JP2011152517A - Drying method of fluorinated hydrocarbon solvent - Google Patents

Drying method of fluorinated hydrocarbon solvent Download PDF

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JP2011152517A
JP2011152517A JP2010016092A JP2010016092A JP2011152517A JP 2011152517 A JP2011152517 A JP 2011152517A JP 2010016092 A JP2010016092 A JP 2010016092A JP 2010016092 A JP2010016092 A JP 2010016092A JP 2011152517 A JP2011152517 A JP 2011152517A
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fluorinated hydrocarbon
hydrocarbon solvent
washed
drying
cleaned
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Hideaki Kikuchi
秀明 菊地
Motosuke Ogawa
素右 小川
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Chemours Mitsui Fluoroproducts Co Ltd
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Du Pont Mitsui Fluorochemicals Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a drying method which minimizes loss of a fluorinated hydrocarbon adhered to substances to be washed scattered out of an apparatus over a short period of time. <P>SOLUTION: In a washing apparatus using a fluorinated hydrocarbon solvent, the drying method of the fluorinated hydrocarbon solvent adhered to the substances to be washed is characterized by making the fluorinated hydrocarbon solvent adhered to the substances to be washed evaporate by jetting the superheated vapor of the fluorinated hydrocarbon with a boiling point in a range of 50-150°C to the substances to be washed. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

本発明は、フッ素化炭化水素溶剤を使用する洗浄装置における、被洗物に付着しているフッ素化炭化水素溶剤の乾燥、詳細には、洗浄目的で使用され、被洗物に付着したフッ素化炭化水素溶剤を、短時間に、なおかつ装置外への飛散ロスを最小限に抑える乾燥方法に関するものである。   The present invention relates to drying of a fluorinated hydrocarbon solvent adhering to an object to be cleaned in a cleaning apparatus using a fluorinated hydrocarbon solvent, and more specifically, fluorination used for cleaning purposes and adhering to an object to be cleaned The present invention relates to a method for drying a hydrocarbon solvent in a short time and to minimize scattering loss to the outside of the apparatus.

従来、フッ素化炭化水素溶剤を使用する洗浄装置としては、たとえば特許文献1や特許文献2などが知られている。
一方、近年環境保護の観点から、洗浄装置、洗浄方法も省エネルギー、省消費量が要求されており、これを満たすため、インライン工程での洗浄装置外への飛散を抑えた洗浄方式が望まれている。
Conventionally, as a cleaning apparatus using a fluorinated hydrocarbon solvent, for example, Patent Document 1 and Patent Document 2 are known.
On the other hand, in recent years, from the viewpoint of environmental protection, cleaning devices and cleaning methods are also required to save energy and consumption, and in order to satisfy this, a cleaning method that suppresses scattering outside the cleaning device in an in-line process is desired. Yes.

米国特許第3881949号明細書U.S. Pat. No. 3,881,949 特公昭63−62276号公報Japanese Patent Publication No. 63-62276

しかしながら、特許文献1で開示されている装置は、洗浄方法がバッチ方式であり、また蒸気による乾燥時間も長く必要である。また、最近では溶剤の装置外への持ち出し飛散を抑制するため、被洗物をフリーボードゾーンで数十秒から数分間静置して乾燥しなければならず、フリーボードゾーンにとどまる時間が数秒程度である連続方式による短時間洗浄に、このような従来の装置は応えられない。   However, the apparatus disclosed in Patent Document 1 requires a batch cleaning method and requires a long drying time with steam. Recently, in order to prevent the solvent from being taken out and scattered, the object to be washed must be left in the freeboard zone for several tens of seconds to several minutes to dry, and the time remaining in the freeboard zone is several seconds. Such a conventional apparatus cannot respond to a short time cleaning by a continuous method.

また、特許文献2で開示されている装置は、乾燥用の溶剤として露点が20〜50℃の塩化フッ化エタンを用いているため、常時高濃度の“湿り溶剤蒸気”が槽上部に滞留し、それにより乾燥速度、被処理物品に制限が加わるという問題があった。   Further, since the apparatus disclosed in Patent Document 2 uses chlorofluoroethane having a dew point of 20 to 50 ° C. as a solvent for drying, a high concentration of “wet solvent vapor” always stays in the upper part of the tank. As a result, there is a problem that the drying speed and the article to be processed are limited.

そこで、本発明者は、上記問題を解決するため、鋭意研究を行った結果、沸点が50〜150℃の範囲であるフッ素化炭化水素の過熱蒸気を被洗物に噴射させることにより、短時間でのフッ素化炭化水素溶剤の乾燥が可能となることを見出し、本発明に至ったものである。   Therefore, the present inventor has conducted extensive research to solve the above problems, and as a result, the superheated vapor of fluorinated hydrocarbon having a boiling point in the range of 50 to 150 ° C. is jetted onto the object to be washed for a short time. The present inventors have found that it is possible to dry the fluorinated hydrocarbon solvent in the present invention.

即ち、本発明は以下の方法に関するものである。
1.フッ素化炭化水素溶剤を使用する洗浄装置において、沸点が50〜150℃の範囲であるフッ素化炭化水素の過熱蒸気を被洗物に噴射させることにより、被洗物に付着しているフッ素化炭化水素溶剤を気化させることを特徴とする、被洗物に付着したフッ素化炭化水素溶剤の乾燥方法。
2.フッ素化炭化水素がフッ素、炭素および水素からなることを特徴とする上記1.記載のフッ素化炭化水素溶剤の乾燥方法。
3.フッ素化炭化水素がさらに酸素、窒素および硫黄の中から選ばれる少なくとも1つの原子を含有することを特徴とする上記1.または2.記載のフッ素化炭化水素溶剤の乾燥方法。
That is, the present invention relates to the following method.
1. In a cleaning apparatus using a fluorinated hydrocarbon solvent, a fluorinated carbonization adhering to an object to be cleaned by injecting the superheated vapor of the fluorinated hydrocarbon having a boiling point in the range of 50 to 150 ° C. onto the object to be cleaned A method for drying a fluorinated hydrocarbon solvent adhering to an object to be cleaned, characterized by evaporating a hydrogen solvent.
2. 1. The fluorinated hydrocarbon is composed of fluorine, carbon and hydrogen. The drying method of the fluorinated hydrocarbon solvent as described.
3. 1. The fluorinated hydrocarbon further contains at least one atom selected from oxygen, nitrogen and sulfur. Or 2. The drying method of the fluorinated hydrocarbon solvent as described.

本発明によれば、被洗物に付着したフッ素化炭化水素を短時間に気化させることができ、装置外への飛散ロスを最小限に抑えることが可能であるため、被洗物のインライン工程における連続方式の洗浄工程を最小限の飛散ロスで実施することができる。   According to the present invention, it is possible to vaporize the fluorinated hydrocarbon adhering to the object to be cleaned in a short time, and it is possible to minimize the scattering loss outside the apparatus. The continuous cleaning process can be carried out with minimal scattering loss.

洗浄装置を示した概略図である。It is the schematic which showed the washing | cleaning apparatus.

本発明のフッ素化炭化水素溶剤の乾燥方法は、フッ素化炭化水素の過熱蒸気を被洗物に噴射させて短時間にフッ素化炭化水素を蒸発気化させることを特徴とする。
本発明において、「フッ素化炭化水素溶剤を使用する洗浄装置」とは、フッ素化炭化水素溶剤を使用して電子・電気・機械部品等、例えば、自動車の小型部品のように形状が小さく連続的に生産、洗浄されるべきものを洗浄する洗浄装置であり、例えば、特許文献1および2に記載されるものをいう。
The method for drying a fluorinated hydrocarbon solvent according to the present invention is characterized by injecting superheated vapor of fluorinated hydrocarbon onto an object to be washed to evaporate the fluorinated hydrocarbon in a short time.
In the present invention, the “cleaning apparatus using a fluorinated hydrocarbon solvent” means that the fluorinated hydrocarbon solvent is used to continuously reduce the shape of electronic, electrical, mechanical parts, such as small parts of automobiles. A cleaning apparatus for cleaning what is to be produced and cleaned, such as those described in Patent Documents 1 and 2.

本発明において、「フッ素化炭化水素」とは、沸点が50℃〜150℃、好ましくは50〜130℃、より好ましくは50℃〜110℃の範囲である、フッ素および炭素、またはフッ素、炭素および水素からなる化合物であって、場合により、さらに酸素、窒素および硫黄からなる群より選ばれる少なくとも1つの原子を含む化合物である。本発明における好適な「フッ素化炭化水素」としては、例えば、1,1,1,2,2,3,4,5,5,5−デカフルオロペンタン、3−H,4−H−パーフルオロヘプタン、メチルトリスデカフルオロヘキシルエーテル、ヘキサフルオロプロピルヘキサフルオロブチルエーテル等が挙げられる。   In the present invention, the “fluorinated hydrocarbon” means fluorine and carbon, or fluorine, carbon and fluorine having a boiling point in the range of 50 ° C. to 150 ° C., preferably 50 to 130 ° C., more preferably 50 ° C. to 110 ° C. A compound comprising hydrogen, optionally further comprising at least one atom selected from the group consisting of oxygen, nitrogen and sulfur. Suitable “fluorinated hydrocarbons” in the present invention include, for example, 1,1,1,2,2,3,4,5,5,5-decafluoropentane, 3-H, 4-H-perfluoro. Examples include heptane, methyl trisdecafluorohexyl ether, hexafluoropropyl hexafluorobutyl ether and the like.

本発明において、「フッ素化炭化水素」は環状であっても鎖状であってもよく、また飽和化合物であっても不飽和化合物であってもよい。   In the present invention, the “fluorinated hydrocarbon” may be cyclic or chain-like, and may be a saturated compound or an unsaturated compound.

本発明において、「フッ素化炭化水素」は単一品であっても2種以上の混合品であってもよい。混合品の場合にその混合比率は特に制限されるものではなく、その洗浄の目的にかなった最適の混合比率でよい。また、その混合物が共沸混合物を形成するのであれば、その混合物の混合比率の保持のために、共沸組成が好ましい。   In the present invention, the “fluorinated hydrocarbon” may be a single product or a mixture of two or more. In the case of a mixed product, the mixing ratio is not particularly limited, and may be an optimum mixing ratio suitable for the purpose of washing. Further, if the mixture forms an azeotropic mixture, an azeotropic composition is preferable for maintaining the mixing ratio of the mixture.

本発明において、「フッ素化炭化水素」は他の溶剤との混合物であってもよく、例えば、メタノールやエタノールなどのアルコール類、アセトンやメチルエチルケトンなどのケトン類、ヘキサメチルジシロキサンなどのシリコーン類、酢酸エチルなどのエステル類、エチレングリコールモノメチルエーテルなどのグリコールエーテル類、ジエチルエーテルなどのエーテル類、など適宜その目的に応じた添加物を混合するこができる。混合物中の他の溶剤の濃度の範囲は、1〜50質量%であって、混合しても不燃性を維持する組成が好ましい。また、共沸混合物を作るものはその共沸組成が望ましい。   In the present invention, the “fluorinated hydrocarbon” may be a mixture with other solvents, for example, alcohols such as methanol and ethanol, ketones such as acetone and methyl ethyl ketone, silicones such as hexamethyldisiloxane, Additives according to the purpose such as esters such as ethyl acetate, glycol ethers such as ethylene glycol monomethyl ether, ethers such as diethyl ether, and the like can be appropriately mixed. The concentration range of the other solvent in the mixture is 1 to 50% by mass, and a composition that maintains nonflammability even when mixed is preferable. Moreover, the azeotropic composition is desirable for the azeotropic mixture.

本発明において、「過熱蒸気」とは、蒸気をさらに加熱した熱量の高い蒸気である。液体は、圧力一定のもとで加熱すると温度が上昇し、一定温度に達すると蒸発し始めるが、加熱を続けても全部の液体が蒸発するまで温度は一定である。液体と蒸気とが共存しているときは湿り飽和蒸気といい、全部蒸気になったものを乾き飽和蒸気というが、乾き飽和蒸気をさらに加熱して蒸気の温度を高くしたものが過熱蒸気である。
本発明において、「乾燥」とは、被洗物に付着したフッ素化炭化水素溶剤を取り去ることを意味する。
In the present invention, “superheated steam” is steam having a high calorific value obtained by further heating the steam. When the liquid is heated under a constant pressure, the temperature rises, and when it reaches a certain temperature, it starts to evaporate. However, even if heating is continued, the temperature is constant until all the liquid evaporates. When the liquid and steam coexist, it is called wet saturated steam, and what is completely vaporized is called dry saturated steam, but what is obtained by further heating dry saturated steam and raising the temperature of the steam is superheated steam. .
In the present invention, “drying” means removing the fluorinated hydrocarbon solvent adhering to the object to be washed.

本発明において、「被洗物」とは、特に限定されるものではないが、電子・電機・機械部品等、例えば、自動車の小型部品のように形状が小さく連続的に生産、洗浄されるべきもの等をいう。   In the present invention, the “object to be washed” is not particularly limited, but it should be continuously produced and washed in a small shape such as a small part of an automobile such as an electronic / electrical / mechanical part. Things etc.

以下、実施例、比較例を挙げて、本発明を更に詳しく説明するが、本発明は、これらの例に限定されるものではない。   EXAMPLES Hereinafter, although an Example and a comparative example are given and this invention is demonstrated in more detail, this invention is not limited to these examples.

実施例1
図1に示すような洗浄装置を用いて、被洗物表面のフッ素化炭化水素溶剤が乾燥するまでに要する時間を測定した。すなわち特許文献1に示されている従前よりフッ素化炭化水素溶剤が使用されている装置の蒸気層内に、過熱されたフッ素化炭化水素を噴射できる装置を用いた。1,1,1,2,2,3,4,5,5,5−デカフルオロペンタンに4質量%のエタノールを混合した溶剤(沸点52度、商品名バートレル(R)XE、三井・デュポンフロロケミカル製)を上記装置内に満たし、ヒーター7にて沸騰槽1内のバートレル(R)XEを沸騰させ、気化したバートレル(R)XEを冷却管4により再度凝縮させて超音波槽2に戻し、オーバーフローにより沸騰槽に戻した。また超音波槽よりバートレル(R)XEの一部をポンプを使用してヒーターゾーン5に送り込み、バートレル(R)XEの過熱蒸気をつくって過熱蒸気ライン6を経て蒸気層3内にバートレル(R)XEの過熱蒸気を噴射させた。過熱蒸気噴射口温度は約60℃となるようヒーターゾーンを調節した。
被洗物を予め40℃に調節された超音波槽に30秒間浸漬した後、バートレル(R)XEの過熱蒸気噴射口より50mm離れた場所で3秒間過熱蒸気をあて、素早く取り出して被洗物質量を測定し、被洗物がテスト前の質量に戻るまでの時間を測定した。被洗物として、自動車用金属部品−1(ニードル)、自動車用金属部品−2(ボディー)、自動車用金属部品−3(吸入シート)を用いた。
Example 1
Using a cleaning apparatus as shown in FIG. 1, the time required for drying the fluorinated hydrocarbon solvent on the surface of the object to be cleaned was measured. That is, the apparatus which can inject the superheated fluorinated hydrocarbon in the vapor layer of the apparatus from which the fluorinated hydrocarbon solvent is used from the former shown by patent document 1 was used. 1,1,1,2,2,3,4,5,5,5-decafluoropentane mixed with 4% by weight of ethanol (boiling point 52 degrees, trade name Bertrell® XE, Mitsui Dupont Fluoro) Chemical) is filled in the above-mentioned apparatus, and the bartrel (R) XE in the boiling tank 1 is boiled by the heater 7, and the vaporized bartrel (R) XE is condensed again by the cooling pipe 4 and returned to the ultrasonic tank 2. Returned to the boiling tank due to overflow. In addition, a part of the Bertle (R) XE is sent from the ultrasonic tank to the heater zone 5 by using a pump, and the superheated steam of the Bertel (R) XE is produced and passed through the superheated steam line 6 into the steam layer (R). ) XE superheated steam was injected. The heater zone was adjusted so that the temperature of the superheated steam outlet was about 60 ° C.
The object to be cleaned is immersed in an ultrasonic bath adjusted to 40 ° C. for 30 seconds in advance, and then heated for 3 seconds at a location 50 mm away from the superheated steam injection port of Bartrel® XE. The amount was measured and the time until the object to be washed returned to the mass before the test was measured. As the objects to be cleaned, automotive metal part-1 (needle), automotive metal part-2 (body), and automotive metal part-3 (suction sheet) were used.

比較例として、実施例1と同様な装置を用い、過熱蒸気を噴射させずに蒸気層内に3秒間静置し、素早く被洗物を取り出して、被洗物がテスト前の重量に戻るまでの時間を測定した。
結果を表1に示す。
As a comparative example, using the same apparatus as in Example 1, let it stand in the steam layer for 3 seconds without injecting superheated steam, quickly take out the object to be washed, and return the object to be washed to the weight before the test. Was measured.
The results are shown in Table 1.

Figure 2011152517
Figure 2011152517

実施例2
60mm×6mm×1mmのよく磨いたステンレススチール(SUS304)に、切削油(カットアーバスKZ260、ユシロ化学製)を4.25mg付着させた。そのスチールに80℃の1,1,1,2,2,3,4,5,5,5−デカフルオロペンタン(沸点55度、商品名バートレル(R)XF、三井・デュポンフロロケミカル製)の過熱蒸気を30秒間噴射させたのち、スチールに残っている油分量を測定した。
比較例として、実施例2と同じテストサンプルをバートレル(R)XFの蒸気(55度)に30秒間噴射した後、テストサンプルに残っている油分量を測定した。
結果を表2に示す。
Example 2
4.25 mg of cutting oil (Cut Arbus KZ260, manufactured by Yushiro Chemical Co., Ltd.) was attached to a well-polished stainless steel (SUS304) of 60 mm × 6 mm × 1 mm. The steel is made of 1,1,1,2,2,3,4,5,5,5-decafluoropentane (boiling point 55 degrees, trade name Bartrel (R) XF, Mitsui DuPont Fluorochemical) After injecting superheated steam for 30 seconds, the amount of oil remaining in the steel was measured.
As a comparative example, the same test sample as in Example 2 was sprayed on the vapor (55 degrees) of Bertrell (R) XF for 30 seconds, and then the amount of oil remaining in the test sample was measured.
The results are shown in Table 2.

Figure 2011152517
過熱蒸気を使用した場合、通常蒸気を使用した場合と比較して油分除去率がはるかに高く、短時間での乾燥に加え、短時間での洗浄も達成された。
Figure 2011152517
When superheated steam was used, the oil removal rate was much higher than when normal steam was used, and in addition to drying in a short time, cleaning in a short time was also achieved.

本発明は、被洗物に付着したフッ素化炭化水素を短時間に気化させることができ、装置外への飛散ロスを最小限に抑えることが可能であるため、部品等のインライン工程における連続方式の洗浄工程を最小限の飛散ロスで実施することができる洗浄装置の用途に好適に用いることができる。   Since the present invention can vaporize fluorinated hydrocarbons adhering to the object to be cleaned in a short time and can minimize scattering loss to the outside of the apparatus, it is a continuous method in the in-line process of parts, etc. This cleaning process can be suitably used for a cleaning apparatus that can carry out the cleaning process with minimum scattering loss.

1沸騰槽
2超音波槽
3蒸気層
4冷却管
5ヒーターゾーン
6過熱蒸気ライン
7ヒーター
8超音波
1 boiling tank 2 ultrasonic tank 3 steam layer 4 cooling pipe 5 heater zone 6 superheated steam line 7 heater 8 ultrasonic

Claims (3)

フッ素化炭化水素溶剤を使用する洗浄装置において、沸点が50〜150℃の範囲であるフッ素化炭化水素の過熱蒸気を被洗物に噴射させることにより、被洗物に付着しているフッ素化炭化水素溶剤を気化させることを特徴とする、被洗物に付着したフッ素化炭化水素溶剤の乾燥方法。   In a cleaning apparatus using a fluorinated hydrocarbon solvent, a fluorinated carbonization adhering to an object to be cleaned by injecting the superheated vapor of the fluorinated hydrocarbon having a boiling point in the range of 50 to 150 ° C. onto the object to be cleaned A method for drying a fluorinated hydrocarbon solvent adhering to an object to be cleaned, characterized by evaporating a hydrogen solvent. フッ素化炭化水素がフッ素、炭素および水素からなることを特徴とする請求項1記載のフッ素化炭化水素溶剤の乾燥方法。   2. The method for drying a fluorinated hydrocarbon solvent according to claim 1, wherein the fluorinated hydrocarbon comprises fluorine, carbon and hydrogen. フッ素化炭化水素がさらに酸素、窒素および硫黄の中から選ばれる少なくとも1つの原子を含有することを特徴とする請求項1または2記載のフッ素化炭化水素溶剤の乾燥方法。   The method for drying a fluorinated hydrocarbon solvent according to claim 1 or 2, wherein the fluorinated hydrocarbon further contains at least one atom selected from oxygen, nitrogen and sulfur.
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JPH08243515A (en) * 1995-03-14 1996-09-24 Du Pont Mitsui Fluorochem Co Ltd Washer and method thereof
JPH10192797A (en) * 1997-01-14 1998-07-28 Du Pont Mitsui Fluorochem Co Ltd Washing method
WO2009110549A1 (en) * 2008-03-07 2009-09-11 三井・デュポンフロロケミカル株式会社 Method and system for washing electronic component

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