JP2021008970A - Freeze dry nozzle, freeze dry device, and granulation method - Google Patents
Freeze dry nozzle, freeze dry device, and granulation method Download PDFInfo
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Abstract
Description
本発明は、凍結乾燥用ノズル、凍結乾燥装置、および、造粒方法に関する。 The present invention relates to a freeze-drying nozzle, a freeze-drying device, and a granulation method.
噴射式の凍結乾燥装置は、真空室内において、凍結乾燥用ノズルから下方に向けて原料液を噴射する。噴射される原料液は、例えば、医薬品、食品、化粧品などの原料を溶媒や分散媒のなかに含む。噴射された原料液は、凍結乾燥用ノズルの下方で、液柱から粒子に変わる。粒子中の原料は、溶媒や分散媒に蒸発潜熱を奪われて自己凍結する(例えば、特許文献1を参照)。 The injection-type freeze-drying device injects the raw material liquid downward from the freeze-drying nozzle in a vacuum chamber. The injected raw material liquid contains, for example, raw materials such as pharmaceuticals, foods, and cosmetics in a solvent or a dispersion medium. The injected raw material liquid changes from a liquid column to particles below the freeze-drying nozzle. The raw material in the particles is deprived of latent heat of vaporization by a solvent or a dispersion medium and self-freezes (see, for example, Patent Document 1).
ところで、噴射された原料液の一部は、液柱として成長せずに、噴射口の周囲に向けて飛散する。飛散した原料液は、噴射口の周囲に付着して瞬時に自己凍結する。噴射口の周囲に一旦付着した凍結乾燥物は、それに他の凍結乾燥物が堆積することを促してしまう。結果として、原料液の進行する方向が堆積物によって曲げられたり、噴射口そのものが塞がれたりする。特に、高分子化合物を含むような高い粘度を有した原料液では、噴射された原料液の一部が噴射口の周囲に向けて飛散しやすいため、上述した課題が深刻なものとなっている。 By the way, a part of the injected raw material liquid does not grow as a liquid column but scatters toward the periphery of the injection port. The scattered raw material liquid adheres to the periphery of the injection port and instantly self-freezes. Once the freeze-dried material adheres to the periphery of the injection port, it promotes the accumulation of other freeze-dried products on it. As a result, the direction of travel of the raw material liquid is bent by the deposit, or the injection port itself is blocked. In particular, in a raw material liquid having a high viscosity such as containing a polymer compound, a part of the injected raw material liquid tends to scatter toward the periphery of the injection port, so that the above-mentioned problem becomes serious. ..
本発明の目的は、原料液を円滑に噴射可能にした凍結乾燥用ノズル、凍結乾燥装置、および、造粒方法を提供することである。 An object of the present invention is to provide a freeze-drying nozzle, a freeze-drying device, and a granulation method that enable smooth injection of a raw material liquid.
上記課題を解決するための凍結乾燥用ノズルは、真空空間に原料液を噴射させて前記原料液からなる粒を前記真空空間で凍結乾燥させるための凍結乾燥用ノズルであって、ノズル外表面の中で前記原料液の噴射口を含む部分が前記原料液のなかの液体成分を撥液する撥液性を有する。 The freeze-drying nozzle for solving the above problems is a freeze-drying nozzle for injecting a raw material liquid into a vacuum space and freeze-drying particles composed of the raw material liquid in the vacuum space, and is a nozzle on the outer surface of the nozzle. Among them, the portion including the injection port of the raw material liquid has a liquid-repellent property of repelling the liquid component in the raw material liquid.
上記構成によれば、ノズル外表面のなかで噴射口を含む部分は、原料液の付着を撥液性によって抑制し、これにより、原料液の自己凍結物が堆積することを抑制する。結果として、噴射口の周囲で自己凍結物が堆積すること、また、噴射口が自己凍結物で塞がれることが抑制されて、真空空間への原料液の噴射が円滑となる。 According to the above configuration, the portion of the outer surface of the nozzle including the injection port suppresses the adhesion of the raw material liquid by the liquid repellency, thereby suppressing the accumulation of the self-frozen product of the raw material liquid. As a result, the accumulation of self-frozen matter around the injection port and the fact that the injection port is not blocked by the self-freezing material are suppressed, so that the raw material liquid is smoothly injected into the vacuum space.
上記凍結乾燥用ノズルにおいて、前記凍結乾燥用ノズルには、前記噴射口に繋がる前記原料液の流路が形成されており、前記流路の内表面、および、前記ノズル外表面が、前記液体成分を撥液する撥液層によって構成されていてもよい。この構成によれば、流路の内表面が撥液層から構成されるため、噴射口に向けて円滑に原料液を導くことが可能ともなる。 In the freeze-drying nozzle, the freeze-drying nozzle is formed with a flow path of the raw material liquid connected to the injection port, and the inner surface of the flow path and the outer surface of the nozzle are the liquid components. It may be composed of a liquid-repellent layer that repels liquid. According to this configuration, since the inner surface of the flow path is composed of a liquid-repellent layer, it is possible to smoothly guide the raw material liquid toward the injection port.
上記凍結乾燥用ノズルにおいて、前記撥液層は、フッ素樹脂であってもよい。フッ素樹脂は、液体成分との相互作用が極めて小さい材料である。上記構成であれば、撥液層がフッ素樹脂から構成されるため、原料液の付着をより高い精度下で抑制することが可能となる。 In the freeze-drying nozzle, the liquid-repellent layer may be a fluororesin. Fluororesin is a material that has extremely small interaction with liquid components. With the above configuration, since the liquid-repellent layer is made of fluororesin, it is possible to suppress the adhesion of the raw material liquid with higher accuracy.
上記凍結乾燥用ノズルにおいて、前記撥液層は、フッ素樹脂と共析されためっき被膜であってもよい。フッ素樹脂と共析されためっき被膜は、フッ素樹脂よりも高い耐摩耗性を有し、また、一部が摩耗しても撥液性を保つ。上記構成であれば、撥液層がフッ素樹脂と共析されためっき被膜であるため、撥液層による原料液の付着抑制と、撥液層そのものの耐久性の向上とが可能となる。 In the freeze-drying nozzle, the liquid-repellent layer may be a plating film co-deposited with a fluororesin. The plating film co-deposited with the fluororesin has higher wear resistance than the fluororesin, and maintains liquid repellency even if a part of the plating film wears. With the above configuration, since the liquid-repellent layer is a plating film co-deposited with the fluororesin, it is possible to suppress the adhesion of the raw material liquid by the liquid-repellent layer and improve the durability of the liquid-repellent layer itself.
上記凍結乾燥ノズルにおいて、前記流路が、第一流路、第二流路、および、前記第一流路と前記第二流路とを接続する第三流路とを備え、前記第一流路は、前記第三流路に向けて先細る錘台筒面状を有して前記原料液の供給部に接続され、前記第二流路は、前記第三流路に向けて先細る錘台筒面状を有して前記真空空間に向けた開口を有し、前記第三流路は、前記噴射口を含み、前記第一流路と第前記二流路とを繋ぐ筒面状を有してもよい。 In the freeze-drying nozzle, the flow path includes a first flow path, a second flow path, and a third flow path connecting the first flow path and the second flow path, and the first flow path is The weight base cylinder surface that tapers toward the third flow path and is connected to the raw material liquid supply unit, and the second flow path tapers toward the third flow path. The third flow path may have a shape and an opening toward the vacuum space, and the third flow path may have a tubular shape including the injection port and connecting the first flow path and the second flow path. ..
第一流路と第二流路とを繋ぐ第三流路は、第一流路と比べて小さい流路断面積を有する。こうした第三流路は、第一流路よりも原料液の流れを規制して、液柱の太さ、ひいては、粒子の大きさを定める。上記構成によれば、第三流路の上流に位置する第一流路が、第三流路に向けた錘台筒状を有して、第三流路に向けて原料液の流れを徐々に抑える。そのため、オリフィスのような流路を備える構成と比べて、第三流路から噴射される原料液が飛散することを抑えることが可能ともなる。また、真空空間に向けて拡開した形状を第二流路が有するため、第三流路から噴射される原料液の一部が飛散するとしても、噴射口や第二流路に原料液が付着しにくい。 The third flow path connecting the first flow path and the second flow path has a flow path cross-sectional area smaller than that of the first flow path. Such a third flow path regulates the flow of the raw material liquid more than the first flow path, and determines the thickness of the liquid column and, by extension, the size of the particles. According to the above configuration, the first flow path located upstream of the third flow path has a pedestal tubular shape toward the third flow path, and the flow of the raw material liquid gradually flows toward the third flow path. suppress. Therefore, it is possible to suppress the scattering of the raw material liquid injected from the third flow path as compared with the configuration provided with the flow path such as the orifice. Further, since the second flow path has a shape that expands toward the vacuum space, even if a part of the raw material liquid injected from the third flow path scatters, the raw material liquid is discharged to the injection port and the second flow path. Hard to adhere.
上記凍結乾燥用ノズルにおいて、噴射口から飛散した原料液を受けるカバーを備え、前記カバーの外表面が前記液体成分を撥液する撥液層によって構成されていてもよい。この構成によれば、噴射口から飛散した原料液がカバー以外に付着することをカバーが抑制する。加えて、こうしたカバーの外表面が撥液層から構成されているため、カバーにおいても、原料液の付着を抑制することが可能ともなる。 The freeze-drying nozzle may include a cover that receives the raw material liquid scattered from the injection port, and the outer surface of the cover may be composed of a liquid-repellent layer that repels the liquid component. According to this configuration, the cover prevents the raw material liquid scattered from the injection port from adhering to other than the cover. In addition, since the outer surface of the cover is composed of a liquid-repellent layer, it is possible to suppress the adhesion of the raw material liquid even on the cover.
上記課題を解決するための凍結乾燥装置は、真空室と、液体を供給する供給部と、前記供給部が供給する液体を前記真空室へ噴射する上記凍結乾燥用ノズルと、を備える。
上記課題を解決するための造粒方法は、真空空間に原料液を噴射させて前記原料液からなる粒を前記真空空間で凍結乾燥させる造粒方法であって、前記原料液を噴射させる凍結乾燥用ノズルのノズル外表面の中で前記原料液の噴射口を含む部分が前記原料液のなかの液体成分を撥液する撥液性を有する。
The freeze-drying device for solving the above problems includes a vacuum chamber, a supply unit for supplying a liquid, and the freeze-drying nozzle for injecting the liquid supplied by the supply unit into the vacuum chamber.
The granulation method for solving the above problems is a granulation method in which a raw material liquid is sprayed into a vacuum space to freeze-dry the particles composed of the raw material liquid in the vacuum space, and freeze-drying is performed by injecting the raw material liquid. The portion of the outer surface of the nozzle of the nozzle including the injection port of the raw material liquid has a liquid repellent property of repelling the liquid component in the raw material liquid.
上記構成によれば、凍結乾燥用ノズルの噴射口における周囲で自己凍結物が堆積すること、また、噴射口が自己凍結物で塞がれることが抑制されて、真空空間への原料液の噴射が円滑となる。 According to the above configuration, the accumulation of self-frozen material around the injection port of the freeze-drying nozzle and the prevention of the injection port being blocked by the self-freezing material are suppressed, and the raw material liquid is injected into the vacuum space. Becomes smooth.
(第1実施形態)
以下、図1および図2を参照して、凍結乾燥装置、および、凍結乾燥用ノズルの第1実施形態を説明する。
(First Embodiment)
Hereinafter, the first embodiment of the freeze-drying apparatus and the freeze-drying nozzle will be described with reference to FIGS. 1 and 2.
図1が示すように、凍結乾燥装置は、原料液を供給する供給部11と、真空室21と、真空室21の内部を排気するための真空ポンプ31と、供給部11から供給される原料液を真空室21の内部に噴射する噴射器41とを備える。 As shown in FIG. 1, the freeze-drying apparatus includes a supply unit 11 for supplying a raw material liquid, a vacuum chamber 21, a vacuum pump 31 for exhausting the inside of the vacuum chamber 21, and a raw material supplied from the supply unit 11. It includes an injector 41 that injects liquid into the vacuum chamber 21.
供給部11が供給する原料液は、例えば、医薬品、食品、化粧品などの原料を含み、原料の粉末が溶媒に溶解された液体や液状体、または、原料の粉末が分散媒に分散した液体や液状体である。液状体は、固体と液体との間に位置付けられる粘度が高い流体である。原料液の一例は、アルブミンを含むアルブミン水溶液や、マンニトールを含むマンニトール水溶液である。 The raw material liquid supplied by the supply unit 11 includes, for example, raw materials such as pharmaceuticals, foods, and cosmetics, and is a liquid or liquid in which the raw material powder is dissolved in a solvent, or a liquid in which the raw material powder is dispersed in a dispersion medium. It is a liquid material. A liquid is a highly viscous fluid that is positioned between a solid and a liquid. An example of the raw material solution is an albumin aqueous solution containing albumin and a mannitol aqueous solution containing mannitol.
供給部11は、例えば、原料液が貯留される容器の内部にガスを供給する。容器に供給されるガスは、窒素、アルゴン、その他の不活性ガスである。供給部11は、容器の内部に供給されるガスの圧力によって、供給部11から供給される原料液の流量を調整する。 The supply unit 11 supplies gas to the inside of the container in which the raw material liquid is stored, for example. The gas supplied to the container is nitrogen, argon or any other inert gas. The supply unit 11 adjusts the flow rate of the raw material liquid supplied from the supply unit 11 by the pressure of the gas supplied to the inside of the container.
真空室21は、例えば、上面と底面とを有した円筒形状を有する。真空室21は、真空室の内部空間である真空空間21Sを区切る。真空空間21Sの圧力は、真空ポンプ31の駆動によって、例えば、0.1Pa以上500Pa以下のなかのいずれかの値に調整される。 The vacuum chamber 21 has, for example, a cylindrical shape having an upper surface and a lower surface. The vacuum chamber 21 divides the vacuum space 21S, which is the internal space of the vacuum chamber. The pressure in the vacuum space 21S is adjusted to any value of, for example, 0.1 Pa or more and 500 Pa or less by driving the vacuum pump 31.
噴射器41は、真空室21の上面に備えられている。噴射器41は、供給部11に接続されている。噴射器41は、凍結乾燥用ノズル43を備える。凍結乾燥用ノズル43は、供給部11から供給される原料液を真空空間21Sの内部に噴射する。 The injector 41 is provided on the upper surface of the vacuum chamber 21. The injector 41 is connected to the supply unit 11. The injector 41 includes a freeze-drying nozzle 43. The freeze-drying nozzle 43 injects the raw material liquid supplied from the supply unit 11 into the vacuum space 21S.
真空空間21Sの内部に噴射される原料液は、凍結乾燥用ノズル43から液柱L1を形成する。液柱L1の長さは、原料液の粘度、凍結乾燥用ノズル43が備える噴射口54の内径、噴射口54から噴射されるときの圧力、真空空間21Sの圧力などによって定まる。例えば、原料液がマンニトール水溶液であり、噴射口54の内径が150μmであり、噴射されるときの圧力が0.5MPaであり、真空空間21Sの圧力が50Paであるとき、液柱L1の長さは、約400mmである。 The raw material liquid injected into the vacuum space 21S forms a liquid column L1 from the freeze-drying nozzle 43. The length of the liquid column L1 is determined by the viscosity of the raw material liquid, the inner diameter of the injection port 54 provided in the freeze-drying nozzle 43, the pressure when injected from the injection port 54, the pressure in the vacuum space 21S, and the like. For example, when the raw material liquid is a mannitol aqueous solution, the inner diameter of the injection port 54 is 150 μm, the pressure at the time of injection is 0.5 MPa, and the pressure of the vacuum space 21S is 50 Pa, the length of the liquid column L1. Is about 400 mm.
液柱L1は、表面張力の作用などを受けて、複数の液滴L2に分断される。液柱L1、および、液滴L2に含まれる液体成分は、真空空間21Sにおいて、原料などから蒸発潜熱を奪って蒸発する。蒸発潜熱を奪われた液滴L2は、自己凍結をはじめて霧状の微粒子L3に変わる。微粒子L3に含まれる液体成分の固化分は、原料などから昇華潜熱を奪って蒸発する。これにより、原料液の凍結乾燥物である微粒子L3が、トレイ21Tの上に堆積する。 The liquid column L1 is divided into a plurality of droplets L2 by the action of surface tension or the like. The liquid component contained in the liquid column L1 and the droplet L2 evaporates in the vacuum space 21S by removing the latent heat of vaporization from the raw material or the like. The droplet L2 deprived of the latent heat of vaporization begins to self-freeze and turns into mist-like fine particles L3. The solidified component of the liquid component contained in the fine particles L3 removes latent heat of sublimation from the raw material and evaporates. As a result, the fine particles L3, which is a freeze-dried product of the raw material liquid, are deposited on the tray 21T.
図2が示すように、噴射器41は、導入管42と凍結乾燥用ノズル43とを備える。導入管42は、例えば、円筒状を有し、真空室21の上面に固定される。導入管42の内部42Sは、供給部11から原料液を受け入れる。導入管42の先端部は、凍結乾燥用ノズル43を支持するための支持リング42Aを備える。 As shown in FIG. 2, the injector 41 includes an introduction pipe 42 and a freeze-drying nozzle 43. The introduction pipe 42 has, for example, a cylindrical shape and is fixed to the upper surface of the vacuum chamber 21. The internal 42S of the introduction pipe 42 receives the raw material liquid from the supply unit 11. The tip of the introduction pipe 42 includes a support ring 42A for supporting the freeze-drying nozzle 43.
凍結乾燥用ノズル43は、例えば、円板状を有し、支持リング42Aと、カバーの一例である固定リング44とに挟持されている。支持リング42Aと固定リング44とは、締付部材45によって固定されている。なお、支持リング42Aと凍結乾燥用ノズル43との間、および、固定リング44と凍結乾燥用ノズル43との間には、Oリングなどの封止部材が介在している。 The freeze-drying nozzle 43 has, for example, a disk shape, and is sandwiched between a support ring 42A and a fixing ring 44, which is an example of a cover. The support ring 42A and the fixing ring 44 are fixed by a tightening member 45. A sealing member such as an O-ring is interposed between the support ring 42A and the freeze-drying nozzle 43, and between the fixing ring 44 and the freeze-drying nozzle 43.
凍結乾燥用ノズル43は、ノズル本体51と撥液層52とを備える。ノズル本体51は、例えば、ステンレス鋼などの金属製の板状部材である。撥液層52は、ノズル本体51の表面のほぼ全体を覆っている。 The freeze-drying nozzle 43 includes a nozzle body 51 and a liquid-repellent layer 52. The nozzle body 51 is, for example, a metal plate-shaped member such as stainless steel. The liquid-repellent layer 52 covers almost the entire surface of the nozzle body 51.
撥液層52は、原料液を構成する液体成分を撥液する。撥液層52を構成する材料は、例えば、ポリテトラフルオロエチレン(PTFE)、パーフルオロアルコキシアルカン(PFA)、パーフルオロエチレンプロペンコポリマー(FEP)からなる群から選択される少なくとも1つである。撥液層52を構成する材料は、例えば、撥水性樹脂と共析されためっき被膜、あるいは、撥水性シランカップリング処理された、亜鉛−ニッケル−シリカ複合めっき被膜である。撥液層52を構成する材料は、高い撥液性が得られる観点において、フッ素樹脂を含むことが好ましい。また、撥液層52は、撥液層52の機械的な耐久性が得られる観点において、フッ素樹脂と共析されためっき被膜であることが好ましい。フッ素樹脂と共析されためっき被膜であれば、撥液層52のなかにフッ素樹脂が均一に分布しやすく、フッ素樹脂による撥液性と、めっき被膜による耐久性とが、撥液層52の全体で均一に得られやすい。 The liquid repellent layer 52 repels liquid components constituting the raw material liquid. The material constituting the liquid repellent layer 52 is, for example, at least one selected from the group consisting of polytetrafluoroethylene (PTFE), perfluoroalkoxy alkane (PFA), and perfluoroethylene propene copolymer (FEP). The material constituting the liquid-repellent layer 52 is, for example, a plating film co-deposited with a water-repellent resin or a zinc-nickel-silica composite plating film that has been subjected to a water-repellent silane coupling treatment. The material constituting the liquid-repellent layer 52 preferably contains a fluororesin from the viewpoint of obtaining high liquid-repellent properties. Further, the liquid-repellent layer 52 is preferably a plating film co-deposited with the fluororesin from the viewpoint of obtaining the mechanical durability of the liquid-repellent layer 52. If the plating film is co-deposited with the fluororesin, the fluororesin is likely to be uniformly distributed in the liquid-repellent layer 52, and the liquid-repellent property of the fluororesin and the durability of the plating film are the characteristics of the liquid-repellent layer 52. It is easy to obtain it uniformly as a whole.
撥液層52は、例えば、PTFEと共析されたニッケルめっき被膜である。ニッケルめっき被膜は、例えば、PTFEを30%含む無電解ニッケルめっき被膜である。無電解ニッケルめっき被膜であれば、フッ素樹脂の一例であるPTFEがニッケルめっき被膜のなかに均一に分布しやすく、これにより、液体成分の撥液性を撥液層52のほぼ全体で均一に得られやすい。また、ニッケルめっき被膜であれば、原料液のなかに粉末などが含まれる場合であっても、粉末に対する耐摩耗を撥液層52において得られる。 The liquid-repellent layer 52 is, for example, a nickel-plated coating co-deposited with PTFE. The nickel plating film is, for example, an electroless nickel plating film containing 30% of PTFE. In the case of an electroless nickel-plated coating, PTFE, which is an example of a fluororesin, is likely to be uniformly distributed in the nickel-plated coating, whereby the liquid-repellent property of the liquid component can be uniformly obtained over almost the entire liquid-repellent layer 52. Easy to get. Further, in the case of the nickel plating film, even when powder or the like is contained in the raw material liquid, wear resistance to the powder can be obtained in the liquid repellent layer 52.
凍結乾燥用ノズル43の中央には、導入管42の内部と、真空空間21Sとの間を貫通するノズル孔53が形成されている。ノズル孔53は、凍結乾燥用ノズル43の下面と直交する方向に延在する円形孔状を有する。凍結乾燥用ノズル43の下面は、凍結乾燥用ノズル43の外表面を構成する。凍結乾燥用ノズル43の下面、および、ノズル孔53の内表面は、これらに共通する撥液層52によって構成されている。 At the center of the freeze-drying nozzle 43, a nozzle hole 53 penetrating between the inside of the introduction pipe 42 and the vacuum space 21S is formed. The nozzle hole 53 has a circular hole shape extending in a direction orthogonal to the lower surface of the freeze-drying nozzle 43. The lower surface of the freeze-drying nozzle 43 constitutes the outer surface of the freeze-drying nozzle 43. The lower surface of the freeze-drying nozzle 43 and the inner surface of the nozzle hole 53 are formed of a liquid-repellent layer 52 common to these.
ノズル孔53が有する開口のなかで真空空間21Sの側に位置する開口は、噴射口54である。噴射口54は、例えば、円形であって、50μm以上500μm以下の内径を有する。噴射口54の内径は、液柱L1の太さ、ひいては、液滴L2の大きさに影響を及ぼす。噴射口54の内径は、微粒子L3の大きさに応じて適宜選択される。ノズル孔53の数量は、導入管42に1つずつであってもよいし、導入管42に2つずつ以上であってもよい。 Among the openings of the nozzle hole 53, the opening located on the side of the vacuum space 21S is the injection port 54. The injection port 54 is, for example, circular and has an inner diameter of 50 μm or more and 500 μm or less. The inner diameter of the injection port 54 affects the thickness of the liquid column L1 and thus the size of the droplet L2. The inner diameter of the injection port 54 is appropriately selected according to the size of the fine particles L3. The number of nozzle holes 53 may be one for each introduction pipe 42, or two or more for each introduction pipe 42.
[作用]
噴射器41に供給された原料液は、導入管42、および、凍結乾燥用ノズル43を通して、真空空間21Sに噴射される。ノズル孔53の内表面を構成する撥液層52は、ノズル孔53での原料液の流れを円滑にして、噴射口54から延在する液柱L1の形成を円滑に進める。
[Action]
The raw material liquid supplied to the injector 41 is injected into the vacuum space 21S through the introduction pipe 42 and the freeze-drying nozzle 43. The liquid-repellent layer 52 forming the inner surface of the nozzle hole 53 facilitates the flow of the raw material liquid in the nozzle hole 53, and smoothly promotes the formation of the liquid column L1 extending from the injection port 54.
一方、液柱L1を形成しない原料液は、噴射口54の周囲に向かって、微小液滴として飛散する。特に、粘度の高い原料液においては、水などの粘度が低い原料液と比べて、より多くの微小液滴が形成され得る。飛散した微小液滴のなかには、噴射口54の周囲において、凍結乾燥用ノズル43の外表面に到達する原料液が含まれる。凍結乾燥用ノズル43の外表面に到達した微小液滴は、液体成分の蒸発に伴って自己凍結し、さらには、液体成分の凍結後の昇華に伴って乾燥する。 On the other hand, the raw material liquid that does not form the liquid column L1 scatters as fine droplets toward the periphery of the injection port 54. In particular, in a raw material liquid having a high viscosity, more fine droplets can be formed as compared with a raw material liquid having a low viscosity such as water. The scattered fine droplets include a raw material liquid that reaches the outer surface of the freeze-drying nozzle 43 around the injection port 54. The fine droplets that reach the outer surface of the freeze-drying nozzle 43 self-freeze as the liquid component evaporates, and further dry as the liquid component sublimates after freezing.
この際、噴射口54を含む凍結乾燥用ノズル43の下面は、撥液層52によって構成されている。撥液層52は、原料液を構成する液体成分のぬれ性を、凍結乾燥用ノズル43の外表面で低下させる。噴射口54に位置する原料液は、噴射口54から若干膨出するように噴射されて液柱L1を形成する。この際、噴射口54から膨出する原料液の一部は、液柱L1を形成するうえで、噴射口54の周囲との親和性に従い、少なからず噴射口54の周囲に向けて引き剥がされる。撥液層52による表面エネルギーの低下や原料液に対する接触角の低下は、噴射口54の周囲に向けたこうした誘導を抑える。すなわち、撥液層52は、噴射口54の周囲に向けて原料液が誘導されることを抑えて、噴射口54から飛散する微小液滴の総量そのものを低減させる。そして、撥液層52は、噴射口54から飛散した原料液が凍結乾燥用ノズル43の外表面に付着することを抑える。外表面に付着せずに自己凍結した微小液滴は、トレイ21Tに回収されたり、真空空間21Sから排気されたりする。 At this time, the lower surface of the freeze-drying nozzle 43 including the injection port 54 is composed of a liquid-repellent layer 52. The liquid-repellent layer 52 reduces the wettability of the liquid component constituting the raw material liquid on the outer surface of the freeze-drying nozzle 43. The raw material liquid located at the injection port 54 is injected so as to slightly bulge from the injection port 54 to form a liquid column L1. At this time, a part of the raw material liquid that swells from the injection port 54 is peeled off not a little toward the periphery of the injection port 54 according to the affinity with the periphery of the injection port 54 in forming the liquid column L1. .. The decrease in surface energy and the decrease in contact angle with the raw material liquid due to the liquid repellent layer 52 suppress such induction toward the periphery of the injection port 54. That is, the liquid-repellent layer 52 suppresses the induction of the raw material liquid toward the periphery of the injection port 54, and reduces the total amount of fine droplets scattered from the injection port 54 itself. The liquid-repellent layer 52 prevents the raw material liquid scattered from the injection port 54 from adhering to the outer surface of the freeze-drying nozzle 43. The fine droplets that are self-frozen without adhering to the outer surface are collected in the tray 21T or exhausted from the vacuum space 21S.
[実施例]
撥液層52として、アルバックテクノ株式会社製の「NIFGRIP(ニフグリップ)」(登録商標)を用いた。JIS K6894:金属素地上のふっ素樹脂塗膜の試験方法に準拠した方法による撥液層52の接触角は、105±3°であった。そして、凍結乾燥用ノズル43からアルブミン水溶液を噴射したところ、撥液層52を備えない構成と比べて、噴射口54の周囲に自己凍結した微小液滴は認められず、原料液を安定して噴射させられることが認められた。また、アルブミン水溶液を長期間にわたり噴射させて撥液層52が6μmの摩耗した状態であっても、撥液層52における接触角の変動は2°以内であって、撥液層52の一部が摩耗するとしても、微小液滴の飛散が抑えられることが確認された。
[Example]
As the liquid repellent layer 52, "NIFGRIP" (registered trademark) manufactured by ULVAC TECHNO CO., LTD. Was used. JIS K6894: The contact angle of the liquid repellent layer 52 by a method based on the test method for a fluororesin coating film on a metal base was 105 ± 3 °. When the albumin aqueous solution was injected from the freeze-drying nozzle 43, no self-frozen fine droplets were observed around the injection port 54 as compared with the configuration without the liquid-repellent layer 52, and the raw material solution was stabilized. It was found to be sprayed. Further, even when the albumin aqueous solution is sprayed for a long period of time and the liquid repellent layer 52 is worn by 6 μm, the fluctuation of the contact angle in the liquid repellent layer 52 is within 2 °, which is a part of the liquid repellent layer 52. It was confirmed that the scattering of fine droplets was suppressed even if the particles were worn.
発明者らは、比較的に高粘度のアルブミン水溶液やマンニトール水溶液を用い、撥液層52を備えた凍結乾燥用ノズルについて、微小液滴の飛散が抑えられることを確認した。また、撥液層52を備えた凍結乾燥用ノズルは、特に、粘度が1.8mPa・sよりも高く、また、分子量が数万から80万程度のタンパク質が原料液に含まれる場合に、より効果的であることも確認した。なお、こうした効果は、真空空間21Sの圧力に応じた飽和水蒸気下で、噴射口54の周囲において、表面に吸着された水分子量の差によるものと推定される。すなわち、撥液層52の表面に存在する水分子量が撥液層52を備えない構成と比べて少ないことは、タンパク質などの高分子タンパク質との接触点における水分子量が少ないことと同じである。そのため、高分子が撥液層52の表面に付着する力は、撥液層52によって弱められている。そして、液柱L1の一部を剥離させて噴射口54の周囲に誘導する起点となるような保持力を高分子が発揮しがたく、このような作用によって上記効果が得られていると言える。 The inventors have confirmed that the scattering of fine droplets can be suppressed in a freeze-drying nozzle provided with a liquid-repellent layer 52 by using a relatively high-viscosity albumin aqueous solution or mannitol aqueous solution. Further, the freeze-drying nozzle provided with the liquid-repellent layer 52 is more suitable especially when the viscosity is higher than 1.8 mPa · s and the raw material liquid contains a protein having a molecular weight of about tens of thousands to 800,000. It was also confirmed to be effective. It is presumed that such an effect is due to the difference in the weight of water molecules adsorbed on the surface around the injection port 54 under saturated water vapor corresponding to the pressure of the vacuum space 21S. That is, the fact that the water molecular weight present on the surface of the liquid repellent layer 52 is smaller than that in the configuration not provided with the liquid repellent layer 52 is the same as the fact that the water molecular weight at the contact point with the polymer protein such as a protein is small. Therefore, the force with which the polymer adheres to the surface of the liquid repellent layer 52 is weakened by the liquid repellent layer 52. Then, it is difficult for the polymer to exert a holding force that serves as a starting point for peeling off a part of the liquid column L1 and inducing it around the injection port 54, and it can be said that the above effect is obtained by such an action. ..
以上、第1実施形態によれば、以下の効果を得ることができる。
(1−1)凍結乾燥用ノズル43の下面のなかで噴射口54を含む部分は、原料液の付着を撥液性によって抑制し、これにより、原料液の自己凍結物が堆積することを抑制する。結果として、噴射口54の周囲で自己凍結物が堆積すること、また、噴射口54が自己凍結物で塞がれることが抑制されて、真空空間21Sへの原料液の噴射が円滑となる。
As described above, according to the first embodiment, the following effects can be obtained.
(1-1) The portion of the lower surface of the freeze-drying nozzle 43 including the injection port 54 suppresses the adhesion of the raw material liquid by its liquid repellency, thereby suppressing the accumulation of self-frozen matter of the raw material liquid. To do. As a result, the accumulation of self-frozen material around the injection port 54 and the fact that the injection port 54 is not blocked by the self-frozen material are suppressed, so that the raw material liquid is smoothly injected into the vacuum space 21S.
(1−2)凍結乾燥用ノズル43における流路の内表面が撥液層52から構成されるため、噴射口54に向けて円滑に原料液を導くことが可能ともなる。
(1−3)固定リング44は、噴射口54の周囲を囲い、噴射口54から飛散した原料液が真空室21の内表面などのようなな固定リング44以外に付着することを抑える。結果として、真空室21の内表面などのメンテナンス性を高めることが可能ともなる。
(1-2) Since the inner surface of the flow path in the freeze-drying nozzle 43 is composed of the liquid-repellent layer 52, the raw material liquid can be smoothly guided toward the injection port 54.
(1-3) The fixing ring 44 surrounds the injection port 54 and prevents the raw material liquid scattered from the injection port 54 from adhering to other than the fixing ring 44 such as the inner surface of the vacuum chamber 21. As a result, it is possible to improve the maintainability of the inner surface of the vacuum chamber 21 and the like.
(1−4)撥液層52が、例えば、PTFEと共析された無電解Niめっき被膜であるから、撥液層52による撥液性の均一化を図ること、また、原料液の通過による撥液層52の摩耗を抑えることが可能ともなる。 (1-4) Since the liquid-repellent layer 52 is, for example, an electroless Ni-plated film co-deposited with PTFE, the liquid-repellent layer 52 can be made uniform in liquid repellency, and the raw material liquid can pass through. It is also possible to suppress wear of the liquid repellent layer 52.
(第2実施形態)
以下、図3を参照して、凍結乾燥装置、および、凍結乾燥用ノズルの第2実施形態を説明する。なお、第2実施形態は、凍結乾燥用ノズルが備えるノズル孔の形状が第1実施形態とは異なる。以下、第1実施形態と異なるノズル孔の形状について主に説明し、第1実施形態と同様の構成についてはその説明を割愛する。
(Second Embodiment)
Hereinafter, a second embodiment of the freeze-drying apparatus and the freeze-drying nozzle will be described with reference to FIG. In the second embodiment, the shape of the nozzle hole provided in the freeze-drying nozzle is different from that in the first embodiment. Hereinafter, the shape of the nozzle hole different from that of the first embodiment will be mainly described, and the description of the same configuration as that of the first embodiment will be omitted.
図3が示すように、凍結乾燥用ノズル43は、流路の一例であるノズル孔53を備える。ノズル孔53は、第一流路53A、第二流路53B、および、第一流路53Aと第二流路53Bとを接続する第三流路53Cを備えている。 As shown in FIG. 3, the freeze-drying nozzle 43 includes a nozzle hole 53 which is an example of a flow path. The nozzle hole 53 includes a first flow path 53A, a second flow path 53B, and a third flow path 53C that connects the first flow path 53A and the second flow path 53B.
第一流路53Aは、導入管42の内部42Sから第三流路53Cに向けて先細る錘台筒面状を有する。錘台筒面を真空空間21Sに向けて延長させた円錐筒面での中心角は、例えば、30°である。第一流路53Aは、原料液が流れる流路の断面積を、導入管42の内部42Sから第三流路53Cに向けて徐々に小さくする。凍結乾燥用ノズル43の厚み方向において、第一流路53Aの有する長さは、例えば、0.2mmである。第一流路53Aは、導入管42の内部42Sに接続されている。第一流路53Aは、第一流路53Aに流入した原料液における流れの乱れを抑えて、第三流路53Cに原料液を流出する。 The first flow path 53A has a weight base tubular surface shape that tapers from the inside 42S of the introduction pipe 42 toward the third flow path 53C. The central angle of the conical cylinder surface in which the weight base cylinder surface is extended toward the vacuum space 21S is, for example, 30 °. The first flow path 53A gradually reduces the cross-sectional area of the flow path through which the raw material liquid flows from the inside 42S of the introduction pipe 42 toward the third flow path 53C. In the thickness direction of the freeze-drying nozzle 43, the length of the first flow path 53A is, for example, 0.2 mm. The first flow path 53A is connected to the inside 42S of the introduction pipe 42. The first flow path 53A suppresses the turbulence of the flow of the raw material liquid that has flowed into the first flow path 53A, and causes the raw material liquid to flow out to the third flow path 53C.
第二流路53Bは、真空空間21Sから第三流路53Cに向けて先細る錘台筒面状を有する。錘台筒面を第三流路53Cに向けて延長させた円錐筒面での中心角は、第一流路53Aでの中心角よりも大きく、例えば、90°である。第二流路53Bは、原料液が通過する流路の断面積を、第三流路53Cから真空空間21Sに向けて徐々に大きくする。凍結乾燥用ノズル43の厚み方向において、第二流路53Bの長さは、例えば、0.2mmである。第二流路53Bは、真空空間21Sに向けた開口を下端に有する。 The second flow path 53B has a cylindrical surface shape of a weight base that tapers from the vacuum space 21S toward the third flow path 53C. The central angle of the conical cylinder surface obtained by extending the weight base cylinder surface toward the third flow path 53C is larger than the central angle of the first flow path 53A, for example, 90 °. The second flow path 53B gradually increases the cross-sectional area of the flow path through which the raw material liquid passes from the third flow path 53C toward the vacuum space 21S. In the thickness direction of the freeze-drying nozzle 43, the length of the second flow path 53B is, for example, 0.2 mm. The second flow path 53B has an opening toward the vacuum space 21S at the lower end.
第三流路53Cは、第一流路53Aと第二流路53Bとを繋ぐ筒面状を有する。第三流路53Cは、原料液が流れる流路の断面積を、第一流路53Aの下端から第三流路53Cの上端までの範囲で、ほぼ一定とする。凍結乾燥用ノズル43の厚み方向において、第三流路53Cの長さは、例えば、0.5mmである。 The third flow path 53C has a tubular surface shape connecting the first flow path 53A and the second flow path 53B. In the third flow path 53C, the cross-sectional area of the flow path through which the raw material liquid flows is substantially constant in the range from the lower end of the first flow path 53A to the upper end of the third flow path 53C. In the thickness direction of the freeze-drying nozzle 43, the length of the third flow path 53C is, for example, 0.5 mm.
第三流路53Cが有する開口のなかで、第一流路53Aに接続された開口には、第一流路53Aから原料液が流れ込む。第三流路53Cが有する開口のなかで、第二流路53Bに接続された開口は、真空空間21Sに原料液を噴射する噴射口として機能する。第三流路53Cは、第一流路53Aから流れ込む原料液から液柱L1を形成する。第三流路53Cから出る液柱L1は、第二流路53Bに触れることなく、真空空間21Sに噴射される。 Among the openings of the third flow path 53C, the raw material liquid flows from the first flow path 53A into the opening connected to the first flow path 53A. Among the openings of the third flow path 53C, the opening connected to the second flow path 53B functions as an injection port for injecting the raw material liquid into the vacuum space 21S. The third flow path 53C forms a liquid column L1 from the raw material liquid flowing from the first flow path 53A. The liquid column L1 exiting from the third flow path 53C is injected into the vacuum space 21S without touching the second flow path 53B.
撥液層52は、凍結乾燥用ノズル43の下面のなかで噴射口を含む外表面、第一流路53Aの内表面、第二流路53Bの内表面、および、第三流路53Cの内表面を構成する。
[作用]
噴射器41に供給された原料液は、導入管42、および、凍結乾燥用ノズル43を通して、真空空間21Sに噴射される。この際、第一流路53Aに流入した原料液は、第一流路53Aが有する錘台形状による乱れの抑制、および、第一流路53Aが有する内表面での撥液性とが相まって、第三流路53Cに向けて円滑に流出する。第三流路53Cに流入した原料液は、第三流路53Cが有する円筒形状による層流の形成、および、第三流路53Cが有する内表面での撥液性とが相まって、真空空間21Sに向けて円滑に液柱L1を形成する。
The liquid-repellent layer 52 is an outer surface including an injection port, an inner surface of the first flow path 53A, an inner surface of the second flow path 53B, and an inner surface of the third flow path 53C in the lower surface of the freeze-drying nozzle 43. To configure.
[Action]
The raw material liquid supplied to the injector 41 is injected into the vacuum space 21S through the introduction pipe 42 and the freeze-drying nozzle 43. At this time, the raw material liquid that has flowed into the first flow path 53A is a third flow due to the suppression of turbulence due to the weight trap shape of the first flow path 53A and the liquid repellency on the inner surface of the first flow path 53A. It flows out smoothly toward the road 53C. The raw material liquid that has flowed into the third flow path 53C is a vacuum space 21S due to the formation of a laminar flow due to the cylindrical shape of the third flow path 53C and the liquid repellency of the inner surface of the third flow path 53C. The liquid column L1 is smoothly formed toward.
一方、液柱L1を形成しない原料液は、噴射口の周囲に向かって、微小液滴として飛散する。この点、噴射口を含む凍結乾燥用ノズル43の下面は、撥液層52によって形成されている。そのため、噴射口から飛散した原料液が凍結乾燥用ノズル43の外表面に付着することが、撥液層52の撥液性によって抑えられる。また、噴射口の周囲は、真空空間21Sに向けて拡開された第二流路53Bの内表面であって、噴射口から飛散した原料液が噴射口の近傍に戻ることを抑えている。結果として、撥液層52による撥液と、第二流路53Bによる噴射口の保護とが相まって、噴射口の近傍で自己凍結物が堆積することを抑える。 On the other hand, the raw material liquid that does not form the liquid column L1 scatters as fine droplets toward the periphery of the injection port. In this respect, the lower surface of the freeze-drying nozzle 43 including the injection port is formed by the liquid-repellent layer 52. Therefore, the liquid-repellent property of the liquid-repellent layer 52 prevents the raw material liquid scattered from the injection port from adhering to the outer surface of the freeze-drying nozzle 43. Further, the periphery of the injection port is the inner surface of the second flow path 53B expanded toward the vacuum space 21S, and prevents the raw material liquid scattered from the injection port from returning to the vicinity of the injection port. As a result, the liquid repellency of the liquid repellent layer 52 and the protection of the injection port by the second flow path 53B combine to prevent self-freezing matter from accumulating in the vicinity of the injection port.
以上、第2実施形態によれば、第1実施形態での効果に加えて以下の効果が得られる。
(2−1)第三流路53Cの内径が小さい構成においても、原料液での流れの乱れが第一流路53Aによって抑えられて、液柱L1の形成が円滑に進められる。これにより、液柱L1を細くすること、ひいては、凍結乾燥物の微小化を図ることが容易となる。
As described above, according to the second embodiment, the following effects can be obtained in addition to the effects of the first embodiment.
(2-1) Even in a configuration in which the inner diameter of the third flow path 53C is small, the turbulence of the flow in the raw material liquid is suppressed by the first flow path 53A, and the formation of the liquid column L1 is smoothly promoted. As a result, it becomes easy to make the liquid column L1 thinner, and by extension, to make the freeze-dried product smaller.
(2−2)第三流路53Cの内径が小さい構成においても、第三流路53Cでの流速を確保することが容易となるため、流速の低下に起因した噴射口の近傍での自己凍結を抑制できる。 (2-2) Even in a configuration in which the inner diameter of the third flow path 53C is small, it is easy to secure the flow velocity in the third flow path 53C, so that self-freezing in the vicinity of the injection port due to the decrease in the flow velocity Can be suppressed.
(2−3)噴射口から飛散した原料液が噴射口の近傍に向けて戻ることを第二流路53Bが抑制する。そして、撥液層52による撥液と、第二流路53Bによる戻りの抑制とが相まって、噴射口の近傍に凍結乾燥物が堆積することがさらに抑制される。 (2-3) The second flow path 53B suppresses the return of the raw material liquid scattered from the injection port toward the vicinity of the injection port. Then, the liquid repellency by the liquid repellent layer 52 and the suppression of the return by the second flow path 53B are combined to further suppress the accumulation of freeze-dried material in the vicinity of the injection port.
なお、上記各実施形態は、以下のように変更して実施できる。
[カバー]
・固定リング44のようなカバーは、噴射口54から真空空間21Sに向けて拡開された孔を有してもよい。すなわち、カバーが有する孔は、噴射口54に向けて先細る錘台筒面状を有してもよい。また、カバーが有する孔は、噴射口54よりも十分に大きい径を有した円筒面状であってもよい。
Each of the above embodiments can be modified as follows.
[cover]
A cover such as the fixing ring 44 may have a hole that is widened from the injection port 54 toward the vacuum space 21S. That is, the hole of the cover may have a cylindrical surface shape of a weight base that tapers toward the injection port 54. Further, the hole of the cover may have a cylindrical surface shape having a diameter sufficiently larger than that of the injection port 54.
・カバーの表面もまた、原料液の液体成分を撥液する撥液性を備えてもよい。この構成であれば、噴射口54の周囲に凍結乾燥物が堆積することを、さらに抑制することが可能ともなる。なお、カバーの表面が備える撥液性は、ノズル本体51と同じく、カバーそのものが撥液性を有した材料から構成されてもよいし、カバーの表面が撥液層から構成されてもよい。 -The surface of the cover may also have a liquid repellent property that repels the liquid component of the raw material liquid. With this configuration, it is possible to further suppress the accumulation of freeze-dried products around the injection port 54. As for the liquid repellency of the surface of the cover, the cover itself may be made of a material having the liquid repellency as in the nozzle body 51, or the surface of the cover may be made of a liquid repellent layer.
[撥液性]
・撥液層52は、ノズル本体51に塗布された撥水性シランカップリング剤であってもよい。
[Liquid repellent]
The liquid-repellent layer 52 may be a water-repellent silane coupling agent applied to the nozzle body 51.
・ノズル本体51を構成する材料は、例えば、PTFE、PFA、および、FEPなどの撥水性樹脂であってもよい。この際、撥液層52が割愛されて、ノズル本体51の外表面が、凍結乾燥用ノズルの外表面であって、撥液性を備えた面であってもよい。すなわち、凍結乾燥用ノズルの外表面における撥液性は、ノズル本体51の撥液性によって担われてもよい。 -The material constituting the nozzle body 51 may be, for example, a water-repellent resin such as PTFE, PFA, and FEP. At this time, the liquid-repellent layer 52 may be omitted, and the outer surface of the nozzle body 51 may be the outer surface of the freeze-drying nozzle, which has liquid-repellent properties. That is, the liquid repellency on the outer surface of the freeze-drying nozzle may be borne by the liquid repellency of the nozzle body 51.
・撥液層52は、ノズル孔53から割愛されて、凍結乾燥用ノズルの下面にのみ位置する構成であってもよい。また、撥液層52は、凍結乾燥用ノズルの下面のなかで、噴射口54を囲う部分にのみ位置する構成であってもよい。なお、噴射口54を囲う部分、および、ノズル孔53の内表面を含む部分に撥液層52が位置する構成であれば、上記(1−3)に準じた効果を得ることが可能ともなる。 The liquid-repellent layer 52 may be omitted from the nozzle hole 53 and may be located only on the lower surface of the freeze-drying nozzle. Further, the liquid repellent layer 52 may be configured to be located only in a portion surrounding the injection port 54 in the lower surface of the freeze-drying nozzle. If the liquid repellent layer 52 is located in the portion surrounding the injection port 54 and the portion including the inner surface of the nozzle hole 53, it is possible to obtain the effect according to the above (1-3). ..
[その他]
・真空室21は、凍結乾燥物を加熱する加熱機構を搭載してもよい。加熱機構を搭載する構成であれば、凍結乾燥物の加熱による乾燥を促すことも可能となる。
[Other]
-The vacuum chamber 21 may be equipped with a heating mechanism for heating the freeze-dried product. If the configuration is equipped with a heating mechanism, it is possible to promote drying by heating the freeze-dried product.
・真空室21は、蒸発した液体成分を捕集するコールドトラップなどの冷却機構を搭載してもよい。冷却機構を搭載する構成であれば、液体成分の蒸気圧を所定値に保つことが可能ともなるため、液体成分の蒸発を安定させること、ひいては、凍結乾燥物の大きさの均一化を図ることが可能ともなる。 -The vacuum chamber 21 may be equipped with a cooling mechanism such as a cold trap that collects evaporated liquid components. If the configuration is equipped with a cooling mechanism, it is possible to maintain the vapor pressure of the liquid component at a predetermined value. Therefore, the evaporation of the liquid component should be stabilized, and the size of the freeze-dried product should be made uniform. Is also possible.
・ノズル孔53、および、ノズル孔53の近傍に位置する撥液層については、接触角を高める目的で突起を設けても良い。特に、複数の突起を設けることで液柱L1に対する固液接触面積が増大し、所謂、超撥水性を付与することが可能となる。超撥水性とは、接触角が120°前後の表面性状を利用して接触角が150°を超える状態にまで強化された状態を言う。これにより、微小液滴の飛散はさらに抑えられる。この突起は、表面粗さを調整することを目的として付与されるが、その設計においては、例えば、濡れに関する式であるWenzel式やCassie式を用いて、求めることができる。 -The nozzle hole 53 and the liquid-repellent layer located in the vicinity of the nozzle hole 53 may be provided with protrusions for the purpose of increasing the contact angle. In particular, by providing a plurality of protrusions, the solid-liquid contact area with respect to the liquid column L1 is increased, and so-called super water repellency can be imparted. The super water repellency refers to a state in which the contact angle is strengthened to a state of exceeding 150 ° by utilizing the surface texture of the contact angle of about 120 °. As a result, the scattering of minute droplets is further suppressed. This protrusion is provided for the purpose of adjusting the surface roughness, but in its design, it can be obtained by using, for example, a Wetting formula or a Cassie formula, which is a formula related to wetting.
L1…液柱、L2…液滴、L3…微粒子、11…供給部、21…真空室、21S…真空空間、21T…トレイ、31…真空ポンプ、41…噴射器、42…導入管、42A…支持リング、42S…内部、43…凍結乾燥用ノズル、44…固定リング、45…締付部材、51…ノズル本体、52…撥液層、53…ノズル孔、53A…第一流路、53B…第二流路、53C…第三流路、54…噴射口。 L1 ... Liquid column, L2 ... Droplet, L3 ... Fine particle, 11 ... Supply unit, 21 ... Vacuum chamber, 21S ... Vacuum space, 21T ... Tray, 31 ... Vacuum pump, 41 ... Injector, 42 ... Introduction tube, 42A ... Support ring, 42S ... Internal, 43 ... Freeze-drying nozzle, 44 ... Fixing ring, 45 ... Tightening member, 51 ... Nozzle body, 52 ... Liquid repellent layer, 53 ... Nozzle hole, 53A ... First flow path, 53B ... No. Two flow paths, 53C ... Third flow path, 54 ... Injection port.
Claims (8)
ノズル外表面のなかで前記原料液の噴射口を含む部分が前記原料液のなかの液体成分を撥液する撥液性を有する
凍結乾燥用ノズル。 A freeze-drying nozzle for injecting a raw material liquid into a vacuum space and freeze-drying particles composed of the raw material liquid in the vacuum space.
A freeze-drying nozzle having a liquid-repellent property in which a portion of the outer surface of the nozzle including the injection port of the raw material liquid repels the liquid component of the raw material liquid.
前記流路の内表面、および、前記ノズル外表面が、前記液体成分を撥液する撥液層によって構成されている
請求項1に記載の凍結乾燥用ノズル。 The freeze-drying nozzle is formed with a flow path of the raw material liquid connected to the injection port.
The freeze-drying nozzle according to claim 1, wherein the inner surface of the flow path and the outer surface of the nozzle are formed of a liquid-repellent layer that repels the liquid component.
請求項2に記載の凍結乾燥用ノズル。 The freeze-drying nozzle according to claim 2, wherein the liquid-repellent layer contains a fluororesin.
請求項3に記載の凍結乾燥用ノズル。 The freeze-drying nozzle according to claim 3, wherein the liquid-repellent layer is a plating film co-deposited with a fluororesin.
前記第一流路は、前記第三流路に向けて先細る錘台筒面状を有して前記液体の供給部に接続され、
前記第二流路は、前記第三流路に向けて先細る錘台筒面状を有して前記噴射口に接続され、
前記第三流路は、前記噴射口を含み、前記第一流路と前記第二流路とを繋ぐ筒面状を有する
請求項2から4のいずれか一項に記載の凍結乾燥用ノズル。 The flow path includes a first flow path, a second flow path, and a third flow path that connects the first flow path and the second flow path.
The first flow path has a cylindrical surface shape of a weight base that tapers toward the third flow path, and is connected to the liquid supply unit.
The second flow path has a cylindrical surface shape of a weight base that tapers toward the third flow path, and is connected to the injection port.
The freeze-drying nozzle according to any one of claims 2 to 4, wherein the third flow path includes the injection port and has a tubular surface shape connecting the first flow path and the second flow path.
前記カバーの外表面が前記液体成分を撥液する撥液層によって構成されている
請求項1から5のいずれか一項に記載の凍結乾燥用ノズル。 A cover for receiving the raw material liquid scattered from the injection port is provided.
The freeze-drying nozzle according to any one of claims 1 to 5, wherein the outer surface of the cover is formed of a liquid-repellent layer that repels the liquid component.
原料液を供給する供給部と、
前記供給部が供給する前記原料液を前記真空室へ噴射する請求項1から6のいずれか一項に記載の凍結乾燥用ノズルと、を備える
凍結乾燥装置。 Vacuum chamber and
The supply unit that supplies the raw material liquid and
A freeze-drying apparatus comprising the freeze-drying nozzle according to any one of claims 1 to 6, which injects the raw material liquid supplied by the supply unit into the vacuum chamber.
前記原料液を噴射させる凍結乾燥用ノズルのノズル外表面のなかで前記原料液の噴射口を含む部分が前記原料液のなかの液体成分を撥液する撥液性を有する
造粒方法。 A granulation method in which a raw material liquid is sprayed into a vacuum space and particles composed of the raw material liquid are freeze-dried in the vacuum space.
A granulation method having a liquid-repellent property in which a portion of the outer surface of the nozzle of a freeze-drying nozzle for injecting the raw material liquid, including an injection port of the raw material liquid, repels a liquid component in the raw material liquid.
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