EP0974642B1 - Reinigungs- und Trocknungsmittel auf Basis von 1,1,1,2,3,4,4,5,5,5-Decafluorpentan und 1,1,1,3,3-pentafluorbutan - Google Patents

Reinigungs- und Trocknungsmittel auf Basis von 1,1,1,2,3,4,4,5,5,5-Decafluorpentan und 1,1,1,3,3-pentafluorbutan Download PDF

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Publication number
EP0974642B1
EP0974642B1 EP99401419A EP99401419A EP0974642B1 EP 0974642 B1 EP0974642 B1 EP 0974642B1 EP 99401419 A EP99401419 A EP 99401419A EP 99401419 A EP99401419 A EP 99401419A EP 0974642 B1 EP0974642 B1 EP 0974642B1
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EP
European Patent Office
Prior art keywords
cleaning
compositions
azeotropic
365mfc
mee
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
Application number
EP99401419A
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English (en)
French (fr)
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EP0974642A1 (de
Inventor
Pascal Michaud
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.)
Arkema France SA
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Atofina SA
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Filing date
Publication date
Application filed by Atofina SA filed Critical Atofina SA
Publication of EP0974642A1 publication Critical patent/EP0974642A1/de
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Publication of EP0974642B1 publication Critical patent/EP0974642B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/50Solvents
    • C11D7/5036Azeotropic mixtures containing halogenated solvents
    • C11D7/504Azeotropic mixtures containing halogenated solvents all solvents being halogenated hydrocarbons
    • C11D7/505Mixtures of (hydro)fluorocarbons
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • C23G5/02Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
    • C23G5/028Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing halogenated hydrocarbons
    • C23G5/02803Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing halogenated hydrocarbons containing fluorine

Definitions

  • the present invention relates to the field of fluorinated hydrocarbons and has more particularly for the purpose of new compositions usable for cleaning or dry solid surfaces.
  • 1,1,2-trichloro-1,2,2-trifluoroethane (known in the art under the designation F113) has been widely used in the industry for cleaning and degreasing of very different solid surfaces (metal parts, glasses, plastics, composites), for which an absence - or at least residual as low as possible - in impurities, in particular of organic nature, is required.
  • F 113 was particularly suitable for this purpose because of its non-aggressive character with regard to the materials used.
  • This product was particularly used in the field of printed circuit manufacturing, to eliminate residues of the substances used to improve the quality of the welds (designated by the term flux welds). This elimination operation is designated in the trade by the term "defluxing".
  • azeotropic mixture is meant in the sense of the present invention a mixture of generally miscible chemical compounds which, under certain particular conditions of proportion, temperature and pressure, butt at substantially constant temperature while maintaining substantially the same composition. When heated to reflux, such a mixture azeotropic is in equilibrium with a vapor phase whose composition is substantially the same as that of the liquid phase. Such behavior azeotropic or near azeotropic is desirable to ensure satisfactory machines in which are performed the operations of aforementioned cleaning, and in particular to ensure the recycling by distillation of cleaning fluid.
  • the F113 is also used in the fields, especially in optics, for which it is required to have water-free surfaces, that is to say surfaces where water is present only in the form of undetectable traces by the method measurement method (Karl Fisher method). F113 is for this purpose implemented in drying (or dewetting) operations of said surfaces, in combination with hydrophobic surfactants.
  • F113-based compositions are now banned because F113 is one of the chlorofluorocarbons (CFCs) suspected of attacking or degrade stratospheric ozone.
  • CFCs chlorofluorocarbons
  • F113 can be replaced by 1,1-dichloro-1-fluoroethane (known as F141b), but the use of this substitute is already regulated because, although weak, its destructive effect vis-à-vis ozone is not zero.
  • F141b 1,1-dichloro-1-fluoroethane
  • the application EP 0512885 describes a composition comprising from 93 to 99% by weight 1,1,1,3,3-pentafluorobutane and 1 to 7% methanol, usable as a substitute for F113.
  • 1,1,1,3,3-Pentafluorobutane also known in the trade under the name of F365mfc, is devoid of destructive effect vis-à-vis ozone.
  • the object of the invention is to propose other compositions which are capable of to be used as a substitute for F113 or F141b, and devoid of effect destructive to ozone.
  • the present invention therefore object of the azeotropic or near azeotropic compositions comprising from 1 to 25% of 1,1,1,2,3,4,4,5,5,5-decafluoropentane, preferably 5 to 20%, and 75 to 99% of 1,1,1,3,3-pentafluorobutane, preferably 80 to 95%. Except otherwise indicated, the percentages used in this text to indicate the The content of the compositions according to the invention are percentages by weight.
  • the 1,1,1,2,3,4,4,5,5,5-Decafluoropentane is a compound (also known as denomination 43-10 mee) totally devoid of destructive effect vis-à-vis ozone.
  • compositions according to the invention make it possible to obtain very good results for the cleaning and degreasing of solid surfaces, as well as in the operations of drying and dewetting the surfaces.
  • these compositions do not have a flash point under the standard conditions of determination (ASTM D 3828) and therefore allow you to work safely.
  • a ternary composition according to the invention includes 5 to 20% of 43-10 mee, 75 to 90% of 365 mfc, and 1 to 10% of methanol. More particularly preferred is a ternary composition containing 10 at 15% of 43-10 mee, 80 to 85% of 365 mfc, and 2 to 8% of methanol. In this domain, there is an azeotrope whose boiling point is 33.2 ° C at the normal atmospheric pressure.
  • cleaning compositions based on 43-10 mee and 365 mfc according to the invention may, if desired, be protected against chemical attack resulting from their contact with water (hydrolysis), with light metals (constituting the solid surfaces to be cleaned), and / or against radical attacks likely to occur in the cleansing process, by adding a conventional stabilizer such as, for example, nitroalkanes (especially nitromethane, nitroethane, nitropropane), acetals (dimethoxymethane) and ethers (1,4-dioxane, 1,3-dioxolane).
  • a conventional stabilizer such as, for example, nitroalkanes (especially nitromethane, nitroethane, nitropropane), acetals (dimethoxymethane) and ethers (1,4-dioxane, 1,3-dioxolane).
  • the proportion of stabilizer can range from 0.01 to 5% by relative to the total weight of the composition.
  • a stabilizer it is preferred to use the dimethoxymethane whose boiling point is close to that of the compositions azeotropic according to the invention; therefore, this stabilizer perfectly follows the cycle of evaporation and condensation of the solvent, which is particularly interesting in cleaning applications.
  • compositions according to the invention can be used in the same applications and be implemented in the same way as the prior compositions based on F113 or F141b. They are therefore suitable especially for use in cleaning and degreasing surfaces solids, preferably for defluxing printed circuits, as well as for surface drying operations.
  • compositions can also be used as an expansion agent polyurethane foams, as an agent for the dry cleaning of textiles, and as a refrigerant.
  • This azeotrope used for the cleaning of welding flux or in degreasing of mechanical parts, gives good results.
  • a mixture containing by weight 9% of 43-10 mee, 90.5% of 365mfc and 0.5% of methylal as stabilizer are introduced. After refluxing the system for one hour, an aliquot of the vapor phase is taken. Its analysis, by gas chromatography, shows the presence of methylal, which indicates that the mixture is also stabilized in the vapor phase.
  • This azeotrope used for the cleaning of welding flux or in degreasing of mechanical parts, gives good results.
  • Example 2 the azeotropic composition above can be stabilized with 0.5% dimethoxymethane.
  • test circuits according to IPC-B-25 described in the IPC Test Methods Manual (Institute for Interconnecting and Packaging Electronic Circuits; Lincolnwood, IL, USA). These circuits are coated with rosin-based solder flux (product marketed by ALPHAMETAL under the name flux R8F) and annealed in an oven at 220 ° C for 30 seconds.
  • rosin-based solder flux product marketed by ALPHAMETAL under the name flux R8F
  • these circuits are cleaned using of the azeotropic composition of Example 3, in a small machine ultrasound for 3 minutes by immersion in the liquid phase and 3 minutes vapor phase.
  • the cleaning is evaluated according to the standard procedure IPC 2.3.26 (also described in the manual cited above) using a precision conductivity meter.
  • the value obtained, 2.2 ⁇ g / cm 2 eq.NaCl, is below the limit of ionic impurities tolerated by the profession (2.5 ⁇ g / cm 2 eq.NaCl).

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Detergent Compositions (AREA)

Claims (7)

  1. Azeotrope oder quasiazeotrope Zusammensetzungen, enthaltend 1 bis 25% 1,1,1,2,3,4,4,5,5,5-Decafluorpentan (43-10 mee), vorzugsweise 5 bis 20%, und 75 bis 99% 1,1,1,3,3-Pentafluorbutan (365 mfc), vorzugsweise 80 bis 95%.
  2. Zusammensetzung nach Anspruch 1 in Form eines Azeotrops mit einem Siedepunkt von 36,5°C bei normalem Atmosphärendruck.
  3. Zusammensetzungen nach Anspruch 1, enthaltend 5 bis 20% 43-10 mee, 75 bis 90% 365 mfc und 1 bis 10% Methanol.
  4. Zusammensetzungen nach Anspruch 3, enthaltend 10 bis 15% 43-10 mee, 80 bis 85% 365 mfc und 2 bis 8% Methanol.
  5. Zusammensetzung nach Anspruch 3 oder 4 in Form eines Azeotrops mit einem Siedepunkt von 33,2°C bei normalem Atmosphärendruck.
  6. Zusammensetzungen nach einem der Ansprüche 1 bis 5, außerdem enthaltend einen Stabilisator, vorzugsweise Dimethoxymethan.
  7. Verwendung der Zusammensetzungen nach einem der Ansprüche 1 bis 6 zur Reinigung und Entfettung fester Oberflächen, vorzugsweise zur Entfernung von Flußmittelresten von Leiterplatten, sowie für Oberflächentrocknungsoperationen.
EP99401419A 1998-07-24 1999-06-11 Reinigungs- und Trocknungsmittel auf Basis von 1,1,1,2,3,4,4,5,5,5-Decafluorpentan und 1,1,1,3,3-pentafluorbutan Expired - Lifetime EP0974642B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9809464A FR2781499B1 (fr) 1998-07-24 1998-07-24 Compositions de nettoyage ou de sechage a base de 1,1,1,2,3,4,4,5,5, 5 - decafluoropentane
FR9809464 1998-07-24

Publications (2)

Publication Number Publication Date
EP0974642A1 EP0974642A1 (de) 2000-01-26
EP0974642B1 true EP0974642B1 (de) 2003-09-03

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EP99401419A Expired - Lifetime EP0974642B1 (de) 1998-07-24 1999-06-11 Reinigungs- und Trocknungsmittel auf Basis von 1,1,1,2,3,4,4,5,5,5-Decafluorpentan und 1,1,1,3,3-pentafluorbutan

Country Status (5)

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US (2) US6174850B1 (de)
EP (1) EP0974642B1 (de)
DE (1) DE69910916T2 (de)
ES (1) ES2207140T3 (de)
FR (1) FR2781499B1 (de)

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Also Published As

Publication number Publication date
EP0974642A1 (de) 2000-01-26
USRE39819E1 (en) 2007-09-04
ES2207140T3 (es) 2004-05-16
DE69910916D1 (de) 2003-10-09
US6174850B1 (en) 2001-01-16
DE69910916T2 (de) 2004-07-15
FR2781499A1 (fr) 2000-01-28
FR2781499B1 (fr) 2000-09-08

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