JP2010242884A - Method of washing vessel valve and washing agent - Google Patents

Method of washing vessel valve and washing agent Download PDF

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JP2010242884A
JP2010242884A JP2009093064A JP2009093064A JP2010242884A JP 2010242884 A JP2010242884 A JP 2010242884A JP 2009093064 A JP2009093064 A JP 2009093064A JP 2009093064 A JP2009093064 A JP 2009093064A JP 2010242884 A JP2010242884 A JP 2010242884A
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hydrogen chloride
container
container valve
washing
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JP5347666B2 (en
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Masahide Tomaru
雅英 登丸
Hiroyuki Akashi
博行 明石
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Tsurumi Soda Co Ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E60/30—Hydrogen technology
    • Y02E60/32—Hydrogen storage

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Abstract

<P>PROBLEM TO BE SOLVED: To provide washing method of a vessel valve and a washing agent, which grasp an end point easily in the case of washing the vessel valve which is attached to a liquefied hydrogen chloride gas vessel. <P>SOLUTION: In the method of washing the vessel valve 10 attached to a high pressure gas vessel G which fills liquefied hydrogen chloride gas, a nozzle 53 of a washing tool 5 is disposed on a gas output port 15 and aqueous ammonia 6 is supplied from the nozzle 53 in such a condition as to close an opening of a gas flow passage 17 by a plug 13. Ammonia and hydrogen chloride react by means of supply of the aqueous ammonia 6, and thereby white smoke S of ammonium chloride is generated from the gas output port 15. After then, the supply of the aqueous ammonia 6 is stopped when the generation of the white smoke S is stopped. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

本発明は、液化塩化水素ガスを充填する高圧ガス容器に装着された容器弁を洗浄する方法に関する。   The present invention relates to a method for cleaning a container valve attached to a high-pressure gas container filled with liquefied hydrogen chloride gas.

半導体製造プロセス等においては、ハロゲン系液化ガスの一種である無水塩化水素（ＨＣｌ）が使用されており、この無水塩化水素（ＨＣｌ）は例えば鉄製の高圧ガス容器に充填されている。図３に示すように前記高圧ガス容器Ｇの開口部には、例えばステンレス製の容器弁１０が装着されている。当該容器弁１０は、容器弁本体１１と容器弁本体１１の上部側に形成されたシリンダ部１２内に螺合して設けられたプラグ１３とこのプラグ１３の上端部にスピンドル１９を介して取り付けられたハンドル１４とを備えている。また、図４にも示すようにプラグ１３の下端部には三フッ化塩化エチレン樹脂よりなるシートディスク１８が設けられている。前記容器弁本体１１の側面側には、高圧ガス容器Ｇ内のガスを取出すためのガス取出し口１５が形成されており、このガス取出し口１５にはアウトレットキャップ１６が配設されている。   In semiconductor manufacturing processes and the like, anhydrous hydrogen chloride (HCl), which is a kind of halogen-based liquefied gas, is used, and this anhydrous hydrogen chloride (HCl) is filled in a high-pressure gas container made of, for example, iron. As shown in FIG. 3, for example, a stainless steel container valve 10 is attached to the opening of the high-pressure gas container G. The container valve 10 is attached via a spindle 19 to a container valve body 11 and a plug 13 screwed into a cylinder portion 12 formed on the upper side of the container valve body 11 and an upper end portion of the plug 13. The handle 14 is provided. Further, as shown in FIG. 4, a sheet disk 18 made of ethylene trifluoride chloride resin is provided at the lower end portion of the plug 13. A gas outlet 15 for taking out gas from the high-pressure gas container G is formed on the side surface of the container valve main body 11, and an outlet cap 16 is disposed in the gas outlet 15.

また、容器弁本体１１の下部側には、その一端側が高圧ガス容器Ｇ内に開口するガス流路１７が形成されており、ハンドル１４を介してプラグ１３を上下動させることで前記ガス流路１７の他端側の開口部の開閉を行うことが可能である。即ち、高圧ガス容器Ｇ内のガスを使用する際には、前記プラグ１３を上昇させてガス流路１７の他端側の開口部を開けることで、前記ガスはガス流路１７を通ってガス取出し口１５から外部に取出されることになる。また、高圧ガス容器Ｇ内のガスの使用を停止する際には、前記プラグ１３を下降させてガス流路１７の他端側の開口部を閉じ、このときプラグ１３の下端部に形成されたシートディスク１８によってガス流路１７の開口部が密閉されることになる。   In addition, a gas flow path 17 having one end opened into the high-pressure gas container G is formed on the lower side of the container valve body 11, and the gas flow path can be moved by moving the plug 13 up and down via a handle 14. It is possible to open and close the opening on the other end side of 17. That is, when using the gas in the high-pressure gas container G, the plug 13 is raised to open the opening on the other end side of the gas flow path 17, so that the gas passes through the gas flow path 17. It is taken out from the take-out port 15 to the outside. When the use of the gas in the high-pressure gas container G is stopped, the plug 13 is lowered to close the opening on the other end side of the gas flow path 17. At this time, the plug 13 is formed at the lower end of the plug 13. The opening of the gas flow path 17 is sealed by the seat disk 18.

このような高圧ガス容器Ｇに液化塩化水素を充填する際には、以下に述べる問題がある。即ち、プラグ１３の下部側周面及び底面（シートディスク１８の周囲部分）に付着している液化塩化水素が外気の温度変化によって気化し、アウトレットキャップ１６の内側空間に充満し、ユーザが当該アウトレットキャップ１６をガス取出し口１５から外すと、ガス取出し口１５から塩化水素ガスが放出され、高圧ガス容器Ｇ内から塩化水素ガスが漏洩しているのか否か判断ができず、高圧ガス容器Ｇを再度点検しなければならない。   When such a high-pressure gas container G is filled with liquefied hydrogen chloride, there are the following problems. That is, the liquefied hydrogen chloride adhering to the lower peripheral surface and the bottom surface (the peripheral portion of the seat disk 18) of the plug 13 is vaporized by the temperature change of the outside air and fills the inner space of the outlet cap 16, and the user can When the cap 16 is removed from the gas outlet 15, hydrogen chloride gas is released from the gas outlet 15, and it cannot be determined whether or not hydrogen chloride gas is leaking from the high pressure gas container G. You must check again.

また、アウトレットキャップ１６をガス取出し口１５に取り付ける際に、容器弁１０内が大気中に晒されることから、容器弁１０内に付着している液化塩化水素が大気中の水分を吸収して塩酸となる。このため、その後アウトレットキャップ１６が閉じられてメーカー側に回収されるまで長時間経過すると、この塩酸により容器弁１０内のプラグ１３等の部品が腐食し、容器弁１０の使用寿命が短くなるといった問題である。   Further, since the inside of the container valve 10 is exposed to the atmosphere when the outlet cap 16 is attached to the gas outlet 15, the liquefied hydrogen chloride adhering to the container valve 10 absorbs the moisture in the atmosphere and hydrochloric acid. It becomes. For this reason, after a long time has passed until the outlet cap 16 is closed and then collected by the manufacturer, the hydrochloric acid corrodes parts such as the plug 13 in the container valve 10 and shortens the service life of the container valve 10. It is a problem.

これらの問題を解決するために特許文献１に開示されているように、噴射剤例えば加圧ガスを発生する液化ガスであるジメチルエーテル（ＤＭＥ）と有機溶剤例えばイソプロピルアルコール（ＩＰＡ）との混合物を洗浄剤として収納した洗浄具より図５に示すようにノズル５３を介して当該洗浄剤をガス取出し口１５へ噴射し、容器弁１０内の液化塩化水素を洗浄する方法がある。   In order to solve these problems, as disclosed in Patent Document 1, a mixture of dimethyl ether (DME), which is a liquefied gas that generates a propellant such as pressurized gas, and an organic solvent such as isopropyl alcohol (IPA) is washed. There is a method of cleaning the liquefied hydrogen chloride in the container valve 10 by injecting the cleaning agent into the gas outlet 15 through the nozzle 53 as shown in FIG.

しかし、当該洗浄方法では、液化塩化水素の洗浄が終わったか否かの判別が難しく、洗浄剤を多量に使用してしまう傾向がある。一方、半導体製造工場内では例えばトルエン、ベンゼン、ジクロロメタン等の揮発性有機化合物（ＶＯＣ：Volatile Organic Compounds）の排出を抑制するために当該揮発性有機化合物を検出するためのセンサー（以下、ＶＯＣセンサーという）を設けているが、前記洗浄剤に含まれるイソプロピルアルコールも揮発性有機化合物の一種であることから、多量に洗浄剤を使用するとＶＯＣセンサーに反応して、半導体の製造ラインが停止し、半導体の生産効率に悪影響を及ぼすおそれがある。   However, in this cleaning method, it is difficult to determine whether or not the liquefied hydrogen chloride has been cleaned, and there is a tendency to use a large amount of cleaning agent. On the other hand, a sensor for detecting volatile organic compounds (hereinafter referred to as a VOC sensor) in order to suppress emission of volatile organic compounds (VOC) such as toluene, benzene, and dichloromethane in a semiconductor manufacturing factory. However, since isopropyl alcohol contained in the cleaning agent is also a kind of volatile organic compound, if a large amount of cleaning agent is used, it reacts with the VOC sensor and the semiconductor production line is stopped. May adversely affect production efficiency.

特開２００７−１６２７８７号公報（段落００２３）JP2007-162787 (paragraph 0023)

本発明はこのような事情の下になされたものであり、その目的は、液化塩化水素ガスを充填する容器に装着されている容器弁を洗浄するにあたり、終点を容易に把握できる容器弁の洗浄方法及び洗浄剤を提供することにある。   The present invention has been made under such circumstances, and its purpose is to clean a container valve that can easily grasp the end point when cleaning a container valve mounted on a container filled with liquefied hydrogen chloride gas. It is to provide a method and a cleaning agent.

本発明に係る容器弁の洗浄方法は、液化塩化水素ガスを充填する高圧ガス容器に装着された容器弁を洗浄する方法において、
高圧ガス容器内に液化塩化水素ガスを充填若しくは高圧ガス容器内の塩化水素ガスを消費した後、前記容器弁を閉じたまま、そのガス取出し口から当該容器弁内に、スプレー容器内からアンモニア水をスプレー状で供給して前記容器弁内に付着している塩化水素を洗浄する工程と、
この洗浄工程において塩化水素がアンモニアとの反応で消費されたときに、前記容器弁内へアンモニア水の供給を停止する工程と、を備えたことを特徴とする。 The container valve cleaning method according to the present invention is a method of cleaning a container valve mounted on a high-pressure gas container filled with liquefied hydrogen chloride gas.
After filling the liquefied hydrogen chloride gas in the high pressure gas container or consuming the hydrogen chloride gas in the high pressure gas container, the container valve is closed, and the ammonia water Supplying hydrogen in a spray form to wash off hydrogen chloride adhering to the container valve;
A step of stopping supply of ammonia water into the container valve when hydrogen chloride is consumed in the reaction with ammonia in the washing step.

本発明によれば、液化塩化水素ガスを充填する容器に装着されている容器弁内にアンモニア水を供給しているため、塩化水素による容器弁内の腐食を防ぐことができ、容器弁の使用寿命が延びる。そして、容器弁内に塩化水素が存在するうちは塩化アンモニウムの白煙が発生し、塩化水素が消費されると白煙の発生が停止するので、容易に容器弁の洗浄が終了したのか否かを判断することできる。従って、過剰にアンモニア水を使用することが抑えられ省資源化を図れる。そして、アンモニア水の使用により、工場内のＶＯＣセンサーが作動することがなく、また噴射剤もアンモニア水に対する含有割合が少ないことから、噴射剤の使用によってもＶＯＣセンサーの作動のおそれはなく、この結果半導体製造工場等の工場のラインが停止するといったおそれがない。   According to the present invention, ammonia water is supplied into a container valve mounted on a container filled with liquefied hydrogen chloride gas, so that corrosion in the container valve due to hydrogen chloride can be prevented, and the use of the container valve Life span is extended. And when hydrogen chloride is present in the container valve, white smoke of ammonium chloride is generated, and when hydrogen chloride is consumed, the generation of white smoke stops, so whether or not the cleaning of the container valve is easily completed Can be judged. Therefore, excessive use of ammonia water can be suppressed and resource saving can be achieved. The use of ammonia water does not activate the VOC sensor in the factory, and the propellant is also contained in a small amount of ammonia water. As a result, there is no fear that the line of a factory such as a semiconductor manufacturing factory will stop.

前記容器弁に接続された洗浄具の縦断面図である。It is a longitudinal cross-sectional view of the cleaning tool connected to the container valve. 前記容器弁の洗浄が行われている様子を模式的に示した模式図である。It is the schematic diagram which showed typically a mode that the washing | cleaning of the said container valve was performed. 従来の容器弁の一例を示す縦断面図である。It is a longitudinal cross-sectional view which shows an example of the conventional container valve. 前記容器弁に用いられるプラグの斜視図である。It is a perspective view of the plug used for the said container valve. 前記容器弁と洗浄具との接続状態を示す説明図である。It is explanatory drawing which shows the connection state of the said container valve and a cleaning tool.

本発明の容器弁の洗浄方法に係る実施の形態を説明する。以下に説明する実施の形態に用いる高圧ガス容器Ｇに装着された容器弁の構造は、従来技術の項で説明した容器弁１０と同一であるため、同じ符号を付し、説明を省略すると共に以下の容器弁の説明については図３に示す容器弁１０を用いて説明する。   An embodiment according to the container valve cleaning method of the present invention will be described. Since the structure of the container valve attached to the high-pressure gas container G used in the embodiment described below is the same as the container valve 10 described in the section of the prior art, the same reference numerals are given and the description is omitted. The following description of the container valve will be made using the container valve 10 shown in FIG.

次に、図１を用いて高圧ガス容器Ｇに装着された容器弁１０内を洗浄する洗浄具５を説明する。洗浄具５は、密閉容器である筒状の缶体部５０と、この缶体部５０の上部に設けられた開閉部５１と、この開閉部５１の側面に設けられたノズル５３とから構成されている。前記缶体部５０にはアンモニア水６と、噴射剤６１例えば加圧ガスを発生する液化ガスであるジメチルエーテル（ＤＭＥ）とが収容されている。前記アンモニア水６は塩化水素を洗浄する洗浄剤の役割を有する。前記噴射剤６１としてはジメチルエーテルの他に液化プロパン又はこれらの混合物であってもよい。また、図２に示すように前記ノズル５３の先端側には噴射口５４が形成されており、この噴射口５４は容器弁１０のガス取出し口１５に挿入されるようになっている。この例では、前記開閉部５１に設けられたボタン５２を押圧することにより、噴射口５４からアンモニア水６が噴射される。   Next, the cleaning tool 5 for cleaning the inside of the container valve 10 attached to the high-pressure gas container G will be described with reference to FIG. The cleaning tool 5 includes a cylindrical can body portion 50 that is a sealed container, an opening / closing portion 51 provided on the upper portion of the can body portion 50, and a nozzle 53 provided on a side surface of the opening / closing portion 51. ing. The can body 50 contains ammonia water 6 and propellant 61, for example, dimethyl ether (DME), which is a liquefied gas that generates pressurized gas. The ammonia water 6 serves as a cleaning agent for cleaning hydrogen chloride. The propellant 61 may be liquefied propane or a mixture thereof in addition to dimethyl ether. As shown in FIG. 2, an injection port 54 is formed on the tip side of the nozzle 53, and this injection port 54 is inserted into the gas extraction port 15 of the container valve 10. In this example, the ammonia water 6 is injected from the injection port 54 by pressing the button 52 provided in the opening / closing part 51.

続いて、容器弁１０内を洗浄する方法を説明する。先ず、高圧ガスの工場内において空の高圧ガス容器Ｇに装着された容器弁１０のガス取出し口１５に充填クランプを介して液化塩化水素供給用（充填用）の配管を接続し、プラグ１３を上昇させてガス流路１７の開口部を開き、塩化水素供給源より配管を介して高圧ガス容器Ｇに無水液化塩化水素を供給して充填する。その後、プラグ１３を下降させてシートディスク１８によりガス流路１７の開口部を密閉した後、配管を外す。しかる後、容器弁１０のガス取出し口１５をホットガンで例えば１分間温め、充填クランプ及びガス取出し口１５に付着している水分を乾燥させる。そして、ガス取出し口１５から充填クランプを取り外し、洗浄具５のノズル５３をガス取出し口１５に差し込む。   Next, a method for cleaning the inside of the container valve 10 will be described. First, in a high-pressure gas factory, a pipe for supplying liquefied hydrogen chloride (for filling) is connected to a gas outlet 15 of a container valve 10 attached to an empty high-pressure gas container G through a filling clamp, and a plug 13 is connected. The gas channel 17 is opened to open, and anhydrous liquefied hydrogen chloride is supplied from the hydrogen chloride supply source to the high-pressure gas container G through a pipe and filled. Thereafter, the plug 13 is lowered and the opening of the gas flow path 17 is sealed with the seat disk 18, and then the pipe is removed. After that, the gas outlet 15 of the container valve 10 is heated with a hot gun for 1 minute, for example, and the moisture adhering to the filling clamp and the gas outlet 15 is dried. Then, the filling clamp is removed from the gas outlet 15, and the nozzle 53 of the cleaning tool 5 is inserted into the gas outlet 15.

そして、前記開閉部５１のボタン５２を例えば作業者が押圧することで缶体部５０に収納されている噴射剤から加圧ガスが発生し、当該缶体部５０内の圧力が増加して、アンモニア水６がノズル５３より噴射され、容器弁１０内が洗浄される。   And, for example, when an operator presses the button 52 of the opening / closing part 51, a pressurized gas is generated from the propellant stored in the can body part 50, and the pressure in the can body part 50 increases, Ammonia water 6 is injected from the nozzle 53, and the inside of the container valve 10 is cleaned.

アンモニア水と加圧ガスとの放出は、霧状（微細な粒子）となりプラグ１３に衝突し、プラグ１３の側周面及び底面におけるガス取出し口１５に臨む部位に衝突し、プラグ１３の表面に沿ってガス取出し口１５の背面側まで回り込み、ガス取出し口１５及びこれに連通する空間に露出する部位にアンモニア水６が接触することになる。これによりプラグ１３のネジ山１周部分を含む下部側周面及び底面（シートディスク１８の周囲部分）に付着していた液化塩化水素がアンモニア水と反応して、塩化アンモニウムが生成され、この塩化アンモニウムは霧状（微細な粒子）となって、ガス取出し口１５より白煙Ｓとして外部へ流出する（図２参照）。   The release of the ammonia water and the pressurized gas becomes a mist (fine particle) and collides with the plug 13, collides with a portion facing the gas outlet 15 on the side peripheral surface and the bottom surface of the plug 13, and hits the surface of the plug 13. The ammonia water 6 comes into contact with the gas extraction port 15 and a portion exposed to the space communicating with the gas extraction port 15. As a result, the liquefied hydrogen chloride adhering to the lower peripheral surface and the bottom surface (the peripheral portion of the sheet disk 18) including the peripheral portion of the screw 13 of the plug 13 reacts with the aqueous ammonia to produce ammonium chloride. Ammonium is atomized (fine particles) and flows out as white smoke S from the gas outlet 15 (see FIG. 2).

引き続き、容器弁１０内にアンモニア水６を供給し続けてゆくとプラグ１３に付着していた液化塩化水素がアンモニア水と反応するか又洗い流され、徐々にその量が減少する。そして液化塩化水素がすべて無くなると、アンモニアとの反応は起こらなくなるため、塩化アンモニウムの発生が停止し、ガス取出し口１５より発生していた塩化アンモニウムの白煙Ｓを視認することができなくなる。塩化アンモニウムの白煙Ｓが視認することができなくなった時、即ち液化塩化水素の洗浄が終了した時に、容器弁１０内へのアンモニア水６の供給を停止する。   When the ammonia water 6 is continuously supplied into the container valve 10, the liquefied hydrogen chloride adhering to the plug 13 reacts with the ammonia water or is washed away, and the amount gradually decreases. When all of the liquefied hydrogen chloride is eliminated, the reaction with ammonia does not occur, so the generation of ammonium chloride stops, and the white smoke S of ammonium chloride generated from the gas outlet 15 cannot be seen. When the white smoke S of ammonium chloride can no longer be seen, that is, when the cleaning of the liquefied hydrogen chloride is completed, the supply of the ammonia water 6 into the container valve 10 is stopped.

容器弁１０内の洗浄が終わった後、液化塩化水素が残っていると容器弁１０内の腐食の原因となるため、ｐＨ試験紙をガス取出し口１５から差込み、ｐＨ試験紙の色が変化しないことを確認して、ガス取出し口１５をウェスで汚れや水分を除去し、ホットガンで乾燥させる。その後、アウトレットキャップ１６をガス取出し口１５に取り付ける。このようにしてメーカー側で高圧ガス容器Ｇ内に液化塩化水素が充填された後、当該高圧ガス容器Ｇはユーザの下へ搬送されることになる。   If liquefied hydrogen chloride remains after the cleaning of the container valve 10, it will cause corrosion in the container valve 10, so the pH test paper is inserted from the gas outlet 15 and the color of the pH test paper does not change. After confirming this, dirt and moisture are removed from the gas outlet 15 with a waste cloth and dried with a hot gun. Thereafter, the outlet cap 16 is attached to the gas outlet 15. After the liquefied hydrogen chloride is filled in the high-pressure gas container G on the manufacturer side in this way, the high-pressure gas container G is transported under the user.

上述の実施の形態によれば、アンモニア水６を洗浄具５のノズル５３からガス取出し口１５を介して、容器弁１０内のガス取出し口１５内に供給しているため、当該アンモニア水と容器弁１０内の例えばプラグ１３の側周面等に付着している液化塩化水素とが反応し、塩化アンモニウムの白煙Ｓがガス取出し口１５より発生すると共にその他の液化塩化水素はアンモニア水６により洗い流される。従って容器弁１０内より塩化水素が除去できるので、容器弁１０内の腐食を防止することができ、またユーザがアウトレットキャップ１６を取り外したときに塩化水素ガスが漏洩しないので、高圧ガス容器Ｇをメーカ側に戻して再点検を依頼するといったトラブルも解消される。   According to the above-described embodiment, since the ammonia water 6 is supplied from the nozzle 53 of the cleaning tool 5 through the gas outlet 15 into the gas outlet 15 in the container valve 10, the ammonia water and the container The liquefied hydrogen chloride adhering to, for example, the side peripheral surface of the plug 13 in the valve 10 reacts, and white smoke S of ammonium chloride is generated from the gas outlet 15 and the other liquefied hydrogen chloride is caused by the ammonia water 6. Washed away. Accordingly, since hydrogen chloride can be removed from the inside of the container valve 10, corrosion inside the container valve 10 can be prevented, and hydrogen chloride gas does not leak when the user removes the outlet cap 16. The trouble of returning to the manufacturer and requesting re-inspection is also eliminated.

また、液化塩化水素が洗浄され、アンモニア水との反応が停止したとき、即ち塩化アンモニウムの白煙Ｓが視認できなくなった時が洗浄の終点であることから、液化塩化水素の洗浄が終了した時点を容易に判断できる。従って、アンモニア水６の過剰な使用を抑制することができ省資源化を図られる。また、アンモニア水の使用により、工場内のＶＯＣセンサーに検出されることもないため、半導体製造工場等の製造ラインが停止するおそれがなく、例えば半導体の生産効率に悪影響を及ぼすおそれも減少する。   When the liquefied hydrogen chloride is washed and the reaction with the ammonia water is stopped, that is, when the white smoke S of ammonium chloride is not visible, the end point of washing is the time when the washing of the liquefied hydrogen chloride is finished. Can be easily determined. Therefore, excessive use of the ammonia water 6 can be suppressed and resource saving can be achieved. Further, since the ammonia water is not detected by the VOC sensor in the factory, there is no possibility that the production line of the semiconductor manufacturing factory or the like is stopped, and the possibility of adversely affecting the semiconductor production efficiency is reduced.

また本発明の洗浄方法は、ユーザ側においても行われる。例えばユーザが高圧ガス容器Ｇ内の塩化水素ガスを使い切った後、上述と同様にしてユーザ側で高圧ガス容器Ｇに装着された容器弁１０内の洗浄が行われる。この場合、容器弁１０のプラグ１３によりガス流路１７を閉じ、次いでガス消費用の配管を容器弁１０から取り外したときに、ガス取出し口１５から大気が容器弁１０内に浸入し、これにより大気中の水分と塩化水素とが反応して塩酸となるが、既述のようにアンモニア水６により洗浄することで容器弁１０内に付着している液化塩化水素又は塩酸が溶解して洗い流される。このため、その後アウトレットキャップ１６が閉じられてメーカ側に回収されるまで、長時間経過してもプラグ１３等の部品の腐食が抑えられるので、部品あるいは容器弁１０の使用寿命が長くなる効果がある。   The cleaning method of the present invention is also performed on the user side. For example, after the user uses up the hydrogen chloride gas in the high pressure gas container G, the inside of the container valve 10 attached to the high pressure gas container G is cleaned on the user side in the same manner as described above. In this case, when the gas flow path 17 is closed by the plug 13 of the container valve 10 and then the gas consumption pipe is removed from the container valve 10, the atmosphere enters the container valve 10 from the gas outlet 15, thereby Moisture in the atmosphere and hydrogen chloride react to form hydrochloric acid, but as described above, the liquid hydrogen chloride or hydrochloric acid adhering to the container valve 10 is dissolved and washed away by washing with the aqueous ammonia 6 as described above. . Therefore, until the outlet cap 16 is subsequently closed and collected by the manufacturer, corrosion of parts such as the plug 13 is suppressed even after a long period of time, so that the service life of the parts or the container valve 10 can be extended. is there.

また、上述した実施形態において、アンモニア水にエタノールを加えた混合物を洗浄剤として用いてもよい。さらに上述の実施の形態では、パックタイプの容器弁について説明を行ったが、ダイヤフラムタイプの容器弁においても上述と同様に容器弁内を洗浄することで、同様の効果を得ることができる。   In the above-described embodiment, a mixture obtained by adding ethanol to aqueous ammonia may be used as a cleaning agent. Furthermore, although the pack type container valve has been described in the above embodiment, the same effect can be obtained by washing the inside of the container valve in the same manner as described above even in the case of the diaphragm type container valve.

次に本発明の効果を確認するために行った実験について述べる。図１に示す洗浄具５において、噴射剤６としてはジメチルエーテル（ＤＭＥ）を用い、ＤＭＥ、エタノール及びアンモニア水との重量比をＤＭＥ：エタノール：アンモニア水（濃度５％）＝３０：６０：１０の混合液を洗浄剤として、既述のように高圧ガス容器Ｇ内に液化塩化水素を充填した後の容器弁１０内の洗浄を行った。そして容器弁１０内の洗浄が終わった後、ガス取出し口１５をホットガンで乾燥させた。その後、ガス取出し口１５にアウトレットキャップ１６を取り付け、一昼夜高圧ガス容器Ｇを放置した。そして翌日アウトレットキャップ１６を外し、ガス取出し口１５に塩化水素ガス検知用の検知器を取り付け、ガス取出し口１５から放出される塩化水素濃度を測定したところ、塩化水素ガスが全く検出されなかった。   Next, an experiment conducted for confirming the effect of the present invention will be described. In the cleaning tool 5 shown in FIG. 1, dimethyl ether (DME) is used as the propellant 6, and the weight ratio of DME, ethanol and aqueous ammonia is DME: ethanol: ammonia water (concentration 5%) = 30:60:10. Using the mixed liquid as a cleaning agent, the container valve 10 was cleaned after the liquefied hydrogen chloride was filled into the high-pressure gas container G as described above. Then, after the cleaning of the container valve 10 was finished, the gas outlet 15 was dried with a hot gun. Thereafter, an outlet cap 16 was attached to the gas outlet 15 and the high-pressure gas container G was left overnight. On the next day, the outlet cap 16 was removed, a detector for detecting hydrogen chloride gas was attached to the gas outlet 15, and the concentration of hydrogen chloride released from the gas outlet 15 was measured. As a result, no hydrogen chloride gas was detected.

Ｇ 高圧ガス容器
１０ 容器弁
１１ 容器弁本体
１２ シリンダ部
１３ プラグ
１５ ガス取出し口
１７ ガス流路
５ 洗浄具
５３ ノズル
６ アンモニア水
Ｓ 白煙 G High-pressure gas container 10 Container valve 11 Container valve body 12 Cylinder part 13 Plug 15 Gas outlet 17 Gas flow path 5 Cleaning tool 53 Nozzle 6 Ammonia water S White smoke

Claims (1)

液化塩化水素ガスを充填する高圧ガス容器に装着された容器弁を洗浄する方法において、
高圧ガス容器内に液化塩化水素ガスを充填若しくは高圧ガス容器内の塩化水素ガスを消費した後、前記容器弁を閉じたまま、そのガス取出し口から当該容器弁内に、スプレー容器内からアンモニア水をスプレー状で供給して前記容器弁内に付着している塩化水素を洗浄する工程と、
この洗浄工程において塩化水素がアンモニアとの反応で消費されたときに、前記容器弁内へアンモニア水の供給を停止する工程と、を備えたことを特徴とする容器弁の洗浄方法。 In a method of cleaning a container valve attached to a high-pressure gas container filled with liquefied hydrogen chloride gas,
After filling the liquefied hydrogen chloride gas in the high pressure gas container or consuming the hydrogen chloride gas in the high pressure gas container, the container valve is closed, and the ammonia water Supplying hydrogen in a spray form to wash off hydrogen chloride adhering to the container valve;
And a step of stopping the supply of aqueous ammonia into the vessel valve when hydrogen chloride is consumed in the reaction with ammonia in the washing step.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07256097A (en) * 1994-03-25 1995-10-09 Tsurumi Soda Co Ltd Corrosive gas absorbent and container valve of gas sealing container
JP2000328070A (en) * 1999-03-12 2000-11-28 Ube Ind Ltd Waste gasification treatment method
JP2003028392A (en) * 2001-05-10 2003-01-29 Mitsui Chemicals Inc High purity hydrogen chloride for semiconductor manufacture
JP2007162787A (en) * 2005-12-12 2007-06-28 Tsurumi Soda Co Ltd Washing method of vessel valve, filling method of halogen based liquefied gas, returning method of high pressure gas vessel, washing tool, and washing agent

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07256097A (en) * 1994-03-25 1995-10-09 Tsurumi Soda Co Ltd Corrosive gas absorbent and container valve of gas sealing container
JP2000328070A (en) * 1999-03-12 2000-11-28 Ube Ind Ltd Waste gasification treatment method
JP2003028392A (en) * 2001-05-10 2003-01-29 Mitsui Chemicals Inc High purity hydrogen chloride for semiconductor manufacture
JP2007162787A (en) * 2005-12-12 2007-06-28 Tsurumi Soda Co Ltd Washing method of vessel valve, filling method of halogen based liquefied gas, returning method of high pressure gas vessel, washing tool, and washing agent

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