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JP2004059802A - Method and apparatus for producing solid fine particles - Google Patents

Method and apparatus for producing solid fine particles Download PDF

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Publication number
JP2004059802A
JP2004059802A JP2002221794A JP2002221794A JP2004059802A JP 2004059802 A JP2004059802 A JP 2004059802A JP 2002221794 A JP2002221794 A JP 2002221794A JP 2002221794 A JP2002221794 A JP 2002221794A JP 2004059802 A JP2004059802 A JP 2004059802A
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Prior art keywords
fine particles
solid fine
producing solid
microdroplets
external action
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Japanese (ja)
Inventor
Toshiro Higuchi
樋口　俊郎
Toru Torii
鳥居　徹
Takashi Nishisako
西迫　貴志
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Japan Science and Technology Agency
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Japan Science and Technology Corp
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Abstract

【課題】生成された微小液滴（微粒子）を固体化して得られる固体微粒子の製造方法およびその装置を提供する。
【解決手段】連続相５中に、分散相６である固体微粒子となる原料液を送り込み、微小液滴７を生成し、この微小液滴７に固化装置８により外部からの作用を施し、前記微小液滴７を固化して固体微粒子９を得る。
【選択図】　　図２An object of the present invention is to provide a method and an apparatus for producing solid fine particles obtained by solidifying generated fine droplets (fine particles).
A raw material liquid to be solid fine particles, which is a dispersed phase, is fed into a continuous phase to generate fine liquid droplets, and the fine liquid droplets are subjected to an external action by a solidifying device. The fine droplets 7 are solidified to obtain solid fine particles 9.
[Selection] Figure 2

Description

【０００１】
【発明の属する技術分野】
本発明は、固体微粒子の製造方法およびその装置に関するものである。
【０００２】
【従来の技術】
従来から、例えばプラスチックの微粒子生成法はあったが、１０〜５００μｍ相当の任意粒径のものを高精度で、しかも効率よく製造することは困難であった。
【０００３】
【発明が解決しようとする課題】
本願発明者らは、水、油等の液体中において微小液滴を迅速、かつ的確に製造する方法及びその装置を、既に特願２００１−２３８６２４号として提案している。
【０００４】
本発明は、更なる研究を進めて、上記によって生成された微小液滴（微粒子）を固体化して得られる固体微粒子の製造方法およびその装置を提供することを目的とする。
【０００５】
【課題を解決するための手段】
本発明は、上記目的を達成するために、
〔１〕固体微粒子の製造方法において、連続相中に、分散相である固体微粒子となる原料液を送り込み、微小液滴を生成し、この微小液滴に外部からの作用を施し、前記微小液滴を固化することを特徴とする。
【０００６】
〔２〕上記〔１〕記載の固体微粒子の製造方法において、前記外部からの作用が光照射であることを特徴とする。
【０００７】
〔３〕上記〔１〕記載の固体微粒子の製造方法において、前記外部からの作用が加熱であることを特徴とする。
【０００８】
〔４〕上記〔１〕記載の固体微粒子の製造方法において、前記外部からの作用が冷却であることを特徴とする。
【０００９】
〔５〕固体微粒子の製造装置において、連続相中に、分散相である固体微粒子となる原料液を送り込み、微小液滴を生成させる手段と、この微小液滴に外部からの作用を施し、前記微小液滴を固化する手段とを具備することを特徴とする。
【００１０】
〔６〕上記〔５〕記載の固体微粒子の製造装置において、前記外部からの作用を与える光照射手段を備えることを特徴とする。
【００１１】
〔７〕上記〔５〕記載の固体微粒子の製造装置において、前記外部からの作用を与える加熱手段を備えることを特徴とする。
【００１２】
〔８〕上記〔５〕記載の固体微粒子の製造装置において、前記外部からの作用を与える冷却手段を備えることを特徴とする。
【００１３】
【発明の実施の形態】
以下、本発明の実施の形態について詳細に説明する。
【００１４】
図１は本発明の概要を示す固体微粒子の生成装置を示す平面図、図２はその模式図、図３はその装置によってポリビニルアルコール水溶液中に生成されるスチレンモノマー微小液滴の生成工程を示す図である。
【００１５】
これらの図において、１は微小液滴の生成装置の本体、２はその本体１に形成された、連続相が流れるマイクロチャンネル、３はそのマイクロチャンネル２に交差する向きに形成される分散相供給チャンネル、４は分散相供給口、５は連続相、６は分散相、７は微小液滴、８はその微小液滴（微粒子）７に作用して固化させるための固化装置、９は固体微粒子である。なお、マイクロチャンネルの材質は、例えば石英ガラスである。
【００１６】
そこで、マイクロチャンネル２中を流れる連続相５に対し、分散相６を、図２に示すように連続相５の流れに交差する向きで供給し、連続相５が分散相供給口４に一部入り込むことにより、分散相供給チャンネル３の幅より径の小さい微小液滴（微粒子）７が生成される。
【００１７】
図３には、連続相としてポリビニルアルコール水溶液中にスチレンモノマー微小液滴７を生成する様子が示されている。なお、図３（ａ）は基準となる時間、図３（ｂ）は基準から３／４５００秒経過時、図３（ｃ）は基準から６／４５００秒経過時を示している。なお、連続相の平均流速は０．５５６ｍ／ｓ、分散相の平均流速は０．００９ｍ／ｓである。
【００１８】
この微小液滴（微粒子）７に外部から固化装置８を作用させて、固体微粒子９を生成することができる。
【００１９】
図４は本発明の第１実施例を示す固体微粒子の生成装置を示す模式図である。
【００２０】
この実施例においては、図２に示した固化装置８として光照射装置１０を配置し、その光照射装置１０からの紫外光１１などの光照射によって微小液滴（微粒子）７を固化して、固体微粒子９を得ることができる。
【００２１】
例えば、連続相としてポリビニルアルコール水溶液（２％）、分散相としてスチレンモノマー（和光純薬製）を用い、下記の表１のような条件で微小液滴の生成を行い、紫外線を２０分照射して固体微粒子の生成を行った。
【００２２】
【表１】

Figure 2004059802
その結果、図５に示すように、直径４４．３μｍのサイズの固体微粒子を生成することができた。
【００２３】
図６は本発明の第２実施例を示す固体微粒子の生成装置を示す模式図である。
【００２４】
この実施例においては、図２に示した固化装置８として、ヒータ板１２を配置して加熱によって微小液滴（微粒子）７を固化して、固体微粒子９を得ることができる。この例ではマイクロチャンネルを大きくした部分にヒータ板１２を配置して、微小液滴（微粒子）７を固化するのが望ましい。
【００２５】
一例を挙げると、連続相としてポリビニルアルコール水溶液（２％）、分散相としてスチレンモノマー（和光純薬製）・重合開始剤の過酸化ベンゾイルを用いて、下記の表２のような条件で微小液滴の生成を行い、温度条件を７５℃、４時間重合させ、固体微粒子の生成を行った。
【００２６】
【表２】
Figure 2004059802
その結果、図７に示すように、直径３３．８μｍのサイズの固体微粒子を生成することができた。
【００２７】
図８は本発明の第３実施例を示す固体微粒子の生成装置を示す模式図である。
【００２８】
この実施例においては、図２に示した固化装置８として、冷却装置１３を配置して冷却によって微小液滴（微粒子）７を固化して、固体微粒子９を得ることができる。例えば、連続相としてシリコンオイル（５０ｃｓ）、分散相としてポリエチレングリコール（分子量１０００）溶液を用いることにより、ポリエチレングリコール液滴を冷却により固化させることができた。
【００２９】
このように、本発明は、連続相中に、分散相である固体微粒子となる原料液を送り込み、微小液滴を生成し、その微小液滴に紫外光などの光照射や加熱又は冷却を施して固化させ固体微粒子を形成するようにしたため、簡単な構成により固体微粒子を得ることができる。
【００３０】
図９は本発明の第４実施例を示す固体微粒子の生成装置を示す平面図、図１０はその模式図である。
【００３１】
これらの図において、２１は微小液滴（微粒子）の生成装置の本体、２２は第１のマイクロチャンネル、２３は第２のマイクロチャンネル、２４は第１の連続相、２５は第２の連続相、２６は第１の連続相２４と第２の連続相２５との合流ポイント、２７は分散相供給チャンネル、２８は分散相、２９は微小液滴（微粒子）、３１は微小液滴（微粒子）２９の固化装置、３２は固体微粒子である。
【００３２】
マイクロチャンネル２２，２３中を流れる連続相２４，２５の合流ポイント２６で、図７に示すように連続相２４，２５の流れに交差するように分散相２８を送り出して微小液滴（微粒子）２９を生成させることができる。
【００３３】
このようにして生成される微小液滴（微粒子）２９を、固化装置３１、例えば、前記第１〜第３実施例で示した光照射、加熱又は冷却などにより固化させて、固体微粒子３２を形成することができる。
【００３４】
また、生成した微粒子を固化させるため、光（紫外光、可視光、赤外光）による重合促進、熱による促進、冷却による固化、連続相に含まれる試薬による重合促進などを行わせることができる。
【００３５】
なお、本発明は上記実施例に限定されるものではなく、本発明の趣旨に基づいて種々の変形が可能であり、これらを本発明の範囲から排除するものではない。
【００３６】
【発明の効果】
以上、詳細に説明したように、本発明によれば、以下に示すような効果を奏することができる。
【００３７】
（Ａ）簡単な構成で、微小液滴（微粒子）を固体微粒子化することができる。
【００３８】
（Ｂ）分散相が連続相に合流する分岐点で微小液滴が生成され、それに紫外光などの光照射や加熱工程や冷却工程を施して固体微粒子を形成することができ、システム内に容易に構築することができる。
【図面の簡単な説明】
【図１】本発明の概要を示す固体微粒子の生成装置を示す平面図である。
【図２】本発明の概要を示す固体微粒子の生成装置を示す模式図である。
【図３】本発明にかかる連続相としてポリビニルアルコール水溶液中にスチレンモノマー微小液滴を生成する工程を示す図である。
【図４】本発明の第１実施例を示す固体微粒子の生成装置を示す模式図である。
【図５】本発明の第１実施例を示すポリビニルアルコール水溶液中にスチレンモノマー微小液滴を示す図である。
【図６】本発明の第２実施例を示す固体微粒子の生成装置を示す模式図である。
【図７】本発明の第２実施例を示すポリビニルアルコール水溶液中に生成されたスチレンモノマー微小液滴を示す図である。
【図８】本発明の第３実施例を示す固体微粒子の生成装置を示す模式図である。
【図９】本発明の第４実施例を示す固体微粒子の生成装置を示す平面図である。
【図１０】本発明の第４実施例を示す固体微粒子の生成装置を示す模式図である。
【符号の説明】
１，２１　　微小液滴（粒子）の生成装置の本体
２　　連続相が流れるマイクロチャンネル
３　　分散相供給チャンネル
４　　分散相供給口
５　　連続相（例えば、ポリビニルアルコール水溶液）
６　　分散相（例えば、スチレンモノマー）
７，２９　　微小液滴（微粒子）
８，３１　　固化装置
９，３２　　固体微粒子
１０　　光照射装置
１１　　紫外光
１２　　ヒータ板
１３　　冷却装置
２２　　第１のマイクロチャンネル
２３　　第２のマイクロチャンネル
２４　　第１の連続相
２５　　第２の連続相
２６　　第１の連続相と第２の連続相との合流ポイント
２７　　分散相供給チャンネル
２８　　分散相[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method for producing solid fine particles and an apparatus therefor.
[0002]
[Prior art]
Conventionally, for example, there has been a method of producing fine particles of plastic, but it has been difficult to efficiently produce plastics having an arbitrary particle size equivalent to 10 to 500 μm with high accuracy.
[0003]
[Problems to be solved by the invention]
The present inventors have already proposed, as Japanese Patent Application No. 2001-238624, a method and an apparatus for quickly and accurately producing microdroplets in a liquid such as water or oil.
[0004]
An object of the present invention is to provide a method for producing solid fine particles obtained by solidifying the fine droplets (fine particles) generated as described above, and an apparatus therefor, by conducting further research.
[0005]
[Means for Solving the Problems]
The present invention, in order to achieve the above object,
[1] In the method for producing solid fine particles, a raw material liquid to be solid fine particles, which is a dispersed phase, is fed into a continuous phase to generate fine liquid droplets, and the fine liquid droplets are subjected to an external action to obtain the fine liquid. It is characterized by solidifying the droplet.
[0006]
[2] The method for producing solid fine particles according to the above [1], wherein the external action is light irradiation.
[0007]
[3] The method for producing solid fine particles according to the above [1], wherein the external action is heating.
[0008]
[4] The method for producing solid fine particles according to the above [1], wherein the external action is cooling.
[0009]
[5] In a device for producing solid fine particles, a means for feeding a raw material liquid to be solid fine particles as a dispersed phase into a continuous phase to generate fine droplets, and applying an external action to the fine droplets, Means for solidifying the microdroplets.
[0010]
[6] The apparatus for producing solid fine particles according to the above [5], further comprising a light irradiating means for giving an external action.
[0011]
[7] The apparatus for producing solid fine particles according to the above [5], further comprising a heating means for giving an external action.
[0012]
[8] The apparatus for producing solid fine particles according to the above [5], further comprising a cooling means for giving an external action.
[0013]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, embodiments of the present invention will be described in detail.
[0014]
FIG. 1 is a plan view showing an apparatus for producing solid fine particles showing an outline of the present invention, FIG. 2 is a schematic view thereof, and FIG. 3 shows a process for producing styrene monomer fine droplets produced in an aqueous polyvinyl alcohol solution by the apparatus. FIG.
[0015]
In these figures, 1 is a main body of a device for generating microdroplets, 2 is a microchannel formed in the main body 1 and through which a continuous phase flows, and 3 is a dispersed phase supply formed in a direction crossing the microchannel 2. Channel 4, dispersed phase supply port, 5 continuous phase, 6 dispersed phase, 7 microdroplets, 8 solidifying device for acting and solidifying the microdroplets (fine particles) 7, 9 solid fine particles It is. The material of the microchannel is, for example, quartz glass.
[0016]
Therefore, the dispersed phase 6 is supplied to the continuous phase 5 flowing in the microchannel 2 in a direction crossing the flow of the continuous phase 5 as shown in FIG. As a result, fine droplets (fine particles) 7 having a diameter smaller than the width of the dispersed phase supply channel 3 are generated.
[0017]
FIG. 3 shows a state in which styrene monomer microdroplets 7 are formed in a polyvinyl alcohol aqueous solution as a continuous phase. 3A shows a reference time, FIG. 3B shows a time when 3/4500 seconds elapse from the reference, and FIG. 3C shows a time when 6/4500 seconds elapse from the reference. The average flow velocity of the continuous phase is 0.556 m / s, and the average flow velocity of the dispersed phase is 0.009 m / s.
[0018]
Solid particles 9 can be generated by externally applying a solidifying device 8 to the minute liquid droplets (fine particles) 7.
[0019]
FIG. 4 is a schematic diagram showing an apparatus for producing solid fine particles according to the first embodiment of the present invention.
[0020]
In this embodiment, a light irradiating device 10 is arranged as the solidifying device 8 shown in FIG. 2, and the minute droplets (fine particles) 7 are solidified by irradiating light such as ultraviolet light 11 from the light irradiating device 10. Solid fine particles 9 can be obtained.
[0021]
For example, using a polyvinyl alcohol aqueous solution (2%) as a continuous phase and a styrene monomer (manufactured by Wako Pure Chemical Industries, Ltd.) as a dispersed phase, microdroplets are generated under the conditions shown in Table 1 below, and irradiated with ultraviolet rays for 20 minutes. Thus, solid fine particles were produced.
[0022]
[Table 1]
Figure 2004059802
As a result, as shown in FIG. 5, solid fine particles having a diameter of 44.3 μm could be produced.
[0023]
FIG. 6 is a schematic diagram showing an apparatus for producing solid fine particles according to a second embodiment of the present invention.
[0024]
In this embodiment, as the solidifying device 8 shown in FIG. 2, a heater plate 12 is arranged, and the minute liquid droplets (fine particles) 7 are solidified by heating, whereby solid fine particles 9 can be obtained. In this example, it is desirable to arrange the heater plate 12 in a portion where the microchannel is enlarged to solidify the minute droplets (fine particles) 7.
[0025]
As an example, using a polyvinyl alcohol aqueous solution (2%) as a continuous phase and a styrene monomer (manufactured by Wako Pure Chemical Industries, Ltd.) and benzoyl peroxide as a polymerization initiator as a dispersed phase, under the conditions shown in Table 2 below, Drops were formed, and polymerization was performed at 75 ° C. for 4 hours to generate solid fine particles.
[0026]
[Table 2]
Figure 2004059802
As a result, as shown in FIG. 7, solid fine particles having a diameter of 33.8 μm could be produced.
[0027]
FIG. 8 is a schematic view showing an apparatus for producing solid fine particles according to a third embodiment of the present invention.
[0028]
In this embodiment, as the solidifying device 8 shown in FIG. 2, a cooling device 13 is provided, and the fine liquid droplets (fine particles) 7 are solidified by cooling to obtain solid fine particles 9. For example, by using a silicone oil (50 cs) as a continuous phase and a polyethylene glycol (molecular weight 1000) solution as a dispersed phase, polyethylene glycol droplets could be solidified by cooling.
[0029]
As described above, the present invention provides a method in which a raw material liquid to be solid fine particles, which is a dispersed phase, is fed into a continuous phase to generate microdroplets, and the microdroplets are irradiated with light such as ultraviolet light or heated or cooled. Thus, solid fine particles are formed by solidification, so that solid fine particles can be obtained with a simple structure.
[0030]
FIG. 9 is a plan view showing an apparatus for producing solid fine particles according to a fourth embodiment of the present invention, and FIG. 10 is a schematic view thereof.
[0031]
In these figures, 21 is a main body of a device for generating microdroplets (fine particles), 22 is a first microchannel, 23 is a second microchannel, 24 is a first continuous phase, and 25 is a second continuous phase. , 26 are the confluence points of the first continuous phase 24 and the second continuous phase 25, 27 is the dispersed phase supply channel, 28 is the dispersed phase, 29 is microdroplets (fine particles), 31 is microdroplets (fine particles) 29 is a solidifying device, and 32 is solid fine particles.
[0032]
At the confluence point 26 of the continuous phases 24 and 25 flowing in the microchannels 22 and 23, the dispersed phase 28 is sent out so as to intersect the flow of the continuous phases 24 and 25 as shown in FIG. Can be generated.
[0033]
The fine droplets (fine particles) 29 thus generated are solidified by a solidifying device 31, for example, the light irradiation, heating or cooling shown in the first to third embodiments, to form solid fine particles 32. can do.
[0034]
Further, in order to solidify the generated fine particles, polymerization promotion by light (ultraviolet light, visible light, infrared light), promotion by heat, solidification by cooling, polymerization promotion by a reagent contained in the continuous phase, and the like can be performed. .
[0035]
It should be noted that the present invention is not limited to the above embodiment, and various modifications are possible based on the spirit of the present invention, and these are not excluded from the scope of the present invention.
[0036]
【The invention's effect】
As described above in detail, according to the present invention, the following effects can be obtained.
[0037]
(A) Fine droplets (fine particles) can be converted into solid fine particles with a simple configuration.
[0038]
(B) Fine droplets are generated at the branch point where the dispersed phase merges with the continuous phase, and solid particles can be formed by applying light such as ultraviolet light, a heating step, and a cooling step to form solid fine particles. Can be built.
[Brief description of the drawings]
FIG. 1 is a plan view showing an apparatus for producing solid fine particles showing an outline of the present invention.
FIG. 2 is a schematic view showing an apparatus for producing solid fine particles showing an outline of the present invention.
FIG. 3 is a diagram showing a step of forming styrene monomer microdroplets in a polyvinyl alcohol aqueous solution as a continuous phase according to the present invention.
FIG. 4 is a schematic view showing an apparatus for producing solid fine particles according to a first embodiment of the present invention.
FIG. 5 is a diagram showing styrene monomer microdroplets in a polyvinyl alcohol aqueous solution showing the first embodiment of the present invention.
FIG. 6 is a schematic view showing a solid particulate generation apparatus according to a second embodiment of the present invention.
FIG. 7 is a view showing styrene monomer microdroplets generated in a polyvinyl alcohol aqueous solution according to a second embodiment of the present invention.
FIG. 8 is a schematic diagram showing an apparatus for producing solid fine particles according to a third embodiment of the present invention.
FIG. 9 is a plan view showing an apparatus for producing solid fine particles according to a fourth embodiment of the present invention.
FIG. 10 is a schematic view showing a solid fine particle generator according to a fourth embodiment of the present invention.
[Explanation of symbols]
1, 21 Main body of microdroplet (particle) generating device 2 Microchannel 3 through which continuous phase flows 3 Dispersed phase supply channel 4 Dispersed phase supply port 5 Continuous phase (for example, aqueous polyvinyl alcohol solution)
6. Disperse phase (for example, styrene monomer)
7,29 Microdroplets (fine particles)
8, 31 Solidification device 9, 32 Solid fine particles 10 Light irradiation device 11 Ultraviolet light 12 Heater plate 13 Cooling device 22 First microchannel 23 Second microchannel 24 First continuous phase 25 Second continuous phase 26 First Confluence point 27 between the continuous phase of the second and the second continuous phase dispersed channel supply channel 28 dispersed phase

Claims (8)

連続相中に、分散相である固体微粒子となる原料液を送り込み、微小液滴を生成し、該微小液滴に外部からの作用を施し、前記微小液滴を固化することを特徴とする固体微粒子の製造方法。Feeding a raw material liquid to be solid fine particles, which is a dispersed phase, into a continuous phase to generate microdroplets; applying an external action to the microdroplets to solidify the microdroplets; A method for producing fine particles. 請求項１記載の固体微粒子の製造方法において、前記外部からの作用が光照射であることを特徴とする固体微粒子の製造方法。The method for producing solid fine particles according to claim 1, wherein the external action is light irradiation. 請求項１記載の固体微粒子の製造方法において、前記外部からの作用が加熱であることを特徴とする固体微粒子の製造方法。2. The method for producing solid fine particles according to claim 1, wherein the external action is heating. 請求項１記載の固体微粒子の製造方法において、前記外部からの作用が冷却であることを特徴とする固体微粒子の製造方法。The method for producing solid fine particles according to claim 1, wherein the external action is cooling. （ａ）連続相中に、分散相である固体微粒子となる原料液を送り込み、微小液滴を生成させる手段と、
（ｂ）前記微小液滴に外部からの作用を施し、前記微小液滴を固化する手段とを具備することを特徴とする固体微粒子の製造装置。(A) means for feeding a raw material liquid to be solid fine particles as a dispersed phase into a continuous phase to generate fine droplets;
(B) means for applying an external action to the microdroplets to solidify the microdroplets. 請求項５記載の固体微粒子の製造装置において、前記外部からの作用を与える光照射手段を備えることを特徴とする固体微粒子の製造装置。6. The apparatus for producing solid fine particles according to claim 5, further comprising a light irradiating means for giving an external action. 請求項５記載の固体微粒子の製造装置において、前記外部からの作用を与える加熱手段を備えることを特徴とする固体微粒子の製造装置。6. The apparatus for producing solid fine particles according to claim 5, further comprising a heating means for applying the external action. 請求項５記載の固体微粒子の製造装置において、前記外部からの作用を与える冷却手段を備えることを特徴とする固体微粒子の製造装置。6. The apparatus for producing solid fine particles according to claim 5, further comprising cooling means for applying the external action.
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