JP3985241B2 - Freeze vacuum dryer - Google Patents

Freeze vacuum dryer Download PDF

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Publication number
JP3985241B2
JP3985241B2 JP26508598A JP26508598A JP3985241B2 JP 3985241 B2 JP3985241 B2 JP 3985241B2 JP 26508598 A JP26508598 A JP 26508598A JP 26508598 A JP26508598 A JP 26508598A JP 3985241 B2 JP3985241 B2 JP 3985241B2
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Japan
Prior art keywords
drying chamber
vacuum
freeze
thin film
light source
Prior art date
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Expired - Fee Related
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JP26508598A
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Japanese (ja)
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JP2000088461A (en
Inventor
昭 藤嶋
久三 中村
敏夫 根岸
健 桃野
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Ulvac Inc
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Ulvac Inc
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Priority to JP26508598A priority Critical patent/JP3985241B2/en
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Description

【0001】
【発明の属する技術分野】
本発明は、食品や医薬品などの水分を含有した被乾燥物を凍結させ、真空下で凍結状態のまま水分や溶剤を蒸発させ乾燥する凍結真空乾燥装置に関する。
【0002】
【従来の技術】
従来、凍結真空乾燥装置は、図4に示すように、被乾燥物aが収容される真空乾燥室bに、コールドトラップcと真空ポンプdを備えた真空排気装置eを接続した構成を有するのが一般的であり、該乾燥室b内を該真空排気装置eで減圧することにより該被乾燥物aを凍結させたのち該真空排気装置eで該乾燥室b内をさらに真空に排気することにより、凍結した水分が昇華して乾燥する。該真空乾燥室b内には上下に移動可能で加熱冷却自在の棚fを設け、乾燥中に該棚fに載せられた被乾燥物aを加熱してその昇華を促進させる構成とすることも行われている。該被乾燥物aが医薬品である場合、薬液を詰めたバイヤル瓶を半打栓状態で該真空乾燥室b内の棚fに並べ、その乾燥が終了したとき、該棚fの上下の間隔を狭めるように移動させて瓶を打栓したのち扉gを開いて外部へ取り出される。
【0003】
また、アナターゼ型結晶の酸化チタンの膜に紫外線を照射すると、該膜に付着した水を分解し、そのとき発生する活性酸素が該膜に付着した汚物を分解させる現象(光触媒機能)が藤嶋らにより見いだされ、さらに細菌をも死滅させる機能をもつことが究明された。
【0004】
【発明が解決しようとする課題】
該被乾燥物aが食品や医薬品である場合、該真空乾燥室b内が細菌などで汚染されることを防止するため、エチレン・オキサイド・ガス(EOG)を該乾燥室b内に流し、或いは高温スチームや無菌洗浄水を流して滅菌・除菌することが行われている。しかし、EOGの該乾燥室b内に残留に関する安全上の不安があり、高温スチームの洗浄を可能にするには、該乾燥室bに耐圧性を持たせる必要があって装置が高価になる欠点がある。また、無菌洗浄水での洗浄を含むこれらの滅菌方法では、凍結真空乾燥装置の運転を止めて定期的に行う必要があり、装置の運転効率が低下して好ましくない。
【0005】
本発明は、長期間に亘り真空乾燥室内を滅菌状態に維持できて運転効率が良く、安価に製作できる凍結真空乾燥装置を提供することを目的とするものである。
【0006】
【課題を解決するための手段】
本発明では、被乾燥物を収容した真空乾燥室内をこれに接続した真空排気装置により真空排気して該被乾燥物を凍結真空乾燥する装置であって、該真空乾燥室の室内に露出した表面を酸化チタンの薄膜で覆い、該薄膜を照射してこれに光分解による滅菌作用を行わせる光源と、表面が酸化チタンの薄膜で覆われた反射鏡とを有することにより、上記目的を達成するようにした。さらに、反射鏡面に加工され、表面が酸化チタンの薄膜で覆われた棚板を有することが好ましい。該紫外線光源には400nm以下の波長の紫外光を照射する光源を使用することが有効である。
【0007】
【発明の実施の形態】
本発明の実施の形態を図面に基づき説明すると、図1及び図2に於いて符号1は複数段の棚板2を内部に設けた真空乾燥室、符号3は該真空乾燥室1に接続したコールドトラップ4及び真空ポンプ5を備えた真空排気装置を示し、該コールドトラップ4には冷凍機6から冷媒を循環させて該乾燥室1内の主として水分を凝縮捕集するようにした。各棚板2にはトレイやバイヤル瓶7に収められた薬液や食品などの被乾燥物8が載せられている。該被乾燥物8は該乾燥室1の扉1aを開いて内部に出し入れされ、被乾燥物8がバイヤル瓶7に収められている場合、該乾燥室1の上方に設けた封栓シリンダ9により該乾燥室1内でバイヤル瓶8を打栓したのち取り出される。10は封栓シリンダ9を作動させるための空気圧縮機、11はコールドトラップ4に凝縮した氷を溶かす融氷水導入管、12は融氷水の排水管、13は無菌室内へ無菌フィルターを介して接続した大気導入管である。
【0008】
こうした構成は従来の凍結真空乾燥装置と特に変わりがなく、被乾燥物8を収めた該乾燥室1内をコールドトラップ4を−45℃程度で作動させながら真空ポンプ5で減圧することにより該被乾燥物8を凍結させ、さらに該乾燥室1内を6.7Pa程度の真空に排気することにより凍結した被乾燥物8中の水分を昇華させて乾燥が行われることも従来のものと同様であるが、本発明では、該乾燥室1の内壁や棚板2などの室内へ露出した表面が細菌で汚染され、或いは汚れが残存することを防止すべく、該表面を酸化チタンの薄膜14で覆い、該乾燥室1内に紫外線光源15を設けるようにした。
【0009】
これを更に説明すると、ステンレスや軟鋼で構成された該乾燥室1の内面及び棚板2の表面に酸化チタンを焼結させて薄膜14を形成し、該乾燥室1内に該表面に多くの暗部を生じないように4本の紫外線光源15を設けた。該薄膜14は厚さ1〜3ミクロン程度とし、紫外線光源15には波長400nm以下の紫外線を照射するものを使用した。該乾燥室1内には封栓シリンダ9の作動部などが内部構成物として存在するが、これらのものにも可能な限り酸化チタンをコーティングしておくことが好ましい。また、該光源14を増設する代わりに、図3に示すように反射鏡16や棚板2を反射鏡面に加工した反射装置を設けて暗部となりやすい部分を減らしてもよく、この場合これら反射鏡16や反射鏡面にも薄膜14が形成される。
【0010】
該乾燥室1内に乾燥室と同じ厚さの酸化チタン薄膜を付けた試験片を置き、その表面に生菌(MRSA,大腸菌)を付着させ、その試験片表面が1000ルックスになるように該紫外線光源15を1時間照射したところ、生菌の99.9%が滅菌された。また、滅菌に関しては、酸化チタンの表面では水が分解され、その時発生する活性酸素の働きが大きいため、真空下だけでなく、乾燥物の出し入れ時のように、乾燥室が大気開放され、室内の水分が多くなっている時に集中的に光を照射すれば更に滅菌効果が大きくなることが分かった。
【0011】
【発明の効果】
以上のように本発明によるときは、凍結真空乾燥装置の真空乾燥室内に露出した表面を酸化チタンの薄膜で覆い、該真空乾燥室内に該薄膜に紫外線を照射する紫外線光源を設けたので、該真空乾燥室内の細菌個数が従来よりも大幅に減少させることができて高クリーンで安全性が高まり、医薬品の凍結乾燥に好都合であり、長時間に亘る運転でもその個数が増大しないので滅菌作業の回数を減らせるから運転効率を高めることができ、生産コストも低下させ得、その製作も容易である等の効果があり、該乾燥室内に複数の紫外線光源を設け或いは反射装置を設けることにより該乾燥室内の暗部を少なくして形成された該薄膜を有効に光触媒作用を営ませ得られ、反射装置を設けることで構成が簡単になり安価に製作できる効果があり、また、該乾燥室が大気に開放されている時に光を集中的に照射すると更に滅菌効果を向上させることができる。
【図面の簡単な説明】
【図1】本発明の実施の形態を示す截断側面図
【図2】図1の2−2線部分の拡大断面図
【図3】本発明の他の実施の形態を示す截断側面図
【図4】従来例の截断側面図
【符号の説明】
1 真空乾燥室、3 真空排気装置、8 被乾燥物、14 薄膜、15 紫外線光源、16 反射鏡、
[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a freeze vacuum drying apparatus that freezes an object to be dried containing moisture such as foods and pharmaceuticals and evaporates and dries the moisture and solvent in a frozen state under vacuum.
[0002]
[Prior art]
Conventionally, as shown in FIG. 4, a freeze vacuum drying apparatus has a configuration in which a vacuum evacuation apparatus e having a cold trap c and a vacuum pump d is connected to a vacuum drying chamber b in which an object to be dried a is accommodated. In general, the inside of the drying chamber b is depressurized by the vacuum exhaust device e to freeze the material to be dried a, and then the drying chamber b is further evacuated by the vacuum exhaust device e. As a result, the frozen water is sublimated and dried. A shelf f that can be moved up and down and heated and cooled is provided in the vacuum drying chamber b, and the object to be dried a placed on the shelf f is heated during drying to promote sublimation. Has been done. When the material to be dried a is a medicine, the vial bottles filled with the chemical solution are arranged on the shelf f in the vacuum drying chamber b in a half-plugged state, and when the drying is finished, the vertical interval of the shelf f is set. After being moved so as to narrow, the bottle is stoppered, and then the door g is opened and taken out to the outside.
[0003]
Moreover, when an anatase-type crystal titanium oxide film is irradiated with ultraviolet light, the phenomenon (photocatalytic function) that decomposes the water adhering to the film and the active oxygen generated at that time decomposes the filth adhering to the film (photocatalytic function). And was found to have a function of killing bacteria.
[0004]
[Problems to be solved by the invention]
When the material to be dried a is a food or a medicine, in order to prevent the inside of the vacuum drying chamber b from being contaminated with bacteria, ethylene oxide gas (EOG) is allowed to flow into the drying chamber b, or Sterilization and sterilization are performed by flowing high-temperature steam and aseptic washing water. However, there is a safety concern regarding the EOG remaining in the drying chamber b, and in order to enable high temperature steam cleaning, it is necessary to provide the drying chamber b with pressure resistance, which makes the apparatus expensive. There is. In addition, these sterilization methods including washing with aseptic washing water are not preferable because the operation of the freeze-drying apparatus needs to be stopped and performed periodically, which reduces the operation efficiency of the apparatus.
[0005]
An object of the present invention is to provide a freeze vacuum drying apparatus that can maintain a vacuum drying chamber in a sterilized state for a long period of time, has high operating efficiency, and can be manufactured at low cost.
[0006]
[Means for Solving the Problems]
In the present invention, a vacuum drying chamber containing a material to be dried is evacuated by a vacuum evacuation device connected thereto, and the material to be dried is freeze-vacuum dried, the surface exposed to the chamber of the vacuum drying chamber The above-mentioned object is achieved by having a light source that covers a thin film of titanium oxide, irradiates the thin film and sterilizes it by photolysis , and a reflecting mirror whose surface is covered with a thin film of titanium oxide. I did it. Furthermore, it is preferable to have a shelf plate which is processed into a reflecting mirror surface and whose surface is covered with a thin film of titanium oxide. It is effective to use a light source that emits ultraviolet light having a wavelength of 400 nm or less as the ultraviolet light source.
[0007]
DETAILED DESCRIPTION OF THE INVENTION
The embodiment of the present invention will be described with reference to the drawings. In FIGS. 1 and 2, reference numeral 1 denotes a vacuum drying chamber provided with a plurality of shelves 2, and reference numeral 3 is connected to the vacuum drying chamber 1. An evacuation apparatus provided with a cold trap 4 and a vacuum pump 5 is shown. A refrigerant is circulated from the refrigerator 6 to the cold trap 4 so that mainly moisture in the drying chamber 1 is condensed and collected. On each shelf plate 2, an object to be dried 8 such as a chemical solution or food stored in a tray or a vial bottle 7 is placed. The object to be dried 8 is opened and removed by opening the door 1 a of the drying chamber 1. When the object to be dried 8 is stored in the vial 7, a sealing cylinder 9 provided above the drying chamber 1 is used. After the vial bottle 8 is capped in the drying chamber 1, it is taken out. 10 is an air compressor for operating the sealing cylinder 9, 11 is a melted water introduction pipe for melting ice condensed in the cold trap 4, 12 is a drain pipe for melted water, and 13 is connected to the sterile room through a sterile filter. This is an atmospheric introduction pipe.
[0008]
Such a configuration is not particularly different from the conventional freeze vacuum drying apparatus, and the inside of the drying chamber 1 containing the material to be dried 8 is decompressed by the vacuum pump 5 while operating the cold trap 4 at about −45 ° C. The dried product 8 is frozen, and the interior of the drying chamber 1 is further evacuated to a vacuum of about 6.7 Pa to sublimate the moisture in the frozen product to be dried 8 so that the drying is performed in the same manner as the conventional one. However, in the present invention, the surface exposed to the interior of the drying chamber 1 such as the inner wall and the shelf 2 is contaminated with bacteria, or the surface is covered with a titanium oxide thin film 14 in order to prevent dirt from remaining. The ultraviolet light source 15 was provided in the drying chamber 1.
[0009]
This will be further explained. A thin film 14 is formed by sintering titanium oxide on the inner surface of the drying chamber 1 and the surface of the shelf plate 2 made of stainless steel or mild steel. Four ultraviolet light sources 15 were provided so as not to cause dark portions. The thin film 14 had a thickness of about 1 to 3 microns, and the ultraviolet light source 15 used was irradiated with ultraviolet light having a wavelength of 400 nm or less. In the drying chamber 1, the operating portion of the sealing cylinder 9 and the like are present as internal components, and it is preferable to coat these with titanium oxide as much as possible. Further, instead of adding the light source 14, as shown in FIG. 3, a reflecting device in which the reflecting mirror 16 and the shelf board 2 are processed into a reflecting mirror surface may be provided to reduce the portion that tends to be a dark part. A thin film 14 is also formed on 16 and the reflecting mirror surface.
[0010]
A test piece with a titanium oxide thin film having the same thickness as that of the drying room is placed in the drying chamber 1, and live bacteria (MRSA, E. coli) are attached to the surface of the test piece so that the surface of the test piece becomes 1000 lux. When the ultraviolet light source 15 was irradiated for 1 hour, 99.9% of viable bacteria were sterilized. As for sterilization, water is decomposed on the surface of titanium oxide, and the action of active oxygen generated at that time is large, so that the drying chamber is opened to the atmosphere not only under vacuum but also when taking in and out dry matter. It was found that the sterilization effect was further increased by irradiating light intensively when the water content of the water was increased.
[0011]
【The invention's effect】
As described above, according to the present invention, the surface exposed in the vacuum drying chamber of the freeze vacuum drying apparatus is covered with a thin film of titanium oxide, and an ultraviolet light source for irradiating the thin film with ultraviolet rays is provided in the vacuum drying chamber. The number of bacteria in the vacuum drying chamber can be greatly reduced compared to the previous one, and it is highly clean and safe. Since the number of times can be reduced, the operation efficiency can be increased, the production cost can be reduced, and the production thereof is easy.Therefore, by providing a plurality of ultraviolet light sources or a reflection device in the drying chamber, The thin film formed by reducing the dark part in the drying chamber can be effectively operated for photocatalysis, and by providing a reflection device, the structure is simplified and can be manufactured at low cost. Drying chamber can be improved further sterilization effect when irradiated with light intensive when that is open to the atmosphere.
[Brief description of the drawings]
FIG. 1 is a cut-away side view showing an embodiment of the present invention. FIG. 2 is an enlarged cross-sectional view taken along line 2-2 in FIG. 1. FIG. 3 is a cut-away side view showing another embodiment of the invention. 4] Cutaway side view of conventional example [Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Vacuum drying chamber, 3 Vacuum exhaust apparatus, 8 To-be-dried object, 14 Thin film, 15 Ultraviolet light source, 16 Reflector,

Claims (4)

被乾燥物を収容した真空乾燥室内をこれに接続した真空排気装置により真空排気して該被乾燥物を凍結真空乾燥する装置であって
該真空乾燥室の室内に露出した表面を酸化チタンの薄膜で覆い、該薄膜を照射してこれに光分解による滅菌作用を行わせる光源と、表面が酸化チタンの薄膜で覆われた反射鏡とを設けたことを特徴とする凍結真空乾燥装置。
An apparatus for vacuum freeze drying該被dried product was evacuated by the vacuum evacuation device connected to a vacuum drying chamber containing the material to be dried thereto,
A light source for covering the surface exposed to the inside of the vacuum drying chamber with a thin film of titanium oxide, irradiating the thin film to effect sterilization by photolysis, a reflecting mirror having a surface covered with a thin film of titanium oxide; A freeze vacuum drying apparatus characterized by comprising:
さらに、反射鏡面に加工され、表面が酸化チタンの薄膜で覆われた棚板とを有することを特徴とする請求項1に記載の凍結真空乾燥装置。The freeze-drying apparatus according to claim 1, further comprising a shelf plate processed into a reflecting mirror surface and having a surface covered with a thin film of titanium oxide. 前記光源は、紫外線光源であり、前記光源が複数設けられていることを特徴とする請求項1または2に記載の凍結真空乾燥装置。The freeze-drying apparatus according to claim 1 or 2, wherein the light source is an ultraviolet light source, and a plurality of the light sources are provided. 上記光源400nm以下の波長の紫外光を照射することを特徴とする請求項1に記載の凍結真空乾燥装置。 The light source vacuum freeze-drying apparatus according to claim 1, wherein the irradiation with ultraviolet light having a wavelength of not more than 400 nm.
JP26508598A 1998-09-18 1998-09-18 Freeze vacuum dryer Expired - Fee Related JP3985241B2 (en)

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CN1938194B (en) * 2004-03-10 2013-06-05 希尔技术股份有限公司 Coated implants, their manufacturing and use thereof
KR101656700B1 (en) * 2015-05-19 2016-09-12 주식회사 일신바이오베이스 Freeze dryer

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EP0278039B1 (en) * 1987-02-13 1991-12-11 FINN-AQUA SANTASALO-SOHLBERG GmbH Freeze-drying apparatus
JPH09152268A (en) * 1995-11-30 1997-06-10 Liquid Gas:Kk Freeze dryer
JP3569837B2 (en) * 1996-01-18 2004-09-29 三菱電機株式会社 Tableware dryer

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