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JPH07138027A - Immersion apparatus for porous material - Google Patents

Immersion apparatus for porous material

Info

Publication number
JPH07138027A
JPH07138027A JP30729393A JP30729393A JPH07138027A JP H07138027 A JPH07138027 A JP H07138027A JP 30729393 A JP30729393 A JP 30729393A JP 30729393 A JP30729393 A JP 30729393A JP H07138027 A JPH07138027 A JP H07138027A
Authority
JP
Japan
Prior art keywords
liquid
porous body
solution
outer container
immersion
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP30729393A
Other languages
Japanese (ja)
Other versions
JP3352190B2 (en
Inventor
Yuko Kurasawa
祐子 倉澤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Olympus Corp
Original Assignee
Olympus Optical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Olympus Optical Co Ltd filed Critical Olympus Optical Co Ltd
Priority to JP30729393A priority Critical patent/JP3352190B2/en
Publication of JPH07138027A publication Critical patent/JPH07138027A/en
Priority to US08/867,043 priority patent/US6178780B1/en
Application granted granted Critical
Publication of JP3352190B2 publication Critical patent/JP3352190B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C23/00Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0095Solution impregnating; Solution doping; Molecular stuffing, e.g. of porous glass

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Melting And Manufacturing (AREA)

Abstract

PURPOSE:To safely and surely perform the immersion treatment of a porous material at a low cost without damaging the porous material. CONSTITUTION:A porous material 4 and a primary immersion solution 6 of an amount to immerse the whole porous material 4 are put into an outer vessel 5 and the porous material is immersed for an arbitrary period. The depth of the outer vessel 5 is larger than the height of the porous material 4. A liquid- discharging member 7 is inserted into the outer vessel 5. The primary immersion solution 6 is over-flowed through the gap between the liquid-discharging member 7 and the outer vessel 5. A secondary immersion solution 8 is poured into the vessel through a feeding port and, simultaneously with the pouring operation, the liquid discharging member 7 is pulled up from the immersion solution. The porous material 4 is immersed in the secondary immersion solution 8 without contacting with outer atmosphere by this process to complete the exchange of the solutions.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、例えば多孔質体を経由
してガラスを作製する方法において使用する、多孔質体
を液体に複数段階に浸漬するための浸漬装置に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a dipping device for immersing a porous body in a liquid in multiple stages, for example, for use in a method for producing glass via a porous body.

【0002】[0002]

【従来の技術】一般に、多孔質ガラス体を溶液に浸漬す
ることにより、多孔質細孔中に金属塩成分を導入する方
法(特開昭56−24307号公報)や、ゾルゲル法に
より細孔中に金属塩を溶解した溶液を含有している多孔
質ゲルを、金属塩の難溶性の溶媒に浸漬することによ
り、多孔質細孔中に金属塩の微結晶を析出する方法(特
開平3−295818号公報)などが知られている。ま
た、特開平3−295818号公報には、表面張力の低
い溶媒に浸漬した後、乾燥処理をすることで乾燥の際の
割れを防止する技術が開示されている。このように、多
孔質ガラス体、多孔質ゲル体等の多孔質体を複数の溶液
に順次浸漬していくことにより細孔中の溶媒系をかえて
いくことで種々の効果が得られている。
2. Description of the Related Art Generally, a method of introducing a metal salt component into porous pores by immersing a porous glass body in a solution (JP-A-56-24307) or a sol-gel method A method of precipitating fine crystals of a metal salt in porous pores by immersing a porous gel containing a solution in which a metal salt is dissolved in a solvent in which the metal salt is poorly soluble (JP-A-3- No. 295818) is known. Further, Japanese Patent Application Laid-Open No. 3-295818 discloses a technique for preventing cracks during drying by performing a drying process after immersing in a solvent having a low surface tension. Thus, various effects are obtained by changing the solvent system in the pores by sequentially immersing the porous body such as the porous glass body and the porous gel body in a plurality of solutions. .

【0003】ところで、従来、溶液中に浸漬した多孔質
体を次の浸漬溶液に漬けかえる方法としては、かご、ピ
ンセット等の治具を用いて溶液中からすくいあげ、次の
浸漬溶液が満たされた容器へ移す方法が一般的であっ
た。また、特開昭62−226832号公報には、図7
に示すように、下部に流入口1を、上部に排出口2を有
する容器3を用いて多孔質体4のリーチングを行う方法
が開示されている。
Conventionally, as a method of submerging a porous body immersed in a solution in the next immersion solution, the jig is scooped out of the solution using a jig such as a basket or tweezers, and the next immersion solution is filled. The method of transferring to a container was common. Moreover, in Japanese Patent Laid-Open No. 62-226832, FIG.
As shown in FIG. 3, a method of leaching the porous body 4 using a container 3 having an inflow port 1 in the lower part and a discharge port 2 in the upper part is disclosed.

【0004】[0004]

【発明が解決しようとする課題】しかし、上記従来の技
術では、多孔質体(多孔質ガラス体やゾルゲル法により
作製したゲル体)を多段階にわたって浸漬する場合、多
孔質体の取り扱い上、次のような問題点を有していた。
第1に、多孔質体を移動させる際に強い力が加わると、
多くの多孔質体は脆いために部分的にくずれたり、傷が
入ったりしやすい。したがって、多孔質体の移動時には
細心の注意が必要である。従来、治具としては、ピンセ
ット状あるいはそれに準ずるはさみ、またかご状のもの
を用いていたが、このようなものを用いて細心の注意を
払うことによっても、多孔質体破損の事故は減少こそす
れ避けられないものであった。
However, in the above conventional technique, when a porous body (a porous glass body or a gel body produced by the sol-gel method) is soaked in multiple stages, the following problems occur in handling the porous body. It had the following problems.
First, when a strong force is applied when moving the porous body,
Since many porous materials are brittle, they are easily broken or damaged. Therefore, great care must be taken when moving the porous body. Conventionally, as a jig, tweezers or similar scissors, or a basket-like jig was used, but even with the utmost care using such a jig, the accident of porous body damage can be reduced. It was unavoidable.

【0005】第2に、多孔質体を移動させて次の溶液に
移す際に、多孔質体を一旦溶液から取り出して次の溶液
に入れるが、多段階処理を行う多孔質体の細孔中は、ア
ルコールなどの溶液が満たされているため、その間に空
気中に出された多孔質体の細孔中の溶媒は急激に揮発
し、細孔中の溶液の表面張力により多孔質体に応力がか
かって亀裂が生じやすい。このような溶媒の急激な揮発
を防ぐためには、処理溶液槽の上方を溶媒が飽和した雰
囲気にしておくという方法も考えられるが、浸漬処理を
多段階行う場合にはこのような雰囲気制御は大変面倒
で、かつコストのかかるものとなる。
Secondly, when the porous body is moved to the next solution, the porous body is once taken out of the solution and put in the next solution. Is filled with a solution such as alcohol, the solvent in the pores of the porous body expelled in the air during that period volatilizes rapidly, and the surface tension of the solution in the pores causes stress on the porous body. It tends to get cracked. In order to prevent such abrupt volatilization of the solvent, it is conceivable to keep the atmosphere above the treatment solution tank saturated with the solvent. However, such an atmosphere control is very difficult when performing the dipping treatment in multiple stages. It is both tedious and costly.

【0006】以上のように、浸漬処理を多段階にわたっ
て行う場合、多孔質体を保持して移動させることに伴う
多孔質体へのダメージや、多孔質体移動中の溶媒揮発に
よるクラックを防止するための雰囲気制御の複雑さなど
が問題となっていた。多孔質体としては、分相熱処理、
酸溶出処理により製造した多孔質ガラス体や、ゾルゲル
法により作製された多孔質ゲル体などがあるが、特にゾ
ルゲル法により作製された多孔質ゲル体は、ゲル骨格が
弱く、クラックが生じやすいという問題を有していた。
As described above, when the immersion treatment is carried out in multiple stages, damage to the porous body caused by holding and moving the porous body and cracks due to solvent volatilization during movement of the porous body are prevented. However, the complexity of atmosphere control has been a problem. As the porous body, phase separation heat treatment,
There are porous glass bodies produced by acid elution treatment and porous gel bodies produced by the sol-gel method, but in particular, porous gel bodies produced by the sol-gel method have a weak gel skeleton and are prone to cracks. Had a problem.

【0007】一方、多孔質体を溶液から出さずに、例え
ば特開昭62−226832号公報に開示されているよ
うな装置(図7参照)を応用して、流入口1より送り込
む溶媒を変えて連続的に溶媒の混合比率を変えていく方
法もあるが、これでは溶媒は徐々にしか変えられず、ま
た2種の溶液が混合してしまうので、完全に次の溶液に
移すためには多量の溶媒が必要になり、高コストになる
という不便があった。
On the other hand, the solvent fed from the inflow port 1 is changed by applying an apparatus (see FIG. 7) as disclosed in, for example, Japanese Patent Laid-Open No. 62-226832 without taking out the porous body from the solution. There is also a method of continuously changing the mixing ratio of the solvent, but with this method the solvent can only be changed gradually, and since the two kinds of solutions mix, it is necessary to completely move to the next solution. There is an inconvenience that a large amount of solvent is required and the cost becomes high.

【0008】本発明は、かかる従来の問題点、すなわち
多孔質体を少なくとも2種の溶液に順次浸漬する工程に
おける、多孔質体の保持および移動に伴う多孔質体への
ダメージや、多孔質体移動中の雰囲気制御をするための
雰囲気制御の複雑さ、あるいは連続的に溶媒の混合比率
を変える方法による溶媒の多量消費等の問題点に鑑みて
なされたもので、多孔質体を破損することなく、安全確
実に低コストで浸漬処理することができる多孔質体の浸
漬装置を提供することを目的とする。
The present invention has the above-mentioned conventional problems, namely, damage to the porous body due to retention and movement of the porous body in the step of successively immersing the porous body in at least two kinds of solutions, and the porous body. It was made in view of the problems such as the complexity of atmosphere control for controlling the atmosphere during movement, or the large amount of solvent consumption due to the method of continuously changing the solvent mixing ratio, and the damage to the porous body. It is an object of the present invention to provide a dipping device for a porous body which can be safely, reliably, and inexpensively dipped.

【0009】[0009]

【課題を解決するための手段】上記課題を解決するため
に、請求項1に係る発明は、多孔質体を少なくとも2種
の液体に連続して順次浸漬する工程で用いられる浸漬装
置において、多孔質体を収納可能で多孔質体の高さより
も深い外容器と、外容器に対して相対的に上下動可能で
あり外容器内に挿入可能な液排出部材と、多孔質体を浸
漬する第1の液体の次に多孔質体を浸漬する第2の液体
を供給する供給口とを備えることとした。また、請求項
2に係る発明は、多孔質体を少なくとも2種の液体に連
続して順次浸漬する工程で用いられる浸漬装置におい
て、多孔質体を収納可能で多孔質体の高さよりも深い外
容器と、外容器内に位置して体積変化可能な液排出部材
と、多孔質体を浸漬する第1の液体の次に多孔質体を浸
漬する第2の液体を供給する供給口とを備えることとし
た。
In order to solve the above-mentioned problems, the invention according to claim 1 is a dipping device used in a step of successively dipping a porous body in at least two kinds of liquids, An outer container capable of accommodating a porous body and deeper than the height of the porous body, a liquid discharge member movable up and down relatively to the outer container and insertable into the outer container, and a first body for immersing the porous body A supply port for supplying a second liquid for immersing the porous body next to the first liquid is provided. The invention according to claim 2 is, in an immersion device used in a step of successively immersing the porous body in at least two kinds of liquids, is capable of accommodating the porous body and is deeper than the height of the porous body. A container, a liquid discharge member located inside the outer container and capable of changing volume, and a supply port for supplying a second liquid for immersing the porous body next to the first liquid for immersing the porous body I decided.

【0010】すなわち、請求項1に係る発明は、多孔質
体を少なくとも2種の液体に連続して順次浸漬する工程
で用いられる浸漬装置において、多孔質体を収納可能で
多孔質体の高さよりも深い外容器と、外容器に対して相
対的に上下動可能であり外容器に挿入可能な液排出部材
と、多孔質体を浸漬する第1の液体の次に多孔質体を浸
漬する第2の液体を供給する供給口とを有し、第1の液
体を満たした外容器内に多孔質体を置き液排出部材を外
容器に挿入した場合、第1の液体を外容器外に流出さ
せ、液排出部材を外容器から離脱した場合、供給口から
第2の液体を供給し、多孔質体を第1の液体と第2の液
体とに連続して順次浸漬することとした。
That is, according to the invention of claim 1, in a dipping device used in a step of successively dipping a porous body in at least two kinds of liquids, the porous body can be housed and the height of the porous body can be changed. A deep outer container, a liquid discharge member that can move up and down relatively to the outer container and can be inserted into the outer container, and a first liquid that dips the porous body next to the first liquid that dips the porous body. When the porous body is placed in the outer container filled with the first liquid and the liquid discharge member is inserted into the outer container, the first liquid flows out of the outer container. Then, when the liquid discharge member is detached from the outer container, the second liquid is supplied from the supply port, and the porous body is successively and successively dipped in the first liquid and the second liquid.

【0011】また、請求項2に係る発明は、多孔質体を
少なくとも2種の液体に連続して順次浸漬する工程で用
いられる浸漬装置において、多孔質体を収納可能で多孔
質体の高さよりも深い外容器と、外容器内に位置して体
積変化可能な液排出部材と、多孔質体を浸漬する第1の
液体の次に多孔質体を浸漬する第2の液体を供給する供
給口とを有し、第1の液体を満たした外容器内に多孔質
体を置き液排出部材の体積を増加させた場合、第1の液
体を外容器外に流出せさ、液排出部材の体積を減少させ
た場合、供給口から第2の液体を供給し、多孔質体を第
1の液体と第2の液体とに連続して順次浸漬することと
した。
Further, according to the invention of claim 2, in a dipping device used in the step of successively dipping the porous body in at least two kinds of liquids, the porous body can be housed and the height of the porous body can be changed. A deep outer container, a liquid discharge member located in the outer container and capable of changing the volume, and a supply port for supplying a second liquid for immersing the porous body next to the first liquid for immersing the porous body And the porous body is placed in an outer container filled with the first liquid to increase the volume of the liquid discharging member, the first liquid is caused to flow out of the outer container, and the volume of the liquid discharging member is increased. In the case of decreasing, the second liquid was supplied from the supply port, and the porous body was successively and successively dipped in the first liquid and the second liquid.

【0012】なお、本発明において、2種の溶液に浸漬
する場合とは、文字通り別個の「2種の」溶液に浸漬す
る場合の他、「1種の」溶液であっても、古くなった溶
液から新鮮な溶液に取り替える場合も含むものである。
In the present invention, the term "immersing in two kinds of solutions" means not only literally immersing in "two kinds of" solutions, but also "one kind of" solution is old. It also includes the case where the solution is replaced with a fresh solution.

【0013】また、上記請求項1または請求項2記載の
発明において、液排出部材の一部に溶液排出供給弁を設
けてもよい。さらに、外容器に溶液排出口を設け、第1
の液体の排出量を制御する排出量制御手段を備えてもよ
い。このように、溶液排出供給弁を設けた液排出部材を
用いた場合、液排出部材が外容器内に挿入されたときま
たは体積変化により体積が増加するとき、溶液排出供給
弁が開いて液排出部材内に第1の液体を取り込むとよ
い。また、溶液排出供給弁を設けた液排出部材を用いた
場合、液排出部材が外容器内に挿入されるときまたは体
積変化により体積が増加するとき、第2の液体が液排出
部材に注入されまたは注入されており、液排出部材の挿
入又は体積増加により外容器内の第1の液体が外容器外
に流出され、溶液排出供給弁が開いて液排出部材内の第
2の液体が外容器内に流出するように構成するとよい。
Further, in the invention described in claim 1 or claim 2, a solution discharge supply valve may be provided in a part of the liquid discharge member. Furthermore, a solution outlet is provided in the outer container to
A discharge amount control means for controlling the discharge amount of the liquid may be provided. As described above, when the liquid discharge member provided with the solution discharge supply valve is used, when the liquid discharge member is inserted into the outer container or when the volume increases due to the volume change, the solution discharge supply valve opens to discharge the liquid. The first liquid may be taken in the member. When the liquid discharge member provided with the solution discharge supply valve is used, the second liquid is injected into the liquid discharge member when the liquid discharge member is inserted into the outer container or when the volume increases due to the volume change. Alternatively, the first liquid in the outer container has been injected and the first liquid in the outer container has flowed out of the outer container due to the insertion or increase in volume of the liquid discharging member. It may be configured to flow into the inside.

【0014】[0014]

【作用】本発明の浸漬装置を用いて、多段階浸漬をする
際の作用を以下に説明する。はじめに、液排出部材と外
容器の少なくともいずれか一方を上下に駆動する装置を
有する場合の作用を以下に説明する。図1(a)に示し
たような有底円筒状の外容器5に多孔質体4と多孔質体
4全体が浸る程の1次浸漬溶液(第1の液体)6を入
れ、任意の時間浸漬する。外容器5は多孔質体4の高さ
よりも深く形成されている。所望の時間浸漬を行った
後、図1(b)に示すように、外容器5内に液排出部材
7を挿入し、1次浸漬溶液6に浸していく。ここで、液
排出部材7は、外径が外容器5の内径よりやや小さい円
柱状で、軸心部には多孔質体4の外径よりもやや大きな
径の貫通孔7aが形成されている。したがって、多孔質
体4を囲繞するようにして液排出部材7を1次浸漬溶液
6に浸していくことにより、外容器5の中の1次浸漬溶
液6は液排出部材7と外容器5の隙間から溢れ出る。図
1(c)は液排出部材7を最後(外容器5の底面)まで
挿入することにより、1次浸漬溶液6の排出を完了した
ところを示す図である。このような方法で1次浸漬溶液
6を排出すれば、1次浸漬溶液6の表面水位は外容器5
の上端より下がることはないので、多孔質体4は1次浸
漬溶液6の外にその表面をさらすことなく、浸漬処理す
ることができる。このとき、外容器5中には、多孔質体
4と液排出部材7および外容器5との各隙間にそれぞれ
若干の1次浸漬溶液6が存在しているが、ここへ図1
(d)に示すように、2次浸漬溶液(第2の液体)8を
供給口から注入し、同時に液排出部材7を引き上げて浸
漬溶液中から取り除いていくことにより、多孔質体4は
外気に触れることなく、2次浸漬溶液8に浸漬された状
態となる。以上のようにして、2次浸漬溶液8への溶液
交換が完結する(図1(e))。
The function of carrying out multi-step immersion using the immersion apparatus of the present invention will be described below. First, the operation when a device for vertically moving at least one of the liquid discharge member and the outer container is provided will be described below. The porous body 4 and the primary dipping solution (first liquid) 6 enough to immerse the entire porous body 4 in an outer container 5 having a cylindrical shape with a bottom as shown in FIG. Soak. The outer container 5 is formed deeper than the height of the porous body 4. After immersion for a desired time, as shown in FIG. 1B, the liquid discharge member 7 is inserted into the outer container 5 and immersed in the primary immersion solution 6. Here, the liquid discharge member 7 has a cylindrical shape having an outer diameter slightly smaller than the inner diameter of the outer container 5, and a through hole 7a having a diameter slightly larger than the outer diameter of the porous body 4 is formed in the shaft center portion. . Therefore, by immersing the liquid draining member 7 in the primary dipping solution 6 so as to surround the porous body 4, the primary dipping solution 6 in the outer container 5 is separated from the liquid draining member 7 and the outer container 5. It overflows from the gap. FIG. 1C is a diagram showing a state where the discharge of the primary dipping solution 6 is completed by inserting the liquid discharge member 7 to the end (bottom surface of the outer container 5). If the primary dipping solution 6 is discharged by such a method, the surface water level of the primary dipping solution 6 will be the outer container 5
Since it does not go below the upper end of the porous body 4, the porous body 4 can be immersed in the primary immersion solution 6 without exposing its surface. At this time, in the outer container 5, some primary dipping solution 6 is present in each of the gaps between the porous body 4, the liquid discharge member 7 and the outer container 5.
As shown in (d), the secondary immersion solution (second liquid) 8 is injected from the supply port, and at the same time, the liquid discharge member 7 is pulled up to remove it from the immersion solution. It is in a state of being immersed in the secondary immersion solution 8 without touching. As described above, the solution exchange to the secondary immersion solution 8 is completed (FIG. 1 (e)).

【0015】浸漬溶液を複数回交換するときにも同様に
して、(N−1)次浸漬溶液の入った外容器5に液排出
部材7を挿入して(N−1)次浸漬溶液を排出した後、
N次浸漬溶液を注入、液排出部材7を引き上げ除去する
操作を繰り返すことにより、N次浸漬溶液まで溶液を交
換することができる(Nは2以上の自然数)。
Similarly, when the immersion solution is exchanged a plurality of times, the liquid discharge member 7 is inserted into the outer container 5 containing the (N-1) -th subsequent immersion solution to discharge the (N-1) -th subsequent immersion solution. After doing
By repeating the operation of injecting the Nth-order immersion solution and pulling up and removing the liquid discharge member 7, the solution can be exchanged up to the Nth-order immersion solution (N is a natural number of 2 or more).

【0016】次に、体積可変の液排出部材を有する本発
明の浸漬装置を用いて多段階浸漬をする際の作用につい
て説明する。液排出部材中の空気や液体を抜き縮めた状
態で、浸漬溶液および多孔質体とともに外容器中に入れ
ておき、徐々にエアまたはN次浸漬溶液もしくは他の溶
液を液排出部材中に送り込んでいくことにより、液排出
部材は膨らんで(N−1)次浸漬溶液を追い出すに十分
な体積を獲得する。このようにして膨らませた液排出部
材は多孔質体の形状にフィットしやすいために、多孔質
体と液排出部材および外容器間の(N−1)次浸漬溶液
の残留量を最少にすることができる。また、フィットさ
せても液排出部材の内部が流体であるために無理な力が
局所的にかかることがなく、多孔質体を傷つけにくいと
いう効果もある。液排出部材を膨らませ、(N−1)次
浸漬溶液を排出した後,N次浸漬溶液の外容器への供給
と、液排出部材の液排出部材の中のエアや溶液の排出を
同時に行うことにより浸漬溶液の交換が完了する。
Next, a description will be given of the operation of multi-step immersion using the immersion apparatus of the present invention having a variable volume liquid discharge member. The air or liquid in the liquid discharging member is compressed and put in the outer container together with the immersion solution and the porous body, and the air or the Nth immersion solution or other solution is gradually fed into the liquid discharging member. As a result, the liquid discharge member swells and acquires a sufficient volume to expel the (N-1) th submersion solution. Since the liquid discharge member inflated in this way easily fits the shape of the porous body, the residual amount of the (N-1) th-order immersion solution between the porous body and the liquid discharge member and the outer container should be minimized. You can Further, even if fitted, since the inside of the liquid discharge member is a fluid, an unreasonable force is not locally applied, and there is an effect that it is difficult to damage the porous body. After inflating the liquid discharging member and discharging the (N-1) th immersion solution, simultaneously supplying the Nth immersion solution to the outer container and discharging the air or the solution in the liquid discharging member of the liquid discharging member. This completes the exchange of the immersion solution.

【0017】体積可変の液排出部材としては、上述のよ
うにエアや溶液を送り込んだときにもれることのない袋
状の部材や、蛇腹状の部材など種々の形状が考えられ
る。また、液体を吸収したときの膨潤率の大きな有機ポ
リマー多孔質体を使用することも可能である。外容器中
の浸漬溶液を排出する方法としては、浸漬溶液の液面を
多孔質体の最上面より下がらないようにすることが必要
であり、そのためには前述の方法のように外容器の深さ
を多孔質体の高さより深くしてもよいし、より好ましく
は、外容器に外容器外へ通じる少なくとも1つの通液口
を設けるとよい。この通液口の高さを多孔質体の浸漬時
の高さより高くしておけば、浸漬液面はその高さより低
くなることはない。また、複数の通液口を高さ方向に並
べて設け、これら複数の通液口をそれぞれ開閉自在とす
ることにより、様々な水位に適用することが可能にな
る。さらに、フロートスイッチや他の水位センサを用い
て浸漬溶液の液面が多孔質体上面より下がらないように
制御する方法をとれば、任意に液面を設定することがで
きる。
As the variable volume liquid discharging member, various shapes such as a bag-shaped member that does not leak when air or a solution is fed, a bellows-shaped member, and the like can be considered. It is also possible to use an organic polymer porous body having a large swelling rate when absorbing a liquid. As a method of discharging the immersion solution in the outer container, it is necessary to keep the liquid level of the immersion solution below the uppermost surface of the porous body. The depth may be deeper than the height of the porous body, and more preferably, the outer container may be provided with at least one liquid passage opening to the outside of the outer container. If the height of the liquid passage port is set higher than the height of the porous body at the time of immersion, the immersion liquid level will not be lower than the height. Further, by providing a plurality of liquid passage ports side by side in the height direction and opening and closing the plurality of liquid passage ports, it is possible to apply to various water levels. Furthermore, if a method is used to control the liquid level of the immersion solution so as not to fall below the upper surface of the porous body by using a float switch or another water level sensor, the liquid level can be set arbitrarily.

【0018】また、液排出部材は内部まで密なものであ
っても、中空であってもよく、液排出部材が中空である
ときには、液排出部材の中空部分から外容器へ通じる開
閉可能な溶液排出供給弁を設ければ、以下のように有効
に作用する。図2は、中空の液排出部材がその中空部分
から外容器へ通じる溶液排出供給弁を有する装置の一例
を示すものである。図2(a)に示したような外容器5
に多孔質体4と多孔質体4全体が浸る程の1次浸漬溶液
6を入れ、任意の時間浸漬を行った後、図2(b)に示
すように、中空の液排出部材7を挿入して1次浸漬溶液
6に浸していくことにより、外容器5の中の1次浸漬溶
液6は液排出部材7の底部の溶液排出供給弁9を通じて
液排出部材7の中空部へ移動する。図2(C)は液排出
部材7を最後まで挿入することにより、液排出部材7中
に1次浸漬溶液6の移動・排出が完了した状態を示す図
である。次に、図2(d)に示すように、溶液排出供給
弁9の弁を閉じ、液排出部材7を取り除いていくと同時
に外容器5中に2次浸漬溶液8を供給口から注入するこ
とにより、多孔質体4は外気に触れることなく、2次浸
漬溶液8に浸漬された状態となる。以上のようにして2
次浸漬溶液8への溶液交換が完結する(図2(e))。
The liquid discharging member may be dense or hollow inside, and when the liquid discharging member is hollow, an openable / closable solution leading from the hollow portion of the liquid discharging member to the outer container. If a discharge supply valve is provided, it works effectively as follows. FIG. 2 shows an example of an apparatus in which a hollow liquid discharge member has a solution discharge supply valve that communicates from its hollow portion to an outer container. The outer container 5 as shown in FIG.
Then, the porous body 4 and the primary dipping solution 6 to the extent that the entire porous body 4 is dipped are put therein, and after dipping for an arbitrary time, a hollow liquid discharge member 7 is inserted as shown in FIG. 2 (b). Then, by immersing in the primary dipping solution 6, the primary dipping solution 6 in the outer container 5 moves to the hollow portion of the liquid discharge member 7 through the solution discharge supply valve 9 at the bottom of the liquid discharge member 7. FIG. 2C is a diagram showing a state in which the movement / discharge of the primary immersion solution 6 in the liquid discharge member 7 is completed by inserting the liquid discharge member 7 to the end. Next, as shown in FIG. 2D, the solution discharge supply valve 9 is closed to remove the liquid discharge member 7, and at the same time, the secondary dipping solution 8 is injected into the outer container 5 from the supply port. As a result, the porous body 4 is in a state of being immersed in the secondary immersion solution 8 without touching the outside air. 2 as above
The solution exchange to the next immersion solution 8 is completed (FIG. 2 (e)).

【0019】このように、中空の液排出部材7が中空部
分から外容器5へ通じる溶液排出供給弁9を有する装置
の作用としては、上記のような、すなわち、液排出部材
7を外容器5内に挿入した際に該溶液排出供給弁9を通
じて第1の液体が液排出部材7内に流れ込み、結果とし
て外容器5内の第1の液体が排出されることとなるとい
う作用を有する。また、この他の作用として、第2の液
体を液排出部材7内に予め導入しておき、外容器5にあ
る第1の液体を排出後に液排出部材7内にある第2の液
体を溶液排出供給弁9を通じて外容器5に供給するとい
う作用をも有し、このような作用を有することから、液
排出部材7を外容器5に挿入した際に第1の液体を外容
器5外に排出させ、その後溶液排出供給弁9を通じて第
2の液体を外容器5に供給しながら、液排出部材7を引
き上げるという方法を採ることによっても、本発明の効
果を奏することができる。
As described above, the operation of the device in which the hollow liquid discharge member 7 has the solution discharge supply valve 9 communicating from the hollow portion to the outer container 5 is as described above, that is, the liquid discharge member 7 is connected to the outer container 5. When inserted into the inside, the first liquid flows into the liquid discharge member 7 through the solution discharge supply valve 9, and as a result, the first liquid in the outer container 5 is discharged. In addition, as another function, the second liquid is introduced into the liquid discharge member 7 in advance, and after the first liquid in the outer container 5 is discharged, the second liquid in the liquid discharge member 7 is dissolved. It also has a function of supplying the liquid to the outer container 5 through the discharge supply valve 9, and since it has such a function, when the liquid discharge member 7 is inserted into the outer container 5, the first liquid is discharged to the outside of the outer container 5. The effect of the present invention can also be obtained by adopting a method of discharging and then pulling up the liquid discharge member 7 while supplying the second liquid to the outer container 5 through the solution discharge supply valve 9.

【0020】また、液排出部材の外容器内における最大
時の総体積が、多孔質体を浸漬した浸漬液の容量の2分
の1以上であるときには、(N−1)次浸漬溶液を追い
出す効率がよく、多孔質体と液排出部材および外容器と
の隙間に存在する(N−1)次浸漬溶液が比較的少なく
なり、(N−1)次浸漬溶液を追い出す効率がよいため
に、効果的である。
Further, when the maximum total volume of the liquid discharge member in the outer container is ½ or more of the volume of the immersion liquid in which the porous body is immersed, the (N-1) th immersion liquid is expelled. Since the (N-1) th order immersion solution existing in the gap between the porous body, the liquid discharge member and the outer container is relatively small in efficiency and the (N-1) th order immersion solution is expelled efficiently, It is effective.

【0021】多孔質体と液排出部材および外容器との隙
間に存在する若干の(N−1)次浸漬溶液の影響をさら
に減らすためには、前述の溶媒交換工程中に以下のよう
な洗浄工程を設ける方法が有効である。洗浄工程とは、
(N−1)次浸漬溶液を適量排出した後に、N次浸漬溶
液を適量注入するとともに液排出部材を操作することに
より、(N−1)次浸漬溶液とN次浸漬溶液とを混合
し、(N−1)次浸漬溶液の比率を小さくした後、再度
液排出部材を操作し、この混合溶液を排出するというも
のである。この操作により(N−1)次浸漬溶液の残留
率は数1となる。
In order to further reduce the influence of a small amount of the (N-1) th order immersion solution existing in the gaps between the porous body, the liquid discharging member and the outer container, the following washing is performed during the solvent exchange step. A method of providing steps is effective. What is a cleaning process?
After discharging an appropriate amount of the (N-1) th immersion solution, by injecting an appropriate amount of the Nth immersion solution and operating the liquid discharge member, the (N-1) th immersion solution and the Nth immersion solution are mixed, (N-1) After reducing the ratio of the next immersion solution, the liquid discharging member is operated again to discharge the mixed solution. By this operation, the residual ratio of the (N-1) th order immersion solution becomes several 1.

【0022】[0022]

【数1】 [Equation 1]

【0023】この操作をX回繰り返すことにより残留率
はX乗で減少するので、(N−1)次浸漬溶液の量の影
響を減らすことができる。
By repeating this operation X times, the residual rate decreases with the Xth power, so that the influence of the amount of the (N-1) th order immersion solution can be reduced.

【0024】また、上下動させることにより、液排出部
材が多孔質体と接触したときにも多孔質体を傷つけたり
することのないようにするためには、液排出部材の多孔
質体側を面取りしたり、衝撃を吸収することのできる弾
性層を液排出部材に設けたりすることも有効である。弾
性層としては、気体または液体を含む流体層を液排出部
材と多孔質体との間に設けてもよいし、液体を含むこと
により膨潤するような有機ポリマー多孔質体材料を使用
することも可能である。
In order to prevent the liquid discharging member from being damaged even when the liquid discharging member comes into contact with the porous member by moving it up and down, the porous member side of the liquid discharging member is chamfered. It is also effective to provide the liquid discharging member with an elastic layer capable of absorbing shock. As the elastic layer, a fluid layer containing gas or liquid may be provided between the liquid discharge member and the porous body, or an organic polymer porous body material that swells by containing the liquid may be used. It is possible.

【0025】液排出部材と多孔質体との接触による事故
を防ぐためには、多孔質体が定位置からずれないように
外容器の側に多孔質体の移動を防ぐガイドを設けること
も有効な方法である。この移動防止ガイドは、浸漬液が
通りやすいように目の粗い網状のもので多孔質体を取り
囲むように設置してもよいし、多孔質体のまわりに細い
円柱状の棒を数本立てたり、リング状のものを用いるな
ど、ガイドの方法は種々考えられ、多孔質体の形状や一
度に処理する多孔質体の個数などに合わせて適切な方法
を用いるのが望ましい。なお、液排出部材が複数に分割
しているときにも同様な効果が得られる。
In order to prevent accidents due to contact between the liquid discharge member and the porous body, it is effective to provide a guide for preventing the porous body from moving on the side of the outer container so that the porous body is not displaced from its fixed position. Is the way. This movement prevention guide may be installed so as to surround the porous body with a coarse mesh so that the immersion liquid can easily pass through, or several thin cylindrical rods may be set around the porous body, Various guide methods are conceivable, such as using a ring-shaped one, and it is desirable to use an appropriate method depending on the shape of the porous body and the number of porous bodies to be treated at one time. The same effect can be obtained when the liquid discharge member is divided into a plurality of parts.

【0026】以上に示した浸漬装置を用いることによ
り、浸漬液を交換する際に多孔質体を破損することがな
くなった。特にゾルゲル法により作製された多孔質ゲル
体は、ゲル骨格が弱いために、従来は破損することが多
かったが、本発明の浸漬装置を用いることにより、破損
率が大幅に減少する。また、消費する浸漬液の量も図7
のタイプの従来の浸漬装置を使用したときと比較して格
段に少なくてすむため、コスト低減につながる。
By using the dipping device shown above, the porous body is not damaged when the dipping liquid is replaced. In particular, a porous gel body produced by the sol-gel method has often been damaged in the past due to its weak gel skeleton, but the use of the dipping device of the present invention greatly reduces the damage rate. The amount of immersion liquid consumed is also shown in FIG.
Since it requires significantly less amount as compared with the case of using the conventional dipping device of this type, the cost is reduced.

【0027】[0027]

【実施例1】図3に本実施例の装置の概略構成図を示
す。多孔質体4を収容する外容器5には、バルブ10を
有する溶液排出口11と、液排出部材7を上下動させる
駆動装置12を制御することにより液面をコントロール
するためのフロートスイッチ13とが配設されている。
フロートスイッチ13により、液面がある一定量より上
昇したときには自動的にバルブ10を開け、また一定量
より下にあるときはバルブ10を閉じるようにすること
により、外容器5の中の浸漬液を排出することができ
る。また、フロートスイッチ13は、N次浸漬溶液を注
入する際に、液面がある一定量より上昇したときに駆動
装置12に作用して液排出部材7を上昇させるスピード
をコントロールすることができるようになっている。
[Embodiment 1] FIG. 3 shows a schematic configuration diagram of an apparatus of this embodiment. The outer container 5 for accommodating the porous body 4 has a solution discharge port 11 having a valve 10 and a float switch 13 for controlling the liquid level by controlling a drive device 12 for vertically moving the liquid discharge member 7. Is provided.
The float switch 13 automatically opens the valve 10 when the liquid level rises above a certain amount, and closes the valve 10 when the liquid level is below a certain amount, so that the immersion liquid in the outer container 5 is closed. Can be discharged. Further, the float switch 13 can control the speed at which the liquid discharge member 7 is raised by acting on the drive device 12 when the liquid level rises above a certain amount when the Nth immersion solution is injected. It has become.

【0028】N次浸漬溶液14の供給はバルブ15を備
えた上方の容器16から行う。また外容器5内の浸漬溶
液全体の濃度、温度等の諸条件を均一に保つために、多
孔質体4の下方には攪拌装置17が配設されている。1
8はモータである。液排出部材7は外容器5内を上下動
できる範囲内でできるだけ外容器5に密着した大きさを
もつものがよい。液排出部材7には駆動装置12が接続
されており、液排出部材7を上下に動かすことができる
ようになっている。また、多孔質体4が液排出部材7の
下に移動してしまうと、液排出部材7を下降させたとき
に液排出部材7により押しつぶされてしまうので、多孔
質体7の移動を防ぐために多孔質体7を囲繞するガイド
19が設けられている。このため、液排出部材7の貫通
孔7aの径はガイド19の径よりも大径に形成されてい
る。
The Nth immersion solution 14 is supplied from an upper container 16 equipped with a valve 15. A stirring device 17 is provided below the porous body 4 in order to keep various conditions such as the concentration and temperature of the entire immersion solution in the outer container 5 uniform. 1
8 is a motor. It is preferable that the liquid discharge member 7 has a size that is in close contact with the outer container 5 as much as possible within a range where it can move up and down in the outer container 5. A drive device 12 is connected to the liquid discharge member 7 so that the liquid discharge member 7 can be moved up and down. If the porous body 4 moves below the liquid discharge member 7, it will be crushed by the liquid discharge member 7 when the liquid discharge member 7 is lowered. Therefore, in order to prevent the porous body 7 from moving. A guide 19 that surrounds the porous body 7 is provided. For this reason, the diameter of the through hole 7 a of the liquid discharge member 7 is formed to be larger than the diameter of the guide 19.

【0029】以上のような構成を有する浸漬装置を用い
て多段階浸漬を行う手順について以下に説明する。外容
器5の中に(N−1)次浸漬溶液20を注入し、その後
に多孔質体4をこの浸漬溶液20中に入れる。適当な時
間(N−1)次浸漬をしたのちに、液排出部材7を徐々
に浸漬溶液20中に降下させる。これにより、液排出部
材7の体積により浸漬溶液20の液面が上昇するために
フロートスイッチ13が作動し、バルブ10が開けら
れ、(N−1)次浸漬溶液20は溶液排出口11から排
出される。フロートスイッチ13は、多孔質体4の高さ
に応じて多孔質体4が液面より上に出ることのないよう
に予めセットしておくので、(N−1)次浸漬溶液20
の排出は浸漬液面が多孔質体4より上方位置にあるとこ
ろで終了する。次に、上方の容器16のバルブ15を開
き、液排出部材7の貫通孔7aを介して外容器5内にN
次浸漬溶液14を注入する。このN次浸漬溶液14の注
入に伴うフロートスイッチ13の作動により、液排出部
材7を徐々に上昇させていくことにより、多孔質体4の
浸漬溶液のN次浸漬溶液14への置換が完了する。
The procedure for carrying out multi-step immersion using the immersion apparatus having the above-mentioned structure will be described below. The (N-1) next immersion solution 20 is poured into the outer container 5, and then the porous body 4 is put into this immersion solution 20. After submergence for an appropriate time (N-1), the liquid discharging member 7 is gradually lowered into the dipping solution 20. As a result, the liquid level of the immersion solution 20 rises due to the volume of the liquid discharge member 7, the float switch 13 is actuated, the valve 10 is opened, and the (N−1) th next immersion solution 20 is discharged from the solution discharge port 11. To be done. Since the float switch 13 is set in advance so that the porous body 4 does not come out above the liquid surface according to the height of the porous body 4, the (N-1) th immersion solution 20
Is finished when the immersion liquid surface is located above the porous body 4. Next, the valve 15 of the upper container 16 is opened, and N is put into the outer container 5 through the through hole 7a of the liquid discharge member 7.
The next immersion solution 14 is injected. By the operation of the float switch 13 associated with the injection of the Nth-order immersion solution 14, the liquid discharge member 7 is gradually raised to complete the replacement of the immersion solution of the porous body 4 with the Nth-order immersion solution 14. .

【0030】以上の全工程において、多孔質体4を移動
させることなく、また多孔質体4を空気中にさらすこと
なく、浸漬溶液の交換ができるので、操作中に多孔質体
4が割れたりすることがなくなった。すなわち、本実施
例の浸漬装置は、浸漬処理において多孔質体4を破損す
ることなく、安全確実に低コストで処理することができ
た。
In all of the above steps, the immersion solution can be exchanged without moving the porous body 4 or exposing the porous body 4 to the air, so that the porous body 4 may break during the operation. There is nothing to do. That is, the dipping device of the present example was able to safely and reliably perform the treatment at low cost without damaging the porous body 4 during the dipping treatment.

【0031】[0031]

【実施例2】図4に本実施例の装置の概略構成図を示
す。図4において、図3に示す装置と同一構成部分につ
いては同一符号をもって示し、その説明は省略する。な
お、図示は省略したが、本実施例においても外容器5内
の浸漬液全体を均一に保つために攪拌装置が配設されて
いる。本実施例では、液排出部材21の体積が可変であ
ることを特徴とする。液排出部材21は、厚さ0.15
mmのテフロン製でエアを送り込むことができる少なく
とも1箇所の注入口22をもち、この注入口22に接続
されたポンプ23によりエアの送り込みと吸い出しを行
うことができ、膨らんだり縮んだりして体積が変化する
ように構成されている。
[Embodiment 2] FIG. 4 shows a schematic configuration diagram of an apparatus of this embodiment. 4, parts that are the same as the parts shown in FIG. 3 are given the same reference numerals, and descriptions thereof will be omitted. Although not shown, a stirring device is also provided in this embodiment to keep the entire immersion liquid in the outer container 5 uniform. The present embodiment is characterized in that the volume of the liquid discharge member 21 is variable. The liquid discharge member 21 has a thickness of 0.15.
It is made of Teflon and has at least one injection port 22 through which air can be sent, and a pump 23 connected to this injection port 22 can send and suck air, and can be inflated or contracted to create a volume. Are configured to change.

【0032】以上のような構成を有する浸漬装置を用い
て多段階浸漬を行う手順について以下に説明する。外容
器5中に(N−1)次浸漬溶液20を注入し、その後に
多孔質体4をこの浸漬溶液20中に入れる。適当な時間
(N−1)次浸漬をした後に、液排出部材21にエアを
送り込むことにより徐々にバックを膨らませる。これに
より、浸漬溶液面が上昇してフロートスイッチ13が作
動し、バルブ10が開けられ、(N−1)次浸漬溶液2
0は溶液排出口11から排出される。前記実施例1と同
様に、フロートスイッチ13は、多孔質体4の高さに応
じて多孔質体4が液面より上に出ることのないように予
めセットしておくので、(N−1)次浸漬溶液20の排
出は浸漬液面が多孔質体4より上方位置にあるところで
終了する。次に、上方の容器16のバルブ15を開いて
N次浸漬溶液14を外容器5内に注入する。N次浸漬溶
液14の注入が終了したら、同時に液排出部材21中の
エアを抜く。ここに、エアを抜いたあとの液排出部材2
1はN次浸漬溶液14から出してもよいし、出さずに液
中に入れておくことも問題なく可能である。これによ
り、多孔質体の浸漬溶液のN次浸漬溶液14への置換が
完了する。
The procedure for carrying out multi-step immersion using the immersion apparatus having the above-mentioned structure will be described below. The (N-1) next immersion solution 20 is poured into the outer container 5, and then the porous body 4 is placed in this immersion solution 20. After submergence for an appropriate time (N-1), air is sent to the liquid discharge member 21 to gradually inflate the bag. As a result, the surface of the immersion solution rises, the float switch 13 operates, the valve 10 is opened, and the (N-1) next immersion solution 2
0 is discharged from the solution discharge port 11. Similar to the first embodiment, the float switch 13 is set in advance so that the porous body 4 does not rise above the liquid surface depending on the height of the porous body 4, so that (N-1 ) The discharge of the next immersion solution 20 ends when the immersion liquid surface is located above the porous body 4. Next, the valve 15 of the upper container 16 is opened to inject the Nth order immersion solution 14 into the outer container 5. When the injection of the Nth immersion solution 14 is completed, the air in the liquid discharge member 21 is simultaneously evacuated. Liquid discharge member 2 after bleeding air here
1 may be taken out from the Nth-order immersion solution 14 or may be put in the solution without being taken out without any problem. This completes the replacement of the immersion solution of the porous body with the Nth order immersion solution 14.

【0033】以上の全工程において、多孔質体4を移動
させることなく、また多孔質体4を空気中にさらすこと
なく、浸漬溶液の交換ができるので、操作中に多孔質体
4が割れたりすることがなくなった。また、エアを導入
する具合により、多孔質体4と液排出部材21の接触の
度合いを加減することができ、実施例1で用いた液排出
部材7と比較して、多孔質体4に密着させることができ
るので、(N−1)次浸漬溶液20の持ち越し量を少な
くすることができ、効率のよい溶液交換が可能となる。
すなわち、本実施例の装置も実施例1と同様に、浸漬処
理において多孔質体4を破損することなく、安全確実に
低コストで処理することができた。
In all of the above steps, the immersion solution can be exchanged without moving the porous body 4 and without exposing the porous body 4 to the air, so that the porous body 4 may break during the operation. There is nothing to do. Further, the degree of contact between the porous body 4 and the liquid discharge member 21 can be adjusted depending on how air is introduced, and compared with the liquid discharge member 7 used in Example 1, the porous body 4 can be closely attached. Since it can be carried out, the carry-over amount of the (N-1) next immersion solution 20 can be reduced, and efficient solution exchange becomes possible.
That is, also in the apparatus of this example, as in Example 1, the porous body 4 could be safely and reliably processed at low cost without damaging the porous body 4 during the immersion process.

【0034】[0034]

【実施例3】図5に本実施例の装置の概略構成図を示
す。図5において、図3に示す装置と同一構成部分につ
いては同一符号をもって示し、その説明は省略する。本
実施例は、N次浸漬溶液14を注入した液排出部材7を
用いて、(N−1)次浸漬溶液20の追い出しを行うこ
とを特徴とする。液排出部材7の底面には、液排出部材
7中に導入しておいたN次浸漬溶液14を放出し、外容
器5中へ移すための開閉自在な溶液排出供給弁9が付設
されている。溶液排出供給弁9を閉じた状態で液排出部
材7中にN次浸漬溶液14を注入し、この液排出部材7
を下降させて実施例1と同様にして(N−1)次浸漬溶
液20を排出した後、溶液排出供給弁9を開け、開けた
まま液排出部材7をゆっくりと引き上げることにより、
液排出部材7中のN次浸漬溶液14が外容器5中へ移動
するので、液排出部材7の引き上げが終了すると浸漬溶
液の交換も終了する。
[Embodiment 3] FIG. 5 shows a schematic configuration diagram of an apparatus of the present embodiment. 5, parts that are the same as the parts shown in FIG. 3 are given the same reference numerals, and descriptions thereof will be omitted. This embodiment is characterized in that the (N-1) th order immersion solution 20 is expelled by using the liquid discharge member 7 into which the Nth order immersion solution 14 is injected. The bottom surface of the liquid discharge member 7 is provided with an openable and closable solution discharge supply valve 9 for discharging the Nth order immersion solution 14 introduced into the liquid discharge member 7 and transferring it into the outer container 5. . The Nth dipping solution 14 is injected into the liquid discharging member 7 with the solution discharging supply valve 9 closed, and the liquid discharging member 7
Is discharged to discharge the (N-1) next immersion solution 20 in the same manner as in Example 1, the solution discharge supply valve 9 is opened, and the liquid discharge member 7 is slowly pulled up with the solution discharge supply valve 9 opened.
Since the Nth order immersion solution 14 in the liquid discharging member 7 moves into the outer container 5, the replacement of the immersion solution is completed when the lifting of the liquid discharging member 7 is completed.

【0035】以上の全工程において、多孔質体4を移動
させることなく、また多孔質体4を空気中にさらすこと
なく、浸漬溶液の交換ができるので、処理操作中に多孔
質体4が割れたりすることがなくなった。すなわち、本
実施例の装置も、浸漬処理において多孔質体4を破損す
ることなく、安全確実に低コストで処理することができ
た。
In all the above steps, the immersion solution can be exchanged without moving the porous body 4 and without exposing the porous body 4 to the air, so that the porous body 4 is broken during the treatment operation. There is no longer any. That is, also in the apparatus of this example, the porous body 4 could be safely and reliably processed at low cost without being damaged in the immersion process.

【0036】[0036]

【実施例4】図6に本実施例の装置の概略構成図を示
す。図6において図4と同一部分については同一符号を
もって示し、その説明は省略する。多孔質体4を収容す
る外容器5には、収容した多孔質体4の上面高さよりも
高い位置に溶液排出口24が配設されており、図示は省
略したが、外容器5内の浸漬液全体を均一に保つために
攪拌装置が配設されている。本実施例は、体積可変の液
排出部材21中に、N次浸漬溶液14を注入して(N−
1)次浸漬溶液20の追い出しを行うことを特徴とす
る。液排出部材21中の液を外容器5中へ放出するため
に開閉可能な溶液排出供給弁25を形成し、また液排出
部材21へN次浸漬溶液14を送り込むことができるよ
うにN次浸漬溶液14を供給する容器23と液排出部材
21との間にポンプ26を介装して、体積可変の液排出
部材21により浸漬溶液の交換を行うものである。すな
わち、このポンプ26を用いて液排出部材21中へN次
浸漬溶液14を送り込むことにより液排出部材21を膨
らませ、実施例2と同様にして溶液排出口24から(N
−1)次浸漬溶液20を排出した後、液排出部材21の
溶液排出供給弁25を開け、開けたままの状態で液排出
部材21をゆっくりと引き上げることにより、液排出部
材21中のN次浸漬溶液14を外容器5中へ移動させ
る。これにより、液排出部材21の引き上げが終了する
と浸漬溶液の交換も終了する。
[Embodiment 4] FIG. 6 shows a schematic configuration diagram of an apparatus of this embodiment. 6, the same parts as those in FIG. 4 are designated by the same reference numerals, and the description thereof will be omitted. The outer container 5 that houses the porous body 4 is provided with the solution discharge port 24 at a position higher than the height of the upper surface of the housed porous body 4, and although not shown in the drawing, the immersion in the outer container 5 is omitted. A stirrer is provided to keep the whole liquid uniform. In this embodiment, the Nth order immersion solution 14 is injected into the volume variable liquid discharge member 21 (N-
1) It is characterized in that the next immersion solution 20 is expelled. A solution discharge supply valve 25 that can be opened and closed is formed to discharge the liquid in the liquid discharge member 21 into the outer container 5, and the Nth order immersion is performed so that the Nth order immersion solution 14 can be sent to the liquid discharge member 21. The pump 26 is interposed between the container 23 for supplying the solution 14 and the liquid discharging member 21, and the immersion liquid is exchanged by the liquid discharging member 21 having a variable volume. That is, the pump 26 is used to send the Nth order immersion solution 14 into the liquid discharging member 21 to inflate the liquid discharging member 21, and in the same manner as the second embodiment, the solution discharging port 24 (N
-1) After discharging the next dipping solution 20, the solution discharge supply valve 25 of the liquid discharge member 21 is opened, and the liquid discharge member 21 is slowly pulled up in the opened state, whereby the Nth order in the liquid discharge member 21 is discharged. The immersion solution 14 is moved into the outer container 5. As a result, when the lifting of the liquid discharge member 21 is completed, the exchange of the immersion solution is also completed.

【0037】以上の全工程において、多孔質体4を移動
させることなく、また多孔質体4を空気中にさらすこと
なく、浸漬溶液の交換ができるので、処理操作中に多孔
質体4が割れたりすることがなくなった。すなわり、本
実施例の装置も、浸漬処理において多孔質体4を破損す
ることなく、安全確実に低コストで処理することができ
た。
In all of the above steps, the immersion solution can be exchanged without moving the porous body 4 and without exposing the porous body 4 to the air, so that the porous body 4 is cracked during the treatment operation. There is no longer any. In other words, the apparatus of the present embodiment was also able to perform the treatment safely, reliably and at low cost without damaging the porous body 4 during the dipping treatment.

【0038】以上に示した方法では、液排出部材7の上
下動あるいは液排出部材21の体積変化とともに浸漬溶
液の排出を行っているが、これらの方法を組み合わせて
用いたときにも優れた効果を発揮することは勿論であ
る。
In the method described above, the immersion solution is discharged as the liquid discharging member 7 moves up and down or the volume of the liquid discharging member 21 changes. However, excellent effects are obtained when these methods are used in combination. Needless to say,

【0039】[0039]

【発明の効果】以上のように、本発明の多孔質体の浸漬
装置によれば、多孔質体を経由して機能性ガラス等を作
製する方法において、浸漬処理を多段階にわたって行う
際の溶液交換に伴う多孔質体へのダメージを最小限にと
どめ、浸漬処理において多孔質体を安全確実に低コスト
で処理することができる。
As described above, according to the apparatus for immersing a porous body of the present invention, in a method for producing a functional glass or the like via a porous body, a solution for performing the dipping treatment in multiple stages. The damage to the porous body due to the replacement can be minimized, and the porous body can be safely and reliably processed at low cost in the dipping treatment.

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明の浸漬装置を用いた浸漬処理工程を示す
工程図である。
FIG. 1 is a process diagram showing an immersion treatment process using an immersion device of the present invention.

【図2】本発明の他の浸漬装置を用いた浸漬処理工程を
示す工程図である。
FIG. 2 is a process drawing showing a dipping treatment process using another dipping device of the present invention.

【図3】本発明の実施例1の浸漬装置を示す概略構成図
である。
FIG. 3 is a schematic configuration diagram showing an immersion device according to a first embodiment of the present invention.

【図4】本発明の実施例2の浸漬装置を示す概略構成図
である。
FIG. 4 is a schematic configuration diagram showing an immersion device according to a second embodiment of the present invention.

【図5】本発明の実施例3の浸漬装置を示す概略構成図
である。
FIG. 5 is a schematic configuration diagram showing an immersion device according to a third embodiment of the present invention.

【図6】本発明の実施例4の浸漬装置を示す概略構成図
である。
FIG. 6 is a schematic configuration diagram showing an immersion device according to a fourth embodiment of the present invention.

【図7】従来の浸漬装置を示す縦断面図である。FIG. 7 is a vertical sectional view showing a conventional dipping device.

【符号の説明】[Explanation of symbols]

4 多孔質体 5 外容器 6 1次浸漬溶液 7,21 液排出部材 8 2次浸漬溶液 9,25 溶液排出供給弁 11,24 溶液排出口 14 N次浸漬溶液 19 ガイド 20 (N−1)次浸漬溶液 4 Porous Body 5 Outer Container 6 Primary Immersion Solution 7,21 Liquid Discharge Member 8 Secondary Immersion Solution 9,25 Solution Discharge Supply Valve 11,24 Solution Discharge Port 14 Nth Immersion Solution 19 Guide 20 (N-1) Next Immersion solution

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】 多孔質体を少なくとも2種の液体に連続
して順次浸漬する工程で用いられる浸漬装置において、
多孔質体を収納可能で多孔質体の高さよりも深い外容器
と、外容器に対して相対的に上下動可能であり外容器内
に挿入可能な液排出部材と、多孔質体を浸漬する第1の
液体の次に多孔質体を浸漬する第2の液体を供給する供
給口とを有し、第1の液体を満たした外容器内に多孔質
体を置き液排出部材を外容器に挿入した場合、第1の液
体を外容器外に流出させ、液排出部材を外容器から離脱
した場合、供給口から第2の液体を供給し、多孔質体を
第1の液体と第2の液体とに連続して順次浸漬すること
となる多孔質体の浸漬装置。
1. A dipping device used in a step of successively dipping a porous body in at least two kinds of liquids,
An outer container capable of accommodating a porous body and deeper than the height of the porous body, a liquid discharge member that can be moved up and down relative to the outer container and can be inserted into the outer container, and the porous body is immersed. A first liquid and a supply port for supplying a second liquid into which the porous body is immersed, and the porous body is placed in an outer container filled with the first liquid, and the liquid discharge member is used as the outer container. When inserted, the first liquid is caused to flow out of the outer container, and when the liquid discharge member is detached from the outer container, the second liquid is supplied from the supply port, and the porous body is separated into the first liquid and the second liquid. A device for immersing a porous body that is successively immersed in a liquid.
【請求項2】 多孔質体を少なくとも2種の液体に連続
して順次浸漬する工程で用いられる浸漬装置において、
多孔質体を収納可能で多孔質体の高さよりも深い外容器
と、外容器内に位置して体積変化可能な液排出部材と、
多孔質体を浸漬する第1の液体の次に多孔質体を浸漬す
る第2の液体を供給する供給口とを有し、第1の液体を
満たした外容器内に多孔質体を置き液排出部材の体積を
増加させた場合、第1の液体を外容器外に流出せさ、液
排出部材の体積を減少させた場合、供給口から第2の液
体を供給し、多孔質体を第1の液体と第2の液体とに連
続して順次浸漬することとなる多孔質体の浸漬装置。
2. A dipping device used in a step of successively dipping a porous body in at least two kinds of liquids,
An outer container capable of accommodating a porous body and deeper than the height of the porous body, and a liquid discharging member located in the outer container and capable of changing volume,
A first liquid for immersing the porous body, and a supply port for supplying a second liquid for immersing the porous body next, and the porous body is placed in an outer container filled with the first liquid. When the volume of the discharge member is increased, the first liquid is caused to flow out of the outer container, and when the volume of the liquid discharge member is decreased, the second liquid is supplied from the supply port to set the porous body to the first position. An apparatus for immersing a porous body which is successively and successively dipped in the first liquid and the second liquid.
JP30729393A 1993-11-12 1993-11-12 Immersion device for porous material Expired - Fee Related JP3352190B2 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP30729393A JP3352190B2 (en) 1993-11-12 1993-11-12 Immersion device for porous material
US08/867,043 US6178780B1 (en) 1993-11-12 1997-06-02 Method of solution doping a sol gel body via immersion

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP30729393A JP3352190B2 (en) 1993-11-12 1993-11-12 Immersion device for porous material

Publications (2)

Publication Number Publication Date
JPH07138027A true JPH07138027A (en) 1995-05-30
JP3352190B2 JP3352190B2 (en) 2002-12-03

Family

ID=17967396

Family Applications (1)

Application Number Title Priority Date Filing Date
JP30729393A Expired - Fee Related JP3352190B2 (en) 1993-11-12 1993-11-12 Immersion device for porous material

Country Status (1)

Country Link
JP (1) JP3352190B2 (en)

Also Published As

Publication number Publication date
JP3352190B2 (en) 2002-12-03

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