JPH04258601A - Production of polymer bead - Google Patents
Production of polymer beadInfo
- Publication number
- JPH04258601A JPH04258601A JP1892191A JP1892191A JPH04258601A JP H04258601 A JPH04258601 A JP H04258601A JP 1892191 A JP1892191 A JP 1892191A JP 1892191 A JP1892191 A JP 1892191A JP H04258601 A JPH04258601 A JP H04258601A
- Authority
- JP
- Japan
- Prior art keywords
- monomer
- porous glass
- solution
- glass membrane
- polymer beads
- 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.)
- Pending
Links
- 229920000642 polymer Polymers 0.000 title claims abstract description 28
- 239000011324 bead Substances 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000000178 monomer Substances 0.000 claims abstract description 79
- 239000012528 membrane Substances 0.000 claims abstract description 33
- 239000005373 porous glass Substances 0.000 claims abstract description 33
- 239000002245 particle Substances 0.000 claims abstract description 32
- 239000000839 emulsion Substances 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract 2
- 239000002612 dispersion medium Substances 0.000 claims description 21
- 239000011148 porous material Substances 0.000 abstract description 11
- 239000002270 dispersing agent Substances 0.000 abstract description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 abstract 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 43
- 238000000034 method Methods 0.000 description 10
- 238000006116 polymerization reaction Methods 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000007720 emulsion polymerization reaction Methods 0.000 description 6
- 239000003094 microcapsule Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 238000010557 suspension polymerization reaction Methods 0.000 description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000004793 Polystyrene Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000693 micelle Substances 0.000 description 3
- 229920002223 polystyrene Polymers 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- 239000004342 Benzoyl peroxide Substances 0.000 description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- 238000012695 Interfacial polymerization Methods 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は、マイクロカプセル等に
利用可能な均一粒径を有するポリマービーズの製造方法
に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing polymer beads having a uniform particle size that can be used for microcapsules and the like.
【０００２】0002
【従来の技術】従来のポリマービーズを製造する方法と
しては、一般に懸濁重合及び乳化重合が採用されている
。懸濁重合とは、非水溶性の重合性モノマーを水中に攪
拌、分散し、モノマー可溶性触媒で重合を開始する方法
である。攪拌により水相に分散したモノマーの小液滴は
０．１ 〜０．５ｍｍ であり、一般に、このモノマー
滴を安定化させるために、ポリビニルアルコール等の分
散剤を使用する。重合は、分散したモノマー滴の中で進
行し、モノマー滴の形態を有する重合体が生成する。2. Description of the Related Art Suspension polymerization and emulsion polymerization are generally employed as conventional methods for producing polymer beads. Suspension polymerization is a method in which water-insoluble polymerizable monomers are stirred and dispersed in water, and polymerization is initiated using a monomer-soluble catalyst. The small droplets of monomer dispersed in the aqueous phase by stirring are 0.1 to 0.5 mm, and a dispersant such as polyvinyl alcohol is generally used to stabilize the monomer droplets. Polymerization proceeds in dispersed monomer droplets, producing a polymer having the morphology of monomer droplets.
【０００３】乳化重合とは、水を媒体として乳化剤を用
いて、水に不溶又は難溶性の重合性モノマーを分散乳化
させ、水溶性開始剤を加えて行う重合方法である。乳化
剤は水媒体中でミセルを形成し、このミセルの中に入れ
込められたモノマー群が重合反応して、ミセル中に重合
体を生成する。[0003] Emulsion polymerization is a polymerization method in which polymerizable monomers that are insoluble or poorly soluble in water are dispersed and emulsified using water as a medium and an emulsifier, and a water-soluble initiator is added. The emulsifier forms micelles in an aqueous medium, and the monomers introduced into the micelles undergo a polymerization reaction to produce a polymer in the micelles.
【０００４】0004
【発明が解決しようとする課題】上記懸濁重合で得られ
るポリマービーズは一般に０．１ 〜０．５ｍｍ 程度
であり、上記乳化重合で得られるポリマービーズは一般
に０．１ 〜１０μｍ 程度である。従って、粒径１０
〜１００ μｍ のポリマービーズを得たい場合、乳化
重合では不充分であり、懸濁重合では粒径が大きすぎる
という問題がある。The polymer beads obtained by the above suspension polymerization are generally about 0.1 to 0.5 mm, and the polymer beads obtained by the emulsion polymerization are generally about 0.1 to 10 μm. Therefore, the particle size is 10
When it is desired to obtain polymer beads of ~100 μm, emulsion polymerization is insufficient, and suspension polymerization has the problem that the particle size is too large.
【０００５】また、懸濁重合又は乳化重合いずれの重合
法も、生成されるポリマービーズの粒径のばらつきは大
きい。このため、単分散のポリマービーズを使用するマ
イクロカプセル等には利用できない。本発明はかかる事
情に鑑みてなされたものであり、その目的とするところ
は、所望の粒径で、かつ単分散に近い粒径分布を有する
ポリマービーズを容易に製造できる方法を提供すること
にある。[0005] Furthermore, in both suspension polymerization and emulsion polymerization, the particle size of the produced polymer beads varies widely. Therefore, it cannot be used for microcapsules using monodispersed polymer beads. The present invention has been made in view of the above circumstances, and its purpose is to provide a method for easily producing polymer beads having a desired particle size and a particle size distribution close to monodisperse. be.
【０００６】[0006]
【課題を解決するための手段】発明者は、多数の細孔を
有する多孔質ガラス膜を用いると、単分散に近い粒径分
布を有するエマルジョン溶液が得られることを利用して
、本発明を完成するに到った。すなわち、本発明のポリ
マービーズの製造方法は、多孔質ガラス膜の一側を流通
しているモノマー溶液を、該多孔質ガラス膜の他側に押
し出して、該多孔質ガラス膜の他側を流通する分散媒中
に均一粒径の重合性モノマー滴が分散したエマルジョン
溶液を調製し、該エマルジョン溶液を加熱して、該エマ
ルジョン溶液中の重合性モノマー滴を構成するモノマー
群を重合させることを特徴とする。[Means for Solving the Problem] The inventor has developed the present invention by taking advantage of the fact that when a porous glass membrane having a large number of pores is used, an emulsion solution having a particle size distribution close to monodisperse can be obtained. It has been completed. That is, in the method for producing polymer beads of the present invention, a monomer solution flowing on one side of a porous glass membrane is extruded to the other side of the porous glass membrane, and the monomer solution is forced to flow on the other side of the porous glass membrane. An emulsion solution in which polymerizable monomer droplets of uniform particle size are dispersed in a dispersion medium is prepared, and the emulsion solution is heated to polymerize the monomer group constituting the polymerizable monomer droplets in the emulsion solution. shall be.
【０００７】[0007]
【作用】モノマー溶液を加圧供給して多孔質ガラス膜を
通過させると、分散媒中に重合性モノマーの小滴（以下
、単にモノマー滴と称する）が分散したエマルジョン溶
液が得られる。かかるエマルジョン溶液に分散している
モノマー滴の大きさは多孔質ガラス膜の細孔径に対応し
ているので、その粒径はほぼ均一となる。[Operation] When a monomer solution is supplied under pressure and passed through a porous glass membrane, an emulsion solution is obtained in which small droplets of polymerizable monomer (hereinafter simply referred to as monomer droplets) are dispersed in a dispersion medium. Since the size of the monomer droplets dispersed in such an emulsion solution corresponds to the pore diameter of the porous glass membrane, the particle diameter is approximately uniform.
【０００８】このエマルジョン溶液を加熱すると、該エ
マルジョン溶液中の分散している個々のモノマー滴中に
おいて、該モノマー滴を構成するモノマー群が重合し、
モノマー滴と同じ粒径及び分布を有するポリマービーズ
が得られる。[0008] When this emulsion solution is heated, the monomer groups constituting the monomer droplets are polymerized in the individual monomer droplets dispersed in the emulsion solution.
Polymer beads are obtained with the same particle size and distribution as the monomer droplets.
【０００９】[0009]
【実施例】はじめに、単分散に近い粒径分布を有するモ
ノマー滴が分散したエマルジョン溶液が得られる機構に
ついて、図２に基づいて説明する。図２において、１１
は筒状に作成された多孔質ガラス膜である。多孔質ガラ
ス膜１１の筒内側に、分散媒１２を流通させる（図中、
分散媒１２の流れを白抜き矢印で示す）。多孔質ガラス
膜の筒外側にモノマー溶液１３（図中、黒色矢印で示す
）を加圧供給すると、モノマー溶液１３は、多孔質ガラ
ス膜１１の細孔を通り抜けて、分散媒１２中にモノマー
滴１４となって分散する。モノマー滴１４は、一般に多
孔質ガラス膜の細孔径の３ 倍程度に膨潤する。[Example] First, a mechanism for obtaining an emulsion solution in which monomer droplets having a particle size distribution close to monodisperse are dispersed will be explained based on FIG. 2. In FIG. 2, 11
is a porous glass membrane made into a cylindrical shape. The dispersion medium 12 is made to flow inside the cylinder of the porous glass membrane 11 (in the figure,
The flow of the dispersion medium 12 is shown by an outline arrow). When a monomer solution 13 (indicated by a black arrow in the figure) is supplied under pressure to the outside of the cylinder of the porous glass membrane, the monomer solution 13 passes through the pores of the porous glass membrane 11 and forms monomer droplets in the dispersion medium 12. 14 and dispersed. The monomer droplets 14 generally swell to about three times the pore diameter of the porous glass membrane.
【００１０】細孔径０．５２μｍ の多孔質ガラス膜を
用いて得られたエマルジョン溶液におけるモノマー滴の
粒径分布を図 ３に示す。図３において、粒径１．５
〜２ μｍ の粒子の割合が８０％以上で、ほぼ単分散
に近い分布を示した。一方、比較例として、攪拌により
モノマー溶液を分散媒に分散させた場合の粒径分布を図
４ に示す。図 ３と比較すると、粒径分布の幅が広く
なっている。FIG. 3 shows the particle size distribution of monomer droplets in an emulsion solution obtained using a porous glass membrane with a pore size of 0.52 μm. In Figure 3, particle size 1.5
The proportion of particles of ~2 μm was 80% or more, indicating a nearly monodisperse distribution. On the other hand, as a comparative example, the particle size distribution when the monomer solution was dispersed in a dispersion medium by stirring is shown in FIG. Compared to Figure 3, the width of the particle size distribution is wider.
【００１１】次に、本発明のポリマービーズの製造方法
について説明する。図１ に、本発明の製造方法を実施
する装置の一実施例を示す。均一粒径のモノマー滴が分
散したエマルジョン溶液を調製するために、複数本の筒
状の多孔質ガラス膜１１を組み合わせて構成した多孔質
ガラス膜のモジュール１を使用した。容器７ には分散
媒２ が入っており、該分散媒２ に分散剤が混合して
いる。分散媒２ 及び分散剤をポンプ６ により送り出
して、モジュール１ を構成する個々の筒状多孔質ガラ
ス膜の内部（又は外部）に流通させる。一方、コンプレ
ッサー、高圧ボンベ、加圧ポンプ等の加圧装置９ を連
結した圧力容器８ には、モノマー溶液３ が入ってい
る。モノマー溶液３ は、重合性モノマー単独でもよい
し、重合性モノマーを適当な溶剤に溶解したものでもよ
い。モノマー溶液３ を、加圧装置９ によりモジュー
ル１ を構成する個々の筒状多孔質ガラス膜の外部（又
は内部）に加圧供給すると、モノマー溶液３ は、加圧
により多孔質ガラス膜の細孔を通り抜け、重合性モノマ
ー滴４ となって分散媒２ 中に分散する。分散媒２
には分散剤が含まれているので、モノマー滴同士が凝集
したり沈澱したりすることがない。モノマー溶液３ の
供給圧力は、約 １〜３ｋｇ／ｃｍ２ 程度が好ましい
。このようにして、分散媒２ 中にモノマー滴４ を分
散させたエマルジョン溶液５ を調製する。Next, the method for producing polymer beads of the present invention will be explained. FIG. 1 shows an embodiment of an apparatus for carrying out the manufacturing method of the present invention. In order to prepare an emulsion solution in which monomer droplets of uniform particle size were dispersed, a porous glass membrane module 1 constructed by combining a plurality of cylindrical porous glass membranes 11 was used. The container 7 contains a dispersion medium 2, and a dispersant is mixed with the dispersion medium 2. The dispersion medium 2 and the dispersant are sent out by a pump 6 and are made to flow inside (or outside) each cylindrical porous glass membrane that constitutes the module 1 . On the other hand, a monomer solution 3 is contained in a pressure vessel 8 connected to a pressurizing device 9 such as a compressor, a high-pressure cylinder, and a pressurizing pump. The monomer solution 3 may be a polymerizable monomer alone or may be a polymerizable monomer dissolved in a suitable solvent. When the monomer solution 3 is supplied under pressure to the outside (or inside) of each cylindrical porous glass membrane constituting the module 1 by the pressurizing device 9, the monomer solution 3 is applied to the pores of the porous glass membrane due to the pressurization. The polymerizable monomer droplets 4 form polymerizable monomer droplets 4 and are dispersed in the dispersion medium 2 . Dispersion medium 2
contains a dispersant, so monomer droplets do not aggregate or precipitate. The supply pressure of the monomer solution 3 is preferably about 1 to 3 kg/cm2. In this way, an emulsion solution 5 in which monomer droplets 4 are dispersed in a dispersion medium 2 is prepared.
【００１２】このエマルジョン溶液５ を加熱すると、
モノマー滴４を構成するモノマー群が重合を開始する。
なお、重合開始剤は、その種類により、分散媒２ 又は
モノマー溶液３ に添加される。重合反応は、モノマー
滴４ の中で起こる。よって、生成されるポリマービー
ズの大きさは、モノマー滴４ の粒径に対応し、かつ、
その粒径分布は、モノマー滴４ の粒径分布と同様にほ
ぼ単分散である。しかも、モノマー滴の粒径は多孔質ガ
ラス膜の細孔径に応じて調節でき、多孔質ガラス膜の細
孔径は、原ガラスの組成、相分離の過程等を制御するこ
とにより０．０１〜１００ μｍ の範囲で任意に調節
することができる。従って、乳化重合や懸濁重合では生
成が困難であった１０〜１００ μｍ のポリマービー
ズ、及び粒径がほぼ均一なポリマービーズを製造するこ
とができる。When this emulsion solution 5 is heated,
The monomer group constituting the monomer droplet 4 starts polymerization. Note that the polymerization initiator is added to the dispersion medium 2 or the monomer solution 3 depending on its type. The polymerization reaction takes place within the monomer droplets 4. Therefore, the size of the polymer beads produced corresponds to the particle size of the monomer droplets 4, and
Its particle size distribution is almost monodisperse, similar to the particle size distribution of the monomer droplets 4. Moreover, the particle size of the monomer droplet can be adjusted according to the pore size of the porous glass membrane, and the pore size of the porous glass membrane can be adjusted to 0.01 to 100 by controlling the composition of the raw glass, the phase separation process, etc. It can be arbitrarily adjusted within the range of μm. Therefore, it is possible to produce polymer beads of 10 to 100 μm, which are difficult to produce by emulsion polymerization or suspension polymerization, and polymer beads with substantially uniform particle size.
【００１３】また、本発明の製造方法によれば、水中油
滴型、油滴水中型のいずれのエマルジョン溶液も調製で
きるので、アクリル酸、メタクリル酸等の水溶性モノマ
ー、スチレン、メタクリル酸メチル等の親油性モノマー
いずれを用いることもできる。また、アクリルアミドの
ように、常温で固体のモノマーを用いることもできる。
固体モノマーの場合、適当な溶剤に溶解してモノマー溶
液にして用いる。Furthermore, according to the production method of the present invention, both oil-in-water type and oil-in-water type emulsion solutions can be prepared. Any lipophilic monomer can be used. Furthermore, monomers that are solid at room temperature, such as acrylamide, can also be used. In the case of a solid monomer, it is used as a monomer solution by dissolving it in an appropriate solvent.
【００１４】分散媒は、重合性モノマーが不溶で、かつ
重合性モノマーを溶剤に溶解させたモノマー溶液を使用
する場合には、該溶剤と混合しても分離しないものが好
ましい。分散媒は、重合性モノマー及び溶剤の種類によ
り適宜選択する。分散剤は、モノマー滴を分散媒中で安
定して分散させるために添加され、その種類はモノマー
及び分散媒により適宜選択する。一般にはラウリル硫酸
ナトリウム、けん化ビニルアルコールなどが用いられる
。When using a monomer solution in which the polymerizable monomer is insoluble and the polymerizable monomer is dissolved in a solvent, the dispersion medium is preferably one that does not separate even when mixed with the solvent. The dispersion medium is appropriately selected depending on the type of polymerizable monomer and solvent. The dispersant is added to stably disperse the monomer droplets in the dispersion medium, and the type thereof is appropriately selected depending on the monomer and the dispersion medium. Generally, sodium lauryl sulfate, saponified vinyl alcohol, etc. are used.
【００１５】重合開始触媒としては、過酸化ベンゾイル
、アゾビスイソブチロニトリルなどが用いられる。なお
、重合開始触媒は、モノマー溶液３ 又は分散媒２ の
いずれか可溶する方に溶解させればよい。
〔具体的実施例〕図１の装置において、容器７ に水２
０００ｇ 及びラウリル硫酸ナトリウム２ｇを入れ、圧
力容器８ にスチレン８５．７１ｇ及び過酸化ベンゾイ
ル８．６ｇを入れた。モジュール１ を構成する個々の
多孔質ガラス膜（ 細孔径５．２ μｍ ）の筒内部に
容器７ の溶液を流通させ、筒外部に圧力容器８ の溶
液を２．５ｋｇ／ｃｍ２ で加圧供給した。両溶液をモ
ジュール１ に流通させた結果、水中にスチレンモノマ
ー滴が分散したエマルジョン溶液が得られた。このエマ
ルジョン溶液を約８０℃にて約９０分間保持したところ
、粒径がほぼ均一（粒径約１５μｍ ）なポリスチレン
のビーズが得られた。
〔比較例〕スチレンに代えてポリスチレンのトルエン溶
液、水の代わりにトルエンと相溶性があるメタノールを
使用した以外は実施例と同様に行った。モジュール１
を流通して得られた混合液にはポリスチレンビーズが沈
澱していた。As the polymerization initiation catalyst, benzoyl peroxide, azobisisobutyronitrile, etc. are used. The polymerization initiation catalyst may be dissolved in either the monomer solution 3 or the dispersion medium 2, whichever is soluble therein. [Specific Example] In the apparatus shown in Fig. 1, water 2 is placed in container 7.
000 g and 2 g of sodium lauryl sulfate were placed in the pressure vessel 8, and 85.71 g of styrene and 8.6 g of benzoyl peroxide were placed in the pressure vessel 8. The solution in container 7 was passed through the cylinder of each porous glass membrane (pore diameter: 5.2 μm) constituting module 1, and the solution in pressure vessel 8 was supplied to the outside of the cylinder under pressure at 2.5 kg/cm2. . Both solutions were passed through module 1, resulting in an emulsion solution in which styrene monomer droplets were dispersed in water. When this emulsion solution was kept at about 80° C. for about 90 minutes, polystyrene beads having a substantially uniform particle size (about 15 μm) were obtained. [Comparative Example] A toluene solution of polystyrene was used instead of styrene, and methanol, which is compatible with toluene, was used instead of water. module 1
Polystyrene beads were precipitated in the mixed solution obtained by passing through the solution.
【００１６】比較例からわかるように、単にポリマー溶
液を多孔質ガラス膜に通過させても均一粒径のポリマー
ビーズを得ることができない。しかし、本発明の製造方
法によれば、ほぼ均一粒径のポリマービーズを得ること
ができる。このようにして得られたポリマービーズは、
均一粒径を要求する種々の分野に利用できる。特に、マ
イクロカプセルの芯物質として好適に利用される。例え
ば、ポリマービーズをマイクロカプセルの外壁を構成す
るモノマー溶液中に分散し、界面重合法や界面反応法等
の適宜方法と組み合わせるとマイクロカプセルを容易に
製造することができる。また、本発明の製造方法におい
て得られるシングルエマルジョン溶液を、重合せずに再
度多孔質ガラス膜を通過させて複層のモノマー滴が分散
したエマルジョン溶液を調製し、このエマルジョン溶液
を適当な方法で重合させることによりマイクロカプセル
を製造することもできる。As can be seen from the comparative example, polymer beads of uniform particle size cannot be obtained simply by passing a polymer solution through a porous glass membrane. However, according to the production method of the present invention, polymer beads having a substantially uniform particle size can be obtained. The polymer beads obtained in this way are
It can be used in various fields that require uniform particle size. In particular, it is suitably used as a core material for microcapsules. For example, microcapsules can be easily produced by dispersing polymer beads in a monomer solution constituting the outer wall of microcapsules and combining this with an appropriate method such as an interfacial polymerization method or an interfacial reaction method. Alternatively, the single emulsion solution obtained in the production method of the present invention is passed through a porous glass membrane again without polymerization to prepare an emulsion solution in which multilayer monomer droplets are dispersed, and this emulsion solution is processed by an appropriate method. Microcapsules can also be produced by polymerization.
【００１７】[0017]
【発明の効果】本発明の製造方法によれば、容易に、均
一粒径を有するポリマービーズを製造することができる
。しかも、ポリマービーズの粒径は、多孔質ガラス膜の
細孔径を選択することにより調節できる。さらに、本発
明の方法では、分散媒及びモノマーを溶解させる溶剤を
適宜選択することにより、水溶性モノマー、油溶性モノ
マー、さらには重合性の固体モノマーなど、種々の重合
性モノマーを使用することができる。従って、種々のポ
リマービーズを製造することができる。[Effects of the Invention] According to the production method of the present invention, polymer beads having a uniform particle size can be easily produced. Furthermore, the particle size of the polymer beads can be adjusted by selecting the pore size of the porous glass membrane. Furthermore, in the method of the present invention, various polymerizable monomers such as water-soluble monomers, oil-soluble monomers, and even polymerizable solid monomers can be used by appropriately selecting the dispersion medium and the solvent for dissolving the monomers. can. Therefore, various polymer beads can be manufactured.
【図１】本発明の製造方法を実施する装置の概要図であ
る。FIG. 1 is a schematic diagram of an apparatus for carrying out the manufacturing method of the present invention.
【図２】本発明の製造方法の一工程を説明するための図
である。FIG. 2 is a diagram for explaining one step of the manufacturing method of the present invention.
【図３】本発明の製造方法により得られるモノマー滴の
粒径分布を示す図である。FIG. 3 is a diagram showing the particle size distribution of monomer droplets obtained by the production method of the present invention.
【図４】従来の攪拌法により得られるモノマー滴の粒径
分布を示す図である。FIG. 4 is a diagram showing the particle size distribution of monomer droplets obtained by a conventional stirring method.
１ 多孔質ガラス膜モジュール ２ 分散媒 ３ モノマー溶液 ４ モノマー滴 ５ エマルジョン溶液 １１ 多孔質ガラス膜 1 Porous glass membrane module 2 Dispersion medium 3 Monomer solution 4 Monomer droplets 5 Emulsion solution 11 Porous glass membrane
Claims (1)
モノマー溶液を、該多孔質ガラス膜の他側に押し出して
、該多孔質ガラス膜の他側を流通する分散媒中に均一粒
径の重合性モノマー滴が分散したエマルジョン溶液を調
製し、該エマルジョン溶液を加熱して、該エマルジョン
溶液中の重合性モノマー滴を構成するモノマー群を重合
させることを特徴とするポリマービーズの製造方法。Claim 1: A monomer solution flowing on one side of the porous glass membrane is extruded to the other side of the porous glass membrane to form uniform particles in a dispersion medium flowing on the other side of the porous glass membrane. A method for producing polymer beads, which comprises preparing an emulsion solution in which polymerizable monomer droplets having a diameter of about 100 mL are dispersed, and heating the emulsion solution to polymerize monomer groups constituting the polymerizable monomer droplets in the emulsion solution. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1892191A JPH04258601A (en) | 1991-02-12 | 1991-02-12 | Production of polymer bead |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1892191A JPH04258601A (en) | 1991-02-12 | 1991-02-12 | Production of polymer bead |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04258601A true JPH04258601A (en) | 1992-09-14 |
Family
ID=11985082
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1892191A Pending JPH04258601A (en) | 1991-02-12 | 1991-02-12 | Production of polymer bead |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04258601A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007067145A1 (en) * | 2005-12-07 | 2007-06-14 | Mip Technologies Ab | Monodisperse molecularly imprinted polymer beads |
| JP2007245151A (en) * | 2007-04-06 | 2007-09-27 | Dainippon Toryo Co Ltd | Method for producing monodisperse particle |
-
1991
- 1991-02-12 JP JP1892191A patent/JPH04258601A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007067145A1 (en) * | 2005-12-07 | 2007-06-14 | Mip Technologies Ab | Monodisperse molecularly imprinted polymer beads |
| JP2007245151A (en) * | 2007-04-06 | 2007-09-27 | Dainippon Toryo Co Ltd | Method for producing monodisperse particle |
| JP4537421B2 (en) * | 2007-04-06 | 2010-09-01 | 大日本塗料株式会社 | Method for producing monodisperse particles |
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