JP2961924B2 - Solvent cleaning method for articles - Google Patents
Solvent cleaning method for articlesInfo
- Publication number
- JP2961924B2 JP2961924B2 JP3071406A JP7140691A JP2961924B2 JP 2961924 B2 JP2961924 B2 JP 2961924B2 JP 3071406 A JP3071406 A JP 3071406A JP 7140691 A JP7140691 A JP 7140691A JP 2961924 B2 JP2961924 B2 JP 2961924B2
- Authority
- JP
- Japan
- Prior art keywords
- solvent
- ether
- solvent composition
- boiling point
- cleaning
- 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.)
- Expired - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/261—Alcohols; Phenols
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5018—Halogenated solvents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5036—Azeotropic mixtures containing halogenated solvents
- C11D7/504—Azeotropic mixtures containing halogenated solvents all solvents being halogenated hydrocarbons
- C11D7/5063—Halogenated hydrocarbons containing heteroatoms, e.g. fluoro alcohols
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
- C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
- C23G5/032—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing oxygen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/28—Organic compounds containing halogen
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、溶剤又は溶剤蒸気を使
用して、金属品、繊維品、ガラス品、プラスチック、電
子部品及び印刷回路板の如き汚染された物品を清浄化す
る、溶剤での清浄化（クリーニング）方法しかもより詳
しく言えば溶剤での清浄化方法での溶剤として低分子量
エーテルの使用に関する。FIELD OF THE INVENTION The present invention relates to a solvent for cleaning contaminated articles such as metal articles, textiles, glass articles, plastics, electronic components and printed circuit boards using a solvent or solvent vapor. And more particularly to the use of low molecular weight ethers as solvents in cleaning methods with solvents.
【０００２】[0002]
【従来の技術及び問題点】汚染された物品をハロゲン化
炭化水素溶剤及び／又はこれの蒸気に浸漬するか又は該
溶剤及び／又はこれの蒸気で洗浄する溶剤清浄化方法は
周知であり、普通に使用されている。浸漬、ゆすぎ及び
乾燥という若干の工程を伴なう溶剤清浄化方法が普通で
あり、多くは超音波攪拌を伴ないながら周囲温度で又は
溶剤の沸点以下の上昇した温度で溶剤を使用することは
周知である。これらの清浄化方法で使用した溶剤の例は
１，１，２−トリクロロ−１，２，２−トリフルオロエ
タン、１，１，１−トリクロロエタン、トリクロロエチ
レン、パークロロエチレン及び塩化メチレンである。こ
れらの溶剤は単独で使用されるか又は脂肪族アルコール
又は他の低分子量極性添加剤の如く補助溶剤と混合して
使用され、しかも清浄化すべき物品に応じて或る程度ま
で光線、熱及び金属類の存在によって誘起される分解を
受けないように安定化されることが多い。2. Description of the Prior Art Solvent cleaning processes in which contaminated articles are immersed in or washed with halogenated hydrocarbon solvents and / or vapors are well known and commonly used. Used in Solvent cleaning methods involving some steps of dipping, rinsing and drying are common, and it is often not possible to use solvents at ambient temperature or elevated temperatures below the boiling point of the solvent without ultrasonic agitation. It is well known. Examples of solvents used in these cleaning methods are 1,1,2-trichloro-1,2,2-trifluoroethane, 1,1,1-trichloroethane, trichloroethylene, perchloroethylene and methylene chloride. These solvents may be used alone or in admixture with co-solvents, such as aliphatic alcohols or other low molecular weight polar additives, and to some extent light, heat and metal depending on the article to be cleaned. It is often stabilized so that it does not undergo degradation induced by the presence of the class.
【０００３】既知の普通の溶剤清浄化方法においてはし
かも特に溶剤を上昇した温度で使用した清浄化方法にお
いては、溶剤蒸気が清浄化系から雰囲気中に消失する傾
向がある。別量の溶剤消失は溶剤を清浄化プラントに装
填し且つこれを取出すのに生起してしまい且つ使用した
溶剤を蒸留により回収するのに生起してしまう。例えば
プラントの設計及び蒸気の回収系を改良することにより
雰囲気中への溶剤の消失を最小とするのに注意を通常払
うけれども、消失を全て防止する経費は法外な程に多大
でありしかも最も実用的な清浄化方法によって雰囲気中
へ溶剤蒸気が若干消失する。[0003] Solvent vapors tend to escape from the cleaning system into the atmosphere in known common solvent cleaning methods, and especially in cleaning methods using elevated temperatures of the solvent. Another amount of solvent loss occurs in loading and unloading the solvent into the cleaning plant and in recovering the used solvent by distillation. Although care is usually taken to minimize the loss of solvent into the atmosphere, for example by improving plant design and steam recovery systems, the cost of preventing all losses is prohibitively large and most significant. Solvent vapors slightly disappear into the atmosphere by a practical cleaning method.
【０００４】最近まで、普通の清浄化溶剤を使用するこ
とは、該溶剤が環境への影響上良好であると考えられる
安定で低毒性の不燃性物質である点で安全に実施される
と考えられていた。然しながら最近の徴候が示唆する所
によれば普通の溶剤の少なくとも若干は成層圏言わゆる
オゾン層に長期の悪影響を及ぼしてしまうので代替溶剤
が望ましいことが見られる。Until recently, the use of ordinary cleaning solvents has been considered to be safe to implement in that they are stable, low toxic, non-flammable materials that are considered to be environmentally benign. Had been. However, recent signs suggest that alternative solvents are desirable because at least some of the common solvents have a long-term adverse effect on the stratosphere, the so-called ozone layer.
【０００５】[0005]
【問題点を解決するための手段、作用及び効果】本発明
によると、清浄化すべき物品に対して２０℃〜１２０℃
の範囲の沸点を有し且つ少なくとも３個の炭素原子と１
個又はそれ以上の水素原子とを有する低分子量のフッ素
化エーテルを含有してなる溶剤組成物を接触させること
からなる物品の溶剤清浄化方法が提供される。According to the present invention, an article to be cleaned has a temperature of 20 ° C to 120 ° C.
And at least 3 carbon atoms and 1
Provided is a method for solvent cleaning an article, comprising contacting a solvent composition comprising a low molecular weight fluorinated ether having at least one hydrogen atom.
【０００６】低分子量のフッ素化エーテル即ちフッ素含
有エーテルは２０℃〜１２０℃の範囲の沸点好ましく
は、２５℃〜８５℃の範囲の沸点を有するのでこれを慣
用の且つ現存する清浄化装置に使用できる。何れかの特
定の清浄化方法については、エーテルはこれが代替して
いる溶剤の沸点に近い沸点を有するように選択できる。[0006] Low molecular weight fluorinated ethers or fluorine-containing ethers have a boiling point in the range of 20 ° C to 120 ° C, preferably in the range of 25 ° C to 85 ° C, and are used in conventional and existing cleaning equipment. it can. For any particular cleaning method, the ether can be selected to have a boiling point close to the boiling point of the solvent it is replacing.
【０００７】本発明で使用するフッ素含有エーテルは既
知の要領でハロゲン化脂肪族オレフィンを場合によりハ
ロゲン化した脂肪族アルコールと反応させることにより
得ることができ、かくして分子中に少なくとも３個の炭
素原子を含有できる。通常フッ素含有エーテルは５個以
下の炭素原子を含有するが、沸点が約１２０℃以下であ
るならば６個又はそれ以上の炭素原子を含有するエーテ
ルも使用できる。The fluorine-containing ethers used according to the invention can be obtained in a known manner by reacting halogenated aliphatic olefins with optionally halogenated aliphatic alcohols, thus obtaining at least 3 carbon atoms in the molecule. Can be contained. Usually, fluorine containing ethers contain up to 5 carbon atoms, but ethers containing 6 or more carbon atoms can also be used provided that the boiling point is below about 120 ° C.
【０００８】フッ素含有エーテルは少なくとも１個のフ
ッ素原子を含有し、通常２個又はそれ以上のフッ素原子
を含有するものであるが、一般には過フッ素化されてい
ない。フッ素原子に加えて、エーテルは塩素原子、臭素
原子及び水素原子を含有できる。塩素及び／又は水素を
含有するエーテルは、１個又は２個の塩素原子及び／又
は１個又は２個の水素原子を含有できる。[0008] Fluorine-containing ethers contain at least one fluorine atom and usually contain two or more fluorine atoms, but are generally not perfluorinated. In addition to fluorine atoms, ethers can contain chlorine, bromine and hydrogen atoms. Ethers containing chlorine and / or hydrogen can contain one or two chlorine atoms and / or one or two hydrogen atoms.
【０００９】エーテルを生成するのに使用できるアルコ
ールの例はメタノール、エタノール、プロパノール及び
ブタノール及びこれらのハロゲン化誘導体である。使用
できるアルケン類にはテトラフルオロエチレン、ヘキサ
フルオロプロペン、クロロトリフルオロエチレン及びク
ロロフルオロプロペン及びこれらの化合物の水素含有同
族体例えばトリフルオロエチレン及びクロロジフルオロ
エチレンがある。[0009] Examples of alcohols which can be used to form the ethers are methanol, ethanol, propanol and butanol and their halogenated derivatives. Alkenes which can be used include tetrafluoroethylene, hexafluoropropene, chlorotrifluoroethylene and chlorofluoropropene and the hydrogen-containing homologs of these compounds, such as trifluoroethylene and chlorodifluoroethylene.
【００１０】使用できるエーテルの例及びそれらの沸点
を次に挙げる： 沸点（℃） １，１−ジフルオロエチルメチルエーテル 47 １，１，２，２−テトラフルオロエチルメチルエーテル 36.5 １−クロロ−１，２，２−トリフルオロエチルメチルエーテル 70.6 １，１−ジクロロ−２，２−ジフルオロエチルメチルエーテル 104.8 １−クロロ−２，２−ジフルオロエチルメチルエーテル 27.5 1 １，１，１，２，３，３−ヘキサフルオロプロピルメチルエーテル 54.5 沸点（℃） １，１−ジフルオロエチルエチルエーテル 65 １，１，２，２−テトラフルオロエチルエチルエーテル 56 １−クロロ−１，２，２−トリフルオロエチルエチルエーテル 82 2 １，１，１，２，３，３−ヘキサフルオロプロピルエチルエーテル 64.5 １，１，２，２−テトラフルオロエチルｎ−プロピルエーテル 71.7 3 １−クロロ−１，２，２−トリフルオロエチルｎ−プロピルエーテル 109 １，１，１，２，３，３−ヘキサフルオロプロピル ｎ−プロピルエーテル 92 １−クロロ−１，２，２−トリフルオロエチルイソプロピルエーテル 100 １−クロロ−２，２−ジフルオロエチルイソプロピルエーテル 53 4 １，１，１，２，３，３−ヘキサフルオロプロピル イソプロピルエーテル 76 １，１，２，２−テトラフルオロエチルｎ−ブチルエーテル 49 5 １，１，１，２，３，３−ヘキサフルオロプロピル ｎ−ブチルエーテル 108 １，２，２−トリフルオロエチル１，１，１− トリフルオロエチルエーテル 75 １，１，２，２−テトラフルオロエチル１，１− ジフルオロエチルエーテル 77 ジ（１，１−ジフルオロエチル）エーテル 103 １−クロロ−１，２，２−トリフルオロエチル１，１− ジフルオロエチルエーテル 102 １，１，２，２−テトラフルオロエチル１，１− ジ（トリフルオロメチル）メチルエーテル 85 1 １３０ｍｍＨｇで沸点測定 2 ６３０ｍｍＨｇ 〃 3 ６２７ｍｍＨｇ 〃 4 １２１ｍｍＨｇ 〃 5 １１３ｍｍＨｇ 〃 共沸混合物を含めてエーテル類の混合物は、１種のエー
テルと１種又はそれ以上の補助溶剤との混合物であり得
るように、所望ならば使用できる。既知の清浄化方法で
の主要溶剤と共に用いたのと同じ補助溶剤を使用でき、
特にアルコール類の如き極性化合物が好ましい補助溶剤
である。本発明の別の要旨によると、フッ素含有エーテ
ルと補助溶剤特に低級アルカノール補助溶剤とを含有し
てなる清浄化組成物が提供される。エーテルとアルコー
ルとの共沸混合物は本発明の好ましい具体例を表わす。
１〜４個の炭素原子を含有する低級脂肪族アルコールは
かゝる混合物中で有用である。The following are examples of ethers which can be used and their boiling points: Boiling point (° C.) 1,1-difluoroethyl methyl ether 47 1,1,2,2-tetrafluoroethyl methyl ether 36.5 1-chloro-1, 2,2-trifluoroethyl methyl ether 70.6 1,1-dichloro-2,2-difluoroethyl methyl ether 104.8 1-chloro-2,2-difluoroethyl methyl ether 27.5 1 1,1,1,2,3,3 -Hexafluoropropyl methyl ether 54.5 boiling point (° C) 1,1-difluoroethyl ethyl ether 65 1,1,2,2-tetrafluoroethyl ethyl ether 56 1-chloro-1,2,2-trifluoroethyl ethyl ether 82 2 1,1,1,2,3,3-hexafluoropropylethyl ether 64.5 1,1,2,2-tetrafluoro Ethyl n-propyl ether 71.7 3 1-chloro-1,2,2-trifluoroethyl n-propyl ether 109 1,1,1,2,3,3-hexafluoropropyl n-propyl ether 92 1-chloro-1 1,2,2-trifluoroethyl isopropyl ether 100 1-chloro-2,2-difluoroethyl isopropyl ether 53 4 1,1,1,2,3,3-hexafluoropropyl isopropyl ether 76 1,1,2,2 -Tetrafluoroethyl n-butyl ether 49 5 1,1,1,2,3,3-hexafluoropropyl n-butyl ether 108 1,2,2-trifluoroethyl 1,1,1-trifluoroethyl ether 75 1, 1,2,2-tetrafluoroethyl 1,1-difluoroethyl ether 77 di (1,1-difluoroethyl) ether 103 1-chloro-1,2,2-trifluoroethyl 1,1-difluoroethyl ether 102 1,1,2,2-tetrafluoroethyl 1,1-di (trifluoromethyl) methyl ether 85 1 Boiling point at 130 mmHg Measurement 2 630 mmHg 〃3 627 mmHg 〃4 121 mmHg 〃5 113 mmHg Can be used. The same co-solvent used with the main solvent in known cleaning methods can be used,
In particular, polar compounds such as alcohols are preferred co-solvents. According to another aspect of the present invention, there is provided a cleaning composition comprising a fluorine-containing ether and a co-solvent, especially a lower alkanol co-solvent. An azeotrope of ether and alcohol represents a preferred embodiment of the present invention.
Lower aliphatic alcohols containing one to four carbon atoms are useful in such mixtures.
【００１１】本発明で使用したフッ素含有エーテルは普
通に用いた溶剤よりもずっと安定である傾向があり、一
般に分解に対する安定化を必要としないものである。然
しながら、所望ならば安定剤を使用でき又は必要ならば
特に厄介な清浄化方法に使用でき、普通の溶剤で用いた
安定剤特にニトロアルカン類及びエポキシド類を使用で
きる。The fluorine-containing ethers used in the present invention tend to be much more stable than commonly used solvents and generally do not require stabilization against decomposition. However, stabilizers can be used if desired or can be used for particularly cumbersome cleaning processes if necessary, and stabilizers used with common solvents, in particular nitroalkanes and epoxides, can be used.
【００１２】フッ素含有エーテルは既知の清浄化方法の
何れかで用いた溶剤類の代りに代替品として使用できし
かも該エーテルが代替する溶剤よりもアルミニウムに対
してずっと安定であるという利点を有し得る。該エーテ
ルを使用して既知の清浄化方法で用いた溶剤類の一部の
代りに代用できる。Fluorine-containing ethers have the advantage that they can be used as a replacement for the solvents used in any of the known cleaning methods, and that they are much more stable to aluminum than the solvents they replace. obtain. The ethers can be used to replace some of the solvents used in known cleaning methods.
【００１３】[0013]
【実施例】本発明を次の実施例により例示する。The invention is illustrated by the following examples.
【００１４】実施例１ 本実施例は銅被覆回路板から融剤残渣を清浄化するのに
２−クロロ−１，１，２−トリフルオロエチルメチルエ
ーテルの使用を例証する。 Example 1 This example illustrates the use of 2-chloro-1,1,2-trifluoroethyl methyl ether to clean flux residues from copper coated circuit boards.
【００１５】銅被覆したＦＲ４（エポキシ／ガラス繊維
積層体）回路板から切り取った供試板（５ｃｍ×７ｃ
ｍ）に既知重量のハンダクリームを塗布し、ハンダクリ
ームをマイクロ（ＭＩＣＲＯ）ＶＰＳハンダ付け装置で
再流動させた。用いたハンダクリームはマルチコア(Mul
ticore) ＰＲＡＢ３として入手できる６２％錫／３８％
鉛のハンダであった。A test board (5 cm × 7 c) cut from a copper-coated FR4 (epoxy / glass fiber laminate) circuit board
m) was coated with a known weight of solder cream and the solder cream was reflowed with a MICRO VPS soldering machine. The solder cream used was multicore (Mul
ticore) 62% tin / 38% available as PRAB3
It was lead solder.
【００１６】冷水を循環させた上部冷却コイルを備えた
ビーカー中で２−クロロ−１，１，２−トリフルオロエ
チルメチルエーテル（６３０ｍｍＨｇで沸点６５℃）を
沸騰させて沸騰中の液相と蒸気相とを生成し、且つ汚染
された回路板を沸騰している液体に６０秒間浸漬し次い
で蒸気相に３０秒間保持した。In a beaker provided with an upper cooling coil in which cold water is circulated, 2-chloro-1,1,2-trifluoroethyl methyl ether (boiling point: 65 ° C. at 630 mmHg) is boiled to obtain a liquid phase and vapor during boiling. The contaminated board was immersed in boiling liquid for 60 seconds and held in the vapor phase for 30 seconds.
【００１７】１ｃｍ2 当りの塩化ナトリウム（ｍｇ）と
して表わした、供試板の残留イオン汚染度は、プロトニ
ク コンタミノメーター(Protonique Contaminometer)
を用いて測定された。未洗浄の供試板のイオン汚染度を
測定し且つイオン汚染度の除去率（％）を算出した。イ
オン系融剤残渣の６１％が供試板から除去された。The residual ionic contamination of the test plate, expressed as sodium chloride (mg) per cm 2 , was measured using a Protonique Contaminometer.
Was measured using The ionic contamination degree of the unwashed test plate was measured, and the ionic contamination degree removal rate (%) was calculated. 61% of the ionic flux residue was removed from the test plate.
【００１８】使用したエーテルを１９０℃に加熱し、エ
ーテルより上方の蒸気圧を５０〜１９０℃の範囲に亘っ
て測定した。大体１２０℃で蒸気圧のわずかな増大が認
められたがこの温度で溶剤分解の徴候は眼で見られなか
った。The ether used was heated to 190 ° C. and the vapor pressure above the ether was measured over the range 50-190 ° C. At about 120 ° C., a slight increase in vapor pressure was observed, at which point no signs of solvent decomposition were visible.
【００１９】溶剤として１，１，２−トリクロロ−１，
２，２−トリフルオロエタンを用いる比較試験では、イ
オン系融剤残渣の４５％が除去された。As a solvent, 1,1,2-trichloro-1,
In a comparative test using 2,2-trifluoroethane, 45% of the ionic flux residue was removed.
【００２０】実施例２〜３ これらの実施例は銅被覆した印刷回路板から融剤残渣を
清浄化するのに２−クロロ−１，１，２−トリフルオロ
エチルメチルエーテルとメタノールとの混合物を使用す
ることを例証する。 Examples 2-3 These examples illustrate the use of a mixture of 2-chloro-1,1,2-trifluoroethyl methyl ether and methanol to clean flux residues from copper-coated printed circuit boards. Illustrate use.
【００２１】実施例２においては、２−クロロ−１，
１，２−トリフルオロエチルメチルエーテルとメタノー
ルとの混合物を一定の沸騰している混合物が得られるま
で沸騰させた。この共沸物は１８．５重量％のメタノー
ルを含有し且つ常圧で５６．８℃で沸騰した。In Example 2, 2-chloro-1,
The mixture of 1,2-trifluoroethyl methyl ether and methanol was boiled until a constant boiling mixture was obtained. This azeotrope contained 18.5% by weight of methanol and boiled at 56.8 ° C. at normal pressure.
【００２２】この共沸混合物を使用して実施例１に記載
の如く供試回路板からイオン系残渣を除去した。イオン
系残渣の６６．９％が除去された。The azeotropic mixture was used to remove ionic residues from the test circuit board as described in Example 1. 66.9% of the ionic residues were removed.
【００２３】実施例３においては、エーテル（９５重量
％）とメタノール（５重量％）との混合物を共沸混合物
の代りに使用した以外は実施例２の方法を反復した。イ
オン系残渣の６５．１％が除去された。In Example 3, the procedure of Example 2 was repeated except that a mixture of ether (95% by weight) and methanol (5% by weight) was used instead of the azeotrope. 65.1% of the ionic residue was removed.
【００２４】実施例４ 本実施例はアルミニウムの存在下での２−クロロ−１，
１，２−トリフルオロエチルメチルエーテルの安定性を
例証する。 Example 4 This example demonstrates the use of 2-chloro-1,2 in the presence of aluminum.
1 illustrates the stability of 1,2-trifluoroethyl methyl ether.
【００２５】該エーテルをアルミニウムと接触させて４
８時間還流させた。アルミニウム試験片の一部は溶剤液
体に浸漬させ、一部は溶剤液体の上方の蒸気に浸漬させ
た。The ether is contacted with aluminum to form 4
Reflux for 8 hours. A portion of the aluminum specimen was immersed in the solvent liquid and a portion was immersed in the vapor above the solvent liquid.
【００２６】この安定性試験では、液相中に塩素イオン
又はフッ素イオンの増大は認められなかったし、試験後
の溶剤のＧＣ（ガスクロマトグラフィー）コン跡は変化
を示さなかった。アルミニウム金属試験片の有意な程大
きな重量変化はなく、試験片は腐食の徴候を有さずに清
浄で輝いたまゝ安定性試験から取出した。In this stability test, no increase in chloride ion or fluorine ion was observed in the liquid phase, and the trace of GC (gas chromatography) of the solvent after the test showed no change. There was no significant change in weight of the aluminum metal specimen, and the specimen was removed from the stability test while remaining clean and shiny without any signs of corrosion.
【００２７】得られた結果が証明する所によれば、エー
テルはアルミニウムの存在下でも高い安定性を有し且つ
アルミニウムの清浄化方法で使用するのに適当である。
エーテルを用いて金属を清浄化する時に安定剤を添加し
てエーテル中に酸度が生成されるのを阻止できる。The results obtained demonstrate that ethers have a high stability in the presence of aluminum and are suitable for use in aluminum cleaning processes.
When cleaning metals with ethers, stabilizers can be added to prevent the formation of acidity in the ether.
【００２８】実施例５ 本実施例は銅被覆した回路板から融剤残渣を清浄化する
のにテトラフルオロエチルメチルエーテルの使用を例証
する。 Example 5 This example illustrates the use of tetrafluoroethyl methyl ether to clean flux residues from copper-coated circuit boards.
【００２９】沸点３３〜３５℃（６３０ｍｍＨｇ）及び
密度（２５℃）１．２８ｇ／ｍｌのテトラフルオロエチ
ルメチルエーテルを使用して実施例１に記載の如く銅被
覆回路板から融剤残渣を清浄化した。イオン系融剤残渣
の６２％が除去された。Clean flux residues from copper-coated circuit boards as described in Example 1 using tetrafluoroethyl methyl ether having a boiling point of 33-35 ° C (630 mmHg) and a density (25 ° C) of 1.28 g / ml. did. 62% of the ionic flux residue was removed.
【００３０】実施例６〜８ これらの実施例は本発明の方法で使用するのに適当な或
る共沸混合物を例証する。 Examples 6-8 These examples illustrate certain azeotropes suitable for use in the process of the present invention.
【００３１】テトラフルオロエチルメチルエーテルはメ
タノールと共に共沸物を形成し、該共沸物は４重量％の
メタノールを含有し３４．５℃の沸点を有する。Tetrafluoroethyl methyl ether forms an azeotrope with methanol, which contains 4% by weight of methanol and has a boiling point of 34.5 ° C.
【００３２】テトラフルオロエチルメチルエーテルは
１，１，２−トリクロロ−１，２，２−トリフルオロエ
タンと共沸物を形成し、該共沸物は３９．５重量％のハ
ロエタンを含有し約３４．９℃の沸点を有する。Tetrafluoroethyl methyl ether forms an azeotrope with 1,1,2-trichloro-1,2,2-trifluoroethane, which contains 39.5% by weight of haloethane and contains It has a boiling point of 34.9 ° C.
【００３３】テトラフルオロエチルメチルエーテルは
１，１，２−トリクロロ−１，２，２−トリフルオロエ
タン及びメタノールと共に三元共沸物を形成し、該共沸
物は４１重量％のハロエタンと３重量％のメタノールと
を含有し約３４．５℃の沸点を有する。Tetrafluoroethyl methyl ether forms a ternary azeotrope with 1,1,2-trichloro-1,2,2-trifluoroethane and methanol, the azeotrope being 41% by weight of haloethane and 3%. It contains about 34.5% by weight methanol and has a boiling point of about 34.5 ° C.
【００３４】実施例９ 本実施例は本発明の方法に三元共沸混合物の使用を例証
する。 Example 9 This example illustrates the use of a ternary azeotrope in the process of the present invention.
【００３５】実施例８で製造したテトラフルオロエチル
メチルエーテルと１，１，２−トリクロロ−１，２，２
−トリフルオロエタンとメタノールとの三元共沸混合物
を使用して、実施例１に記載した方法により回路板から
ハンダの融剤残渣を除去した。イオン系融剤残渣の４
８．２％が除去された。The tetrafluoroethyl methyl ether prepared in Example 8 and 1,1,2-trichloro-1,2,2
Using a ternary azeotrope of trifluoroethane and methanol, the solder flux residue was removed from the circuit board by the method described in Example 1. 4 of ionic flux residue
8.2% were removed.
【００３６】実施例１０〜１１ 本実施例は本発明の方法に使用するのに別の共沸混合物
を例証する。 Examples 10-11 This example illustrates another azeotrope for use in the method of the present invention.
【００３７】沸点５６℃、密度１．２１ｇ／ｍｌのテト
ラフルオロエチルエチルエーテルはメタノールと共沸物
を形成し、該共沸物は１０．６重量％のメタノールを含
有し４８．６℃の沸点を有する。Tetrafluoroethylethyl ether having a boiling point of 56 ° C. and a density of 1.21 g / ml forms an azeotrope with methanol, which contains 10.6% by weight of methanol and has a boiling point of 48.6 ° C. Having.
【００３８】該テトラフルオロエチルエチルエーテルは
エタノールと共沸物を形成し、該共沸物は３８．５重量
％の１，１，２−トリクロロ−１，２，２−トリフルオ
ロエタンを含有し４６．３℃の沸点を有する。The tetrafluoroethyl ethyl ether forms an azeotrope with ethanol, the azeotrope containing 38.5% by weight of 1,1,2-trichloro-1,2,2-trifluoroethane. It has a boiling point of 46.3 ° C.
フロントページの続き (56)参考文献 米国特許3957672（ＵＳ，Ａ) (58)調査した分野(Int.Cl.6，ＤＢ名) C11D 7/28 B08B 3/08 C11D 7/50 Continuation of the front page (56) References US Patent 3,976,672 (US, A) (58) Fields investigated (Int. Cl. 6 , DB name) C11D 7/28 B08B 3/08 C11D 7/50
Claims (9)
の範囲の沸点を有し且つ少なくとも３個の炭素原子と１
個又はそれ以上の水素原子とを有する低分子量のフッ素
化エーテル又はその蒸気又はその両方を含有してなる溶
剤組成物と接触することからなる物品の溶剤清浄化方
法。1. The method according to claim 1, wherein the article to be cleaned is at 20.degree.
And at least 3 carbon atoms and 1
A method for solvent cleaning an article comprising contacting with a solvent composition comprising a low molecular weight fluorinated ether having one or more hydrogen atoms and / or a vapor thereof.
求項１記載の方法。2. The method of claim 1, wherein the solvent composition further comprises a co-solvent.
載の方法。3. The method according to claim 2, wherein the co-solvent is an alcohol.
低級脂肪族アルカノールである請求項３記載の方法。4. The method according to claim 3, wherein the co-solvent is a lower aliphatic alkanol having 1 to 4 carbon atoms.
合物よりなる請求項１記載の方法。5. The method of claim 1 wherein the solvent composition comprises an azeotropic mixture of a fluorinated ether.
る三元共沸混合物よりなる請求項１記載の方法。6. The method of claim 1 wherein the solvent composition comprises a ternary azeotrope containing a fluorinated ether.
有し且つ少なくとも３個の炭素原子と１個又はそれ以上
の水素原子とを有する低分子量のフッ素化エーテル及び
（ii）補助溶剤としての極性化合物を含有してなる溶剤
組成物。7. A low molecular weight fluorinated ether having (i) a boiling point in the range of 20 ° C. to 120 ° C. and having at least 3 carbon atoms and one or more hydrogen atoms; and (ii) an auxiliary. A solvent composition containing a polar compound as a solvent.
求項７記載の溶剤組成物。8. The solvent composition according to claim 7, wherein the polar compound is an alcohol.
アルコールとの共沸混合物よりなる請求項７記載の溶剤
組成物。9. The solvent composition according to claim 7, wherein the solvent composition comprises an azeotropic mixture of the fluorinated ether and an alcohol.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB9007645:6 | 1990-04-04 | ||
| GB909007645A GB9007645D0 (en) | 1990-04-04 | 1990-04-04 | Solvent cleaning of articles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05271692A JPH05271692A (en) | 1993-10-19 |
| JP2961924B2 true JP2961924B2 (en) | 1999-10-12 |
Family
ID=10673894
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3071406A Expired - Lifetime JP2961924B2 (en) | 1990-04-04 | 1991-04-04 | Solvent cleaning method for articles |
Country Status (11)
| Country | Link |
|---|---|
| EP (1) | EP0450855B1 (en) |
| JP (1) | JP2961924B2 (en) |
| KR (1) | KR100205296B1 (en) |
| AT (1) | ATE186071T1 (en) |
| AU (1) | AU640760B2 (en) |
| CA (1) | CA2039828C (en) |
| DE (1) | DE69131737T2 (en) |
| ES (1) | ES2140382T3 (en) |
| GB (1) | GB9007645D0 (en) |
| IE (1) | IE911028A1 (en) |
| NZ (1) | NZ237628A (en) |
Families Citing this family (30)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE1005181A3 (en) * | 1991-08-19 | 1993-05-18 | Solvay | Composition containing a fluorinated ether and use thereof. |
| US5273592A (en) * | 1991-11-01 | 1993-12-28 | Alliesignal Inc. | Method of cleaning using partially fluorinated ethers having a tertiary structure |
| US6355113B1 (en) | 1991-12-02 | 2002-03-12 | 3M Innovative Properties Company | Multiple solvent cleaning system |
| JPH07504889A (en) * | 1991-12-03 | 1995-06-01 | ユナイテッド ステーツ インバイオロンメンタル プロテクション エイジェンシー | Refrigerant composition and method of use thereof |
| US5888418A (en) * | 1992-03-20 | 1999-03-30 | The United States Of America As Represented By The Secretary Of Commerce | Azeotropic refrigerant comprising bis-(difluoromethyl)ether and 1,1,2-trifluoroethane |
| US5278342A (en) * | 1992-03-25 | 1994-01-11 | Hampshire Chemical Corp. | Vapor phase chlorination of difluoromethyl methyl ether |
| US5605882A (en) * | 1992-05-28 | 1997-02-25 | E. I. Du Pont De Nemours And Company | Azeotrope(like) compositions of pentafluorodimethyl ether and difluoromethane |
| BE1006433A3 (en) * | 1992-12-03 | 1994-08-23 | Solvay | Composition containing fluorinated ether and use thereof. |
| US5484546A (en) * | 1993-05-19 | 1996-01-16 | E. I. Du Pont De Nemours And Company | Refrigerant compositions including an acylic fluoroether |
| US5658962A (en) | 1994-05-20 | 1997-08-19 | Minnesota Mining And Manufacturing Company | Omega-hydrofluoroalkyl ethers, precursor carboxylic acids and derivatives thereof, and their preparation and application |
| US5562854A (en) * | 1994-09-29 | 1996-10-08 | E. I. Du Pont De Nemours And Company | Octafluorobutane compositions |
| US6548471B2 (en) | 1995-01-20 | 2003-04-15 | 3M Innovative Properties Company | Alkoxy-substituted perfluorocompounds |
| US6506459B2 (en) | 1995-01-20 | 2003-01-14 | 3M Innovative Properties Company | Coating compositions containing alkoxy substituted perfluoro compounds |
| US5718293A (en) * | 1995-01-20 | 1998-02-17 | Minnesota Mining And Manufacturing Company | Fire extinguishing process and composition |
| US5925611A (en) * | 1995-01-20 | 1999-07-20 | Minnesota Mining And Manufacturing Company | Cleaning process and composition |
| JP2870577B2 (en) * | 1995-03-28 | 1999-03-17 | 工業技術院長 | Solvent composition |
| US6008179A (en) * | 1995-05-16 | 1999-12-28 | 3M Innovative Properties Company | Azeotrope-like compositions and their use |
| CA2218890A1 (en) | 1995-05-16 | 1996-11-21 | Dean S. Milbrath | Azeotrope-like compositions and their use |
| CN1192088C (en) * | 1995-05-16 | 2005-03-09 | 美国3M公司 | Azeotrope-like compositions and their use |
| US5543055A (en) * | 1995-06-06 | 1996-08-06 | Hampshire Chemical Corp. | Purifications of flourinated dimethyl ethers |
| JP3783047B2 (en) | 1995-12-15 | 2006-06-07 | スリーエム カンパニー | Cleaning method and composition |
| US6030934A (en) * | 1997-02-19 | 2000-02-29 | 3M Innovative Properties Company | Azeotropic compositions of methoxy-perfluoropropane and their use |
| US6552090B1 (en) | 1997-09-15 | 2003-04-22 | 3M Innovative Properties Company | Perfluoroalkyl haloalkyl ethers and compositions and applications thereof |
| US6022842A (en) * | 1998-02-11 | 2000-02-08 | 3M Innovative Properties Company | Azeotrope-like compositions including perfluorobutyl methyl ether, 1- bromopropane and alcohol |
| US6127430A (en) * | 1998-12-16 | 2000-10-03 | 3M Innovative Properties Company | Microemulsions containing water and hydrofluroethers |
| US6159917A (en) * | 1998-12-16 | 2000-12-12 | 3M Innovative Properties Company | Dry cleaning compositions containing hydrofluoroether |
| GB0203315D0 (en) * | 2002-02-13 | 2002-03-27 | Henly Stephen R | Method of sterilising an article |
| JP4655931B2 (en) | 2003-06-27 | 2011-03-23 | 旭硝子株式会社 | Cleaning rinse method |
| JP5109556B2 (en) * | 2006-11-01 | 2012-12-26 | セントラル硝子株式会社 | Azeotropic and azeotrope-like compositions comprising 1,1,2,2-tetrafluoro-1-methoxyethane |
| JP6264510B2 (en) * | 2015-07-27 | 2018-01-24 | 旭硝子株式会社 | Solvent composition, cleaning method, coating film forming method, heat transfer medium and thermal cycle system |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3957672A (en) * | 1973-11-23 | 1976-05-18 | The United States Of America As Represented By The Secretary Of The Navy | Displacement of organic liquid films from solid surfaces by non aqueous systems |
| IT1213537B (en) * | 1986-11-21 | 1989-12-20 | Ausimont Spa | PROCEDURE FOR THE PREPARATION OF PERFLUOROETERS BY FLUORURATION WITH ELEMENTARY FLUORINE. |
| US4948526A (en) * | 1989-09-26 | 1990-08-14 | Allied-Signal Inc. | Azeotrope-like compositions of pentafluorodimethyl ether and monochlorodifluoromethane |
-
1990
- 1990-04-04 GB GB909007645A patent/GB9007645D0/en active Pending
-
1991
- 1991-03-27 IE IE102891A patent/IE911028A1/en unknown
- 1991-03-27 EP EP91302698A patent/EP0450855B1/en not_active Expired - Lifetime
- 1991-03-27 ES ES91302698T patent/ES2140382T3/en not_active Expired - Lifetime
- 1991-03-27 AT AT91302698T patent/ATE186071T1/en not_active IP Right Cessation
- 1991-03-27 DE DE69131737T patent/DE69131737T2/en not_active Expired - Fee Related
- 1991-03-28 NZ NZ23762891A patent/NZ237628A/en unknown
- 1991-03-28 AU AU73913/91A patent/AU640760B2/en not_active Ceased
- 1991-04-04 CA CA002039828A patent/CA2039828C/en not_active Expired - Fee Related
- 1991-04-04 JP JP3071406A patent/JP2961924B2/en not_active Expired - Lifetime
- 1991-04-04 KR KR1019910005446A patent/KR100205296B1/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| DE69131737T2 (en) | 2000-06-08 |
| AU7391391A (en) | 1991-10-10 |
| IE911028A1 (en) | 1991-10-09 |
| EP0450855B1 (en) | 1999-10-27 |
| GB9007645D0 (en) | 1990-05-30 |
| ATE186071T1 (en) | 1999-11-15 |
| EP0450855A3 (en) | 1992-01-15 |
| JPH05271692A (en) | 1993-10-19 |
| CA2039828A1 (en) | 1991-10-05 |
| KR910018532A (en) | 1991-11-30 |
| DE69131737D1 (en) | 1999-12-02 |
| ES2140382T3 (en) | 2000-03-01 |
| CA2039828C (en) | 2001-01-23 |
| EP0450855A2 (en) | 1991-10-09 |
| AU640760B2 (en) | 1993-09-02 |
| NZ237628A (en) | 1994-07-26 |
| KR100205296B1 (en) | 1999-07-01 |
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