JP2007125535A - Emulsification process and emulsification apparatus - Google Patents

Emulsification process and emulsification apparatus Download PDF

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JP2007125535A
JP2007125535A JP2005347020A JP2005347020A JP2007125535A JP 2007125535 A JP2007125535 A JP 2007125535A JP 2005347020 A JP2005347020 A JP 2005347020A JP 2005347020 A JP2005347020 A JP 2005347020A JP 2007125535 A JP2007125535 A JP 2007125535A
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emulsified composition
emulsified
emulsification
composition
wall part
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JP4981312B2 (en
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Kenji Fujimoto
健二 藤本
Yoshihiko Iwasaki
義彦 岩崎
Masataka Shimizu
正高 清水
Kiyoshi Torigoe
清 鳥越
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Kiyomoto Iron & Machinery Work
Miyazaki Prefecture
Kiyomoto Iron and Machinery Works Co Ltd
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Miyazaki Prefecture
Kiyomoto Iron and Machinery Works Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide an emulsification process for easily producing a fine emulsion excellent in evenness and stability and apparatus for producing the emulsion by the process. <P>SOLUTION: The emulsion composition production process for producing an emulsion composition involves previously producing a preliminary emulsion composition of two kind liquids which are not dissolved in each other using an emulsifier and re-emulsifying the produced preliminary emulsion composition by passing the preliminary emulsion composition through a porous membrane having a uniform pre diameter. In the process, pressure is applied to pass the preliminary emulsion composition through the porous membrane while the preliminary emulsion composition is dispersed and the preliminary emulsion composition is emulsified in an emulsified composition liquid to produce an emulsion composition. Accordingly, an aimed emulsion composition can be produced in a short time and the quantity of the emulsification treatment per unit time can be increased. The apparatus can be made compact and is provided with high processing capability. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、膜乳化方法及び膜乳化装置に関し、特に、安定した微小粒子径の均一な各種タイプのエマルション、例えば、Ｏ／Ｗ型（水中油型）エマルション、Ｗ／Ｏ型（油中水型）エマルション、Ｗ／Ｏ／Ｗ型（水中油中水型）エマルション又はＯ／Ｗ／Ｏ型（油中水中油型）エマルションを製造することができる膜乳化方法及びその膜乳化装置に関する。
また、本発明は、少量のエマルション製造用の膜乳化方法及び小形の膜乳化装置に関し、特に、５０ｎｍ乃至１００μｍ、好ましくは５０ｎｍ乃至１００μｍの微小粒子のエマルションを製造するに適した単分散乳化組成物製造用の膜乳化法及びその乳化装置に関する。そしてまた、本発明は、このような乳化を連続式に行うことができる乳化方法及び装置に関する。The present invention relates to a membrane emulsification method and a membrane emulsification device, and in particular, various types of emulsions having a stable and fine particle diameter, such as O / W type (oil-in-water type) emulsion, W / O type (water-in-oil type). The present invention relates to a film emulsification method and a film emulsification apparatus capable of producing an emulsion, a W / O / W type (water-in-oil-in-water) emulsion or an O / W / O type (oil-in-water-in-oil) emulsion.
The present invention also relates to a membrane emulsification method and a small membrane emulsification apparatus for producing a small amount of emulsion, and in particular, a monodisperse emulsion composition suitable for producing an emulsion of fine particles of 50 nm to 100 μm, preferably 50 nm to 100 μm. The present invention relates to a membrane emulsification method and an emulsification apparatus for the production. The present invention also relates to an emulsification method and apparatus capable of continuously performing such emulsification.

予備乳化組成物を、孔径が微細で且つ均一な多孔質ガラス膜等の多孔質乳化膜を通して乳化して、分散粒子の粒径が１乃至１０ミクロンの微細なエマルションを製造されている。この方法は、急激な粘度上昇や温度上昇を生ずることなく、乳化精度が高い乳化物を製造することができ、また、該分散素子の孔径の大きさを変えることが容易であり、エマルションの用途に見合ったエマルションの粒子設計も可能であるために、広く使用されている。
特開平６−３９２５９号公報 The pre-emulsified composition is emulsified through a porous emulsified membrane such as a porous glass membrane having a fine pore size, and a fine emulsion having a dispersed particle size of 1 to 10 microns is produced. This method can produce an emulsion with high emulsification accuracy without causing a sudden increase in viscosity or temperature, and it is easy to change the pore size of the dispersion element. It is widely used because it is possible to design emulsion particles suitable for
JP-A-6-39259

しかし、この方法は、膜乳化に先立って、分散相の液体及び連続相の液体を予め乳化させて予備乳化液とすることを必要とし、さらに、多孔質膜に対する一方の空間を大気等の気相の空間とし、前記多孔質膜に対するもう一方の空間を予備乳化液相の空間として、比較的低い圧力で、予備乳化組成物を多孔質膜に通して乳化させるために、乳化処理量が小さく、問題とされている。また、予備乳化組成物が乳化されるまでの間に、粒子径分布が変化して、乳化の効率を低下させて問題とされている。さらに、予備乳化組成物を乳化させる際に、乳化膜が気相空間に接しているために、乳化液の乳化粒子に変形を生じ、乳化後に、乳化組成物の分散相と連続相の分離を生じて、乳化組成物の粒子径分布が変化して、乳化の効率を低下させて問題とされている。  However, this method requires that the liquid in the dispersed phase and the liquid in the continuous phase be pre-emulsified prior to membrane emulsification to form a preliminary emulsified liquid, and that one space with respect to the porous membrane is left in the atmosphere such as the atmosphere. In order to emulsify the pre-emulsified composition through the porous membrane at a relatively low pressure with the other space for the porous membrane as the space for the pre-emulsified liquid phase, the emulsification throughput is small. Has been a problem. In addition, the particle size distribution is changed before the pre-emulsified composition is emulsified, which lowers the efficiency of emulsification. Furthermore, when the preliminary emulsified composition is emulsified, the emulsion film is in contact with the gas phase space, so that the emulsified particles of the emulsion are deformed. After emulsification, the dispersed phase and the continuous phase of the emulsified composition are separated. As a result, the particle size distribution of the emulsified composition is changed, which lowers the efficiency of emulsification and is problematic.

問題を解決するための手段Means to solve the problem

殊に、近年、医療用新薬の開発や乳化系抗癌剤の臨床投与において、また高価な乳化原料を使用する液晶材料の開発や希少な界面活性剤を用いる新規なエマルションの研究開発の現場において、少量でありながら均一で、乳化精度が高く、且つ安定性に優れたエマルションの製造が必要とされており、そのようなエマルション製造のための乳化方法及び乳化装置が切望されている。  In particular, in recent years in the development of new medical drugs and clinical administration of emulsified anticancer agents, in the development of liquid crystal materials that use expensive emulsifying raw materials, and in the field of research and development of new emulsions that use rare surfactants. However, it is necessary to produce an emulsion that is uniform, has high emulsification accuracy, and is excellent in stability, and an emulsification method and an emulsification apparatus for producing such an emulsion are desired.

本発明者らは、予備乳化液による乳化法において、予備乳化の攪拌により、温度の上昇及び空気の混入は避けられず、これにより予備乳化される物質の変性等を生じることを発見し、また、予備乳化液の調製後における分散相の液体粒子同士の凝集や解膠により、膜乳化の効果が上がり難いことを発見した。本発明は、予備乳化の際の攪拌により、温度の上昇及び空気の混入は避け、予備乳化液の調製後における分散相の液体粒子同士の凝集や解膠を避けることを目的としている。  In the emulsification method using a pre-emulsified liquid, the present inventors have found that stirring of the pre-emulsification inevitably causes an increase in temperature and mixing of air, thereby causing modification of the pre-emulsified substance. It was discovered that the effect of membrane emulsification is difficult to increase due to aggregation and peptization of the liquid particles in the dispersed phase after preparation of the preliminary emulsion. An object of the present invention is to avoid temperature rise and air mixing by stirring during preliminary emulsification, and avoid aggregation and peptization of liquid particles in a dispersed phase after preparation of the preliminary emulsion.

本発明は、均一で且つ安定性に優れた微細なエマルションを、容易に製造することができる乳化方法及びその製造装置を提供することを目的としている。
即ち、本発明は、互いに溶解しない二種の液体の予備乳化組成物を、乳化剤を用いて予め製造し、この製造された予備乳化組成物を均一な孔径を有する多孔質膜を通過させて再乳化させることにより乳化組成物を製造する乳化組成物の製造方法において、予備乳化組成物を分散させながら圧力を加えて、多孔質膜を通して乳化組成物液中に乳化させることにより、乳化組成物を製造することを特徴とする乳化組成物の製造方法にあり、また、本発明は、互いに溶解しない二種の液体の予備乳化組成物を、乳化剤を用いて予め製造し、この製造された予備乳化組成物を均一な孔径を有する多孔質膜を通過させて再乳化させることにより乳化組成物を製造する乳化組成物の製造方法において、予備乳化組成物中の分散相をさらに分散させながら１ＭＰａ以上の圧力を加えて、多孔質膜を通して乳化組成物液中に乳化させることにより、前記多孔質膜の孔径より小さい平均粒子径を有する乳化組成物を製造することを特徴とする乳化組成物の製造方法にあり、さらに、本発明は、多孔質膜を通過して得られた乳化組成物中の分散相を、さらに分散させながら圧力を加えて、前記通過した多孔質膜を再度通して乳化組成物液中に乳化させることにより、前記多孔質膜の孔径より小さい平均粒子径を有する乳化組成物を製造することを特徴とする請求項１又は２に記載の乳化組成物の製造方法にあり、さらにまた、本発明は、天井壁部、側壁部及び底壁部により囲まれて形成される乳化容器と、該乳化容器の内部を仕切る多孔質膜と、多孔質膜で仕切られた一方の側に形成される予備乳化組成物形成室と、乳化膜で仕切られた他方の側に形成される乳化組成物室とを備えることを特徴とする乳化装置にあり、更に加えて、本発明は、天井壁部、側壁部及び底壁部により囲まれて形成される乳化容器と、該乳化容器の内部を仕切る多孔質膜と、前記多孔質膜で仕切られた一方の側に、分散相液体導入口、連続相液体導入口、加圧用気体導入口及び撹拌具が設けられて形成されている予備乳化組成物形成室と、多孔質膜で仕切られた他方の側に乳化組成物取出し口を設けて形成されている乳化組成物室とを備えることを特徴とする乳化装置にあり、これらの他に、本発明は、天井壁部、側壁部及び底壁部により囲まれて形成される乳化容器と、該乳化容器の内部を仕切る多孔質膜と、前記多孔質膜で仕切られた一方の側に、予備乳化組成物導入口が設けられて形成されている予備乳化組成物形成室と、前記多孔質膜で仕切られた他方の側に乳化組成物取出し口を設けて形成されている乳化組成物室とを備えることを特徴とする乳化装置にあり、またこれらの他に、本発明は、天井壁部、側壁部及び底壁部により囲まれている乳化容器と、該乳化容器の底部下方に設けられている乳化組成物取出し室と、夫々、前記乳化容器の内部を、上端開口部が大気に連通し、下端開口部が乳化組成物取出し室内に突き出して設けられている一以上の中空筒形多孔質膜と、前記多孔質膜の周囲に設けられる撹拌具と、前記乳化容器の天井壁又は側壁に形成されている連続相液体導入口、分散相液体導入口及び加圧流体導入口とを備えていることを特徴とする乳化装置にあり、そしてこれらの他に、本発明は、天井壁部、側壁部及び底壁部により囲まれている乳化容器と、該乳化容器の底部下方に設けられている乳化組成物取出し室と、夫々、前記乳化容器の内部を、上端開口部が大気に連通し、下端開口部が乳化組成物取出し室内に突き出して設けられている一以上の中空筒形多孔質膜と、前記乳化容器の天井壁又は側壁に形成されている予備乳化組成物導入口と、該予備乳化組成物導入口に送液ポンプを有する予備乳化組成物供給管とを備えていることを特徴とする乳化装置にあり、さらにこれらの他に、本発明は、中空筒形多孔質膜は、夫々の両端部が、弾性リング部材により支持されており、該弾性リング部材は、袋ナットの雌ネジ部と螺合する雄ねじ部材の前記乳化容器壁に設けられる予備乳化組成物導入口及び加圧流体導入口とを備えており、前記乳化容器の予備乳化組成物導入口は、槽内に攪拌装置を備えて、連続相液体導入口及び分散相液体導入口を備える予備乳化容器にポンプを介して接続していることを特徴とする乳化装置にある。An object of this invention is to provide the emulsification method and its manufacturing apparatus which can manufacture easily the fine emulsion which was uniform and excellent in stability.
That is, according to the present invention, two types of preliminarily emulsified compositions that do not dissolve each other are produced in advance using an emulsifier, and the produced preliminarily emulsified composition is allowed to pass through a porous membrane having a uniform pore size and re-applied. In the method for producing an emulsified composition by emulsifying, the emulsified composition is emulsified in the emulsified composition liquid through a porous membrane by applying pressure while dispersing the pre-emulsified composition. The present invention relates to a method for producing an emulsified composition, and the present invention relates to two preliminarily emulsified compositions that do not dissolve in each other using an emulsifier in advance. In the method for producing an emulsified composition, wherein the composition is passed through a porous membrane having a uniform pore size and re-emulsified, the dispersion phase in the pre-emulsified composition is further dispersed 1 An emulsified composition having an average particle size smaller than the pore size of the porous membrane is produced by emulsifying the emulsified composition liquid through the porous membrane by applying a pressure of Pa or higher. In addition, the present invention further applies pressure while further dispersing the dispersed phase in the emulsified composition obtained by passing through the porous membrane, and passing the porous membrane again through the passed porous membrane. The method for producing an emulsified composition according to claim 1 or 2, wherein an emulsified composition having an average particle size smaller than the pore size of the porous membrane is produced by emulsification in an emulsified composition liquid. Furthermore, the present invention provides an emulsification container formed by being surrounded by a ceiling wall part, a side wall part and a bottom wall part, a porous film partitioning the inside of the emulsification container, and one of the parts partitioned by the porous film Pre-emulsified composition formed on the side of An emulsification apparatus comprising: a forming chamber; and an emulsified composition chamber formed on the other side partitioned by an emulsifying film. Further, the present invention includes a ceiling wall portion, a side wall portion, and a bottom. An emulsification container surrounded by a wall, a porous film partitioning the interior of the emulsification container, and one side partitioned by the porous film, a dispersed phase liquid inlet, a continuous phase liquid inlet, A pre-emulsified composition forming chamber formed by providing a gas inlet for pressurization and a stirrer, and an emulsified composition formed by providing an emulsified composition outlet on the other side partitioned by the porous membrane In addition to these, the present invention includes an emulsification container surrounded by a ceiling wall part, a side wall part, and a bottom wall part, and an interior of the emulsification container. A preliminarily emulsified composition on one side partitioned by a porous membrane partitioning the porous membrane; A pre-emulsified composition forming chamber formed with an introduction port; and an emulsified composition chamber formed by providing an emulsified composition take-out port on the other side partitioned by the porous membrane. In addition to these, the present invention also includes an emulsification container surrounded by a ceiling wall part, a side wall part and a bottom wall part, and emulsification provided below the bottom part of the emulsification container. One or more hollow cylindrical porous membranes provided inside the emulsification container, each having an upper end opening communicating with the atmosphere and a lower end opening projecting into the emulsification composition take-out chamber A stirring tool provided around the porous membrane, and a continuous phase liquid inlet, a dispersed phase liquid inlet, and a pressurized fluid inlet formed on the ceiling wall or side wall of the emulsification container. In addition to these emulsifying devices The present invention includes an emulsification container surrounded by a ceiling wall part, a side wall part and a bottom wall part, an emulsified composition take-out chamber provided below the bottom part of the emulsification container, and the inside of the emulsification container, One or more hollow cylindrical porous membranes whose upper end opening communicates with the atmosphere and whose lower end opening protrudes into the emulsified composition take-out chamber, and a spare formed on the ceiling wall or side wall of the emulsification container An emulsifying apparatus comprising: an emulsified composition introduction port; and a pre-emulsified composition supply pipe having a liquid feed pump at the pre-emulsified composition introduction port. Both ends of the hollow cylindrical porous membrane are supported by elastic ring members, and the elastic ring members are provided on the emulsification container wall of the male screw member that is screwed with the female screw portion of the cap nut. Pre-emulsified composition inlet and pressurized fluid introduction The pre-emulsified composition inlet of the emulsification container is provided with a stirrer in the tank and connected to a pre-emulsification container having a continuous phase liquid inlet and a dispersed phase liquid inlet via a pump. It is in the emulsification apparatus characterized by having.

発明の効果The invention's effect

本発明においては、互いに溶解しない二種の液体の予備乳化組成物を、乳化剤を用いて予め製造し、この製造された予備乳化組成物を均一な孔径を有する多孔質膜を通過させて再乳化させることにより乳化組成物を製造する乳化組成物の製造方法において、予備乳化組成物を分散させながら圧力を加えて、多孔質膜を通して乳化組成物液中に乳化させるので、予備乳化組成物は、乳化組成物に接している多孔質膜の孔内を通過することとなり、前記多孔質膜の孔径より小さい平均粒子径を有する乳化組成物を、短時間で高い乳化精度の乳化組成物を容易に製造することができる。また、気泡の混入が殆ど無く、質のよい微細に分散された乳化組成物を温度上昇を小さくして製造でき、さらに、熱による変性のない乳化組成物を得ることができる。
そしてまた、本発明の乳化装置は、天井壁部、側壁部及び底壁部により囲まれている乳化容器と、該乳化容器の底部下方に設けられている乳化組成物取出し室と、夫々、前記乳化容器内に設けられ、上端開口部が大気に連通し、下端開口部が乳化組成物取出し室内に突き出して設けられている一以上の中空筒状の多孔質乳化膜部材と、前記多孔質乳化膜部材の周囲に配置されている攪拌装置と、前記乳化容器の天井壁又は側壁に設けられ前記多孔質乳化膜部材の周囲の空間内に開口する連続相液体導入管、分散相液体導入管及び加圧流体導入管とを備えているので、乳化容器内で、予備乳化組成物を製造し、この製造された予備乳化組成物を、ただちに、中空筒状の多孔質乳化膜部材を通して乳化することができることとなり、目的の乳化組成物を短時間で製造することができ、時間当たりの乳化処理量を大きくすることができる。In the present invention, two liquid pre-emulsified compositions that do not dissolve in each other are produced in advance using an emulsifier, and the produced pre-emulsified composition is re-emulsified through a porous membrane having a uniform pore size. In the method for producing an emulsified composition, the pre-emulsified composition is emulsified in the emulsified composition liquid through the porous membrane by applying pressure while dispersing the pre-emulsified composition. An emulsion composition having an average particle size smaller than the pore size of the porous membrane that passes through the pores of the porous membrane in contact with the emulsion composition can be easily converted into an emulsion composition with high emulsification accuracy in a short time. Can be manufactured. In addition, a finely dispersed emulsified composition of good quality with almost no air bubbles can be produced with a small increase in temperature, and an emulsified composition free from heat denaturation can be obtained.
And the emulsification device of the present invention comprises an emulsification container surrounded by a ceiling wall part, a side wall part and a bottom wall part, an emulsified composition take-out chamber provided below the bottom part of the emulsification container, One or more hollow cylindrical porous emulsified membrane members provided in the emulsification container, the upper end opening communicating with the atmosphere, and the lower end opening projecting into the emulsified composition take-out chamber, and the porous emulsification A stirrer disposed around the membrane member, a continuous phase liquid introduction tube provided in a ceiling wall or a side wall of the emulsification container and opening into a space around the porous emulsification membrane member, a dispersed phase liquid introduction tube, and Since a pressurized fluid introduction tube is provided, a pre-emulsified composition is produced in an emulsification container, and the produced pre-emulsified composition is immediately emulsified through a hollow cylindrical porous emulsified membrane member. The desired emulsification group Can be produced in a short time things, it is possible to increase the emulsification process amount per unit time.

本発明において、「互いに溶解しない二種の液体」は、例えば水と油のように互いに殆ど溶解しない二種の液体を意味し、「互いに溶解しない二種の液体の乳化組成物」は、互いに殆ど溶解し合わない二種の液体の乳化物（即ち、エマルション）又は互いに殆ど混ざり合わない二種の液体の乳化物（即ち、エマルション）を意味する。このような乳化組成物としては、化学薬品、医薬品、化粧品、食品、及び農薬等における種々の乳化物（即ち、エマルション）があり、さらに、化学薬品、医薬品、化粧品、食品、若しくは農薬等における各種のタイプのエマルション（乳化物）、例えば、Ｏ／Ｗ型（水中油型）エマルション、Ｗ／Ｏ型（油中水型）エマルション、Ｗ／Ｏ／Ｗ型（水中油中水型）エマルション又はＯ／Ｗ／Ｏ型（油中水中油型）エマルションがある。  In the present invention, “two types of liquids that do not dissolve each other” mean two types of liquids that hardly dissolve each other, such as water and oil, and “an emulsion composition of two types of liquids that do not dissolve each other” By two liquid emulsions (i.e. emulsions) that are hardly soluble or two liquid emulsions (i.e. emulsions) that are hardly miscible with each other. Such emulsified compositions include various emulsions (ie, emulsions) in chemicals, pharmaceuticals, cosmetics, foods, agricultural chemicals, and the like, and various chemicals, pharmaceuticals, cosmetics, foods, agricultural chemicals, and the like. Type emulsion (emulsion), for example, O / W type (oil-in-water type) emulsion, W / O type (water-in-oil type) emulsion, W / O / W type (water-in-oil-in-water type) emulsion or O There is a / W / O type (oil-in-oil-in-oil) emulsion.

本発明においては、予備乳化組成物は精密な膜乳化に先立って形成される乳化物であり、所謂、粗乳化物である。本発明においては、分散相の液体を連続相の液体中に分散させて、予備乳化組成物を形成し、さらに、分散相液体粒を連続相の液体中に分散させながら、圧力を加えて乳化膜を通して、乳化組成物中に分散相液体の微細粒を形成するものである。本発明における膜乳化において、乳化膜は、一方の側で、予備乳化された組成物即ち予備乳化組成物に接し、他方の側で、乳化された組成物即ち乳化組成物に接して設けられる。  In the present invention, the pre-emulsified composition is an emulsion formed prior to precise membrane emulsification, and is a so-called crude emulsion. In the present invention, the liquid in the dispersed phase is dispersed in the liquid in the continuous phase to form a preliminary emulsified composition, and further emulsified by applying pressure while dispersing the dispersed phase liquid particles in the liquid in the continuous phase. Through the membrane, fine particles of the dispersed phase liquid are formed in the emulsified composition. In the membrane emulsification in the present invention, the emulsion membrane is provided on one side in contact with the pre-emulsified composition, ie, the pre-emulsified composition, and on the other side, in contact with the emulsified composition, ie, the emulsion composition.

本発明においては、予備乳化組成物は、乳化膜である多孔質膜の周囲において、攪拌されて、その分散相の液体を、さらに、連続相の液体中に強制的に分散させて乳化させて形成することができる。そして、本発明においては、このように、多孔質膜の周囲において、乳化が進行する状態で、予備乳化組成物を、加圧して、多孔質乳化膜の細孔を通過させて乳化することができる。本発明においては、膜モジュール等の多孔質乳化膜部材を備える膜乳化装置内で、予備乳化組成物は、その分散相の液体が連続相の液体中に強制的に分散させられている状態において、膜乳化される。本発明において、乳化膜は、一方の側で、予備乳化液、即ち予備乳化組成物に接し、他方の側、即ち反対側で、乳化液、即ち乳化組成物に接して配置される。このように乳化膜を配置することにより、乳化の際の剪断力による変形を少なくでき、乳化された粒子の粒子径を狭い範囲に収めることができ、即ち乳化精度を上げることができる。
予備乳化組成物の膜乳化は、筒状又は管状に形成されている多孔質乳化膜部材を内部に備える膜乳化装置において、管状多孔質膜の周囲に撹拌羽根等の攪拌装置を設け、攪拌装置による攪拌下において行うことができる。また、本発明においては、一旦膜乳化させた乳化組成物を予備乳化組成物として、多孔質乳化膜部材を通して再度膜乳化させてもよい。In the present invention, the pre-emulsified composition is stirred around the porous membrane, which is an emulsified membrane, and the liquid in the dispersed phase is forcibly dispersed and emulsified in the liquid in the continuous phase. Can be formed. In the present invention, the pre-emulsified composition is pressurized and passed through the pores of the porous emulsion film while emulsification proceeds around the porous film as described above. it can. In the present invention, a pre-emulsified composition in a membrane emulsification apparatus comprising a porous emulsion membrane member such as a membrane module is in a state where the liquid in the dispersed phase is forcibly dispersed in the liquid in the continuous phase. The film is emulsified. In the present invention, the emulsion membrane is disposed on one side in contact with the pre-emulsion, i.e., the pre-emulsion composition, and on the other side, i.e., on the opposite side, in contact with the emulsion, i.e., emulsion composition. By disposing the emulsified film in this manner, deformation due to shearing force during emulsification can be reduced, and the particle diameter of the emulsified particles can be kept within a narrow range, that is, the emulsification accuracy can be increased.
Membrane emulsification of the pre-emulsified composition is a membrane emulsification apparatus provided with a porous emulsification membrane member formed in a cylindrical shape or a tube, and a stirring device such as a stirring blade is provided around the tubular porous membrane. Can be carried out with stirring. In the present invention, the emulsified composition once emulsified into a film may be preliminarily emulsified as a pre-emulsified composition and may be emulsified again through a porous emulsified film member.

本発明においては、多孔質の中空筒状の乳化膜部材で形成された乳化膜装置の周囲に、前記中空筒状の多孔質乳化膜部材を中心に撹拌羽根を配置して、前記中空筒部材を囲む周囲の空間を撹拌領域とし、予備乳化組成物の供給槽から、撹拌領域の前記多孔質乳化膜部材を囲む周囲の空間内に、互いに溶解しない二種の液体の予備乳化組成物を加圧下に供給し、撹拌羽根を回転させて撹拌乳化をさせながら、多孔質乳化膜部材の乳化膜を透過させて乳化を行うことができる。また、本発明においては、互いに溶解しない二種の液体を、夫々の液体の供給槽からポンプにより混合機に供給して混合して予備乳化させ、この予備乳化した予備乳化組成物をポンプによる撹乱状態でさらに乳化させながら、乳化膜装置に送り乳化膜を通してさらに乳化させることができる。このようにポンプで予備乳化組成物を乳化膜装置に送り、乳化させる場合は、絶えず乳化膜を通して乳化を行うことができるので、連続式に乳化を行うことが可能となる。  In the present invention, a stirring blade is disposed around the emulsified membrane device formed of a porous hollow cylindrical emulsified membrane member around the hollow cylindrical porous emulsified membrane member, and the hollow cylindrical member The surrounding space surrounding the porous emulsified membrane member is added from the pre-emulsified composition supply tank to the surrounding space surrounding the porous emulsified membrane member in the stirring region. Emulsification can be carried out by passing through the emulsified membrane of the porous emulsified membrane member while supplying under pressure and rotating the stirring blade to emulsify and emulsify. Further, in the present invention, two types of liquids that do not dissolve each other are supplied to a mixer by pumps from the respective liquid supply tanks, mixed and pre-emulsified, and the pre-emulsified pre-emulsified composition is disturbed by the pump. While being further emulsified in the state, it can be sent to the emulsifying membrane device and further emulsified through the emulsifying membrane. In this way, when the pre-emulsified composition is sent to the emulsifying membrane device by the pump and emulsified, it can be continuously emulsified through the emulsifying membrane, so that it is possible to emulsify continuously.

本発明において、撹拌領域の前記多孔質乳化膜部材を囲む周囲の空間内の予備乳化組成物の撹拌を、該空間内に設けられた撹拌子を回転させることにより行うことができる。撹拌子の回転は、マグネチックスターラにより行うことができ、また、膜乳化装置の乳化組成物取出し流路を、撹拌子の回転軸の内側を貫通して設けて、乳化組成物の取出しを行いながら、撹拌子の回転を行うことができる。  In the present invention, the preliminary emulsified composition in the space surrounding the porous emulsified membrane member in the stirring region can be stirred by rotating a stirrer provided in the space. The stirring bar can be rotated by a magnetic stirrer, and the emulsified composition take-out channel of the membrane emulsifying apparatus is provided through the inside of the rotating shaft of the stirring bar to take out the emulsified composition. However, the stirring bar can be rotated.

本発明において、膜乳化される予備乳化組成物を、前記多孔質乳化膜部材を囲む周囲の撹拌領域の空間内を通してポンプで強制循環させて膜乳化させることができる。この場合、予備乳化組成物はその動圧により、乳化膜の細孔を通過させることになる。膜乳化されない予備乳化組成物は、膜乳化装置の攪拌領域からポンプにより汲み出されて、攪拌乳化装置に送られて、強制的に攪拌され乳化されて、再度膜乳化させることができる。このようにポンプを使用して予備乳化組成物を継続して膜乳化装置に送り、連続式に乳化を行うことができ、また、繰り返し乳化を行うことができる。  In the present invention, the pre-emulsified composition to be membrane-emulsified can be forcibly circulated by the pump through the space in the surrounding stirring region surrounding the porous emulsified membrane member to be membrane-emulsified. In this case, the preliminary emulsified composition passes through the pores of the emulsified membrane due to its dynamic pressure. The pre-emulsified composition not subjected to membrane emulsification can be pumped out of the stirring region of the membrane emulsifying device, sent to the stirring emulsifying device, forcibly stirred and emulsified, and membrane emulsified again. In this way, the pre-emulsified composition can be continuously sent to the membrane emulsifier using the pump, and emulsification can be carried out continuously, and repeated emulsification can be carried out.

本発明において、連続式で多段階に乳化を行うことができる。この場合、高圧ポンプにより、予備乳化組成物を、流動抵抗の少ない乳化膜から順次流動抵抗の大きい乳化膜に送って精製エマルションを製造することができる。例えば、高圧ポンプを使用して、最初、大孔径の乳化膜に送り、この大孔径の乳化膜の乳化組成物を中孔径の乳化膜に送り、この中孔径の乳化膜の乳化組成物を小孔径の乳化膜に送り、さらに、この小孔径の乳化膜の乳化組成物を極小孔径の乳化膜に送って、精製エマルションを製造することができる。また、連続式で多段階に乳化を行う場合、例えば、１ＭＰａの低圧ポンプを使用して、大孔径の乳化膜に送り、この大孔径の乳化膜の乳化組成物を、例えば、３ＭＰａの中圧ポンプを使用して、中孔径の乳化膜に送り、この中孔径の乳化膜の乳化組成物を、例えば、１０ＭＰａの高圧ポンプを使用して、小孔径の乳化膜に送って、精製エマルションを製造することもできる。  In the present invention, it is possible to carry out emulsification in a continuous manner and in multiple stages. In this case, the pre-emulsified composition can be sequentially sent from the emulsion film having a low flow resistance to the emulsion film having a high flow resistance by a high-pressure pump to produce a purified emulsion. For example, using a high-pressure pump, first, the emulsion composition of the large pore diameter emulsion is sent to the emulsion composition of the large pore diameter emulsion and the emulsion composition of the medium pore diameter emulsion is sent to the small emulsion emulsion composition of the medium pore diameter. The purified emulsion can be produced by feeding the emulsion composition having a small pore diameter and further sending the emulsion composition of the emulsion film having a small pore diameter to the emulsion film having a very small pore diameter. Also, when emulsifying in a multi-stage continuous manner, for example, using a 1 MPa low-pressure pump, the emulsion is sent to a large pore emulsion membrane, and the emulsion composition of this large pore emulsion membrane is, for example, 3 MPa medium pressure Using a pump, the emulsion is sent to a medium-pore emulsion film, and the emulsion composition of the medium-pore emulsion film is sent to a small-pore emulsion film using, for example, a 10 MPa high-pressure pump to produce a purified emulsion. You can also

本発明においては、多孔質管状膜を使用して膜乳化する場合は、膜乳化時における乳化圧を、５ＭＰａ以上の高圧にすることができる。このように高圧下で膜乳化を行う場合、管状の乳化膜と乳化組成物の取出し管状流路との接続部が、液密に封じられていないと、乳化前の予備乳化組成物が、前記接続部から乳化組成物内に混入して、単一粒子の乳化組成物を得ることができない。そこで、本発明においては、乳化膜と乳化組成物の取出し流路との接続部をガラス皮膜により封じることにより、前記接続部からの、乳化前の予備乳化組成物の乳化組成物内への漏洩を防止することができる。この場合、ガラス皮膜を構成するガラス材は、熱膨張率が乳化膜の熱膨張率と同じガラス材から選ばれる。  In the present invention, when membrane emulsification is performed using a porous tubular membrane, the emulsification pressure during membrane emulsification can be set to a high pressure of 5 MPa or more. When membrane emulsification is carried out under high pressure in this way, the pre-emulsified composition before emulsification is obtained when the connection portion between the tubular emulsion membrane and the take-out tubular flow path of the emulsion composition is not liquid-tightly sealed. It cannot mix in an emulsion composition from a connection part and can obtain the emulsion composition of a single particle. Therefore, in the present invention, by leaking the pre-emulsified composition before emulsification from the connecting portion into the emulsified composition by sealing the connecting portion between the emulsified film and the take-out flow path of the emulsified composition with a glass film. Can be prevented. In this case, the glass material constituting the glass film is selected from glass materials having the same thermal expansion coefficient as that of the emulsion film.

本発明においては、平膜状の乳化膜を通して、高圧の液体ポンプによる、高圧下に乳化を行うことにより、例えば、５０ｎｍの粒径の、所謂、ナノサイズのエマルション（乳化組成物）を製造することができる。また、この場合、エマルションの製造が、分散相体積比が７０容積％以下で、また、粘度が１Ｐａ・ｓ以下で製造が可能であり、１ミリリットル以上の量で製造することができる。この場合、平膜状の乳化膜を、多孔板の耐食性材料の板状物で挟持して、高圧に備えることが好ましい。また、本発明において、予備乳化組成物の粒径が小さい場合には、例えば、０．１μｍ以下の場合には、一般には、撹拌しなくとも、乳化物の分離が起こらなくなるので、特に撹拌手段は必要でない。しかし、予備乳化組成物の乳化を行うためには、例えば、回転翼による攪拌乳化、超音波による攪拌乳化、振動による攪拌乳化及び回転による攪拌乳化を行うことができる。  In the present invention, a so-called nano-sized emulsion (emulsion composition) having a particle size of, for example, 50 nm is produced by emulsifying under a high pressure with a high-pressure liquid pump through a flat membrane-like emulsion film. be able to. In this case, the emulsion can be produced with a volume ratio of the dispersed phase of 70% by volume or less and with a viscosity of 1 Pa · s or less, and can be produced in an amount of 1 ml or more. In this case, it is preferable to prepare for a high pressure by sandwiching a flat membrane-like emulsified membrane with a plate-like material made of a corrosion-resistant material of a porous plate. In the present invention, when the particle size of the preliminary emulsified composition is small, for example, when it is 0.1 μm or less, in general, separation of the emulsion does not occur without stirring. Is not necessary. However, in order to emulsify the pre-emulsified composition, for example, stirring emulsification using a rotary blade, stirring emulsification using ultrasonic waves, stirring emulsification using vibration, and stirring emulsification using rotation can be performed.

以下に、添付図面を参照して本発明の実施例について説明するが、本発明は、以下の例示及び説明の内容により、何ら限定されるものではない。
図１は、本発明の乳化装置の一実施例について、その構造の概略を示す断面図である。図２は、本発明の乳化装置の別の一実施例について、その構造の概略を示す一部断面図である。図３は、本発明の乳化方法の一実施例について、その概略を示すフロー図である。図４は、図１及び図２に示す実施例とマグネチックスターラ２６の配置位置が相違する本発明の一実施例について、その構造の概略を示す部分断面図である。図５は、図１乃至図４に示す実施例と平板状の乳化膜部材を設けた点で相違するについて、その構造の概略を示す一部断面図である。図６は、図３に示す実施例とは異なる本発明の乳化方法の一実施例について、その概略を示すフロー図である。
図１乃至６において、対応する箇所には同一の符号が付されている。Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings, but the present invention is not limited to the contents of the following examples and descriptions.
FIG. 1 is a sectional view schematically showing the structure of an emulsifying device according to an embodiment of the present invention. FIG. 2 is a partial cross-sectional view showing an outline of the structure of another embodiment of the emulsification apparatus of the present invention. FIG. 3 is a flowchart showing an outline of one embodiment of the emulsification method of the present invention. FIG. 4 is a partial cross-sectional view schematically showing the structure of an embodiment of the present invention in which the magnetic stirrer 26 is disposed at a different position from the embodiment shown in FIGS. FIG. 5 is a partial cross-sectional view showing an outline of the structure of the embodiment shown in FIGS. 1 to 4 in that a flat emulsion film member is provided. FIG. 6 is a flowchart showing an outline of an embodiment of the emulsification method of the present invention different from the embodiment shown in FIG.
1 to 6, corresponding portions are denoted by the same reference numerals.

図１に示す実施例においては、乳化槽１は、天井部２、側壁部３及び底部４により筒形に形成されており、支柱に取り付け具（何れも図示されていない）を介して取り付けられている。本例において、天井部２及び底部４の間には、槽内を貫通して管状の乳化膜５が設けられており、管状の乳化膜５の上部開口部６は、天井部２に液密に保持されており、下部開口部７は底部４により液密に保持されている。天井部２には、中央部に乳化膜５の挿通用の孔８が設けられ、天井部２の孔８の周囲には、孔８から後退して環状部９が立設されている。環状部９の外側面は、ネジ部１０となっており、そのネジ部１０は、環状部９の外側に設けられるナット１１の内側ネジ部１２に螺合する。環状部９の内側面１３と孔８の間には、前記孔８を囲んで、孔８の径より大きい内径を有する、例えば、Ｏリング等の環状弾性密封部材１４が配置されている。環状弾性密封部材１４の上面に接触可能の筒形部１５を備える密封用のキャップ型の押圧部材１６は、筒形部１５を環状部９内に差し込んで配置される。押圧部材１６の上部には外方に突き出る外向きフランジ部１７が形成されており、このフランジ部１７は、前記ナット１１の上端開口部１８の内側に突き出る縁部１９に当接して、ナット１１を環状部９に締め付けることにより、押圧部材１６が環状弾性密封部材１４を押圧変形させて、天井部２の挿通用の孔８とそこを挿通する乳化膜５との間の隙間を液密に封鎖する。  In the embodiment shown in FIG. 1, the emulsification tank 1 is formed in a cylindrical shape by a ceiling part 2, a side wall part 3 and a bottom part 4, and is attached to a column via an attachment tool (none of which is shown). ing. In this example, a tubular emulsified film 5 is provided between the ceiling part 2 and the bottom part 4 so as to penetrate the tank, and the upper opening 6 of the tubular emulsified film 5 is liquid-tight to the ceiling part 2. The lower opening 7 is liquid-tightly held by the bottom 4. In the ceiling portion 2, a hole 8 for inserting the emulsified film 5 is provided in the center portion, and an annular portion 9 is erected around the hole 8 of the ceiling portion 2 so as to recede from the hole 8. The outer surface of the annular portion 9 is a screw portion 10, and the screw portion 10 is screwed into an inner screw portion 12 of a nut 11 provided on the outer side of the annular portion 9. Between the inner side surface 13 of the annular portion 9 and the hole 8, an annular elastic sealing member 14 such as an O-ring having an inner diameter larger than the diameter of the hole 8 is disposed so as to surround the hole 8. A sealing cap-type pressing member 16 having a cylindrical portion 15 that can contact the upper surface of the annular elastic sealing member 14 is disposed by inserting the cylindrical portion 15 into the annular portion 9. An outward flange portion 17 that protrudes outward is formed on the upper portion of the pressing member 16, and this flange portion 17 abuts on an edge portion 19 that protrudes inside the upper end opening 18 of the nut 11, and thereby the nut 11. Is tightened to the annular portion 9, the pressing member 16 presses and deforms the annular elastic sealing member 14, and the gap between the insertion hole 8 of the ceiling portion 2 and the emulsifying film 5 inserted therethrough is liquid-tight. Blockade.

本例において、天井部２には、加圧用気体の導入管部２０が形成されており、乳化槽１の側壁部３の上部には、乳化される分散相液体導入管接続口２１及び連続相液体導入管接続口２２が形成されている。本例においては、底部４には、管状の乳化膜５の下部の周囲に、中空の軸受け部２３が立設されており、該軸受け部２３には、磁性体の撹拌羽根２４が取り付けられている攪拌軸２５が軸支されており、乳化槽１の外側には、撹拌羽根２４が位置する周囲に、マグネチックスターラ２６が設けられている。本例において、乳化槽１内の管状の乳化膜５の周囲は、攪拌乳化空間２７となっており、マグネチックスターラ２６の作動により、磁性体の撹拌羽根２４を、管状の乳化膜５の下部の周囲で回転させて、攪拌乳化空間２７内で、粗乳化組成物をさらに攪拌乳化させることができる。本例において、管状の乳化膜５の下部は、底部４の中央部の挿通用の孔２８に挿通されて支持されている。この構造は天井部２における構造と同様である。即ち、底部４には、中央部に乳化膜５の挿通用の孔２８が設けられ、底部４の乳化膜５の挿通用の孔２８の周囲には、乳化膜５の挿通用の孔２８から後退して環状部２９が立設されている。環状部２９の外側面は、ネジ部３０となっており、そのネジ部３０は、環状部２９の外側に設けられるナット３１の内側ネジ部３２に螺合するようになっている。環状部２９の内側面３３と乳化膜５の挿通用の孔２８の間には、前記乳化膜５の挿通用の孔２８を囲んで、乳化膜５の挿通用の孔２８の径より大きい内径を有する、例えば、Ｏリング等の環状弾性密封部材３４が配置されている。環状弾性密封部材３４の下面に接触可能の筒形部３５を備える密封用のキャップ型の押圧部材３６は、筒形部３５を環状部２９内に差し込んで配置される。押圧部材３６の中間部には外方に突き出る外向きフランジ部３７が形成されており、このフランジ部３７は、前記ナット３１の下端開口部３８の内側に突き出る縁部３９′に当接して、ナット３１を環状部２９に締め付けることにより、押圧部材３６が環状弾性密封部材３４を押圧変形させて、底部４の挿通用の孔２８とそこを挿通する乳化膜５との間の隙間を液密に密封する。本例において、押圧部材３６には、管状の乳化膜５の下端開口部７が接続する乳化組成物取出し室４０′が形成されており、乳化組成物取出し室４０′には、乳化組成物取出し管４１′が接続しており、乳化膜５を通して乳化された乳化組成物は、乳化組成物取出し管４１′から取り出される。  In this example, a pressurizing gas introduction pipe part 20 is formed in the ceiling part 2, and the dispersed phase liquid introduction pipe connection port 21 to be emulsified and the continuous phase are provided above the side wall part 3 of the emulsification tank 1. A liquid introduction pipe connection port 22 is formed. In this example, a hollow bearing portion 23 is erected on the bottom portion 4 around the lower portion of the tubular emulsion film 5, and a magnetic stirring blade 24 is attached to the bearing portion 23. A stirring shaft 25 is supported, and a magnetic stirrer 26 is provided outside the emulsification tank 1 around the stirring blade 24. In this example, the periphery of the tubular emulsion film 5 in the emulsification tank 1 is a stirring emulsification space 27, and the magnetic stirrer blade 24 is moved under the tubular emulsion film 5 by the operation of the magnetic stirrer 26. , The coarsely emulsified composition can be further stirred and emulsified in the stirring emulsification space 27. In this example, the lower part of the tubular emulsion film 5 is inserted into and supported by the insertion hole 28 in the center of the bottom part 4. This structure is the same as the structure in the ceiling portion 2. That is, the bottom 4 is provided with a hole 28 for insertion of the emulsion film 5 at the center, and the hole 28 for insertion of the emulsion film 5 around the insertion hole 28 of the emulsion film 5 from the hole 28 for insertion of the emulsion film 5. The annular portion 29 is erected by retreating. The outer surface of the annular portion 29 is a threaded portion 30, and the threaded portion 30 is screwed into an inner threaded portion 32 of a nut 31 provided outside the annular portion 29. Between the inner surface 33 of the annular portion 29 and the hole 28 for insertion of the emulsion film 5, the inner diameter larger than the diameter of the hole 28 for insertion of the emulsion film 5 is surrounded by the hole 28 for insertion of the emulsion film 5. For example, an annular elastic sealing member 34 such as an O-ring is disposed. A sealing cap-type pressing member 36 having a cylindrical portion 35 that can contact the lower surface of the annular elastic sealing member 34 is disposed by inserting the cylindrical portion 35 into the annular portion 29. An outward flange portion 37 protruding outward is formed at the intermediate portion of the pressing member 36, and this flange portion 37 abuts on an edge 39 ′ protruding inside the lower end opening 38 of the nut 31, By tightening the nut 31 to the annular portion 29, the pressing member 36 presses and deforms the annular elastic sealing member 34, and the gap between the insertion hole 28 of the bottom portion 4 and the emulsifying film 5 inserted therethrough is liquid-tight. To seal. In this example, an emulsified composition take-out chamber 40 ′ to which the lower end opening 7 of the tubular emulsified film 5 is connected is formed in the pressing member 36, and the emulsified composition take-out chamber 40 ′ has an emulsified composition take-out chamber 40 ′. The pipe | tube 41 'is connected and the emulsified composition emulsified through the emulsified film 5 is taken out from the emulsified composition take-out pipe 41'.

本例は、以上のように構成されているので、乳化される食用油等の分散相液体を分散相液体導入管入口２１から乳化槽１に供給すると共に、乳化剤を混合した水等の連続相液体を連続相液体導入管入口２２から乳化槽１に供給して、マグネチックスターラ２６を作動させて、磁性体の撹拌羽根２４を回転させ、食用油等の分散相液体と乳化剤を混合した水等の連続相液体を混合して、攪拌乳化空間２７内に、予備乳化組成物を調製する。その後も攪拌羽根による攪拌乳化を続けながら、加圧用気体の窒素ガスを導入管部２０から、攪拌乳化空間２７内に導入し、攪拌乳化空間２７内の気圧を５ＭＰａ以上に高めて、例えば、平均細孔径が１．０μｍの乳化膜を使用して乳化した。乳化組成物は、乳化組成物取出し室４０′から乳化液組成物出し管４１′により取り出した。本例において、多孔質の管状乳化膜５の端部は、その侭、環状弾性部材に支持させているが、多孔質の管状乳化膜５の端部を、同じ熱膨張係数を有する液密のガラス部材で被覆することにより、外部の予備乳化組成物の多孔質の管状乳化膜５内への侵入を防止して、乳化精度を高めることが出来る。  Since this example is configured as described above, a dispersed phase liquid such as edible oil to be emulsified is supplied from the dispersed phase liquid inlet pipe inlet 21 to the emulsification tank 1 and a continuous phase such as water mixed with an emulsifier. The liquid is supplied from the continuous phase liquid inlet pipe inlet 22 to the emulsification tank 1, the magnetic stirrer 26 is operated, the magnetic stirring blade 24 is rotated, and water in which the dispersed phase liquid such as edible oil and the emulsifier are mixed is mixed. A pre-emulsified composition is prepared in the stirring emulsification space 27 by mixing continuous phase liquids such as the above. After that, while continuing the stirring and emulsification with the stirring blade, a nitrogen gas as a pressurizing gas is introduced into the stirring and emulsifying space 27 from the introduction pipe portion 20, and the atmospheric pressure in the stirring and emulsifying space 27 is increased to 5 MPa or more. Emulsification was performed using an emulsified membrane having a pore size of 1.0 μm. The emulsified composition was taken out from the emulsified composition take-out chamber 40 ′ through an emulsified liquid composition take-out tube 41 ′. In this example, the end portion of the porous tubular emulsion film 5 is supported by the ring-shaped elastic member, but the end portion of the porous tubular emulsion film 5 is liquid-tight having the same thermal expansion coefficient. By covering with a glass member, it is possible to prevent the external preliminary emulsified composition from entering the porous tubular emulsion film 5 and to improve the emulsification accuracy.

本例においては、乳化槽１内に分散相を形成する液体と、連続相を形成する液体とを槽内に導入して攪拌乳化して予備乳化組成物を形成し、乳化膜を通して乳化組成物を製造しているが、予備乳化組成物を別の槽で形成し、形成された予備乳化組成物を乳化槽１内に導入して、槽内で攪拌乳化させながら、加圧気体の加圧圧力により多孔質の管状乳化膜５を通して乳化させて、乳化組成物とすることができる。本例において、撹拌羽根を磁性材料で形成し、マグネチックスターラにより回転させているが、側壁部に複数個の撹拌羽根を設けて、夫々、電動機により回転させて行うことが出来る。  In this example, a liquid for forming a dispersed phase in the emulsifying tank 1 and a liquid for forming a continuous phase are introduced into the tank and stirred and emulsified to form a pre-emulsified composition, and the emulsified composition is passed through the emulsion film. The pre-emulsified composition is formed in a separate tank, and the pre-emulsified composition thus formed is introduced into the emulsification tank 1 and stirred and emulsified in the tank while pressurizing the pressurized gas. An emulsified composition can be obtained by emulsifying through the porous tubular emulsion film 5 under pressure. In this example, the stirring blade is made of a magnetic material and is rotated by a magnetic stirrer. However, a plurality of stirring blades are provided on the side wall, and each of them can be rotated by an electric motor.

図２に示す実施例においては、乳化槽１は、天井板部２０１、側壁部３及び底板部４０１により筒形に形成されており、天井板部２０１及び底板部４０１間には、槽内を貫通して複数の管状の乳化膜５（図にはその内の一個のみが示され、他は省略されて図示されていない）が同一円周上に並設されている。本例において、夫々の管状の乳化膜５の上部開口部６は、天井板部２０１に液密に保持されており、また、下部開口部７は底板部４０１に液密に保持されている。天井板部２０１には、管状の乳化膜５の配置箇所に夫々対応して、乳化膜５の挿通用孔３９が設けられている。本例において、天井板部２０１の挿通用孔３９には、その下部に、例えば、Ｏリング等の環状弾性密封部材４０が配置可能の大きさで中央に張り出す内向きフランジ部４１が形成されており、またその上部に、ネジ部４２が形成されており、該ネジ部４２に中空状のナット４３を上から下に向けて螺着することにより、ネジ部４２内に配置され、例えば、Ｏリング等の環状弾性密封部材４０を押圧変形させて、天井板部２０１の挿通用孔３９とそこを挿通する乳化膜５との間の隙間を液密に封鎖する。同様に底板部４０１においても、底板部４０１の挿通用孔４４には、その上部に、例えば、Ｏリング等の環状弾性密封部材４５が配置可能の大きさで中央に張り出す内向きフランジ部４６が形成されており、またその上部にネジ部４２が形成されており、該ネジ部４２に中空状のナット４５を下から上に向けて螺着することにより、ネジ部４２内に配置される、例えば、Ｏリング等の環状弾性密封部材４５を押圧変形させて、底板部４０１の挿通用の孔４４とそこを挿通する乳化膜５との間の隙間を液密に封鎖する。    In the embodiment shown in FIG. 2, the emulsification tank 1 is formed in a cylindrical shape by the ceiling plate part 201, the side wall part 3 and the bottom plate part 401, and the inside of the tank is interposed between the ceiling plate part 201 and the bottom plate part 401. A plurality of tubular emulsified membranes 5 (only one of them is shown in the figure and the others are omitted and are not shown) are arranged in parallel on the same circumference. In this example, the upper opening 6 of each tubular emulsified film 5 is liquid-tightly held on the ceiling plate portion 201, and the lower opening 7 is held liquid-tight on the bottom plate portion 401. The ceiling plate portion 201 is provided with insertion holes 39 for the emulsified film 5 corresponding to the arrangement positions of the tubular emulsified film 5. In this example, the insertion hole 39 of the ceiling plate portion 201 is formed with an inward flange portion 41 projecting to the center with a size such that an annular elastic sealing member 40 such as an O-ring can be disposed, for example. Further, a screw portion 42 is formed on the upper portion thereof, and a hollow nut 43 is screwed onto the screw portion 42 from the top to the bottom. The annular elastic sealing member 40 such as an O-ring is pressed and deformed, and the gap between the insertion hole 39 of the ceiling plate portion 201 and the emulsified film 5 inserted therethrough is sealed in a liquid-tight manner. Similarly, in the bottom plate portion 401, the inward flange portion 46 projects to the center with a size that allows the annular elastic sealing member 45 such as an O-ring to be disposed on the insertion hole 44 of the bottom plate portion 401. Further, a screw part 42 is formed on the upper part thereof, and a hollow nut 45 is screwed onto the screw part 42 from below to be arranged in the screw part 42. For example, the annular elastic sealing member 45 such as an O-ring is pressed and deformed to liquid-tightly seal a gap between the insertion hole 44 of the bottom plate portion 401 and the emulsified film 5 inserted therethrough.

本例において、天井板部２０１の上方には、乳化組成物の上部取出し室４８が形成されており、底部板部４０１の下方には、乳化組成物の下部取出し室４８が形成されている。乳化組成物の上部取出し室４７には、乳化組成物の上部取出し管４９が接続し、また、乳化組成物の下部取出し室４８には、乳化組成物の下部取出し管５０が接続している。乳化槽１の側壁部３の中央部には、予備乳化組成物導入用入口５１が設けられており、側壁部３の上部には、圧力計接続部５２及び開閉弁５３を備える空気抜き用開口部５４（図３）が設けられている。本例においては、乳化槽１内には、管状の乳化膜５が円周上に複数個配置されており、複数の管状の乳化膜５に囲まれた乳化槽１の底部中心部には、回転軸５２に取り付けられて撹拌羽根２４が設けられている。撹拌羽根２４を中心にして管状の乳化膜５の周囲は、攪拌乳化領域２７となっている。本例において、撹拌羽根２４が取り付けられている回転軸５２は、上端部が天井板部２０１に回動可能に取り付けられ、下端部が底板部４０１に回動可能に取り付けられており、側壁部３の外側の撹拌羽根２４の周囲にはマグネチックスターラ２６が配置されている。  In this example, an upper take-out chamber 48 for the emulsified composition is formed above the ceiling plate portion 201, and a lower take-out chamber 48 for the emulsified composition is formed below the bottom plate portion 401. The emulsified composition upper take-out pipe 47 is connected to the upper take-out chamber 47 of the emulsified composition, and the lower take-out pipe 50 of the emulsified composition is connected to the lower take-out chamber 48 of the emulsified composition. A pre-emulsified composition introduction inlet 51 is provided at the center of the side wall 3 of the emulsification tank 1, and an air vent opening provided with a pressure gauge connection 52 and an on-off valve 53 at the top of the side wall 3. 54 (FIG. 3) is provided. In this example, a plurality of tubular emulsion films 5 are arranged on the circumference in the emulsification tank 1, and at the center of the bottom of the emulsion tank 1 surrounded by the plurality of tubular emulsion films 5, A stirring blade 24 is provided attached to the rotary shaft 52. A stirring emulsification region 27 is formed around the tubular emulsification film 5 around the stirring blade 24. In this example, the rotating shaft 52 to which the stirring blade 24 is attached has an upper end portion that is rotatably attached to the ceiling plate portion 201 and a lower end portion that is rotatably attached to the bottom plate portion 401. A magnetic stirrer 26 is disposed around the outer agitating blade 24 of the third.

本例は、以上のように構成されているので、空気抜き用開口部５４の開閉弁５３を開いて、乳化される食用油等の分散相液体と、乳化剤を混合した水等の連続相液体とを混合して調製された予備乳化組成物を、予備乳化組成物導入管入口５１から乳化槽１内に圧送を開始する。予備乳化組成物の圧送を開始すると共に予備乳化組成物のマグネチックスターラ２６を作動させて、撹拌羽根２４を回転させる。予備乳化組成物の圧送を継続して、乳化槽１内が予備乳化組成物で満たされたところで、開閉弁５３を閉じる。開閉弁５３が閉じられた後も、撹拌羽根２４の攪拌下に、予備乳化組成物の圧送を継続して行い、予備乳化組成物を攪拌乳化する。この乳化槽１内に導入され、攪拌乳化された予備乳化組成物は、乳化されながら、乳化膜５の細孔を通過してより乳化される。乳化された組成物は、乳化組成物の下部取出し室４８に集められ、乳化組成物の下部取出し管５０から取り出される。  Since this example is configured as described above, the on-off valve 53 of the air vent opening 54 is opened, and a dispersed phase liquid such as edible oil to be emulsified and a continuous phase liquid such as water mixed with an emulsifier The pre-emulsified composition prepared by mixing the pre-emulsified composition into the emulsification tank 1 from the pre-emulsified composition introduction pipe inlet 51 is started. The pumping of the pre-emulsified composition is started and the magnetic stirrer 26 of the pre-emulsified composition is operated to rotate the stirring blade 24. The pre-emulsified composition is continuously pumped, and the on-off valve 53 is closed when the emulsification tank 1 is filled with the pre-emulsified composition. Even after the on-off valve 53 is closed, the preliminary emulsified composition is continuously fed under stirring by the stirring blade 24 to stir and emulsify the preliminary emulsified composition. The pre-emulsified composition introduced into the emulsification tank 1 and stirred and emulsified passes through the pores of the emulsified film 5 and is emulsified while being emulsified. The emulsified composition is collected in the lower take-out chamber 48 of the emulsified composition and taken out from the lower take-out pipe 50 of the emulsified composition.

図３は、図２に示す実施例の装置を使用したフロー図である。
図３において、撹拌装置５５を備える分散相供給槽５６は、供給用開閉弁５７を備える分散相供給管５８及び流量計５９を介して第一Ｔ字形分岐管６０の第一分岐流路６１に接続しており、また、撹拌装置６２を備える連続相供給槽６３は、供給用開閉弁６４を備える分散相供給管６５を介して第一Ｔ字形分岐管６０の第二分岐流路６７に接続している。第一Ｔ字形分岐管６０の第三分岐流路６８は、開閉弁６９を備える粗混合組成物供給管７０に接続している。粗混合組成物供給管７０は、第二Ｔ字形分岐管７１の第一分岐流路７２に接続しており、第二Ｔ字形分岐管７１の第二分岐流路７３は、送液ポンプ７４を備える予備乳化組成物供給管７５に接続している。予備乳化組成物供給管７５は、乳化槽１の予備乳化組成物導入用入り口５１に接続している。本例において、乳化槽１の乳化組成物の下部取出し管５０は、乳化槽１からの乳化組成物が、乳化組成物収容槽７６に収集されるように、管路７７を介して乳化物収容槽７６に接続している。乳化物収容槽７６の乳化組成物取出し管７８は、第三Ｔ字形分岐管７９の第一分岐流路８０に接続している。本例において、第三Ｔ字形分岐管７９の第二分岐流路８１は、開閉弁８２を備える乳化組成物供給管８３を介して、第二Ｔ字形分岐管７１の第三分岐流路８４に接続している。FIG. 3 is a flow diagram using the apparatus of the embodiment shown in FIG.
In FIG. 3, the dispersed phase supply tank 56 provided with the stirring device 55 is connected to the first branch flow path 61 of the first T-shaped branch pipe 60 via the dispersed phase supply pipe 58 provided with the supply opening / closing valve 57 and the flow meter 59. The continuous phase supply tank 63 connected with the stirring device 62 is connected to the second branch flow path 67 of the first T-shaped branch pipe 60 via the dispersed phase supply pipe 65 including the supply on-off valve 64. is doing. The third branch flow path 68 of the first T-shaped branch pipe 60 is connected to a crude mixed composition supply pipe 70 including an on-off valve 69. The crude mixed composition supply pipe 70 is connected to the first branch flow path 72 of the second T-shaped branch pipe 71, and the second branch flow path 73 of the second T-shaped branch pipe 71 is connected to the liquid feed pump 74. The pre-emulsified composition supply pipe 75 provided is connected. The pre-emulsified composition supply pipe 75 is connected to the pre-emulsified composition introduction inlet 51 of the emulsification tank 1. In this example, the lower take-out pipe 50 of the emulsified composition in the emulsifying tank 1 accommodates the emulsion via the conduit 77 so that the emulsified composition from the emulsifying tank 1 is collected in the emulsified composition accommodating tank 76. It is connected to the tank 76. The emulsion composition take-out pipe 78 of the emulsion storage tank 76 is connected to the first branch flow path 80 of the third T-shaped branch pipe 79. In this example, the second branch flow path 81 of the third T-shaped branch pipe 79 is connected to the third branch flow path 84 of the second T-shaped branch pipe 71 via the emulsion composition supply pipe 83 provided with the on-off valve 82. Connected.

本例は、以上のように構成されているので、分散相供給槽５６に入れられている乳化される食用油等の分散相液体は、分散相供給管５８から流量計５９を介して、その所定流量が、送液ポンプ７４により、第一Ｔ字形分岐管６０の第二分岐流路６１に送られ、他方、連続相供給槽６３に入れられている乳化剤を混合した水等の連続相液体は、連続相供給管６５から流量計６６を介して、その所定流量が、送液ポンプ７４により、第一Ｔ字形分岐管６０の第二分岐流路６７に送られ、第一Ｔ字形分岐管６０内で混合されて、粗混合組成物が形成される。粗混合組成物は、開閉弁６９を通ってさらに混合されて、第二Ｔ字形分岐管７１の第一分岐流路７２に送られる。他方、乳化物収容槽７６の乳化物は、乳化物供給管８３から、第二Ｔ字形分岐管７１の第三分岐流路８４に送られ、第二Ｔ字形分岐管７１内で、第二Ｔ字形分岐管７１の第一分岐流路７２から送られる粗混合組成物と混合して、予備乳化組成物が形成される。この予備乳化組成物は、送液ポンプ７４内で更に均一に混合されて、乳化槽１内に予備乳化組成物導入管入口５１から乳化槽１内に圧送される。予備乳化組成物が圧送されると共に予備乳化組成物のマグネチックスターラ２６を作動させて、撹拌羽根２４を回転させる。予備乳化組成物の圧送を継続して、乳化槽１内が予備乳化組成物で満たされたところで、開閉弁５３を閉じる。開閉弁５３が閉じられた後も、撹拌羽根２４の攪拌下に、予備乳化組成物の圧送を継続して行い、予備乳化組成物を攪拌乳化する。この乳化槽１内に導入され、攪拌乳化される。本例において、予備乳化組成物は、乳化されながら、乳化膜５の細孔を通過して乳化され、より微細な粒子の乳化組成物になる。乳化された乳化物は、下部取出し室４８に集められ、乳化組成物の下部取出し管５０から取り出され、乳化物収容槽７６に収容される。  Since this example is configured as described above, the dispersed phase liquid such as edible oil to be emulsified contained in the dispersed phase supply tank 56 passes through the flow meter 59 from the dispersed phase supply pipe 58. A predetermined flow rate is sent to the second branch flow path 61 of the first T-shaped branch pipe 60 by the liquid feed pump 74, and on the other hand, a continuous phase liquid such as water mixed with an emulsifier placed in the continuous phase supply tank 63. The predetermined flow rate is sent from the continuous phase supply pipe 65 through the flow meter 66 to the second branch channel 67 of the first T-shaped branch pipe 60 by the liquid feed pump 74, and the first T-shaped branch pipe Mix within 60 to form a crude mixed composition. The coarsely mixed composition is further mixed through the on-off valve 69 and sent to the first branch flow path 72 of the second T-shaped branch pipe 71. On the other hand, the emulsion in the emulsion storage tank 76 is sent from the emulsion supply pipe 83 to the third branch channel 84 of the second T-shaped branch pipe 71, and in the second T-shaped branch pipe 71, the second T The pre-emulsified composition is formed by mixing with the coarsely mixed composition sent from the first branch flow path 72 of the letter-shaped branch pipe 71. The preliminary emulsified composition is further uniformly mixed in the liquid feeding pump 74 and is pumped into the emulsifying tank 1 from the preliminary emulsified composition introduction pipe inlet 51 into the emulsifying tank 1. The pre-emulsified composition is pumped and the magnetic stirrer 26 of the pre-emulsified composition is operated to rotate the stirring blade 24. The pre-emulsified composition is continuously pumped, and the on-off valve 53 is closed when the emulsification tank 1 is filled with the pre-emulsified composition. Even after the on-off valve 53 is closed, the preliminary emulsified composition is continuously fed under stirring by the stirring blade 24 to stir and emulsify the preliminary emulsified composition. It introduce | transduces in this emulsification tank 1, and is stirred and emulsified. In this example, the pre-emulsified composition is emulsified and emulsified through the pores of the emulsified film 5 to become an emulsified composition of finer particles. The emulsified emulsion is collected in the lower take-out chamber 48, taken out from the lower take-out pipe 50 of the emulsified composition, and stored in the emulsion storage tank 76.

図４に示す実施例は、図１及び図２に示す実施例とマグネチックスターラ２６の配置位置が相違する例である。
本例において、マグネチックスターラ２６は、底板部４０１の下方に、モータ８５の回転軸８６に永久磁石８７を取り付けて形成されており、磁石撹拌羽根２４は、天井板部２０１に延びる回転軸８８に設けられている。モータの作動により永久磁石８７を回転させ、この永久磁石８７の回転による磁気作用により磁石撹拌羽根２４を回転させて、予備乳化組成物形成域２７内の予備乳化組成物を撹拌し、乳化させる。The embodiment shown in FIG. 4 is an example in which the arrangement position of the magnetic stirrer 26 is different from the embodiment shown in FIGS. 1 and 2.
In this example, the magnetic stirrer 26 is formed by attaching a permanent magnet 87 to a rotating shaft 86 of a motor 85 below the bottom plate portion 401, and the magnet stirring blade 24 has a rotating shaft 88 extending to the ceiling plate portion 201. Is provided. The permanent magnet 87 is rotated by the operation of the motor, and the magnetic stirring blade 24 is rotated by the magnetic action caused by the rotation of the permanent magnet 87 to stir and emulsify the pre-emulsified composition in the pre-emulsified composition forming area 27.

本例において、底板部４０１には、管状の乳化膜５の挿通用孔４４が設けられている。この管状の乳化膜５の挿通用孔４４には、その上部に、例えば、Ｏリング等の環状弾性密封部材４３が配置可能の大きさで中央に張り出す内向きフランジ部４６が形成されており、またその下部にネジ部４７が形成されており、該ネジ部４７に中空状のナット４５を下から上に向けて螺着することにより、ネジ部４７内に配置される、例えば、Ｏリング等の環状弾性密封部材４３を押圧変形させて、底板部４０１の挿通用の孔４４とそこを挿通する乳化膜５との間の隙間を液密に封鎖する。乳化された組成物、即ち乳化組成物は、下部取出し室４８に集められ、下部取出し管５０から取り出される。  In this example, the bottom plate 401 is provided with an insertion hole 44 for the tubular emulsion film 5. The insertion hole 44 of the tubular emulsified membrane 5 is formed with an inward flange portion 46 projecting to the center with a size that allows an annular elastic sealing member 43 such as an O-ring to be arranged, for example. Further, a screw part 47 is formed in the lower part thereof, and a hollow nut 45 is screwed into the screw part 47 from below to be arranged in the screw part 47, for example, an O-ring. The annular elastic sealing member 43 is pressed and deformed, and the gap between the insertion hole 44 of the bottom plate portion 401 and the emulsified film 5 inserted therethrough is liquid-tightly sealed. The emulsified composition, that is, the emulsified composition is collected in the lower take-out chamber 48 and taken out from the lower take-out pipe 50.

図５に示す実施例は、図１乃至図４に示す実施例と相違して、平板状の乳化膜部材８９を設けた例である。平板状の乳化膜部材８９は、上側の多孔板９０と下側の多孔板９１の間に乳化膜９２を挟着して形成されている。上側の多孔板９０の周縁部９３及び下側の多孔板９１の周辺部９４には共に孔が形成されておらず、多孔板９０及び９１は、夫々その周辺部９３及び９４をそれぞれＯリング等の環状弾性密封部材４３に密着させることにより、少なくとも液密に密封されている。本例において、乳化膜８９で仕切られた上部は蓋部９４で囲まれた空間であり、乳化室９５となっており、その天井部には予備乳化組成物導入口９６が形成されている。この予備乳化物導入口９６は、例えば、分散相供給槽５６及び連続相供給槽６３にポンプ６９を備える予備乳化組成物供給管７５に接続させることができる。蓋体部９４は、本体部９７の上部側壁部９８の上端開口部内に嵌入し、蓋部９４の外周面は本体部９７の上部側壁部９８に囲われている。本例において、本体部９７の上部側壁部９８を覆って蓋部押さえナット９９が設けられており、上部側壁９８の外周部と蓋部押さえナット９９の内周部には、夫々ネジ部が形成されて、ネジ係合部１００が形成されている。本体部９７の上部側壁部９８と蓋部押さえナット９９をネジ係合部１００で互いに螺合させて、本体部９７に対して押さえナット１００を押し下げることにより。本体部９７の内側棚状部の溝１０１内に配置されているＯリング４３及び蓋体部９４の外周下端部の切欠き部１０２内に配置されているＯリング４３を押圧して蓋体部９４と、本体部９７の間を密封する。本例において、本体部９７の底部には乳化物排出口が形成されている。
本例において、乳化膜８９で仕切られた下部は本体部９７で囲まれた空間であり、乳化組成物室１０３となっており、その底部には乳化組成物取出し口１０４が形成されている。The embodiment shown in FIG. 5 is an example in which a flat emulsion film member 89 is provided, unlike the embodiment shown in FIGS. The flat emulsion film member 89 is formed by sandwiching an emulsion film 92 between an upper porous plate 90 and a lower porous plate 91. No holes are formed in the peripheral portion 93 of the upper porous plate 90 and the peripheral portion 94 of the lower porous plate 91, and the porous plates 90 and 91 are respectively connected to the peripheral portions 93 and 94 by O-rings or the like. The ring-shaped elastic sealing member 43 is in close contact with the ring-shaped elastic sealing member 43 to at least liquid-tightly seal. In this example, the upper part partitioned by the emulsifying film 89 is a space surrounded by a lid part 94, which is an emulsifying chamber 95, and a pre-emulsified composition inlet 96 is formed in the ceiling part. The preliminary emulsion introduction port 96 can be connected to, for example, a preliminary emulsion composition supply pipe 75 provided with a pump 69 in the dispersed phase supply tank 56 and the continuous phase supply tank 63. The lid body portion 94 is fitted into the upper end opening of the upper side wall portion 98 of the main body portion 97, and the outer peripheral surface of the lid portion 94 is surrounded by the upper side wall portion 98 of the main body portion 97. In this example, a lid holding nut 99 is provided so as to cover the upper side wall portion 98 of the main body portion 97, and screw portions are formed on the outer peripheral portion of the upper side wall 98 and the inner peripheral portion of the lid portion pressing nut 99, respectively. Thus, a screw engaging portion 100 is formed. The upper side wall portion 98 of the main body portion 97 and the lid portion pressing nut 99 are screwed together by the screw engaging portion 100, and the pressing nut 100 is pressed down against the main body portion 97. The O-ring 43 arranged in the groove 101 of the inner shelf-like portion of the main body 97 and the O-ring 43 arranged in the notch 102 at the lower end of the outer periphery of the lid 94 are pressed to form the lid. 94 and the body 97 are sealed. In this example, an emulsion discharge port is formed at the bottom of the main body 97.
In this example, the lower part partitioned by the emulsifying film 89 is a space surrounded by a main body part 97, which is an emulsified composition chamber 103, and an emulsified composition outlet 104 is formed at the bottom.

本例は、以上のように構成されているので、予備乳化組成物導入口９６から乳化槽１内に予備乳化組成物を混合しながら供給し、ポンプによる加圧により、例えば、６．５ＭＰａ圧力下で、乳化膜５を通して膜乳化を行う。乳化膜５を通って乳化された乳化組成物は、乳化精度が高い乳化組成物であり、乳化組成物室１０３に集められ、乳化組成物取出し口１０４から取り出される。本例は、予備乳化組成物をポンプで圧入して、予備乳化組成物の乳化を行うものであり、予備乳化組成物の乳化処理時間を短縮すると共に、予備乳化組成物の微細な乳化物を得ることができる。  Since this example is configured as described above, the pre-emulsified composition is supplied from the pre-emulsified composition inlet 96 into the emulsification tank 1 while being mixed, and is pressurized by a pump, for example, at a pressure of 6.5 MPa. Below, membrane emulsification is performed through the emulsion membrane 5. The emulsified composition emulsified through the emulsified film 5 is an emulsified composition having high emulsification accuracy, and is collected in the emulsified composition chamber 103 and taken out from the emulsified composition outlet 104. In this example, the pre-emulsified composition is press-fitted with a pump to emulsify the pre-emulsified composition, the emulsification time of the pre-emulsified composition is shortened, and a fine emulsion of the pre-emulsified composition is reduced. Obtainable.

図６は、図５に示す実施例の装置を使用したフロー図である。
図６に示す実施例において、乳化装置はバッチ式の予備乳化組成物形成槽１０５と、平膜型の膜透過モジュール１０６で構成されており、予備乳化組成物形成槽１０５と、平膜型の膜透過モジュール１０６は予備乳化組成物供給管１０７により接続している。予備乳化組成物形成槽１０５には、ガス圧による加圧を行うための加圧ガス供給管１０８と、予備乳化組成物形成槽１０５内のガス抜きを行うためのガス抜き管１０９が設けられている。本例において、加圧ガス供給管１０８は加圧用ガス供給源（図示されていない）に接続している。本例において、バッチ式の予備乳化組成物形成槽１０５には、内部に磁石製の撹拌羽根が設けられており、予備乳化組成物形成槽１０５の底部下方には、マグネチックスターラ２６が設けられている。予備乳化組成物形成槽１０５の磁石製の撹拌羽根は、マグネチックスターラ２６のモータ８５の作動により、モータ８５の回転軸に取り付けられている磁石８７を回転させ、この永久磁石８７の回転による磁気作用により磁石撹拌羽根を回転させて、予備乳化組成物形成槽１０５内の予備乳化組成物を撹拌乳化させて、より微細な予備乳化組成物とすることができる。本例において、予備乳化組成物形成槽１０５の容積は、膜透過モジュール１０６の容積より遥かに大きく形成されている。予備乳化組成物形成槽１０５は、膜透過モジュール１０６の容積より遥かに大きく形成されている。予備乳化組成物形成槽１０５を複数設け、夫々の予備乳化組成物形成槽１０５を、流路切り替え弁を介して膜透過モジュール１０６に接続させることができる。本例において、１１０は安全弁であり、１１１は圧力計である。FIG. 6 is a flowchart using the apparatus of the embodiment shown in FIG.
In the embodiment shown in FIG. 6, the emulsifying apparatus is composed of a batch type pre-emulsified composition forming tank 105 and a flat membrane type membrane permeation module 106, and the pre-emulsified composition forming tank 105 and the flat membrane type The membrane permeation module 106 is connected by a pre-emulsified composition supply pipe 107. The pre-emulsified composition forming tank 105 is provided with a pressurized gas supply pipe 108 for performing pressurization by gas pressure and a degassing pipe 109 for degassing the pre-emulsified composition forming tank 105. Yes. In this example, the pressurized gas supply pipe 108 is connected to a pressurized gas supply source (not shown). In this example, the batch-type pre-emulsified composition forming tank 105 is provided with a magnetic stirring blade inside, and a magnetic stirrer 26 is provided below the bottom of the pre-emulsified composition forming tank 105. ing. The magnetic stirring blades of the pre-emulsified composition forming tank 105 rotate the magnet 87 attached to the rotating shaft of the motor 85 by the operation of the motor 85 of the magnetic stirrer 26, and the magnetic force generated by the rotation of the permanent magnet 87. By rotating the magnet stirring blade by the action, the pre-emulsified composition in the pre-emulsified composition forming tank 105 can be stirred and emulsified to obtain a finer pre-emulsified composition. In this example, the volume of the pre-emulsified composition forming tank 105 is much larger than the volume of the membrane permeation module 106. The preliminary emulsified composition forming tank 105 is formed to be much larger than the volume of the membrane permeation module 106. A plurality of preliminary emulsified composition forming tanks 105 can be provided, and each of the preliminary emulsified composition forming tanks 105 can be connected to the membrane permeation module 106 via a flow path switching valve. In this example, 110 is a safety valve and 111 is a pressure gauge.

本例は以上のように構成されているので、分散相の液体と、界面活性剤を予め混合させた連続相の液体を予備乳化組成物形成槽１０５内に入れて、マグネチックスターラ２６のモータ８５を作動させ、モータ８５の回転軸に取り付けられている永久磁石８７を回転させる。この永久磁石８７の回転による磁気作用により磁石撹拌羽根を回転させて、予備乳化組成物形成槽１０５内の分散相の液体を連続相の液体と撹拌混合させて乳化させる。撹拌により乳化された予備乳化組成物は加圧ガス供給管から送られる加圧ガスにより押し出されて、平膜型の膜透過モジュール１０６に送られる。平膜型の膜透過モジュール１０６には、平均孔径が５０ｎｍの平膜型の乳化膜が設けられており、この平均孔径が５０ｎｍの平膜型の乳化膜を通過させることにより、５０ｎｍ以下の粒径の乳化組成物に精密乳化すもことができる。  Since this example is configured as described above, a liquid of a dispersed phase and a liquid of a continuous phase in which a surfactant is preliminarily mixed are placed in the pre-emulsified composition forming tank 105, and a motor of the magnetic stirrer 26 is obtained. 85 is operated to rotate the permanent magnet 87 attached to the rotating shaft of the motor 85. The magnetic stirring blade is rotated by the magnetic action caused by the rotation of the permanent magnet 87, and the liquid in the dispersed phase in the preliminary emulsion composition forming tank 105 is stirred and mixed with the liquid in the continuous phase to emulsify. The pre-emulsified composition emulsified by stirring is pushed out by the pressurized gas sent from the pressurized gas supply pipe and sent to the flat membrane type membrane permeation module 106. The flat membrane type membrane permeation module 106 is provided with a flat membrane type emulsion membrane having an average pore size of 50 nm. By passing the flat membrane type emulsion membrane having an average pore size of 50 nm, particles having a size of 50 nm or less are passed. It is also possible to finely emulsify into an emulsion composition having a diameter.

例１
図１に示す実施例により、大豆油３０重量％の水中油型の乳化組成物を製造した。
３０重量部の大豆油を、０．２重量部のＳＤＳ（硫酸ドデシルナトリウム）を含む１００重量部の水に加えて撹拌混合し、大豆油粒子の平均粒子径が１０７μｍの予備乳化組成物を調製した。この予備乳化組成物を、ゲージ圧で０．３ＭＰａのガス圧及び４０ｍ３／ｍ２・ｈの透過流速で、孔径が４．８μｍの乳化膜を通して乳化した。得られた乳化組成物の大豆の平均粒子径は４．５μｍであった。Example 1
According to the example shown in FIG. 1, an oil-in-water emulsion composition of 30% by weight soybean oil was produced.
30 parts by weight of soybean oil was added to 100 parts by weight of water containing 0.2 part by weight of SDS (sodium dodecyl sulfate) and mixed by stirring to prepare a pre-emulsified composition having an average particle diameter of soybean oil particles of 107 μm. did. The pre-emulsified composition was emulsified through an emulsified membrane having a pore size of 4.8 μm at a gauge pressure of 0.3 MPa and a gas flow rate of 40 m 3 / m 2 · h. The average particle size of soybean in the obtained emulsified composition was 4.5 μm.

図１に示す実施例により、大豆油３０重量％の水中油型の乳化組成物を製造した。
３０重量部の大豆油を、０．２重量部のＴｗｅｅｎ２０（）を含む１００重量部の水に加えて撹拌混合し、大豆油粒子の平均粒子径が１７１μｍの予備乳化組成物を調製した。この予備乳化組成物を、ゲージ圧で３ＭＰａのガス圧及び５０ｍ３／ｍ２・ｈの透過流速で、孔径が２．５６μｍの乳化膜を通して乳化した。得られた乳化組成物の大豆の平均粒子径は０．６７μｍであった。According to the example shown in FIG. 1, an oil-in-water emulsion composition of 30% by weight soybean oil was produced.
30 parts by weight of soybean oil was added to 100 parts by weight of water containing 0.2 parts by weight of Tween 20 () and mixed by stirring to prepare a pre-emulsified composition having an average particle diameter of soybean oil particles of 171 μm. This pre-emulsified composition was emulsified through an emulsified membrane having a pore size of 2.56 μm at a gas pressure of 3 MPa as a gauge pressure and a permeation flow rate of 50 m 3 / m 2 · h. The average particle size of soybean in the obtained emulsified composition was 0.67 μm.

例３
図３に示す実施例により、大豆油３０重量％の水中油型の乳化組成物を製造した。
３０重量部の大豆油を、０．２重量部のＳＤＳを含む１００重量部の水に加えて、ポンプ撹拌により混合し、大豆油粒子の平均粒子径が１７４μｍの予備乳化組成物を調製した。この予備乳化組成物を、７ＭＰａのポンプ圧及び、２８ｍ３／ｍ２・ｈの透過流速で、孔径が０．７２μｍの乳化膜を通して乳化した。得られた乳化組成物の大豆の平均粒子径は０．６９μｍであった。Example 3
According to the example shown in FIG. 3, an oil-in-water emulsion composition of 30% by weight of soybean oil was produced.
30 parts by weight of soybean oil was added to 100 parts by weight of water containing 0.2 part by weight of SDS and mixed by pump stirring to prepare a pre-emulsified composition having an average particle diameter of soybean oil particles of 174 μm. The pre-emulsified composition was emulsified through an emulsified membrane having a pore diameter of 0.72 μm at a pump pressure of 7 MPa and a permeation flow rate of 28 m 3 / m 2 · h. The average particle size of soybean in the obtained emulsified composition was 0.69 μm.

例４
図３に示す実施例により、大豆油３０重量％の水中油型の乳化組成物を製造した。
３０重量部の大豆油を、０．２重量部のＳＤＳを含む１００重量部の水に加えて、ポンプ撹拌により混合し、大豆油粒子の平均粒子径が１７４．４μｍの予備乳化組成物を調製した。この予備乳化組成物を、７ＭＰａのポンプ圧及び、２８ｍ３／ｍ２・ｈの透過流速で、孔径が０．７２４μｍの乳化膜を通して乳化した。得られた乳化組成物をポンプに吸引して、前記乳化膜により再度乳化し、以下、これを繰り返して乳化した。１分４０秒を経過した時の乳化組成物の大豆の平均粒子径は０．７４６μｍであり、２分４０秒を経過した時の乳化組成物の大豆の平均粒子径は０．７０６μｍとなり、４分４０秒を経過した時の乳化組成物の大豆の平均粒子径は０．６９７μｍとなり、大豆油の粒子径の微細な乳化組成物が得られた。Example 4
According to the example shown in FIG. 3, an oil-in-water emulsion composition of 30% by weight of soybean oil was produced.
30 parts by weight of soybean oil is added to 100 parts by weight of water containing 0.2 parts by weight of SDS and mixed by pump stirring to prepare a pre-emulsified composition having an average particle diameter of soybean oil particles of 174.4 μm. did. The pre-emulsified composition was emulsified through an emulsified membrane having a pore size of 0.724 μm at a pump pressure of 7 MPa and a permeation flow rate of 28 m 3 / m 2 · h. The obtained emulsified composition was sucked into a pump and emulsified again with the emulsified membrane, and thereafter this was repeated to emulsify. The average particle diameter of soybean in the emulsified composition when 1 minute and 40 seconds have elapsed is 0.746 μm, and the average particle diameter of soybean in the emulsion composition when 2 minutes and 40 seconds have elapsed is 0.706 μm. The average particle size of soybean in the emulsified composition after a lapse of 40 minutes was 0.697 μm, and a fine emulsion composition having a soybean oil particle size was obtained.

例５
図３に示す実施例により、大豆油３０重量％の水中油型の乳化組成物を製造した。
３０重量部の大豆油を、０．２重量部のＳＤＳを含む１００重量部の水に加えて、ポンプ撹拌により混合し、大豆油粒子の平均粒子径が１９７．２μｍの予備乳化組成物を調製した。この予備乳化組成物を、７ＭＰａのポンプ圧及び、２８ｍ３／ｍ２・ｈの透過流速で、孔径が０．７２４μｍの乳化膜を通して乳化した。得られた乳化組成物をポンプに吸引して、前記乳化膜により再度乳化し、以下、これを繰り返して乳化した。１分４０秒を経過した時の乳化組成物の大豆の平均粒子径は０．７０４μｍであり、３分を経過した時の乳化組成物の大豆の平均粒子径は０．６９５μｍとなり、７分を経過した時の乳化組成物の大豆の平均粒子径は０．６８９μｍとなり、大豆油の粒子径の微細な乳化組成物が得られた。Example 5
According to the example shown in FIG. 3, an oil-in-water emulsion composition of 30% by weight of soybean oil was produced.
30 parts by weight of soybean oil is added to 100 parts by weight of water containing 0.2 parts by weight of SDS and mixed by pump stirring to prepare a pre-emulsified composition having an average particle diameter of soybean oil particles of 197.2 μm. did. The pre-emulsified composition was emulsified through an emulsified membrane having a pore size of 0.724 μm at a pump pressure of 7 MPa and a permeation flow rate of 28 m 3 / m 2 · h. The obtained emulsified composition was sucked into a pump and emulsified again with the emulsified membrane, and thereafter this was repeated to emulsify. The average particle diameter of soybean in the emulsified composition after 1 minute and 40 seconds is 0.704 μm, and the average particle diameter of soybean in the emulsion composition after 3 minutes is 0.695 μm and 7 minutes When the elapsed time, the average particle size of soybean in the emulsified composition was 0.689 μm, and a finely emulsified composition having a particle size of soybean oil was obtained.

互いに溶解しない二種の液体の予備乳化組成物を、乳化剤を用いて予め製造し、この製造された予備乳化組成物を均一な孔径を有する多孔質膜を通過させて再乳化させることにより乳化組成物を製造する乳化組成物の製造方法において、予備乳化組成物を分散させながら圧力を加えて、乳化組成物に接している多孔質膜を通して乳化組成物液中に乳化させるにことにより乳化組成物を製造するので、目的の乳化組成物を短時間で製造することができ、時間当たりの乳化処理量を大きくでき、装置として、処理能力が装置をコンパクトにすることができる。  Two kinds of liquid pre-emulsified compositions that do not dissolve each other are prepared in advance using an emulsifier, and the prepared pre-emulsified composition is passed through a porous membrane having a uniform pore size and re-emulsified. In the method for producing an emulsified composition, a pressure is applied while dispersing the pre-emulsified composition, and the emulsified composition is emulsified in the emulsified composition liquid through the porous membrane in contact with the emulsified composition. Therefore, the target emulsified composition can be produced in a short time, the amount of emulsification treatment per hour can be increased, and the apparatus can be made compact in terms of processing capacity.

本発明の乳化装置の一実施例について、その構造の概略を示す断面図である。  It is sectional drawing which shows the outline of the structure about one Example of the emulsification apparatus of this invention. 本発明の乳化装置の別の一実施例について、その構造の概略を示す二部断面図である。  It is a two-part sectional view showing the outline of the structure about another example of the emulsification device of the present invention. 本発明の乳化方法の一実施例について、その概略を示すフロー図である。  It is a flowchart which shows the outline about one Example of the emulsification method of this invention. 図１及び図２に示す本発明の乳化装置の実施例と、マグネチックスターラ２６の配置位置が相違する本発明の一実施例について、その構造の概略を示す部分断面図である。  It is a fragmentary sectional view which shows the outline of the structure about the Example of the emulsification apparatus of this invention shown in FIG.1 and FIG.2, and one Example of this invention from which the arrangement position of the magnetic stirrer 26 differs. 図１、２及び図４に示す本発明の乳化装置の実施例と平膜状の乳化膜部材を設けた点で相違するについて、その構造の概略を示す一部断面図である。  FIG. 5 is a partial cross-sectional view showing an outline of the structure of the emulsifying apparatus of the present invention shown in FIGS. 図３に示す実施例とは異なる本発明の乳化方法の一実施例について、その概略を示すフロー図である。  It is a flowchart which shows the outline about one Example of the emulsification method of this invention different from the Example shown in FIG.

符号の説明Explanation of symbols

１ 乳化槽
２ 乳化槽１の天井部
２０１ 天井板部
３ 乳化槽１の側壁部
４ 乳化槽１の底部
４０１ 底板部
５ 管状の乳化膜
６ 管状の乳化膜５の上部開口部
７ 管状の乳化膜５の下部開口部
８、２８、３９、４４ 管状の乳化膜５の挿通用の孔
９、２９ 環状部
１０、３０、４２ ネジ部
１１、３１、４３ ナット
１２、３２ 内側ネジ部
１３ 環状部９の内側面
１４、３４、４０及び４５ 環状弾性密封部材
１５、３５ 筒形部
１６、３６ 押圧部材
１７、３７ フランジ部
１８ ナット１１の上端開口部
１９ 縁部
２０ 加圧気体の導入管部
２１ 分散相液体導入管接続口
２２ 分散相液体導入管接続口
２３ 中空の軸受け部
２４ 撹拌羽根
２５ 撹拌軸
２６ マグネチックスターラ
２７ 攪拌乳化空間
３３ 環状部２９の内側面
３８ ナット３１の下端開口部
１９、３９′ 縁部
４０′ 乳化組成物取出し室
４１′ 乳化組成物取出し管
４７ 乳化組成物の上部取出し室
４８ 乳化組成物の下部取出し室
４９ 乳化組成物の上部取出し管
５０ 乳化組成物の下部取出し管DESCRIPTION OF SYMBOLS 1 Emulsification tank 2 Ceiling part 201 of the emulsification tank 1 Ceiling plate part 3 Side wall part of the emulsification tank 1 4 Bottom part 401 of the emulsification tank 1 Bottom plate part 5 Tubular emulsification film 6 Upper opening part of the tubular emulsification film 5 7 Tubular emulsification film 5, lower opening portion 8, 28, 39, 44 Tubular emulsification membrane 5 insertion hole 9, 29 annular portion 10, 30, 42 screw portion 11, 31, 43 nut 12, 32 inner screw portion 13 annular portion 9 Inner side surfaces 14, 34, 40 and 45 Annular elastic sealing members 15, 35 Cylindrical parts 16, 36 Press members 17, 37 Flange part 18 Upper end opening part 19 of nut 11 Edge part 20 Introducing pipe part 21 of pressurized gas Dispersion Phase liquid introduction pipe connection port 22 Dispersed phase liquid introduction pipe connection port 23 Hollow bearing portion 24 Stirrer blade 25 Stir shaft 26 Magnetic stirrer 27 Stir emulsification space 33 Inner side surface 38 of annular portion 29 Lower end openings 19 and 39 of nut 31 Lower extraction pipe edge 40 'emulsion composition unloading chamber 41' upper takeout tube 50 emulsified composition of the lower extraction chamber 49 emulsified composition of the upper unloading chamber 48 emulsified composition of the emulsion composition takeout tube 47 emulsion composition

Claims (25)

互いに溶解しない二種の液体の予備乳化組成物を、乳化剤を用いて予め製造し、この製造された予備乳化組成物を均一な孔径を有する多孔質膜を通過させて再乳化させることにより乳化組成物を製造する乳化組成物の製造方法において、予備乳化組成物を分散させながら圧力を加えて、多孔質膜を通して乳化させることにより、乳化組成物を製造することを特徴とする乳化組成物の製造方法。  Two kinds of liquid pre-emulsified compositions that do not dissolve each other are prepared in advance using an emulsifier, and the prepared pre-emulsified composition is passed through a porous membrane having a uniform pore size and re-emulsified. In the manufacturing method of an emulsified composition for manufacturing a product, an emulsified composition is manufactured by applying pressure while dispersing the pre-emulsified composition and emulsifying through a porous membrane. Method. 互いに溶解しない二種の液体の予備乳化組成物を、乳化剤を用いて予め製造し、この製造された予備乳化組成物を均一な孔径を有する多孔質膜を通過させて再乳化させることにより乳化組成物を製造する乳化組成物の製造方法において、予備乳化組成物中の分散相をさらに分散させながら０．１ＭＰａ以上の圧力を加えて、多孔質膜を通して乳化させることにより、前記多孔質膜の孔径より小さい平均粒子径を有する乳化組成物を製造することを特徴とする乳化組成物の製造方法。  Two kinds of liquid pre-emulsified compositions that do not dissolve each other are prepared in advance using an emulsifier, and the prepared pre-emulsified composition is passed through a porous membrane having a uniform pore size and re-emulsified. In the method for producing an emulsified composition for producing a product, the pore size of the porous membrane is obtained by emulsifying the porous membrane by applying a pressure of 0.1 MPa or more while further dispersing the dispersed phase in the pre-emulsified composition. A method for producing an emulsion composition, comprising producing an emulsion composition having a smaller average particle size. 互いに溶解しない二種の液体の予備乳化組成物を、乳化剤を用いて予め製造し、この製造された予備乳化組成物を均一な孔径を有する多孔質膜を通過させて再乳化させることにより乳化組成物を製造する乳化組成物の製造方法において、予備乳化組成物中の分散相をさらに分散させながら０．１ＭＰａ以上の圧力を加えて、多孔質膜を通して乳化させることにより得られた乳化組成物を、さらに分散させながら圧力を加えて、前記通過した多孔質膜を再度通過させて乳化させることにより、前記多孔質膜の孔径より小さい平均粒子径を有する乳化組成物を製造することを特徴とする請求項１又は２に記載の乳化組成物の製造方法。  Two kinds of liquid pre-emulsified compositions that do not dissolve each other are prepared in advance using an emulsifier, and the prepared pre-emulsified composition is passed through a porous membrane having a uniform pore size and re-emulsified. In the method for producing an emulsified composition for producing a product, an emulsified composition obtained by emulsifying through a porous membrane by applying a pressure of 0.1 MPa or more while further dispersing the dispersed phase in the pre-emulsified composition The emulsified composition having an average particle size smaller than the pore size of the porous membrane is produced by applying pressure while further dispersing and passing the porous membrane again through the emulsification. The manufacturing method of the emulsion composition of Claim 1 or 2. 互いに溶解しない二種の液体の予備乳化組成物を、乳化剤を用いて予め製造し、この製造された予備乳化組成物を均一な孔径を有する多孔質膜を通過させて再乳化させることにより乳化組成物を製造する乳化組成物の製造方法において、予備乳化組成物を、０．１ＭＰａ以上の圧力を加えて、第一の多孔質膜を通して乳化させて、第一の乳化組成物を製造し、この製造された第一の乳化組成物を、第一の多孔質膜より孔径が小さい第二の多孔質膜に通して乳化させることを特徴とする乳化組成物の製造方法。  Two kinds of liquid pre-emulsified compositions that do not dissolve each other are prepared in advance using an emulsifier, and the prepared pre-emulsified composition is passed through a porous membrane having a uniform pore size and re-emulsified. In the method for producing an emulsified composition for producing a product, a pre-emulsified composition is emulsified through a first porous membrane by applying a pressure of 0.1 MPa or more to produce a first emulsified composition, A method for producing an emulsified composition, comprising emulsifying the produced first emulsified composition through a second porous membrane having a pore size smaller than that of the first porous membrane. 圧力が、ガスによる圧力又はポンプによる圧力であることを特徴とする請求項１乃至４の何れか一項に記載の乳化組成物の製造方法。  The method for producing an emulsified composition according to any one of claims 1 to 4, wherein the pressure is a gas pressure or a pump pressure. 多孔質膜の平均孔径が０．１μｍ以下であることを特徴とする請求項１乃至３の何れか一項に記載の乳化組成物の製造方法。  The method for producing an emulsified composition according to any one of claims 1 to 3, wherein an average pore size of the porous membrane is 0.1 µm or less. 第二の多孔質膜の平均孔径が０．１μｍ以下であることを特徴とする請求項４に記載の乳化組成物の製造方法。  The method for producing an emulsified composition according to claim 4, wherein the average pore size of the second porous membrane is 0.1 µm or less. 天井壁部、側壁部及び底壁部により囲まれて形成される乳化容器と、該乳化容器の内部を仕切る多孔質膜と、多孔質膜で仕切られた一方の側に圧力源に接続する圧力導入口を設けて形成されている予備乳化組成物形成室と、乳化膜で仕切られた他方の側に形成されている乳化組成物室とを備えることを特徴とする乳化装置。  An emulsification container formed by being surrounded by a ceiling wall part, a side wall part and a bottom wall part, a porous film partitioning the inside of the emulsification container, and a pressure connected to a pressure source on one side partitioned by the porous film An emulsifying apparatus comprising: a pre-emulsified composition forming chamber formed with an introduction port; and an emulsified composition chamber formed on the other side partitioned by an emulsifying film. 天井壁部、側壁部及び底壁部により囲まれて形成される乳化容器と、該乳化容器の内部を仕切る多孔質膜と、多孔質膜で仕切られた一方の側に圧力源に接続する圧力導入口及び予備乳化組成物導入口を設けて形成されている予備乳化組成物形成室と、乳化膜で仕切られた他方の側に乳化組成物取出し口を備えて形成されている乳化組成物室とを備えることを特徴とする乳化装置。  An emulsification container formed by being surrounded by a ceiling wall part, a side wall part and a bottom wall part, a porous film partitioning the inside of the emulsification container, and a pressure connected to a pressure source on one side partitioned by the porous film A pre-emulsified composition forming chamber formed by providing an inlet and a pre-emulsified composition inlet, and an emulsified composition chamber formed by providing an emulsified composition outlet on the other side partitioned by the emulsion film And an emulsifying device. 天井壁部、側壁部及び底壁部により囲まれて形成される乳化容器と、該乳化容器の内部を仕切る多孔質膜と、前記多孔質膜で仕切られた一方の側に、分散相液体導入口、連続相液体導入口、加圧用気体導入口及び撹拌具を設けて形成されている予備乳化組成物形成室と、多孔質膜で仕切られた他方の側に乳化組成物取出し口を設けて形成されている乳化組成物室とを備えることを特徴とする乳化装置。  An emulsification container formed by being surrounded by a ceiling wall part, a side wall part and a bottom wall part, a porous film partitioning the inside of the emulsification container, and a dispersed phase liquid introduction on one side partitioned by the porous film A pre-emulsified composition forming chamber formed by providing a mouth, a continuous-phase liquid inlet, a pressurizing gas inlet and a stirrer, and an emulsified composition outlet on the other side partitioned by the porous membrane An emulsification apparatus comprising: an emulsified composition chamber formed. 天井壁部、側壁部及び底壁部により囲まれて形成される乳化容器と、該乳化容器の内部を仕切る多孔質膜と、前記多孔質膜で仕切られた一方の側に、予備乳化組成物導入口を設けて形成されている予備乳化組成物形成室と、前記多孔質膜で仕切られた他方の側に乳化組成物取出し口を設けて形成されている乳化組成物室とを備えることを特徴とする乳化装置。  An emulsification container formed by being surrounded by a ceiling wall part, a side wall part and a bottom wall part, a porous film partitioning the inside of the emulsification container, and a pre-emulsification composition on one side partitioned by the porous film A pre-emulsified composition forming chamber formed by providing an inlet, and an emulsified composition chamber formed by providing an emulsified composition outlet on the other side partitioned by the porous membrane. A characteristic emulsification apparatus. 天井壁部、側壁部及び底壁部により囲まれている乳化容器と、該乳化容器の底部下方に設けられている乳化組成物室と、夫々、前記乳化容器の内部を、上端開口部が大気に連通し、下端開口部が乳化組成物取出し室内に突き出して設けられている一以上の中空筒形多孔質膜と、前記多孔質膜の周囲に設けられている撹拌具と、前記乳化容器の天井壁又は側壁に形成されている連続相液体導入口、分散相液体導入口及び加圧流体導入口とを備えていることを特徴とする乳化装置。  The emulsification container surrounded by the ceiling wall part, the side wall part and the bottom wall part, the emulsification composition chamber provided below the bottom part of the emulsification container, and the interior of the emulsification container, respectively, the upper end opening being the atmosphere One or more hollow cylindrical porous membranes provided with a lower end opening protruding into the emulsion composition take-out chamber, an agitator provided around the porous membrane, and the emulsification container An emulsifying apparatus comprising a continuous phase liquid inlet, a dispersed phase liquid inlet, and a pressurized fluid inlet formed on a ceiling wall or a side wall. 天井壁部、側壁部及び底壁部により囲まれている乳化容器と、該乳化容器の底部下方に設けられている乳化組成物取出し室と、夫々、前記乳化容器の内部を、上端開口部が大気に連通し、下端開口部が乳化組成物取出し室内に突き出して設けられている一以上の中空筒形多孔質膜と、前記乳化容器の天井壁又は側壁に形成されている予備乳化組成物導入口と、該予備乳化組成物導入口に送液ポンプを有する予備乳化組成物供給管とを備えていることを特徴とする乳化装置。  An emulsification container surrounded by a ceiling wall part, a side wall part, and a bottom wall part, an emulsified composition take-out chamber provided below the bottom part of the emulsification container, and an upper end opening respectively inside the emulsification container One or more hollow cylindrical porous membranes communicating with the atmosphere and having a lower end opening projecting into the emulsified composition take-out chamber, and a pre-emulsified composition introduced on the ceiling wall or side wall of the emulsification container An emulsifying apparatus comprising a mouth and a pre-emulsified composition supply pipe having a liquid feed pump at the pre-emulsified composition introduction port. 天井壁部、側壁部及び底壁部により囲まれている乳化容器と、該乳化容器の底部下方に設けられている乳化組成物取出し室と、夫々、前記乳化容器の内部を、上端開口部が大気に連通し、下端開口部が乳化組成物取出し室内に突き出して設けられている一以上の中空筒形多孔質膜と、前記乳化容器の天井壁又は側壁に形成されている予備乳化組成物導入口と、該予備乳化組成物導入口に送液ポンプを有する予備乳化組成物供給管とを備えている乳化容器を複数設け、第一の乳化容器の乳化組成物取出し室が、第二の乳化容器の予備乳化組成物導入口に接続していることを特徴とする乳化装置。  An emulsification container surrounded by a ceiling wall part, a side wall part, and a bottom wall part, an emulsified composition take-out chamber provided below the bottom part of the emulsification container, and an upper end opening respectively inside the emulsification container One or more hollow cylindrical porous membranes communicating with the atmosphere and having a lower end opening projecting into the emulsified composition take-out chamber, and a pre-emulsified composition introduced on the ceiling wall or side wall of the emulsification container A plurality of emulsification containers having a mouth and a pre-emulsification composition supply pipe having a liquid feed pump at the preliminary emulsification composition introduction port are provided, and the emulsification composition take-out chamber of the first emulsification container is a second emulsification An emulsifying apparatus connected to a preliminary emulsified composition inlet of a container. 天井壁部、側壁部及び底壁部により囲まれている乳化容器と、乳化容器内を仕切って設けられている平膜状の多孔質膜と、該多孔質膜により仕切られた一方の室は予備乳化組成物形成室であり、多孔質膜により仕切られた他方の室は乳化組成物室であり、前記予備乳化組成物形成室には、予備乳化組成物導入口が設けられ、予備乳化組成物導入口には、送液ポンプを有する予備乳化組成物供給管が接続しており、乳化組成物室には乳化組成物取出し口が設けられていることを特徴とする乳化装置。  The emulsification container surrounded by the ceiling wall part, the side wall part and the bottom wall part, the flat membrane-like porous film provided by partitioning the inside of the emulsification container, and one chamber partitioned by the porous film are The pre-emulsified composition forming chamber, the other chamber partitioned by the porous membrane is an emulsified composition chamber, the pre-emulsified composition forming chamber is provided with a pre-emulsified composition inlet, and the pre-emulsified composition A pre-emulsified composition supply pipe having a liquid feed pump is connected to the product introduction port, and an emulsified composition take-out port is provided in the emulsion composition chamber. 天井壁部、側壁部及び底壁部により囲まれている乳化容器と、該乳化容器内を仕切って設けられている平膜状の多孔質膜と、該多孔質膜により仕切られた一方の室は予備乳化組成物形成室であり、多孔質膜により仕切られた他方の室は乳化組成物室であり、前記予備乳化組成物形成室には、予備乳化組成物導入口が設けられ、予備乳化組成物導入口には、送液ポンプを有する予備乳化組成物供給管が接続しており、乳化組成物室には乳化組成物取出し口が設けられており、該いることを特徴とする乳化装置。  An emulsification container surrounded by a ceiling wall part, a side wall part and a bottom wall part, a flat membrane-like porous film provided by partitioning the inside of the emulsification container, and one chamber partitioned by the porous film Is a pre-emulsified composition forming chamber, the other chamber partitioned by the porous membrane is an emulsified composition chamber, and the pre-emulsified composition forming chamber is provided with a pre-emulsified composition inlet, and pre-emulsified A pre-emulsified composition supply pipe having a liquid feed pump is connected to the composition introduction port, and an emulsified composition take-out port is provided in the emulsified composition chamber. . 天井壁部、側壁部及び底壁部により囲まれている乳化容器と、乳化容器内を仕切って設けられている平膜状の多孔質膜ど多孔質膜により仕切られた一方の室は予備乳化組成物形成室であり、多孔質膜により仕切られた他方の室は乳化組成物室であり、前記予備乳化組成物形成室には、予備乳化組成物導入口が設けられ、予備乳化組成物導入口には、送液ポンプを有する予備乳化組成物供給管が接続しており、乳化組成物室には乳化組成物取出し口が設けられている乳化容器が複数設けられており、第一の乳化容器の乳化組成物取出し口は、第二の乳化容器の予備乳化組成物導入口に接続していることを特徴とする乳化装置。  The emulsification container surrounded by the ceiling wall part, the side wall part, and the bottom wall part, and one chamber partitioned by a porous membrane such as a flat membrane-like porous film provided by partitioning the emulsification container is preliminarily emulsified The other chamber partitioned by the porous membrane is an emulsified composition chamber. The preliminary emulsified composition forming chamber is provided with a preliminary emulsified composition inlet, and the preliminary emulsified composition is introduced. A pre-emulsified composition supply pipe having a liquid feed pump is connected to the mouth, and the emulsified composition chamber is provided with a plurality of emulsification containers provided with an emulsified composition take-out port. An emulsifying device, wherein the emulsified composition outlet of the container is connected to the preliminary emulsified composition inlet of the second emulsified container. 天井壁部、側壁部及び底壁部により囲まれている乳化容器と、乳化容器内を仕切って設けられている平膜状の多孔質膜と、多孔質膜により仕切られた一方の室は予備乳化組成物形成室であり、多孔質膜により仕切られた他方の室は乳化組成物室であり、前記予備乳化組成物形成室には、予備乳化組成物導入口が設けられ、予備乳化組成物導入口には、送液ポンプを有する予備乳化組成物供給管が接続しており、乳化組成物室には乳化組成物取出し口が設けられている乳化容器が複数設けられており、第一の乳化容器の乳化組成物取出し口は、送液ポンプを介して第二の乳化容器の予備乳化組成物導入口に接続していることを特徴とする乳化装置。  The emulsification container surrounded by the ceiling wall part, the side wall part and the bottom wall part, the flat membrane-like porous film provided by partitioning the inside of the emulsification container, and one chamber partitioned by the porous film are spare The emulsified composition forming chamber, the other chamber partitioned by the porous membrane is an emulsified composition chamber, and the preliminary emulsified composition forming chamber is provided with a preliminary emulsified composition inlet, and the preliminary emulsified composition A pre-emulsified composition supply pipe having a liquid feed pump is connected to the introduction port, and a plurality of emulsification containers provided with an emulsified composition take-out port are provided in the emulsion composition chamber. An emulsification apparatus, wherein the emulsified composition take-out port of the emulsification container is connected to the preliminary emulsified composition introduction port of the second emulsification container via a liquid feed pump. 天井壁部、側壁部及び底壁部により囲まれている乳化容器と、乳化容器内を仕切って設けられている平膜状の多孔質膜と、多孔質膜により仕切られた一方の室は予備乳化組成物形成室であり、多孔質膜により仕切られた他方の室は乳化組成物室であり、前記予備乳化組成物形成室には、予備乳化組成物導入口が設けられ、予備乳化組成物導入口には、送液ポンプを有する予備乳化組成物供給管が接続しており、乳化組成物室には乳化組成物取出し口が設けられており、該乳化組成物取出し口は、前記送液ポンプの吸い込み側に接続していることを特徴とする乳化装置。  The emulsification container surrounded by the ceiling wall part, the side wall part and the bottom wall part, the flat membrane-like porous film provided by partitioning the inside of the emulsification container, and one chamber partitioned by the porous film are spare The emulsified composition forming chamber, the other chamber partitioned by the porous membrane is an emulsified composition chamber, and the preliminary emulsified composition forming chamber is provided with a preliminary emulsified composition inlet, and the preliminary emulsified composition A pre-emulsified composition supply pipe having a liquid feed pump is connected to the introduction port, and an emulsion composition take-out port is provided in the emulsion composition chamber. An emulsifying device connected to the suction side of the pump. 第一の乳化容器の平膜状の多孔質膜の孔径が第二の乳化容器の平膜状の多孔質膜の孔径より大きいことを特徴とする請求項１６又は１７に記載の乳化装置。  The emulsification apparatus according to claim 16 or 17, wherein the pore diameter of the flat membrane-like porous membrane of the first emulsification container is larger than the pore diameter of the flat membrane-like porous membrane of the second emulsification container. 撹拌具は、前記多孔質膜部材中心に回転可能に設けられている撹拌羽根であることを特徴とする請求項１０乃至又は１９の何れか一項に記載の乳化装置。  The emulsifying apparatus according to any one of claims 10 to 19, wherein the stirring tool is a stirring blade rotatably provided at the center of the porous membrane member. 撹拌具は、乳化容器内に乳化容器の側壁部に回転可能に設けられていることを特徴とする請求項１０乃至又は１９の何れか一項に記載の乳化装置。  The emulsifying apparatus according to any one of claims 10 to 19, wherein the stirrer is rotatably provided in a side wall portion of the emulsification container in the emulsification container. 平形多孔質膜が、多孔板により支持されて、夫々の周辺部が、収容容器の蓋体部及び本体部間に、弾性リング部材により密着支持されていることを特徴とする請求項請求項１５０乃至又は１９の何れか一項に記載の乳化装置。  150. The flat porous membrane is supported by a perforated plate, and each peripheral portion is closely supported by an elastic ring member between a lid portion and a main body portion of the container. The emulsification apparatus as described in any one of thru | or 19. 中空筒形多孔質膜は、夫々の両端部が、弾性リング部材により支持されており、該弾性リング部材は、袋ナットの雌ネジ部と螺合する雄ねじ部材の前記乳化容器壁に設けられる予備乳化組成物導入口及び加圧流体導入口とを備えており、前記乳化容器の予備乳化組成物導入口は、槽内に攪拌装置を備えて、連続相液体導入口及び分散相液体導入口を備える予備乳化容器にポンプを介して接続していることを特徴とする乳化装置。  Both ends of the hollow cylindrical porous membrane are supported by an elastic ring member, and the elastic ring member is a spare provided on the emulsification container wall of the male screw member screwed with the female screw portion of the cap nut. An emulsified composition inlet and a pressurized fluid inlet, and the preliminary emulsified composition inlet of the emulsification container includes a stirrer in the tank, and a continuous phase liquid inlet and a dispersed phase liquid inlet. An emulsification apparatus, wherein the emulsification apparatus is connected to a pre-emulsification container with a pump. 中空筒形多孔質膜は、夫々の両端部が、収容容器の天井壁部及び底壁部の孔内に、弾性リング部材により密着支持されていることを特徴とする請求項１２乃至１４及び請求項２５の何れか一項に記載の乳化装置。  The hollow cylindrical porous membrane is characterized in that both end portions thereof are closely supported by elastic ring members in the holes of the ceiling wall portion and the bottom wall portion of the container. Item 26. The emulsifier according to any one of Items 25.
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JP5801974B1 (en) * 2015-02-12 2015-10-28 株式会社Ｎｅｘｔコロイド分散凝集技術研究所 Multilayer emulsion manufacturing method and capsule manufacturing method
CN108854153A (en) * 2018-08-01 2018-11-23 中国科学技术大学 Film emulsification and extraction device and film emulsification and extraction method
WO2021171701A1 (en) * 2020-02-27 2021-09-02 日東電工株式会社 Method and apparatus for producing emulsion
JP7450146B2 (en) 2019-10-16 2024-03-15 エス・ピー・ジーテクノ株式会社 Disc-shaped porous membrane holder

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JP2009297612A (en) * 2008-06-11 2009-12-24 Spg Techno Kk Porous film emulsifying apparatus
GB2469087A (en) * 2009-04-02 2010-10-06 Ct Angewandte Nanotech Can Preparation of colloidal dispersion
WO2010112379A1 (en) 2009-04-02 2010-10-07 Centrum Für Angewandte Nanotechnologie (Can) Gmbh Method and apparatus for the manufacture of a colloidal dispersion using controlled micro-channel flow
CN103007793A (en) * 2011-09-20 2013-04-03 中国科学院过程工程研究所 Multi-stage temperature control type membrane emulsifier
CN103007793B (en) * 2011-09-20 2014-12-24 中国科学院过程工程研究所 Multi-stage temperature control type membrane emulsifier
JP2012176401A (en) * 2012-02-21 2012-09-13 Sumitomo Chemical Co Ltd Cylindrical container
JP5801974B1 (en) * 2015-02-12 2015-10-28 株式会社Ｎｅｘｔコロイド分散凝集技術研究所 Multilayer emulsion manufacturing method and capsule manufacturing method
JP2016147233A (en) * 2015-02-12 2016-08-18 株式会社Ｎｅｘｔコロイド分散凝集技術研究所 Manufacturing method of multilayer emulsion and manufacturing method of capsule
CN108854153A (en) * 2018-08-01 2018-11-23 中国科学技术大学 Film emulsification and extraction device and film emulsification and extraction method
JP7450146B2 (en) 2019-10-16 2024-03-15 エス・ピー・ジーテクノ株式会社 Disc-shaped porous membrane holder
WO2021171701A1 (en) * 2020-02-27 2021-09-02 日東電工株式会社 Method and apparatus for producing emulsion
JP2021133300A (en) * 2020-02-27 2021-09-13 日東電工株式会社 Method and apparatus for manufacturing emulsion
CN115175756A (en) * 2020-02-27 2022-10-11 日东电工株式会社 Method and apparatus for producing emulsion

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