, and the projection 16 is brought into contact with the inside of the plate 3 by the elastic force (elastic force) of the partition member 18. ing. The supply port 5 for the composition for dispersed phase (O) is opened in the inner region surrounded by the partition member 18, and the supply port 6 for the continuous phase (W) and the emulsion (E) are collected in the outer region. The outlet 7 is open. A camera 19 connected to a video system is arranged outside the plate 3.
【００２２】単分散エマルションを生成する装置として
は、上記の構成に限定されるものではない。例えば、図
１〜５の例にあっては、プレート３、蓋体４及び基板１
２を縦方向に配置したが、これらを水平方向に配置して
もよい。また、他の装置としては、ケース内に基板を配
置し、この基板とプレートとの間に連続相の流路を形成
し、この流路に対し交差する方向に開口するマイクロチ
ャネルを上記基板に形成し、流動状態にある連続相に対
して交差する方向から分散相用組成物を供給するクロス
フロータイプとしてもよい。The apparatus for producing a monodisperse emulsion is not limited to the above-described configuration. For example, in the example of FIGS. 1 to 5, the plate 3, the lid 4, and the substrate 1
2 are arranged in the vertical direction, but they may be arranged in the horizontal direction. Further, as another device, a substrate is disposed in a case, a continuous phase flow path is formed between the substrate and the plate, and a microchannel opening in a direction intersecting the flow path is formed on the substrate. It may be of a cross-flow type in which a composition for a dispersed phase is formed and supplied from a direction intersecting a continuous phase in a fluidized state.
【００２３】[0023]
【実施例】以下に実施例を掲げて本発明を更に詳しく説
明するが、本発明はこれら実施例のみに限定されるもの
ではない。The present invention will be described in more detail with reference to the following examples, but the present invention is not limited to these examples.
【００２４】分散相用組成物として、ラジカル重合開始
剤である過酸化ベンゾイルの２５％含水物を２％の濃度
で溶解したジビニルベンゼンを用い、連続相に０．３％
ドデシルベンゼンスルホン酸ナトリウム水溶液を用いて
常温でマイクロチャネル乳化を行った。分散相用組成物
の供給圧力は４．９〜６．９ｋＰａ（０．０５〜０．０
７ｋｇ／ｃｍ2 ）の範囲とした。生成したエマルション
１００部を２％ポリビニルアルコール溶液１００部と攪
拌混合した後、９０℃で反応を行った。この後、このサ
スペンジョンを乾燥して白色の固体微粒子を得た。得ら
れた微粒子は平均粒径が１６．４μｍで、標準偏差が
１．１８μｍであった。As the composition for the dispersed phase, divinylbenzene in which 25% hydrate of benzoyl peroxide as a radical polymerization initiator was dissolved at a concentration of 2% was used.
Microchannel emulsification was performed at room temperature using an aqueous solution of sodium dodecylbenzenesulfonate. The supply pressure of the composition for a dispersed phase is 4.9 to 6.9 kPa (0.05 to 0.0 kPa).
7 kg / cm 2 ). After 100 parts of the produced emulsion was stirred and mixed with 100 parts of a 2% polyvinyl alcohol solution, a reaction was performed at 90 ° C. Thereafter, the suspension was dried to obtain white solid fine particles. The obtained fine particles had an average particle size of 16.4 μm and a standard deviation of 1.18 μm.
【００２５】[0025]
【発明の効果】本発明の固体微粒子の製造方法は、上述
の構成からなるので、液晶表示装置用スペーサ等に用い
ることができる粒径が数μｍ以上の単分散固体微粒子を
製造することができる。Since the method for producing solid fine particles of the present invention has the above-described structure, monodisperse solid fine particles having a particle size of several μm or more which can be used for spacers for liquid crystal display devices can be produced. .
【図面の簡単な説明】[Brief description of the drawings]
【図１】本発明の概略を工程順に示したブロック図であ
る。FIG. 1 is a block diagram showing an outline of the present invention in the order of steps.
【図２】本発明の一実施形態として用いるエマルション
生成装置の全体図である。FIG. 2 is an overall view of an emulsion generating apparatus used as an embodiment of the present invention.
【図３】図２のエマルション生成装置における要部の拡
大模式図である。FIG. 3 is an enlarged schematic diagram of a main part in the emulsion generation device of FIG. 2;
【図４】（ａ）は、図２のエマルション生成装置におけ
る基板の平面図である。（ｂ）は、図２のエマルション
生成装置における基板の裏面図である。FIG. 4A is a plan view of a substrate in the emulsion generation device of FIG. 2; FIG. 3B is a back view of the substrate in the emulsion generation device of FIG. 2.
【図５】図２のエマルション生成装置におけるマイクロ
チャネルの部分の拡大斜視図である。FIG. 5 is an enlarged perspective view of a microchannel portion in the emulsion generation device of FIG. 2;
１ エマルション生成装置本体 ２ 恒温槽 ３ プレート ４ 蓋体 ５ 分散相用組成物（Ｏ）の供給口 ６ 連続相（Ｗ）の供給口 ７ エマルション（Ｅ）の取出口 ８ 分散相用組成物リザーバ ９ ヒータ １０ 連続相リザーバ １１ 回収用配管 １２ 基板 １３ 開口 １４ 突条 １５ テラス １６ 突部 １７ マイクロチャネル １８ 隔壁部材 １９ ビデオカメラ ２０ 分散相用組成物（Ｏ） ２１ 連続相（Ｗ） ２２ マイクロスフィア REFERENCE SIGNS LIST 1 Emulsion generating apparatus main body 2 Constant temperature bath 3 Plate 4 Lid 5 Supply port for composition for dispersed phase (O) 6 Supply port for continuous phase (W) 7 Outlet for emulsion (E) 8 Composition reservoir for dispersed phase 9 Heater 10 Continuous phase reservoir 11 Collection pipe 12 Substrate 13 Opening 14 Ridge 15 Terrace 16 Protrusion 17 Microchannel 18 Partition member 19 Video camera 20 Composition for dispersed phase (O) 21 Continuous phase (W) 22 Microsphere
フロントページの続き (72)発明者 鍋谷 浩志 茨城県つくば市観音台２−１−２ 農林水 産省 食品総合研究所内 (72)発明者 伊藤 央乙 茨城県つくば市観音台２−１−２ 農林水 産省 食品総合研究所内 (72)発明者 向井 克典 大阪府大阪市北区西天満２−４−４ 積水 化学工業株式会社内 Ｆターム(参考） 2H089 LA19 MA03X NA17 4J011 DB11 KA01 KB08 KB11 4J100 FA20 GC07 GC25 Continued on the front page (72) Inventor Hiroshi Nabeya 2-1-2 Kannondai, Tsukuba-shi, Ibaraki Prefectural Ministry of Agriculture, Forestry and Fisheries Food Research Institute (72) Inventor Hirotoshi Ito 2-1-2 Kannondai, Tsukuba-shi, Ibaraki Agriculture and Forestry Within the Food Research Institute of the Ministry of Fisheries (72) Katsunori Mukai 2-4-4 Nishitenma, Kita-ku, Osaka City, Osaka Prefecture Sekisui Chemical Co., Ltd.F-term (reference)
Claims (2)
固体微粒子を製造する方法であって、（１）反応性モノ
マーを含む分散相用組成物を加圧し、前記分散相用組成
物をマイクロチャネルを介して連続相中に分散せしめて
エマルションを生成する工程、（２）前記エマルション
を重合させることにより固体微粒子のサスペンジョンを
作製する工程、及び、（３）前記サスペンジョンから連
続相を除去することにより固体微粒子を回収する工程か
らなることを特徴とする単分散固体微粒子の製造方法。1. A method for producing monodisperse solid fine particles obtained by polymerizing a reactive monomer, comprising the steps of: (1) applying pressure to a composition for a dispersed phase containing a reactive monomer; Dispersing in a continuous phase through a channel to form an emulsion, (2) producing a suspension of solid fine particles by polymerizing the emulsion, and (3) removing the continuous phase from the suspension A method for producing monodisperse solid fine particles, comprising the step of recovering solid fine particles by a method.
示装置用スペーサを製造する方法であって、（１）反応
性モノマーを含む分散相用組成物を加圧し、前記分散相
用組成物をマイクロチャネルを介して連続相中に分散せ
しめてエマルションを生成する工程、（２）前記エマル
ションを重合させることにより固体微粒子のサスペンジ
ョンを作製する工程、及び、（３）前記サスペンジョン
から連続相を除去することにより液晶表示装置用スペー
サを固体微粒子として回収する工程からなることを特徴
とする液晶表示装置用スペーサの製造方法。2. A method for producing a spacer for a liquid crystal display device by polymerizing a reactive monomer, comprising the steps of: (1) applying pressure to a composition for a dispersed phase containing a reactive monomer; Dispersing in a continuous phase through a microchannel to form an emulsion; (2) preparing a suspension of solid fine particles by polymerizing the emulsion; and (3) removing the continuous phase from the suspension. A method of recovering the liquid crystal display device spacer as solid fine particles.
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|---|---|---|---|
| JP36925699A JP3616909B2 (en) | 1999-12-27 | 1999-12-27 | Method for producing monodispersed solid fine particles |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP36925699A JP3616909B2 (en) | 1999-12-27 | 1999-12-27 | Method for producing monodispersed solid fine particles |
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| JP2001181309A true JP2001181309A (en) | 2001-07-03 |
| JP3616909B2 JP3616909B2 (en) | 2005-02-02 |
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|---|---|---|---|
| JP36925699A Expired - Fee Related JP3616909B2 (en) | 1999-12-27 | 1999-12-27 | Method for producing monodispersed solid fine particles |
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